aerated pet food composition and method of preparation

专利摘要:
COMPOSITION OF FOOD FOR AERATED PETS AND ITS PREPARATION METHOD The present invention provides pet treats and teethers that were aerated during production by a supercritical fluid. The aeration process results in pet treats and teethers that have a lower density and increased oral hygiene properties, compared to treats of similar composition that have not been aerated in the same way.
公开号:BR112015011300B1
申请号:R112015011300-1
申请日:2013-10-22
公开日:2021-02-02
发明作者:Ralf Bela Reiser；Chad A. Cepeda；Matthew Elliott
申请人:Mars, Incorporated；
IPC主号:

专利说明:

FIELD OF THE INVENTION
[001] The present invention in general refers to edible teethers for pets and the methods of making and using them. More particularly, the present invention relates to edible pet teethers that have a structure that includes bubbles. More particularly, the present invention relates to an edible and nutritional pet teether or treat. Even more particularly, the present invention relates to an edible, nutritional and aerated (or foamed) pet bite or treat. More particularly, the present invention relates to a bite or treat as described above, in which the bite or treat facilitates weight loss or weight control properties. In some embodiments, aeration, or foaming of the treat is done before, during, or after extrusion or injection molding. SUMMARY OF THE INVENTION
[002] The present invention generally provides an aerated pet teether composition (or foamed as the terms are used interchangeably) comprising 15-90% by weight of protein, 5-25% by weight of glycerin , 5-25% by weight of water and an amount of supercritical fluid sufficient to occupy 5-55% of the total volume of the composition when the supercritical fluid is transformed into gas. In some preferred forms, the composition further comprises up to 40% by weight of plasticizer. In other preferred forms, the composition further comprises from 0.05 - 27.55% by weight of an additional ingredient selected from the group consisting of flavor enhancers, fat, vitamins, minerals, colorants, preservatives and combinations thereof. The gas transformed from the supercritical fluid preferably produces bubbles in the composition. In general, such bubbles have an average diameter between 0.05 to 200 μm. In the preferred forms, the bubbles have a density greater than 2 x 104 bubbles / cc. Preferably, the bubbles are substantially uniform in distribution throughout the composition. However, in the alternative modalities, the bubbles can be distributed unevenly within the composition. In such cases, the bubbles may be more concentrated in one area than in another and the density of the composition may vary. In the preferred forms, the distribution of the bubbles will be intentional.
[003] Preferably, the surface roughness of the teether or treat of the present invention is greater than that of a pet teether that does not have a supercritical fluid in it. The Ra (μm) value of the pet teether of the present invention is preferably about 4 to 15.
[004] The average friction coefficient of the pet teether of the present invention is preferably from about 0.136 ± 0.001 to 0.235 ± 0.049.
[005] Preferably, the delicacy stiffness using Vickers analysis ranges from about 0.003 to 0.02.
[006] The tensile strength of the product of the present invention that includes a supercritical fluid preferably has about 15% to 50% of the tensile strength of a pet teether that does not include a supercritical fluid. Preferably, the maximum distance to maximum force ratio is about 6: 1 to 8: 1 when compared to a pet teether that includes a supercritical fluid with that which does not include a supercritical fluid.
[007] The present invention also provides new methods for making the compositions according to the invention. Such compositions are preferably injection molded or extruded to produce a final pet teether or treat from the composition. In some preferred forms when injection molding is used, the supercritical fluid comes into contact with the composition during the injection molding process. In some preferred injection molding processes, the composition is extruded prior to the injection molding process. In some forms, supercritical fluid is added to the composition during the extrusion process and before the injection molding process. When the composition is extruded to produce the final product of the pet teether, the supercritical fluid comes into contact with the composition during the extrusion process. BRIEF DESCRIPTION OF THE DRAWINGS
[008] FIGURE 1 is a diagram of an exemplary method of producing a pet teether, according to the invention, where the powder components are added in the mixing step and the liquids in the extrusion step;
[009] FIGURE 2 is another diagram of an exemplary method of producing the pet biting product, according to the invention which additionally comprises the steps of packaging and additional de-agglutination;
[0010] FIGURE 3 is another diagram of an exemplary method of producing the pet bite product, according to the invention, where the powdered components and liquids are added together in the mixing step;
[0011] FIGURE 4 is a schematic drawing of the injection molding process that can be used to make the pet bite product according to the invention;
[0012] FIGURE 5 is an illustration of a particularly preferred pet teether of the present invention;
[0013] FIGURE 6 is a graph showing the cell size distribution for a 1 cubic centimeter sample size of the pet bite product according to the present invention;
[0014] FIGURE 7 is a graph showing the average force / distance curve for the control and a modality of the treats of the present invention;
[0015] FIGURE 8 is a graph showing the results of resistance to tension for the control and a modality of the treats of the present invention.
[0016] FIGURE 9 is a diagram of an exemplary method of producing a pet teether, according to the invention by adding a supercritical fluid;
[0017] FIGURE 10 is another diagram of an exemplary method of producing a pet biting product, according to the invention by adding a supercritical fluid in the injection molding step and the additional packaging and de-agglutination steps;
[0018] FIGURE 11 is another diagram of an exemplary method of producing a pet biting product, according to the invention, where powder components and liquids are added together in the mixing step, and adding a fluid supercritical in the injection molding stage;
[0019] FIGURE 12 is a schematic drawing of the injection molding process that can be used to make the pet bite product according to the invention by adding the supercritical fluid; and
[0020] FIGURE 13 is a diagram of an exemplary method of producing a pet teether, according to the invention, where powder components are added in the mixing step and liquids are added in the extrusion step together with the supercritical fluid; DETAILED DESCRIPTION
[0021] The modalities of the invention described in this document are illustrations of the present invention and are not intended to limit.
[0022] In general, the present invention is directed to a bite or edible treat for pet and to the methods of manufacturing a nutritious product that is designed to remove plaque or tartar, by means of mechanical abrasion, while providing fun and function safe. The inventive pet teether provides rapid degradation of the product once ingested by the animal and demonstrates a significant reduction in plaque and tartar compared to a standard diet. The composition of the pet teether creates a functional and nutritious treat that will promote a healthier lifestyle for the animal.
[0023] The composition of the edible pet teether of the invention is, in general, formed by a thermoplastic material, preferably comprising a protein, a water-absorbing polymer, a plasticizer and water. The pet teether of the invention is preferably a one-component / monotexture product. As used here, the monocomponent / monotexture product means that the biting product is a substantially homogeneous molded mass that can be formed into any shape desired for a bite or pet treat.
[0024] The pet teether has malleable properties, so when chewed the animal's teeth penetrate the product causing the product to degrade in a controlled manner under repetitive strain. The edible thermoplastic material can be shaped in a variety of ways to provide good strength and stiffness and other desired physical properties to enhance functionality and chewing pleasure.
[0025] The soft chewable texture of this pet teether improves the fun of the animal and demonstrates enhanced effectiveness in oral hygiene. The inventive pet teether composition provides a balanced blend of highly digestible proteins in a matrix of water-soluble materials to improve nutritional performance and safety for the animal.
[0026] The protein can be composed of any protein, such as fibrous protein and / or gelation protein. The fibrous protein for the pet bite can be derived from animals, but it can be formulated in such a way that it does not include muscle protein, or plants. A person skilled in the art could recognize that insignificant amounts of muscle protein may be present. Fibrous proteins are generally strong and relatively insoluble. Due to these properties, fibrous proteins are important in providing the main structure of the pet bite product. Exemplary fibrous proteins include, but are not limited to, wheat protein, wheat gluten, corn zein, corn gluten, soy protein, peanut protein, casein, keratin and mixtures thereof. Particularly preferred fibrous proteins include, but are not limited to, wheat protein isolate, soy protein isolate, sodium caseinate and mixtures thereof. A highly preferred fibrous protein is a mixture of wheat protein isolate, soy protein isolate and sodium caseinate.
[0027] The water-absorbent polymer in the pet teether can be a gelling protein, a hydrocolloid, an edible hydrogel or mixtures thereof. Gelling proteins, sometimes known as globular proteins, generally comprise proteins with a globular shape that are relatively soluble in aqueous solutions where they form gels or colloidal solutions. Exemplary gelling proteins include, but are not limited to, gelatin, albumin, plasma, pea proteins, lactoglobulins, surimi (fish) proteins, whey protein and mixtures thereof. A highly preferred gelling protein is gelatin.
[0028] A hydrocolloid can be used in the composition of the pet teether as the water-absorbing polymer. A hydrocolloid is generally defined as a macromolecule (for example, a carbohydrate polymer or protein) that is soluble in water and forms a gel when combined with water. Exemplary hydrocolloids include, among others, pectins, alginates, agar, carrageenan, xanthan gum and guar gum.
[0029] An edible hydrogel can be used in the composition of the pet teether as the water-absorbing polymer. The edible hydrogel can be of a natural or synthetic material that swells in water or some liquid, keeping a large amount of liquid without dissolving. Exemplary hydrogels include, but are not limited to, maltodextrins, cetyl alcohol, chitosan, lecithins, polypeptides, waxes and edible polymers.
[0030] In a preferred embodiment, the water-absorbing polymer is a gelation polymer. In a more preferred embodiment, the gelling polymer is gelatin, preferably having a Bloom resistance in the range of about 100 to about 400. More preferably, the gelatin will have a Bloom resistance in the range of about 100 to about 200.
[0031] Plasticizers dissolve in the polymer, separating the polymer chains and thus facilitating molecular movement. Plasticizers are commonly used to increase the functionality, flexibility and extensibility of polymers. Plasticizers also reduce water activity in feed systems by connecting water that is otherwise available through biological reactions, such as microbial growth. Exemplary plasticizers, in general, used in food applications include, but are not limited to, water, polyalcohols (eg, sorbitol, mannitol, maltitol, glycerol and polyethylene glycol), gum arabic, hydrogenated starch hydrolyzate and hydrolyzed protein. In a preferred embodiment, the plasticizer is glycerol. In another preferred embodiment, the plasticizer is a hydrogenated starch hydrolyzate.
[0032] Yet another embodiment of the invention is directed to a composition of the pet teether which is a mixture comprising a fibrous protein in an amount of about 15 to about 90%, preferably from about 20 to about 80%, even more preferably between about 25% to about 60%, even more preferably from about 30 to about 50% by weight of the composition, a water-absorbing polymer in an amount of about 5 to about 35 %, preferably about 10 to about 30%, more preferably about 15 to about 25% by weight of the composition, a plasticizer in an amount of about 40%, preferably about 5 to about from 40%, preferably from about 10 to about 35%, more preferably from about 15 to about 30% by weight of the composition, and water in an amount from about 1 to about 20%, preferably from about from 2 to about 18%, more preferably from about 5 to about 15% by weight of the composition. In a preferred embodiment the composition of the pet teether will contain starch in an amount of less than about 5%, preferably less than about 4% and more preferably less than about 3% by weight of the composition. The present composition is thermoplasticized, preferably by extrusion and molded to form the pet biting product. The pet biting product is preferably formed by injection molding. A person skilled in the art will readily recognize that the pet teether of this invention can also be prepared by compression molding, extrusion without molding or compression techniques.
[0033] The properties of the proteinaceous materials used in the pet teether are subject to physical and chemical interactions (for example, protein / protein and with other materials including water-absorbing polymers) to improve its solubility and textural properties to intensify the benefits of oral hygiene and animal safety. Animal safety is achieved through product design to minimize risk in all areas. Texture control minimizes the risk of tooth fractures; the controlled reduction in the size of the product through chewing reduces the risk of suffocation; and superior solubility / digestibility eliminates the risk of intestinal obstruction.
[0034] The composition of the pet teether can also contain at least one additional ingredient selected from the group consisting of fat, flavor enhancers, preservatives, nutrients and / or colorants. As used here, the fat includes edible oils and will preferably be liquid fat at room temperature. Exemplary fats include corn oil, soybean oil, peanut oil, sunflower oil, grape seed oil, sunflower oil, flaxseed oil (and other sources of omega 3 and omega 6 fatty acids), vegetable oil, palm kernel oil, olive oil, tallow, lard, vegetable fat, butter and combinations thereof. In a preferred embodiment, the fat is vegetable oil. If fat is present, it will generally be in the range of about 1 to about 20%, preferably about 1.5 to about 10% and most preferably about 2 to about 5% in weight of the composition of the teether for pet. Flavor enhancers are well known and the use of any and all flavor enhancers is covered in the present invention. Other ingredients can also be included in the composition, for example, release agents, stabilizers and emulsifiers.
[0035] The pet teether of the present invention preferably contains an amount of supercritical fluid to occupy 5-55% of the total volume of the composition after the supercritical fluid is transformed into gas within the teether matrix. A variety of amounts of supercritical fluid is predicted depending on the desired density of the teether resulting from the present invention. Preferably, the total volume of the pet teether of the present invention occupied by the supercritical fluid can be, among others, any of the following amounts: 5-50% of the total volume, 10-50% of the total volume, 15-40 % of the total volume, 2035% of the total volume, 5-10% of the total volume, 10-15% of the total volume, 1520% of the total volume, 20-25% of the total volume, 25-30% of the total volume, 3035 % of the total volume, 35-40% of the total volume, 40-45% of the total volume, 4550% of the total volume and 50-55% of the total volume after the supercritical fluid is transformed into gas inside the teether matrix.
[0036] In one embodiment, the composition of the pet teether may contain an amount of supercritical fluid that is 0.050.25% by weight, while this amount may have an amount of supercritical fluid sufficient to occupy 5-55% of the total volume of the composition when the supercritical fluid is transformed into gas. Various amounts of supercritical fluid are anticipated, including, but not limited to, about 0.05% to 0.1% by weight; 0.05 to 0.15% by weight; 0.1 to about 0.15% by weight and any amounts thereof, as well as within the greater range provided above. The amount of supercritical fluid, of about 0.15% by weight, in some applications may be sufficient to occupy a volume of about 25%; 0.10% by weight, while this amount may be sufficient to occupy a volume of about 15%; and about 0.05%, a volume of 5%, or any range among them, as well as within the largest range provided above. In this embodiment, the supercritical fluid is preferably nitrogen. In an alternative modality in which CO2 is used as a supercritical fluid, other than nitrogen, the amount of supercritical fluid can be changed to occupy a certain desired volume of the product of the present invention.
[0037] In one embodiment, the thermoplastic composition may also contain active ingredients for removing plaque and tartar, and materials for fresh breath and oral hygiene in general.
[0038] The pet teether of the present invention demonstrates high elastic properties and flexibility to improve chewing pleasure and to be long lasting. The product is developed to degrade in a controlled way under repetitive chewing. The texture of the pet teether ensures an appropriate balance between the safety of the animal, effectiveness in oral hygiene, fun and prolonged duration. In addition, the degradation or fracture of the invention's pet teether under mechanical stress is controlled to prevent the release of large pieces that can be swallowed intact and increase the risk of digestive obstruction and asphyxiation.
[0039] In one embodiment of the invention, the surface roughness of the pet teether of the present invention is greater when compared to a pet teether that does not include a supercritical fluid in it. The surface roughness refers to the surface texture of the internal cross-sectional area, where this area causes the surface to come into contact with a tooth during the lower bite and the upward attraction involved with chewing. In one embodiment of the present invention, a pet teether of the present invention having a supercritical fluid demonstrates similar flexibility, stiffness and elastic properties when compared to a pet teether that does not include a supercritical fluid in it. Preferably, the recipe or formulation of the pet teether of the present invention can be changed, just as the stiffness, elasticity and flexibility can be changed. In another embodiment, the pet teether of the present invention has textural properties when compared to a pet teether that does not include a supercritical fluid in it. EXAMPLE 1 Formulation of a pet teether composition of the invention: TABLE 1
The water activity of the final products varies from 0.2-0.85. In addition, the individual ingredient levels and ratios from liquid to powder can be modified to obtain various textures of the final product. In addition, substituting ingredients for alternatives can also result in different textures than the final product. For example, using 200-bloom gelatin instead of 100-bloom gelatin can result in a firmer product. EXAMPLE 2 Formulation of a pet teether composition: TABLE 2
EXAMPLE 3 Formulation of another composition of the 10-pet animal bite: TABLE 3
EXAMPLE 4 Formulation of another composition of the pet teether: TABLE 4
EXAMPLE 5 Formulation of another preferred pet teether composition:
[0040] The performance of the pet bite product is measured against a variety of criteria including plaque and tartar reduction, fresh breath, prolonged duration, palatability as measured by paired preference, solubility, textural attributes including stiffness, density , elasticity, friability, water absorption capacity, and solubilization speed.
[0041] Texture measurements were performed with the TA.HDi Texture Analyzer (Texture Technologies Corp., Scarsdale, N.Y.) equipped with 250-500 kg load cells. A 5 mm diameter cylindrical probe was used for the uniaxial puncture or compression tests, and the tests were conducted at an ambient temperature of 25 ° C. The data were collected using Texture Expert software (version 2.12) from Texture Technologies Corp. Two different uniaxial puncture or compression tests were performed. These tests were selected because they are most similar to the biting and chewing of the test samples by dogs.
[0042] The parameters of the compression analysis are as follows. Work (W) is defined as an estimate of work; and therefore shows the toughness of the product. A tough product will have a higher work value than a less tough product. The area shows the “force” or load that can be applied to the product that can cause it to break. The area under the curve represents toughness. The units of “area” expressed are derived from multiplying the y-axis by the x-axis as N * mm. To convert the “Area” to Work-W- (F / d) multiply by 0.1020408 m.sup.2 / mm / s.sup.2.
[0043] The Maximum Force (N) is defined as the maximum amount of force necessary to overcome the rigidity of the product. In general, a rigid product will be associated with high ordinate values (y-axis). The unit "Force" expressed derives from a direct association with the weight of the mass in kg. To convert “Force” to “Maximum Force” multiply -N- by 9.81 m / s.sup.2 (the acceleration due to gravity).
[0044] Travel (mm) is represented as the point (distance) at which the maximum force is reached. Thus, it emulates the strength of the product as a combination of toughness and stiffness, in addition to elasticity, attributed to a measurement of how far the probe has traveled to achieve maximum strength. Larger travel numbers indicate more elastic products. The tensile strength is directly proportional to the travel values.
[0045] Linear distance (mm) is calculated by measuring the length of a stretched imaginary line that joins all points of the trajectory. This measure describes the cohesive versus friable attributes of the product. It is a direct assessment of fragility where a fragile product will produce more sharp peaks, resulting in a longer linear distance.
[0046] The values of stiffness, toughness, elasticity were determined using whole samples of the product. A base platform, as seen with the TA.HDi provided by Texture Technologies, was used to measure the force / distance. An exemplary sample of the product, which has been made and tested, is shown in FIGURE 5.
[0047] The sample was centered on the platform so that the knife comes in contact with one location along the length of the sample structure at a time. The chosen locations include the brush head. The site comes into contact with the knife at an angle of 90 °, while the sample is placed horizontally on the flat surface of the platform. The brush head, the shaft joint for the brush head and the gasket at the end of the shaft of a pet teether are clearly visible in FIGURE 5. SOLUBILITY
[0048] The in vitro measurement of the solubility / digestibility of a pet teether can be used to indicate the amount of pet teether that could be solubilized or digested in a pet's gastrointestinal tract, and so particularly a dog. The test performed is based on a part or whole piece of a pet biting product. A specific size piece or part, for example, a 32 gram pet teether part, can be used so that different formulations can be compared accurately. The result is expressed as a percentage (%) of disappearance in vitro (IVD). The measurement of solubility is performed by subjecting a specific amount of the product to a number of solutions that represent a pet's stomach and intestinal environments. In general, the stomach environment is relatively acidic and the intestinal environment is relatively more alkaline compared to the stomach. After subjecting the product to these environments, any product left is filtered and dried. This left product is weighed and compared to the weight of the starting product. The percentage of IVD is the percentage of the weight of the dissolved product compared to the weight of the initial product. The solubility test is best described below. USED SOLUTIONS:
[0049] Phosphate Buffer Solution, 0.1M, pH 6.0: 2.1 grams of anhydrous dibasic sodium phosphate and 11.76 grams of monobasic sodium phosphate monohydrate were dissolved in a 1 liter volumetric flask and taken volume with distilled / deionized water (dd).
[0050] HCl solution: 17.0 ml of concentrated HCl were added to a 1 liter volumetric flask containing 500 ml of dd water and made up to volume with dd water. When 100 ml of HCl: pepsin is added to 250 ml of phosphate buffer, the pH should be close to 2.0. One way to achieve this is to use 850 ml of 0.1 N HCl +150 ml of 1 N HCl to make 1000 ml of the HCl stock solution. When 100 ml of HCl: pepsin is added to 250 ml of phosphate buffer, the pH of the solution is about 1.9-2.0.
[0051] HCl solution: Pepsin: The appropriate amount of pepsin (Sigma P-7000, amount of pepsin depends on the size of the sample to be tested. 0.01 gram of pepsin per 1 gram of sample must be obtained in the final mixture in Procedure step 6. For example, 0.3 grams of pepsin should be used for 30 grams of sample) was placed in a 1 liter volumetric flask and made up to volume with the HCl solution made above.
[0052] Chloramphenicol solution: 0.5 gram of chloramphenicol (Sigma C-0378) was brought to volume in a 100 ml volumetric flask with 95% ethanol.
[0053] Sodium Hydroxide Solution, 0.5N: 20 grams of NaOH were brought to the volumes in a 1 liter volumetric flask with dd water.
[0054] Phosphate Buffer Solution, 0.2M, pH 6.8: 16.5 grams of anhydrous dibasic sodium phosphate and 11.56 grams of monobasic sodium phosphate monohydrate were dissolved in a 1 liter volumetric flask and taken volume with distilled water.
[0055] Pancreatin Solution: Phosphate Buffer: The appropriate amount of porcine pancreatin (Sigma P-1750, amount of enzyme depends on the size of the sample to be tested. 0.05 grams of porcine pancreatin per 1 gram sample should obtained in the final mixture from Step 8. For example, 1.5 grams of pancreatin should be used for 30-gram samples) was dissolved in a 500 ml volumetric flask and made up to volume with a 0% phosphate buffer solution , 2M, pH 6.8 made above. PROCEDURE EXAMPLE
[0056] 1. Place numbered pieces of Dacron® fabric in an oven at 57 ° C overnight and weigh the next day.
[0057] 2. Weigh the samples in the Erlenmeyers balloons. (Weigh the additional sample to dry as a control along with the residue to account for moisture loss when calculating the% IVD). Add 250 ml of 0.1 M Phosphate Buffer Solution, pH 6.8 to each flask.
[0058] 3. Add 100 ml of the HCl: Pepsin Solution to each flask. Check that the pH of the mixture is about 2. Adjust with HCl, if necessary.
[0059] 4. Add 5 ml of the Chloramphenicol Solution to each flask.
[0060] 5. Cap the balloons. Mix gently. Incubate at 39 ° C for 6 hours. Mix regularly using a shaking water bath, set at a speed that causes the samples to move steadily in the flask while keeping the products submerged in the solution.
[0061] 6. After incubation, add sufficient 0.5N Sodium Hydroxide Solution to each flask to obtain a final pH of 6.8 for the mixture.
[0062] 7. Add 100 ml of Pancreatin Solution: Phosphate Buffer to each flask. Mix gently.
[0063] 8. Cap the balloons. Incubate at 39 ° C for 18 hours. Mix regularly using a shaking water bath, set at a speed that causes the samples to move steadily in the flask while keeping the products submerged in the solution.
[0064] 9. Filter the sample through tared pieces of the Dacron® fabric from Step 1. Rinse three times with dd water. Keep at 57 ° C until the weight is constant.
[0065] 10. Record the pH in the following phases: a. In step 4. b. After 6 hours of digestion. c.After adding the NaOH solution in step 7. d. After adding the pancreatin solution: phosphate buffer. and. After 24 hours. Calculations:

[0066] In certain embodiments, the composition of the pet teether has a solubility of at least 60% IVD, preferably at least 70% IVD and more preferably at least 75% IVD based on a piece of maximum 32 grams (if the pet teether is less than 32 grams, then typically a single teether product of a certain gram weight will be used. It is not recommended to use a piece larger than 32 grams for a realistic reading. Obviously , one of ordinary skill will recognize that the mass of the analyzed pieces must be substantially equivalent to make a comparison of the solubility numbers). While the solubility of the pet teether of this invention may be close to 100%, it will generally be in the range of about 60 to about 95% IVD. The solubility of a pet teether made from the formulation of Example 2 by extrusion and injection molding as described in this document was about 85% IVD.
[0067] In a preferred embodiment, when the process material was exposed to the supercritical fluid, the resulting pet teether IVD had an increased IVD in the range of about 5 to about 10% when compared to an animal teether that does not include a supercritical fluid in it. The increased IVD of the pet teether of the present invention could also have an IVD range that is 5-25% greater, including ranges such as, but not limited to, 5-15%, 5-20%, 525%, 10- 25%, 15-25% and 20-25%. In general, the IVD of the pet teether of the present invention increases as the amount of supercritical fluid increases. EXTRUSION
[0068] In a preferred embodiment, the extrusion can be used to manufacture the products according to the present invention, preferably an extrusion with double screw screw for the production of the pellets. The pellets are subsequently melted and formed into specific shapes by post-extrusion formation, preferably by injection molding. Thereafter, for injection molding, individual pieces of the products are trimmed by instant removal followed by cooling before packaging.
[0069] FIGURE 1 shows a diagram of an exemplary method of producing the pet bite product according to the invention. As shown in FIGURE 1, the manufacturing process for mixing the ingredients for packaging the finished product takes place on a continuous basis. The powdered ingredients are mixed in the mixer for about 5-30 minutes. The uniform mixture of the powdered ingredients is then inserted into an extruder, preferably an extruder with a double screw. Downstream of the powder insertion, the liquid ingredients are added to transform the mixture of the powder and liquid ingredients into a uniformly plasticized moldable mass in the presence of heat and shear. During this process, the moldable dough is also baked by increasing the temperature in the extruder barrels. The temperature profile of the extruder barrels is determined by, among others, the composition, pressure, residence time in the extruder barrels, screw profile, screw speed and shear rate.
[0070] The temperature and shear in the extruder zones will be set to provide sufficient thermoplasticization. This can be achieved with temperatures in the range of about 88 ° C to about 141 ° C in the middle zones and lower temperatures at both ends of the barrel. Obviously, higher temperatures can be used in the middle zones.
[0071] Thus, the temperature can be controlled through the barrel to allow optional ventilation of energy and humidity throughout the extruder. Forced ventilation can also be achieved using ventilation / vacuum fillers at the end of the process section where most of the cooking is achieved in the moldable mass inside the extruder barrel.
[0072] At the extruder outlet, the extrudate is forced through a die with small holes. Immediately behind the die, the extrudate is exposed to increased pressure and temperature due to the restriction imposed by small openings in the die, so the use of extra cooling becomes increasingly important to ensure the quality of the pellet.
[0073] Immediately after the extruder die leaves, the plasticized extrudate is cut on the die surface by a surface cutter equipped with at least one blade in small pellets. The rotational speed of the cutter can be adjusted depending on the size requirements of the pellets in addition to the flow properties of the extrudate. The temperature of the product at the exit of the die can vary from about 82 ° C to about 95 ° C and is more preferably about 85 ° C.
[0074] After cutting, the pellets are placed on moving belts to transport the pellets from the extruder outlet. This process also facilitates the cooling of the pellets to avoid hardening which reduces the need for a later de-agglutination step in the sequence of the process. The mats can be kept at room temperature, however, in order to reduce the cooling time, forced air circulation with cooler air can be applied to induce rapid cooling.
[0075] Depending on the formulation, speed and degree of cooling, the pellets can be together forming groups of different sizes. These groups must be reduced in size, obtained by de-agglutination, to guarantee a constant and stable injection molding process.
[0076] After cooling and de-agglutination, the pellets are transported to injection molding, where the shape of the final product is obtained.
[0077] An alternative manufacturing process can be seen in FIGURE 2. FIGURE 2 shows a diagram of another exemplary method of producing the pet bite product according to the invention, in which the pellets are well manufactured before being used in injection molding.
[0078] While the mixing, extrusion, cooling and de-agglutination steps may be similar to that described above (see FIGURE 1), in the alternative manufacturing process illustrated in FIGURE 2, the pellets are packaged in suitable containers by cooling or de-agglutination. For packing, bags, bags, super bags, barrels, boxes etc. can be used for storage and transfer. The selection of packaging depends, among others, on the packaging characteristics of the pellets, safety and environmental regulations, handling / transport requirements, frequencies of use and sizes.
[0079] Pellet containers must be suitable for target use and inert enough to protect their contents from external elements, such as insects, birds, dust, temperature and humidity fluctuations, sun exposure, aroma / flavor transfer / leaching of the containers.
[0080] Prior to injection molding, an additional de-agglutination process may be necessary to separate groups into individual pellets again, if the packaging or agglutination of the pellets is observed in the containers during storage or transportation. Upon de-agglutination, the pellets are molded into the final product by injection molding as described below.
[0081] In the preferred variations of the processes shown in FIGURES 9 and 10, a supercritical fluid is added to the extruded product, either before or during the injection molding process. A more detailed explanation of the various methods that can be used with this variation is provided below. As can be appreciated, the use of a supercritical fluid and the control of temperature and pressure parameters will form the advantageous bubbles or foam in the final product.
[0082] FIGURE 3 shows yet another diagram of an exemplary method of producing the pet biting product according to the invention. The process, shown in FIGURE 3, combines the powder and liquid ingredients together in a high-shear mixer to form a uniform dough. According to the process shown in FIGURE 3, the pellet production step is also eliminated, feeding the uniform mass directly into the injection molder's barrel.
[0083] In a preferred variation of the process shown in FIGURE 11, a supercritical fluid is added to the mixed product, either before or during the injection molding process. As noted below, the size and density of the bubbles will preferably be controlled, so that the desired concentration and size of the bubbles are produced in the finished finished product.
[0084] After injection molding, the product is cooled and subjected to a trimming process where excess material is removed from the product. Trimming can be achieved by vibrating the product within the vibration hoppers, tables and / or vibration drums. INJECTION MOLDING
[0085] FIGURE 4 shows a schematic drawing of the injection molding process that can be used to prepare the pet biting product according to the invention. The material for the injection molding process can be distributed in containers 1 in the form of pellets. Occasionally, due to transport, the pressure of the cargo, and the nature of the recipe, pellets have a tendency to be packed together and form large adhesive blocks. Thus, if necessary, each container is transferred to a deglutinant 2 to break and separate the individual pellets to allow feeding in the injection molders 4. The individual pellets are collected in a container 3 and then vacuum fed to a feeder 5 taking injection molders for forming.
[0086] As the pellets are transported through the injection molder screw 6, the high temperatures, shear and pressure generated by the screw transform the solid pellets into a melted product that can be injected into the mold 7 and take shape. The melted product travels through sprays and / or manifolds, channels and / or nozzles and then the cavities to form the shape of the final product. When the dose is complete, the injection screw will retract and refill with the melted product for the next dose.
[0087] As the injection molder is being filled, the products formed in the cavities are either cooled or heated as necessary to cool and / or establish the products. Once the desired cooling or defined time is obtained, the mold opens and the products are released from the cavities by means of the ejector pins on the back of the product. Molded products fall onto a mechanical conveyor, from which they are later collected for cooling. If the channels are present, they are removed and the molded products are placed on a cooling table to allow the temperature of the structures to reach room temperature before being packaged. An exemplary molded pet teether is shown in FIGURE 5.
[0088] As explained in more detail below, in the preferred variations of the process shown in FIGURE 12, a supercritical fluid can be added to the process at several points. First, some variations will add the supercritical fluid inside the extruder barrel during the extrusion process. Obviously, care must be taken to ensure that the pressure and temperature parameters are controlled, so that the supercritical nature of the fluid is maintained as desired. Other variations will add the supercritical fluid to the mixed material, moving from the extruder to the injection molding apparatus. Further variations will add the supercritical fluid to the material in the injection molder. As can be appreciated, the nucleation and expansion of the cell resulting from the manipulation of temperature and pressure can be carried out at any desired location or any desired period of time to produce foam products.
[0089] The parameters of the exemplary injection molding process for forming the molded products are shown in Table 5. TABLE 5

[0090] It is also possible to simply mix the ingredients for the formulation and go directly to the injection molder as long as the parameters are controlled to obtain the thermoplasticization of the formulation.
[0091] In another aspect of the present invention, any of the formulations shown in Tables 1-4 are used to produce a treat or pet teether of the present invention. First, the liquid ingredients, not including the oil, are mixed together and kept below the desired temperature, preferably below 50 ° F (-10 ° C). The dry ingredients are also added to a mixer and mixed together. The mixture of the liquid ingredient and the oil is then added to the dry ingredient mixture in several stages to produce a mesh. The various phases are used to prevent clumping and to distribute the liquid evenly. After all the ingredients have been added and mixed uniformly together, the resulting mesh is transferred to a compensation tank for later transport to the injection molders or is transported directly to the injection molders after the mixing process is complete. As described in this document, when making a treat or foam-shaped bite, a supercritical fluid is added or injected into the foundry and the temperature and pressure parameters are controlled to maintain the supercritical state of the fluid until the expansion and nucleation of the cell is desired. , where the temperature and pressure parameters are modified or manipulated to produce a desired bubble concentration and bubble size for the final product. This manipulation can be done before or during the current injection molding process.
[0092] The treats and teethers of the present invention can be formed, so that they are of any desired size and / or shape. In preferred shapes, the volume ranges from 0.15 - 8 cubic inches, the width ranges from 8-25 mm, the height ranges from 14-40 mm and the length ranges from 52 - 153 mm.
[0093] Typical water activity will vary between 0.45 - 0.65, more preferably between 0.48 - 0.62, and even more preferably between 0.52 - 0.59.
[0094] In particularly preferred forms of the invention, the formulations described above are subjected to contact with a supercritical fluid as described below. Contact of such formulations with a supercritical fluid will impart many beneficial aspects to the products of the present invention. For example, treats and teethers having the formulas described above, but which are in contact with a supercritical fluid as described below will have increased oral hygiene properties due to greater interaction with the surface structure, as well as the fragmented internal surface of the product formed by foam. This increased oral hygiene will be evident throughout the mouth including the teeth, gums, inside the cheeks and palate. The surface of the product will have a more rigid or varied texture than the composition of the similar candy that has not been subjected to or has come into contact with a supercritical fluid. This is due to the presence of the microbubbles that are formed by the supercritical fluid. In addition, when the bubbles break, they provide an increased surface area with which the product fragments can come into contact or interact with the mouth and the parts in it. The concentration and distribution of the bubbles will affect each of these properties so that the concentration and distribution of the bubble will increase, the beneficial impact will also increase. In addition, due to the improved mechanics and structure of the bite that results from biting and chewing a product as described here, friction is also increased in the lower bite and in the upward attraction.
[0095] Other advantages of the present invention include greater digestibility compared to treats and teethers having a similar formulation, but which have not had contact with a supercritical fluid. Due to greater digestibility, the stool will also be improved. Finally, treats and teethers will have fewer calories compared to similarly designed and sized treats and teethers due to the microbubbles created by the supercritical fluid.
[0096] In general, the cells (or bubbles) will have an average diameter between 0.05 to 200 μm, more preferably, between 0.1 to 150 μm, even more preferably, between 1 to 100 μm, and even more preferably, between 2 to 80 μm. Preferably, the cell distribution within the candy will be substantially uniform. Substantially uniform in this context will mean, in general, that the density of the cell will not vary by more than 10% over any section of the treat or bite that comprises at least 10% of the total volume of the treat or bite. More preferably, the density of the cell will not vary by more than 7%, even more preferably by no more than 5%, and even more preferably by no more than 3% over such a section. The cell density will generally be greater than 2 x 104 cells / cc, preferably between 2 x 106 to 2 x 1016 cells / cc, more preferably between 2 x 107 to 2 x 1015 cells / cc, even more preferably between 2 x 108 to 2 x 1014 cells / cc, even more preferably between 2 x 109 to 2 x 1013 cells / cc, and more preferably between 2 x 1010 to 2 x 1012 cells / cc. Such cell densities and cell sizes will result in treats that have less calories and less mass per treat compared to treats that have not had contact with a supercritical fluid as described in this document. Preferably, the process parameters will be designed to result in a treat that has a reduction of at least 5% in both mass and calorie when compared to conventional treats, more preferably, the reduction will be at least 10%, even more preferably at least 15%, even more preferably at least 20%, and even more preferably at least 25% or more.
[0097] The provision of extremely small cell sizes and high cell densities in an aerated material, as obtained when using supercritical fluids to provide an aeration operation, as described with reference to the modalities and aspects of the invention causes substantially improved properties for the aerated materials obtained, particularly compared to standard aerated cellular or microcellular materials. For the purposes of the present invention the aerated or foamed material is used interchangeably. In addition, the material formed with little candy is used in the process and, therefore, this material is conserved and their costs are reduced.
[0098] In accordance with one aspect of the invention, an aerated injection molded animal treat is provided. In general, gases such as nitrogen and carbon dioxide in a non-critical state are supplied to a high pressure chamber via a high pressure valve. The pressure inside the high pressure chamber is set higher than the critical point of the gas used, or the chamber is pressurized by means of a compressor higher than the critical point. Similarly, the temperature inside the high pressure chamber is set at or above the critical point for the gas being used or the chamber is heated to that point. Once the pressure and temperature have exceeded the respective critical points of the gas used, the gas is transformed into a supercritical liquid. Preferably, the temperature of the chamber is controllable by conventional means, known in the art. For example, the high pressure chamber can be controlled thermostatically by cooling and selective heating, so that the temperature inside the high pressure chamber can be adjusted and maintained to keep the liquid / gas used in the supercritical state. A polymeric treat, such as those made using recipes similar to those in Tables 1-4, is then placed in the high pressure chamber with the supercritical fluid in it. The candy is then left in the high pressure chamber for a period of time that depends on the thickness, density and stiffness of the candy, as well as the desired amount of cell nucleation and eventual foaming. Once the desired amount of time has passed, the high pressure chamber is opened and the candy is removed from it. Expansion and nucleation of the cell, or foaming, then occurs within the candy due to the pressure and temperature rapidly assuming room temperature conditions after removal of the high pressure chamber. In general, the foaming time can vary from 1 second to 15 minutes, more preferably between 30 seconds and 10 minutes, even more preferably between 45 seconds and 5 minutes, and most preferably between 1 minute and 3 minutes. It will be appreciated that the size and density or concentration of cells within the candy can be adjusted by manipulating the time the candy remains inside the high pressure chamber, as well as the rigidity or permeability of the candy. Those skilled in the art will understand better than the desired amount of reduction in both mass and calorie will be directly related to the amount of supercritical fluid used in the process, the hardness of the treat, the time spent in the high pressure chamber and the temperature in the heating chamber. high pressure.
[0099] When using carbon dioxide as the supercritical fluid, the processes of the present invention will need to be performed at a temperature above 31.1 ° C and a pressure above 1071.3 psi. It will be appreciated that higher pressures and temperatures can be used depending on the desired sweetener and bite characteristics. The key is that the temperature and pressure must be above the critical point in order to keep the fluid in a supercritical state. Critical temperatures and pressures are known in the art for each fluid.
[00100] When using nitrogen as the supercritical fluid, the processes of the present invention will need to be performed at a temperature above - 147 ° C and a pressure above 493 psi. It will be appreciated that higher pressures and temperatures can be used depending on the desired sweetness characteristics. The key is that the temperature and pressure must be above the critical point in order to keep the fluid in a supercritical state. Critical temperatures and pressures are known in the art for each fluid.
[00101] In another aspect of the present invention, dog treats according to the present invention are made using a continuous process. In this process, an extruder is used to deliver a quantity of extruded animal-forming material to a high pressure chamber in which the material is in contact with a supercritical fluid. After leaving the extruder barrel, the material is supplied to a chamber with a supercritical fluid in it. The chamber includes a supercritical fluid in it and the environment within the chamber is maintained under conditions that will maintain the desired state of the supercritical fluid. The material is then improved through the chamber at a rate that will produce the desired level of foam of the material, as described above. In some embodiments, the product flow will be supplied to the chamber as a continuous sheet and the rate at which it progresses through the chamber will be controlled by a series of rollers. Preferably, the rollers will be kept at a constant temperature. In some embodiments, the supercritical fluid is supplied to the chamber after being pressurized and heated to supercritical levels. As the extrudate travels through a series of rollers, the supercritical fluid and the extrudate form a fluid / extrudate system, sufficient fluid being supplied, so that the extrudate is effectively saturated with the fluid as soon as it leaves the chamber. Once the extrudate leaves the chamber, it is subjected to ambient temperatures and pressures, which causes nucleation and expansion of cells within the liquid / extruded material. The extrudate is then heated if further expansion of the cells is desired, thus forming the foam of the extruded material. Obviously, the extrudate can still be heated or re-treated after the foaming process. As described above, the process can be manipulated to control cell density and size in order to form products with the desired characteristics.
[00102] In another aspect of the invention, the supercritical fluid is supplied to an extruded stream at a selected point, so that the supercritical fluid is added to the material as it progresses through the extrusion process, to produce an extrudate that is saturated with the supercritical fluid to a desired level. When the extrudate leaves the barrel of the extruder, it is supplied to a die and then transported to a chamber, where foaming occurs due to the subcritical conditions maintained therein. The pressure in the chamber is maintained at a level lower than that of the extruder barrel outlet and as the pressure drops with the entry of the polymer / fluid material into the chamber, cell nucleation and some expansion occur within the material. If another expansion is desired, the material is heated. As with the other aspects described here, the amount of nucleation and expansion can be controlled by a variety of parameters, by means of which a product with the desired characteristics is produced.
[00103] In another aspect of the present invention, the animal candy forming material can be foamed using a stamping molding process. In general, a stamping molding apparatus includes a mold cavity or form and an alternative mold structure. In this regard, the stamping molding apparatus is housed within a chamber capable of pressurizing. The conditions inside the chamber are maintained so that the supercritical state of the fluid is maintained. A supercritical fluid is supplied to the chamber together with an animal candy forming material, which is positioned between the mold cavity and the alternative mold structure. Once the supercritical fluid and animal candy forming material are in contact for a sufficient time to properly saturate the material with the supercritical fluid, the alternative mold structure presses the material into the mold cavity to make a molded product in the shape of the mold cavity. The pressure and temperature inside the chamber can be adjusted / reduced to subcritical conditions, preferably ambient, immediately before, simultaneously with, or shortly after the material is pressed into the cavity. The time period of the changing conditions will be selected based on the desired effect on the foaming of the material. When the pressure and temperature conditions are reduced simultaneously with the formation of the molded product by pressing the material into the cavity, the nucleation of the cell and the expansion of the cell within the material occur simultaneously with the molding of the product. In such an embodiment, the product has a super microcellular structure and the product is both formed by foam and formed at room temperature in a global operation.
[00104] In a preferred variation of the process shown in FIGURE 13, the candy-forming material comes into contact with a supercritical fluid, during the extrusion process and inside an extrusion barrel. This can be done by injecting the supercritical fluid into an extruder during an extrusion process, in which conditions within the extruder are designed to keep the fluid in its supercritical state. In such an embodiment, supercritical conditions cease when exiting the extruder and cell nucleation and cell expansion occur rapidly. As noted above, nucleation and expansion can be controlled by manipulating both pressure and temperature conditions near the extruder outlet port. For example, the extruder can be connected to a chamber that includes both pressure and heat controls in it, so that individual changes in pressure and / or heat can be adjusted slowly to achieve a desired cell nucleation and expansion characteristic. In another aspect, the sub supercritical gas can be injected into an extruder during an extrusion process, in which the temperature and pressure are brought to a point that exceeds the levels necessary to transform the gas into a supercritical fluid. The gas can be injected into the extruder before or after the point, at which the temperature and / or pressure were above the critical level. Again, nucleation and / or expansion can be controlled as noted above. In another aspect, the extrudate with the supercritical fluid in it is injected into a mold. The mold can be designed to maintain supercritical conditions (for example, with air compression or physical mold compression) and by expanding the mold cavity and the pressure in it is reduced quickly, cell growth occurs. In all of these modalities, the extruder mixing screw assists in the formation of a solution of the extrudate and the supercritical fluid. The shear created by the rotation of the mixing screws elongates the bubbles of the supercritical fluid in the shear direction and stops the rotation of the screw to create progressively smaller bubbles. The use of irregular blades in the mixing screw can facilitate changes in the orientation of the gas / extruded interface in relation to the agility of the shear, thus increasing the efficiency of the laminar mixture that occurs in it.
[00105] In some embodiments, the gas / extrudate mixture is supplied to a static mixer that continuously changes the orientation of the gas / extrudate interface in relation to the agility of the shear and, thus, also intensifies the mixing process. As is known in the art, the diameter of the static mixer must be small to increase the flow rate and overcome the effect of tension on the surface of the gas bubbles. In general, a greater number of mixing elements, as well as small mixing elements are also preferred. As is known in the art, during static gas / extrusion mixing, the gas molecules in the bubbles also tend to diffuse somewhat in the extruded material surrounding each bubble. However, diffusion can also take place in a separate diffusion chamber, into which the two-phase gas / extrudate mixture is introduced. The mixture then becomes a complete single-phase solution in the diffusion chamber as the gas diffuses into the extrudate. The gas concentration in the produced single-phase gas / extruded solution is thus substantially uniform throughout the solution and the solution is effectively homogeneous. If the supercritical fluid does not diffuse in and saturates the extrudate, uniformly and homogeneously, the foamed structure that is formed last will not be uniform because the cell's morphology depends a lot on the concentration of local gas in the solution. In such a modality, the homogeneous and uniform fluid / extruded solution in the diffusion chamber is then heated in a heating section of the same, where the solution is heated quickly (in a typical case, the temperature can rise from about 190 ° C to about 245 ° C, in about 1 second, for example), in order to form nucleated cells in the saturated solution due to the thermodynamic instability that is created because of the decreased solubility of the fluid / extruded solutions at the most elevated. The greater the decrease in solubility that occurs, the greater the nucleation rate of the cell and the greater the number of nucleated cells. To prevent the nucleated cells from growing in the extrusion barrel, high pressure is maintained in the barrel. The nucleated cell solution is then injected into a mold cavity in a mold and cell growth during the mold filling process is prevented by using back pressure to control the pressure in the mold cavity. As noted above, back pressure can be provided by the insertion of air under pressure from a source in the source by means of a shut-off valve. Finally, cell growth occurs within the mold cavity when the mold cavity is expanded and the pressure in it is reduced rapidly, thus producing pressure instability that intensifies cell growth.
[00106] In this sense, the expansion of the mold provides an article molded and formed by foam, having the desired small cell sizes and high cell densities. Using a mixing screw to provide a shear field that produces a laminar flow of the mixed materials and then using either a static mixer having small diameter mixing elements or a selected number of such mixing elements and a diffusion chamber, occurs the saturation of the extruded material with the supercritical fluid. The period of time required to provide such saturation can be reduced from that required in the modalities of the invention discussed above, so that it is possible to obtain continuous operation at relatively high production rates, which would not be possible when longer periods of saturation are necessary.
[00107] In another aspect of the present invention, an injection molded animal treat is provided by a system that includes an extruder operatively connected to an injection molding chamber. The polymeric material for forming animal treats is supplied to the extruder inlet, advanced by the extruder into an attached passage connected to the molding chamber and through the passage to the molding chamber. In the preferred forms, the attached passage receives a single-phase solution of homogeneous non-nucleated fluid from the polymeric material, and a blowing agent maintains that material containing the fluid and blowing agent in a fluid state at a high pressure within the passage, and advances the solution as a flow of fluid into the passage in a direction downstream of the inlet end towards the molding chamber. Preferably, the annexed passage further includes a nucleation pathway in which the blowing agent is nucleated in the single-phase solution that passes through it. The nucleation pathway is constructed to include a polymer receiving end that receives a monophasic solution of homogeneous fluid from a polymeric material and a non-nucleated blowing agent, a nucleated polymer release end constructed and arranged to release the nucleated polymeric material, and a fluid pathway that connects the receiving end to the release end. Optionally, the polymer release end can define a hole in the molding chamber, or it can be in fluid communication with the molding chamber. The nucleation pathway is constructed to have transverse length and dimensions, so that the system is able to subject the mixed fluid polymer homogeneously to the blowing agent at a rate of pressure drop, as it passes through the pathway, through the at least about 0.1 GPa / s, or at least about 0.3 GPa / s, or at least about 1.0 GPa / s or at least about 3 GPa / s, or at least about 10 GPa / s, or at least about 100 GPa / s. The nucleation pathway can also be constructed to have a variable transverse dimension, so that a polymer of the fluid flowing through the pathway is subject to a variable pressure drop rate and / or temperature increase.
[00108] In another aspect of the invention, a system is provided having a molding chamber constructed and arranged to contain a nucleated polymeric material at high pressure in order to prevent cell growth at high pressure. The pressurized molding chamber can be fluidly and mechanically pressurized in order to contain the nucleated polymeric material at a certain high pressure. After reducing the pressure in the pressurized molding chamber, the polymeric material can solidify the desired shape of a microcellular polymeric article, as the molding chamber is constructed and arranged to have such an interior shape.
[00109] In another aspect of the invention, the system is provided having a barrel with an inlet designed to receive a precursor of the extruded material, an outlet designed to release an un-nucleated mixture of fluid from the blowing agent and from the precursor of polymeric article formed by foam for the precursor, a hole connected to a source of the blowing agent, and a reciprocally mounted screw inside the barrel. The extrusion system can also have at least two holes connected to a source of the blowing agent and the hole can be arranged longitudinally along the axis of the barrel, in order to insert the non-nucleated mixture sequentially by means of at least at least two holes in the barrel due to reciprocity of the screw. The system may also include a second extrusion barrel connected in parallel to the first barrel where the second barrel has an inlet designed to receive the non-nucleated mixture of fluid and has a reciprocally mounted screw inside the barrel.
[00110] In another aspect of the invention, a method is provided for the establishment of a continuous flow of the monophasic solution of non-nucleated fluid of the polymeric precursor and blowing agent, for the nucleation of the flow to create a nucleated flow of the mixture, for the passage of the nucleated flow in the shell and for the release of the mixture to solidify in the shape of the shell. Optionally, the flow can be continuously nucleated, subjecting it continuously to a pressure drop of a rate of at least about 0.1 GPa / s when passing the flow in the housing to create a continuous flow of the nucleated material. Alternatively, the method involves intermittent nucleation of the flow subjecting it to a pressure drop at a rate of at least about 0.1 GPa / s, while the flow passes into the shell, so that the non-nucleated material passes through first of the wrapper, followed by the nucleated material. On the other hand, the nucleated flow can be passed into the casing, so that the nucleated material passes through the casing, first followed by the non-nucleated material. The method also involves removing a microcellular article from the wrapper, and in less than about 10 minutes, providing a second nucleated mixture in the wrapper, allowing the second mixture to solidify into the wrapper shape and removing one second solidified microcellular article of the casing.
[00111] In another aspect of the present invention, a method is provided involving the accumulation of a charge from a precursor of the polymeric material formed by foam and a blowing agent, heating a first part of the charge defining at least 2% of the charge at a temperature of at least 10 ° C higher than the average load temperature and the injection of the load in a molding chamber.
[00112] In another aspect of the present invention, a method is provided for the accumulation, in an accumulator fluidly connected to a molding chamber, of a charge including a first part comprising a fluid polymeric material essentially free of the blowing agent and a second part comprising a polymeric material of the fluid mixed with a blowing agent and the injection of the accumulator charge in a molding chamber.
[00113] In another aspect of the present invention, a method is provided which involves the injection of a fluid, a single-phase solution of a precursor of the polymeric material formed by foam and a blowing agent in a molding chamber of an accumulator in communication of fluid with the extrusion apparatus, while the solution is nucleated to create a nucleated mixture and allows the mixture to solidify as a polymeric microcellular article in the molding chamber.
[00114] In another aspect of the present invention, a method is provided which involves injecting a blowing agent into a barrel of the polymer extrusion apparatus extruder while an extrusion screw is moving axially within the barrel.
[00115] In another aspect of the present invention, a method is provided which involves injecting an extrusion screw blowing agent into a barrel of the polymer extrusion apparatus.
[00116] In another aspect of the present invention, a method is provided which involves the establishment of a barrel extrusion apparatus in a precursor of the polymeric fluid article, the removal of a part of the fluid precursor from the barrel, the mixing of the part of the fluid precursor with the blowing agent to form a mixture of the blowing agent and the fluid precursor part, and introducing the mixture into the barrel.
[00117] In another aspect of the present invention, a method is provided that involves introducing a polymeric material mixed with the supercritical fluid into a mold including a part having an internal dimension of less than about 0.125 inch and releasing the polymeric material for solidify in the mold.
[00118] In another aspect of the present invention, a method is provided which involves the injection of a monophasic solution of the polymeric material and blowing agent in an open mold, then the closing of the mold and the formation of a microcellular article in the form of the mold.
[00119] In another aspect of the present invention, a method is provided which involves the establishment of a single-phase non-nucleated solution of a polymeric material and blowing agent, the introduction of the solution into a molding chamber while the solution is nucleated, rupture of the mold, thus allowing cell growth to occur and the recovery of a microcellular polymeric article having a shape similar to that of the molding chamber, but being larger than the molding chamber.
[00120] In another aspect of the present invention, a method is provided which involves forming in an extruder a single-phase solution of homogeneous non-nucleated fluid of a precursor of microcellular polymeric material and a blowing agent, filling a molding chamber with the solution while the solution is nucleated to form within the molding chamber a precursor of nucleated microcellular polymeric material.
[00121] In another aspect of the present invention, a method is provided which involves injecting a mixture of the polymeric / blowing agent in a molding chamber at a melting temperature below 400 ° F, and molding in a molding chamber. a solid foam polymer article having a dead volume of at least about 5% and a length-to-thickness ratio of at least about 50: 1. In certain embodiments of this method, the melting temperature is less than 380 F, in some embodiments less than about 300 F, in other embodiments less than about 200 F, and in other embodiments less than about 100 F.
[00122] In another aspect of the present invention, a method is provided which involves the injection of non-foamed polymeric material into a molding chamber and the release of the polymeric material to form a microcellular polymeric article, having an essentially identical shape to that of the molding chamber. The article includes at least a portion having transverse dimensions of at least about 1/2 inch on each of the three transverse axes perpendicular to the intersection and a dead volume of at least 50%.
[00123] In another aspect of the present invention, a method is provided which involves injecting a fluid precursor of the polymeric material formed by foam into a molding chamber at a molding chamber temperature below about 100 ° C, and releasing the mixture to solidify in the molding chamber as a polymeric microcellular article. The article includes at least a portion having transverse dimensions of at least 1/2 inch in each of the three transverse axes perpendicular to the intersection and a dead volume of at least 50%. The temperature of the molding chamber can be less than about 75 ° C, 50 ° C or 30 ° C.
[00124] In another aspect of the present invention, a method is provided which involves the injection of a single-phase solution of the fluid of the polymeric material and the blowing agent into a molding chamber, while the solution is subjected to a rapid pressure drop at a first rate of pressure drop that is sufficient to cause microcellular nucleation. Essentially, just after the cell growth is released and controlled by subjecting the material to a second pressure drop that is less than the first pressure drop and at a decreasing rate.
[00125] In another aspect of the present invention, a system is provided including an accumulator having an inlet to receive a precursor of the polymeric material formed by foam and a blowing agent, and an outlet, a molding chamber having an input in communication fluid with the outlet of the accumulator and heating devices associated with the accumulator built and disposed of heat, during the operation of the system, a first section of the accumulator close to the molding chamber at a temperature of at least about 10 ° C more than at the average temperature of the accumulator.
[00126] In another aspect of the present invention, a system is provided for the production of injection-molded microcellular material, including an extruder having an outlet at an outlet end thereof designed to release a monophasic solution of homogeneous fluid not nucleated from a polymeric material and a blowing agent and a molding chamber with an inlet in fluid communication with the outlet of the extruder. The system is constructed and arranged to distribute the single-phase solution from the extruder outlet to the entrance of the molding chamber, and during the filling of the molding chamber, nuclear the single-phase solution to form within the chamber a precursor of nucleated microcellular polymeric material.
[00127] In another aspect of the present invention, an extrusion system is provided including a barrel with an inlet designed to receive a precursor of the extruded material, an outlet designed to release a mixture of fluid from the non-nucleated blowing agent and the precursor, a hole connected to a blowing agent source, and a reciprocally mounted screw inside the barrel.
[00128] In another aspect of the present invention, a system is provided for the production of injection molded microcellular material, including an extruder having an outlet at an outlet end thereof designed to release a precursor of the microcellular polymeric material and an blow molding chamber with an inlet in fluid communication with the outlet of the extruder. The system is constructed and arranged to cyclically inject the precursor of the microcellular polymeric material and the blowing agent in a molding chamber.
[00129] In another aspect of the present invention, an extrusion system is provided including a barrel with an inlet designed to receive a precursor of the extruded material, an outlet designed to release a mixture of fluid from the non-nucleated blowing agent and the precursor, a hole connected to a blowing agent source. A screw is preferably mounted by reciprocity within the barrel.
[00130] In another aspect of the present invention, a system for producing a fused polymeric microcellular material includes an entrance instructed and arranged to receive a precursor of fused polymeric microcellular material, a molding chamber and a channel that connects the entrance with the molding. The channel includes a divergent part between the entrance and the molding chamber that increases in width by at least about 100%, while maintaining a transverse area changing no more than about 25%.
[00131] In another aspect of the present invention, a system of the invention includes an entrance constructed and arranged to receive a precursor of molten polymeric microcellular material, a molding chamber and a channel that connects the entrance with the molding chamber. The channel includes a nucleation pathway having a transverse length and dimensions which, when a monophasic solution of the fluid from the polymeric material and blowing agent is passed through the pathway at rates at which the system is built, creates a pressure drop in the pathway. fluid at a rate of pressure drop sufficient to cause microcellular nucleation. The channel includes a region of cell growth between the nucleation pathway and the molding chamber that increases in transversal dimension in the direction of the molding chamber.
[00132] In another aspect of the present invention, a system as described just above, but not necessarily including the region of cell growth that increases in transverse dimension, includes a nucleation pathway having a width to height ratio of at least about 1.5 :1.
[00133] In another aspect of the present invention, a system similar to the one described above, but in which the nucleation pathway does not necessarily need to have a width-to-height range of at least 1.5: 1, has a width equal to one dimension of the molding chamber.
[00134] In another aspect of the present invention, a method is provided which involves injecting a blowing agent into a barrel of the polymer extrusion apparatus while an extrusion screw is moving axially within the barrel. In a preferred embodiment, the method involves injecting a blowing agent from an extrusion screw into a barrel of the polymer extrusion apparatus. This injection technique can be used with any wide variety of conventional and microcellular techniques. In another embodiment, an extrusion screw is constructed and arranged for rotation within a barrel of the polymer extrusion apparatus that includes, within the screw, a lumen communication with a hole in a surface of the screw. The lumen can be used to inject the blowing agent into the extrusion barrel.
[00135] In another aspect of the present invention, a system is provided for producing injection molded articles. The system generally includes an extruder, a molding chamber, a channel that fluidly connects the extruder and the molding chamber and a temperature control device in thermal communication with the channel.
[00136] In another aspect of the present invention, the invention involves the establishment of a fluid mixing blowing agent and a precursor of the injection molded material in an extruder, the passage of the mixture through a channel in a molding chamber , the solidification of the fluid mixture part in the chamber, while maintaining a part of the mixture in the channel in a fluid state, and the injection of the additional fluid mixture into the channel, thereby stimulating the fluid mixture part and the channel within the camera.
[00137] In another aspect of the present invention, a method is provided which involves removing a part of a precursor from the polymeric fluid article from an extrusion barrel, mixing the part of the fluid precursor with the blowing agent to form a mixture, and the reinsertion of the mixture into the barrel.
[00138] In another aspect of the present invention, a system is provided including an extruder with an extruder barrel, a molding chamber and a mixing chamber in fluid communication with a first orifice upstream in the barrel, a second orifice downstream in the barrel and a source of a blowing agent.
[00139] In another aspect of the present invention, a foam-shaped article having a shape essentially identical to that of the molding chamber is provided, including at least a part having a transverse dimension of no more than about 0.125 inch.
[00140] In another aspect of the present invention, there is provided a three-dimensional polymeric foam article having main axes of intersection corresponding to the three dimensions, one of the dimensions associated with a first axis varying as a function of position along the second perpendicular axis. The article includes at least a part having a cross-sectional dimension of no more than 0.125 inches and has a dead volume of at least about 20%.
[00141] Another aspect of the present invention involves a three-dimensional polymeric foam article having three main axes of intersection corresponding to the three dimensions, one of the dimensions associated with a first axis varying as a function of position along the second perpendicular axis. The article includes at least one part having a cross-sectional dimension of no more than 0.125 inches.
[00142] In another aspect of the present invention, an injection molded polymeric part having a length-to-thickness ratio of at least about 50: 1, the polymer having a melt index of less than 10, is provided.
[00143] In another aspect of the present invention, an injection molded polymeric part having a length-to-thickness ratio of at least about 120: 1, the polymer having a melt index of less than 40, is provided.
[00144] In another aspect of the present invention, an injection-molded polymer foam is provided having a dead volume of at least about 5%, and having a surface that is free of opening and spiral visible to the naked eye.
[00145] In another aspect of the present invention, an article having a thickness of less than 0.125 inch at a dead volume of at least about 20% is provided. A method of preparing such an article is also provided, which may involve inserting a mixture of polymeric material with a supercritical fluid into a mold including a part having an internal dimension of less than about 0.125 inch, and releasing the polymeric material to solidify in the mold, the insertion and release of the steps that occur within a period of time less than 10 seconds.
[00146] In another aspect of the present invention, there is provided a molded polymeric article having a shape essentially identical to that of the molding chamber, including at least a part having a transverse dimension of at least% inch in each of the three transversal axes of intersection perpendicular. The article preferably has a dead volume of at least about 50% and is defined by cells including cell walls of medium thickness of the cell wall. The article is free of periodic solid edges with a thickness greater than about five times the thickness of the cell wall.
[00147] In another aspect of the present invention, there is provided a foam-molded polymeric article including at least a part having a transverse dimension of no more than about 0.075 inch and a dead volume of at least about 5%.
[00148] In another aspect of the present invention, there is provided a foam-molded polymeric article including at least a part having a transverse dimension of between about 0.075 inch and about 0.125 inch and a dead volume of at least about 10% .
[00149] In another aspect of the present invention, there is provided a foam-molded polymeric article including at least a part having a transverse dimension of between about 0.125 inch and about 0.150 inch and a dead volume of at least about 15% .
[00150] In another aspect of the present invention, there is provided a foam-molded polymeric article including at least a part having a cross-sectional dimension of between about 0.150 inch and about 0.350 inch and a dead volume of at least about 20% .
[00151] In another aspect of the present invention, there is provided a molded polymeric article including a plurality of cells, wherein at least 70% of the total number of cells have a cell size of less than 150 microns.
[00152] In another aspect of the present invention, a system is provided including a barrel having an inlet at an upstream end designated to receive a polymeric precursor, and an outlet at a downstream end. The barrel includes a blowing agent port between the upstream end and the downstream end, fluidly connectable to a blowing agent source for inserting the source blowing agent into the precursor in the barrel to form a mixture of the precursor material and the blowing agent in the barrel. The system also includes a measuring device having an input connected to the blowing agent source and an output connected to the barrel. The measuring device constructed and arranged to measure the mass flow rate of the blowing agent from the blowing agent source to the blowing agent door. The system also includes a molding chamber having an inlet in the fluid communication with the outlet of the barrel to receive the mixture of the precursor material and the blowing agent of the barrel.
[00153] In another aspect of the present invention, a method of forming a polymeric foam article is provided. The method includes stimulating a flow of the precursor of polymeric article floating in a downstream direction within a barrel of an extrusion apparatus. The method further includes the insertion of a blowing agent into the stream, at a rate measured by the mass flow of the blowing agent to form a mixture of a precursor of the fluid polymeric article and a blowing agent. The method also includes injecting the mixture of the polymeric fluid precursor into a molding chamber fluidly connected to the barrel.
[00154] In another aspect of the present invention, a system is provided including a barrel having an inlet at an upstream end designated to receive a precursor of polymeric article, and an outlet at a downstream end. The barrel includes between the upstream end and the downstream end, a blowing agent port having a plurality of holes. The blowing agent port is fluidly connected to a blowing agent source by introducing the blowing agent from the source into the precursor in the barrel, through the respective holes, to form a mixture of the precursor material and the blowing agent in the barrel . The system also includes a molding chamber having an inlet in the fluid communication with the outlet of the barrel to receive the mixture of the precursor material and the blowing agent of the barrel.
[00155] In another aspect of the present invention, a method of forming a polymeric article is provided. The method includes stimulating a flow of the precursor of polymeric article floating in a downstream direction within a barrel of an extrusion apparatus. The method further includes inserting a blowing agent from a blowing agent source into a stream, through a plurality of holes, in a blowing agent port fluidly connected to the barrel with the blowing agent source. to form a mixture of the precursor material and the blowing agent, and injecting the mixture of the precursor material into a molding chamber fluidly connected to the barrel.
[00156] In another aspect of the present invention, a system is provided for producing an injection molded microcellular material. The system preferably includes an accumulator constructed and arranged to accumulate a precursor of the microcellular material and a blowing agent, and including an outlet. Preferably, the system also includes an injector constructed and arranged to cyclically inject the precursor of the microcellular material through the outlet of the accumulator. Preferably, the system further includes a molding chamber having an inlet in fluid communication with the outlet of the accumulator. The molding chamber is preferably constructed and arranged to receive the precursor to the microcellular material.
[00157] In another aspect of the present invention, a method includes accumulating a charge from a precursor of the microcellular polymeric material and a blowing agent, and injecting the charge into the molding chamber.
[00158] In yet another aspect of the present invention, the product has an average cell count of about 368,976 cells per cubic centimeter. Preferably, the product of the present invention has at least 50,000 cells, more preferably, at least 75,000 cells, more preferably, at least 100,000 cells, even more preferably, at least 125,000 cells, more preferably, at least 150,000 cells , even more preferably at least 175,000 cells, more preferably at least 200,000 cells, more preferably at least 225,000 cells, even more preferably at least 250,000 cells, most preferably at least 275,000 cells, even more preferably at least 300,000 cells, more preferably at least 325,000 cells, more preferably at least 350,000 cells, more preferably at least 360,000 cells, most preferably at least 375,000 cells, more preferably at least 400,000 cells, more preferably at least 500,000 cells per cubic centimeter, where the most preferred range is 300,000 to 400,000 cells per r cubic centimeter. In a preferred embodiment, the cell number of the product of the present invention is at least 2 times more cells than a pet teether that does not include a supercritical fluid in it, more preferably at least 3 times more cells, more preferably at least 5 times more cells, more preferably at least 10 times more cells, more preferably at least 15 times more cells, even more preferably at least 20 times more cells, and more preferably at least 26 times more cells than the pet teether that does not include supercritical fluid in it.
[00159] The average cell volume is preferably about 50,000 to 200,000 μm3, with the most preferred average cell volume being about 107,000 μm3. Preferably, the average cell volume is about 86% less than the cell volume in a pet teether that does not include a supercritical fluid in it. However, the average cell volume can be 80% less, 70% less, 60% less, 50% less, 40% less, 30% less, and 20% less than the cell volume of a pet teether that doesn’t include a supercritical fluid in it.
[00160] In another embodiment of the present invention, the product has a surface roughness greater than a pet teether that does not include a supercritical fluid in it. For the purposes of the present invention, the surface roughness refers to the surface texture of the internal cross-sectional area, where this area causes the surface to come into contact with a tooth during the lower bite and the upward attraction involved with chewing. The surface roughness is preferably measured as a Ra value (μm), where Ra is the arithmetic mean of the absolute values of the profile height deviations from the midline, recorded in the length assessment. In other words, Ra is the average of a set of individual measurements of surface undulations.
[00161] However, the surface roughness can be measured using any known measurement, including, among others, Sq, the standard deviation of the distribution height or in other words, RMS, surface roughness; Ssk, the asymmetry of the height distribution; Sku, the kurtosis of the height distribution that qualifies the leveling; Sp (μm), the height between the highest peak and the middle plane; Sv (μm), the depth between the median plane and the deepest fall; Sz (μm), the height between the highest peak and the deepest drop or Sa (μm), the arithmetic mean height or in other words, the roughness of the average surface. Preferably, the Ra value of the product of the present invention is about 4 to 15, where the values, such as, among others, 4.8, 5, 5.1, 5.5, 5.8, 5.9 , 6, 6.3, 7, 7.6, 8, 9, 10, 11, and 11.8 are predicted to be the Ra value of the product of the present invention. Preferably, the Ra value of the product of the present invention is greater than that of a pet teether that does not include a supercritical fluid in it. In a preferred embodiment, the Ra value of the product of the present invention is at least 1.5 to 4 times the Ra value of a pet teether that does not include a supercritical fluid in it, more preferably at least 2 3 times the Ra value of a pet teether that does not include supercritical fluid in it.
[00162] In another aspect of the present invention, the delicacy of the present invention preferably has an average friction coefficient of about 0.136 ± 0.001 to 0.235 ± 0.049, where the average friction coefficient can also be 0.198 ± 0.063, 0.138 ± 0.001, and the intermediate values. The formula of the pet teether of the present invention can be changed, as is known to those skilled in the art, so that the coefficient of friction, elasticity, flexibility and stiffness can be modified.
[00163] In another aspect of the present invention, the delicacy stiffness of the present invention is preferably less than that of a pet teether that does not include a supercritical fluid in it. Rigidity and / or hardness can be expressed using Vickers, MPa, Young's Modulus (MPa) and Maximum Depth (nm). Preferably, when the sweetness stiffness is measured using Vickers analysis, the stiffness ranges from about 0.003 to 0.02, more preferably from about 0.005 to 0.1, where values, such as, among others, 0 .0061 ± 0.0005, 0.0074 ± 0.0005, 0.0099 ± 0.0021, and 0.109 ± 0.0005 are predicted. In an embodiment using the Young Modulus hardness value [Mpa], the value for the pet teether of the present invention is preferably 20 or less, more preferably, from about 2 to 20, where values, such as, among others, 3, 3.8, 4, 5, 6, 7, 8, 8.1, 8.5, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, and 19 too are foreseen. Preferably, the Young's Modulus of the product of the present invention is about 20% to 90% less than the Young's Modulus [Mpa] of a pet teether that does not include a supercritical fluid in it, where values, such as , among others 30% smaller, 40% smaller, 50% smaller, 60% smaller, 70% smaller, and 80% smaller are predicted.
[00164] The tensile strength of the product of the present invention is preferably less than that of a pet teether that does not include a supercritical fluid in it. Preferably, the average stress resistance for the total product area of the present invention is preferably about 15% to 50%, of the stress resistance for a pet teether that does not include a supercritical fluid in it. In a more preferred embodiment, the average stress resistance for the total area of the product of the present invention is about 34% of the stress resistance for a pet teether that does not include a supercritical fluid in it. When letting the treats age, the average stress resistance of the total area of the product of the present invention is preferably about 30% to 60% of the stress resistance for a pet teether that does not include a supercritical fluid in it. In a more preferred embodiment, the average stress resistance for the total area of the aged product of the present invention is about 47% of the stress resistance for a pet teether that does not include a supercritical fluid in it. Preferably, the maximum strength of the product of the present invention is preferably about 4-10, where a preferred value is about 5.5. The maximum strength value of the product of the present invention is preferably about half the maximum strength value of a pet teether that does not include a supercritical fluid in it. Preferably, the breaking distance of the product of the present invention is preferably about 40-53, where a more preferred value is about 42. Preferably, the breaking distance is about 15-30% less than the of a pet teether that does not include a supercritical fluid in it, more preferably, the breaking distance is about 25% less than that of a pet teether that does not include a supercritical fluid in it. Preferably, the ratio of the maximum distance to the maximum force is greater for the product of the present invention when compared to a pet teether that does not include a supercritical fluid in it. Preferably, the ratio of the maximum distance to the maximum force is about 6: 1 to 8: 1 when compared to 4: 1 for a pet teether that does not include a supercritical fluid in it. Thus, an embodiment of the present invention allows easier penetration of the tooth than a pet teether that does not include a supercritical fluid in it.
[00165] In another aspect of the present invention, an incorporation of meat, dried meat or emulsified meat ("meat slurry") is added to a polymeric delicacy by means of a controlled medium.
[00166] In all aspects described, the control of temperature and pressure is important for the operation of the supercritical fluid. Such temperature and pressure control systems are well known in compression and extruder molding techniques. For example, heating and cooling elements, covers, bands, rings and the like can be used. Likewise, pressure conditions can be controlled in any conventional way, including adjusting the speed of the extruder screw, adjusting the barrel diameters, applying an external pressure source, and the like. In some ways, temperature and pressure can be controlled separately regardless of the extrusion or molding process. Alternatively, temperature and pressure conditions can be controlled as part of the overall processes. Preferably, the pressure and temperature monitors are positioned in the correct locations to ensure that such supercritical fluid is maintained in the supercritical state when desired, and released from the supercritical state in a controlled and deliberate manner.
[00167] The above description and drawings merely explain and illustrate the invention and it is not limited to them, since those skilled in the art, who are in possession of the description, will be able to make modifications and variations in it without departing from the scope of the invention . EXAMPLE 6
[00168] Analysis of surface roughness MATERIALS AND METHODS:
[00169] The samples were prepared by removing the ends of the goodies using a standard peeling knife, exposing the cross-sectional area of the experimental and control goodies. The length was between 2-3 centimeters. Equipment: Nanovea ST400 Optical Profiler Measurement Parameters: Probe = 300 μm / MG7 Acquisition rate = 1000 Hz Average = 1 Surface measurement = 5 X 2 mm Step size = 2.5 μm X 2.5 μm Scanning mode = Constant speed Scan time per line = 00:40:19 Probe specifications: Z resolution = 12 nm Z accuracy = 60 Lateral resolution = 2.6μm PRINCIPLE AND METHOD OF MEASUREMENT:
[00170] The axial chromatism technique used a white light source, where the light passed through an objective lens with a high degree of chromatic aberration. The refractive index of the objective lens will vary in relation to the wavelength of the light. In effect, each wavelength separated from the incident white light will recur at a different distance from the lens (different height). When the measured sample is within the range of possible heights, a single monochromatic point will be focused to form the image. Due to the confocal configuration of the system, only the concentrated wavelength will pass through the spatial filter with high efficiency, thus making all other wavelengths out of focus. Spectral analysis was performed using a diffraction grid. This technique deflects each wavelength to a different position, intercepting a CCD line, which in turn indicates the position of the maximum intensity and 1 allows direct correspondence to the height Z position.
[00171] Unlike the errors caused by the contact of the probe or the manipulative interferometry technique, the Axial Chromatism technology with White Light measures the height directly from the detection of the wavelength that reaches the surface of the sample in focus. This is a direct measurement without any manipulation of math software. This type of measurement was used on a series of pieces of the present treat's candy to determine the surface roughness of the treat. RESULTS AND CONCLUSIONS:
EXAMPLE 7 These examples illustrate how the friction coefficient was determined. MATERIALS AND METHODS
[00172] Sample Preparation: The ends of the goodies were cut using a standard peeling knife, exposing the cross-sectional area of the experimental and control goodies. The length was between 2-3 centimeters. Equipment: Nanovea TRB Settings: 10 Load = 15 N Test duration = 20 min. Speed rate = 100 rpm Length = 5.5 mm Revolutions = 2000 15 Spherical Diameter = 6 mm Spherical Material = Steel Substrate Material = Sample Environmental Conditions: Lubricant = N / A Atmosphere = Air Temperature = 24 ° C Humidity = 40% PRINCIPLE AND METHOD OF MEASUREMENT:
[00173] The base of the instrument was first, leveled in the horizontal position by screwing or unscrewing the adjustable rubber plates in each corner. A ball support containing a spherical diameter of 3 or 6 mm was maintained on a load clamp and placed at a height, which allows the tribometer clamp to be leveled horizontally when resting on the sample to ensure that the normal load is applied vertically . The cuff was then balanced with the counterweight to ensure that the ball and cuff support initially did not apply force to the sample surface. Finally, the weights corresponding to the load required for the test clamp were placed carefully on the clamp on the ball holder. Through the software, the test was then started and the test was performed at a specific speed, for a specific duration and the frictional force was recorded over time. RESULTS AND CONCLUSIONS:
EXAMPLE 8 This example illustrates how the stiffness was determined. MATERIALS AND METHODS Sample Preparation: The ends of the goodies were cut using a standard peeling knife, exposing the cross-sectional area of the experimental and control goodies. The length was between 2-3 centimeters. Equipment: Nanovea Nano Module Machine Parameters: Control Sample * Test Samples Maximum force (mN) = 101 Charge rate (mN / min) = 202 Discharge rate (mN / min) = 202 Displacement (s) = 3030 Calculation = ASTEM E-2546 & Oliver & Pharr Type of indenter = 1 mm spherical 1 mm spherical * Note: Because the control sample was harder and softer than the other samples, a higher maximum force was used. PRINCIPLE AND MEASUREMENT METHOD: The Nano Mechanical Tester is based on the instrumented indentation standards, ASTM E2546 and ISO 14577. It uses an already established method, where an indentator tip with a known geometry is driven to a specific location of the material to be tested by applying an increasing normal load. Upon reaching a pre-established maximum value, the normal load is reduced until complete relaxation occurs. The load is applied by a piezoelectric actuator and the load is measured in a controlled circuit with a highly sensitive load cell. During the experiment, the position of the indenter in relation to the sample surface is precisely monitored with a high-precision capacitive sensor. The resulting load / displacement curves provide specific data regarding the mechanical nature of the material under analysis. The established models are used to calculate the quantitative values of stiffness and modulus for such data. This method was performed on a series of parts of the candy to determine the rigidity of the candy of the present invention. RESULTS AND CONCLUSIONS:
EXAMPLE 9
[00174] This example illustrates how the voltage resistance was determined.
[00175] Sample Preparation: The Base Material was injected and molded into shapes on the Tension Bar. PRINCIPLE AND METHOD OF MEASUREMENT:
[00176] The test method followed the standards described in ASTM D638, ISO 527.
[00177] The sample was placed in the claws of the test machine, which separated the sample at a rate of 1 mm s-1. The force required to separate the sample and the amount of filament in the sample were measured. These values together with the cross-sectional area of the sample in the gauge region were used to calculate the stress properties. This process was repeated several times to determine the total stress resistance of the treats of the present invention. RESULTS AND CONCLUSIONS:
These data are illustrated in Figure 7.
These data are illustrated in Figure 8. EXAMPLE 10 This example illustrates how the distribution and size of the cell were determined. Sample Preparation: The base material was injected and molded in the form of candy and analyzed. Equipment: NSI Imagix microCT system ParameterConfiguration Point SizeSmall 10 Voltage 50.0 kV Amperage200 μA No. of Projections2160 Structure Average1 Structures / s1 15 Small Calibration Tool (0.762 mm) Beam Hardening Correction0Step Method MEASUREMENT METHOD:
[00178] All samples were photographed at a size of 18.2 microns voxel. This means that only the aeration greater than the value of 18.2 microns will be observed and precisely segmented by the system. The samples were thoroughly tested, but only a 2.5 to 3 cm section of the toothbrush handle was photographed for each sample.
[00179] An x-ray tomography was used, which allowed visualizing the internal structures that have different densities without cutting or altering the sample. The darker (blacker) an area appears, the lower the x-ray density of the material in that area. The lighter an area appears, the greater the x-ray density of the material in that area.
[00180] Aeration in Dog Hygiene samples appears dark. The dog's matrix appears gray under these conditions. The unknown shiny white dots seen in all three samples are numbers of atoms or densities greater than the material in the dog matrix. Some typical higher density materials are bone meal, salt, calcium carbonate and sodium bicarbonate.
[00181] Aeration was determined by exporting the slices of y from the x-ray tomography in the Amira software. The slices were reconstructed in three-dimensional structures. The air bubbles were segmented and their percentage of total volume was determined. RESULTS AND CONCLUSIONS:
These data are illustrated in Figure 6.

权利要求:
Claims (21)
[0001]
1. Aerated pet food composition FEATURED by the fact that it comprises: 15-90% by weight of protein; 5-25% by weight of glycerin; 5-25% by weight of water; and between 2 x 106 and 2 x 1016 cells per cubic centimeter (cc), in which the cells are created by releasing an amount of supercritical fluid sufficient to occupy 5-55% of the total volume of the composition when the supercritical fluid is transformed into gas, and the supercritical fluid is nitrogen or CO2.
[0002]
2. Composition according to claim 1, CHARACTERIZED by the fact that the protein comprises 30-50% by weight of fibrous protein and 1525% by gelation protein, wherein the gelation protein comprises gelatin.
[0003]
3. Composition, according to claim 1, CHARACTERIZED by the fact that it still comprises up to 40% by weight of a plasticizer.
[0004]
4. Composition according to claim 3, CHARACTERIZED by the fact that it also comprises 0.05-27.55% by weight of an additional ingredient selected from the group consisting of flavor enhancers, fat, vitamins, minerals, dyes , preservatives, and combinations thereof.
[0005]
5. Composition, according to claim 1, CHARACTERIZED by the fact that the cells have an average diameter between 0.05-200 μm.
[0006]
6. Composition according to claim 5, CHARACTERIZED by the fact that the cell density is between 2 x 108 and 2 x 1014 cells per cubic centimeter.
[0007]
7. Composition, according to claim 5, CHARACTERIZED by the fact that the cells are substantially uniform in distribution throughout the composition.
[0008]
8. Composition, according to claim 5, CHARACTERIZED by the fact that the cells are varied in distribution within the food.
[0009]
9. Composition, according to claim 1, CHARACTERIZED by the fact that the aforementioned aerated pet food has a surface roughness with an Ra value of 4 to 15 μm.
[0010]
10. Composition, according to claim 1, CHARACTERIZED by the fact that Young's Modulus, stiffness value, of said aerated pet food is 20 MPa or less.
[0011]
11. Composition according to claim 1, CHARACTERIZED by the fact that the ratio of the peak distance to the peak force is greater than that of a pet food that does not include a supercritical fluid.
[0012]
12. Composition, according to claim 1, CHARACTERIZED by the fact that the ratio of the peak distance to the peak force is from 6: 1 to 8: 1.
[0013]
13. Composition, according to claim 2, CHARACTERIZED by the fact that gelatin has a Bloom resistance between 100 and 400.
[0014]
14. Method of preparing a pet food composition in accordance with claim 1, CHARACTERIZED by the fact that said composition is extruded prior to the injection molding process.
[0015]
15. Method, according to claim 14, CHARACTERIZED by the fact that the supercritical fluid comes into contact with the composition during the injection molding process.
[0016]
16. Method according to claim 14, CHARACTERIZED by the fact that the composition is injection molded to produce the final pet food product.
[0017]
17. Method, according to claim 16, CHARACTERIZED by the fact that the supercritical fluid is added to the composition during the extrusion process.
[0018]
18. Method of preparing a pet food composition in accordance with claim 1, CHARACTERIZED by the fact that the composition is extruded to produce the final pet food product.
[0019]
19. Method, according to claim 18, CHARACTERIZED by the fact that the supercritical fluid comes into contact with the composition during the extrusion process.
[0020]
20. Composition, according to claim 1, CHARACTERIZED by the fact that the protein comprises gelatin and in which the supercritical fluid is nitrogen.
[0021]
21. Composition, according to claim 1, CHARACTERIZED by the fact that the supercritical fluid is nitrogen.

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法律状态:
2018-05-29| B06F| Objections, documents and/or translations needed after an examination request according art. 34 industrial property law|

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2019-09-03| B06U| Preliminary requirement: requests with searches performed by other patent offices: suspension of the patent application procedure|

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2020-05-12| B15K| Others concerning applications: alteration of classification|Free format text: AS CLASSIFICACOES ANTERIORES ERAM: A23K 1/00 , A23K 1/16 , A23K 1/18 , B01J 3/00 Ipc: A23K 50/40 (2016.01), A23K 20/10 (2016.01), A23K 2 |

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2020-05-12| B06A| Notification to applicant to reply to the report for non-patentability or inadequacy of the application according art. 36 industrial patent law|

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2020-12-01| B09A| Decision: intention to grant|

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2021-02-02| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 22/10/2013, OBSERVADAS AS CONDICOES LEGAIS. |

优先权:

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申请号 | 申请日 | 专利标题

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US201261716913P| true| 2012-10-22|2012-10-22|

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US61/716,913|2012-10-22|

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PCT/US2013/066255|WO2014066438A1|2012-10-22|2013-10-22|Aerated injection molded pet chew|

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