• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Composition pour l'alimentation des ruminants contenant une substance biologiquement active hydrosoluble, stable dans un milieu dont le pH est supérieur ou égal à 5 et qui permet la libération de la substance active dans un milieu dont le pH est inférieur à 3,5 comprenant :- un noyau contenant la substance active, ayant éventuellement subi un traitement de surface- une première couche d'enrobage constituée d'une substance filmogène sensible aux variations du pH éventuellement associée à une charge minérale, et- une seconde couche d'enrobage constituée d'une substance hydrophobe éventuellement associée à une charge minérale.
    公开号:SU1651775A3
    申请号:SU874203664
    申请日:1987-11-16
    公开日:1991-05-23
    发明作者:Отан Пьер；Буррэн Поль；Картиллье Андре
    申请人:Рон-Пуленк Санте (Фирма)；
    IPC主号:
    专利说明:

    FIELD: feed production.
    The purpose of the invention is to increase the stability of the feed pellets in an environment with a pH greater than or equal to 5.5 and selected
    biologically active substance &; at pH less than or equal to 3.5.
    The ruminant feed pellet consists of a core containing lysine hydrochloride, which is hung
    with microcrystalline cellulose, with the formation of granules with a diameter of 0.8 to 1.0 mm, the last surface treatment
    The first protective layer (precoating) is formed by a substance or composition sensitive to changes in pH.
    The second protective layer (final or topcoat) is formed by a hydrophobic substance or a hydrophobic composition that may contain mineral filler. The resulting product is stable in an environment with a pH equal to Pl exceeding 5.53 and releases the active substance in an environment with a pH equal to or less. 3; 5 „
    Surface treatment of the core in the form of granules consists in spraying a hydrophobic type binder solution containing dispersed mineral filler, preferably hydrophilic type, onto their surface.
    The binder is selected from hydrophobic polymers such as zein, ethyl cellulose or cellulose acetobutyrate.
    Mineral fillers are chosen, in particular, from silica or precipitated silica, such as aerosil (Aerosil) 300 and levilite calcium carbonate or kaolin.
    Since the stability of the surface-treated granule at pH 6 increases with increasing binder content, theoretically there is no upper limit for binder content. However, to obtain a finished granule with a biologically active substance content that is acceptable, it is particularly preferable to limit the binder content to about 10% by weight from covered granules
    with
    The hydrophilic mineral filler usually constitutes up to 10% of the total syrup content of the coated granule, and a higher content does not lead to a noticeable increase in stability at PH 6.
    The precoat layer (the first protective coating layer) usually consists of a base film-forming polymer that is sensitive to pH changes, in some cases in conjunction with a water-insoluble polymer and / or a hydrophobic substance.



    ten
    15
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    25
    517754
    Among the basic amine-containing polymers can be called polymers containing at least one basic amino group and with a basic nitrogen content of 2-14%. For example, copolymers of styrene with isomers or derivatives of vinylpyridine, and especially copolymers of styrene with 2-vinylpyridine,
    The water-insoluble polymer is usually chosen from cellulose derivatives such as ethyl cellulose or zein.
    Hydrophobic substances are usually chosen from fatty acids, fatty alcohols, and mixtures thereof. Of particular interest are hydrophobic substances with a higher melting point, and especially stearic acid with a purity greater than 90%.
    In the pre-coating composition of the base polymer, in known cases, in combination with a water-insoluble polymer, it is 0.5-10%, preferably 4% of the mass of the core.
    Usually the precoat layer has a thickness of 5-10 microns.
    After surface treatment, it is advisable to coat the core with a basic copolymer in combination with a hydrophobic substance having a melting point above 60 ° C in order to limit the amount of the basic amino-containing polymer. The ratio of basic copolymer / hydrophobic substance 35 B0 is 5 / 95-50 / 50 and, in particular, 20/80 wt.%.
    The final coating layer (second protective layer) is usually a mixture of hydrophobic substances. Hydrophobic substances are chosen so that the outer layer of the coating has a structure with the possibility of diffusion or penetration of an external liquid medium. In addition to poor water permeability, hydrophobic substances should have appropriate mechanical properties, such as increased resistance to stretching and elongation and ability to film formation.
    Among the hydrophobic substances include fatty substances, paraffins, natural waxes (carnauba wax, beeswax), synthetic waxes 55 (polyethylene wax), polymers such as polyethylene, paraffins. Hydrophobic substances can be used individually, but prefer
    thirty
    40
    45
    50
    516
    blend to form an outer layer with desired mechanical properties.
    The thickness of the second layer, the upper (final) coating, depends on the viscosity of the hydrophobic composition in the molten state.
    In order to obtain a thin final coating, it is recommended, in particular, that the viscosity in the molten state is 2-100 P.
    Coating unsatisfactory with too low viscosity. With an ingot of high viscosity, the final coating layer is too thick and agglomeration phenomena occur.
    It is most advisable to use a film-forming hydrophobic polymer (for example, polyethylene), a diluent that reduces the viscosity of the molten phase (for example, paraffin melting at about 60 ° C) and an agent that provides mechanical stability for the final coating. which has a high fluidity in the melting state and a high hardness in the solid state (for example, Polymax 580 or polyethylene wax), which gives good mechanical stoicity and prevents adhesion when and USE temperature.
    In the compositions, the outer layer of the coating, the average thickness of which may vary from 5 to 200 µm, depending on the size of the granule to be coated, is 25-35% of the total mass of the composition.
    In order to improve the properties of the compositions, it is possible to add to the hydrophobic composition of the final coating a powdered mineral filler selected among the fumed or precipitated silica. The content of the mineral filler is 0.1- 30 wt.% And preferably 1-15 wt. composition of the final coating.
    The compositions may contain additives, the role of which is to facilitate the preparation of these compositions and to improve their physicochemical properties.
    Plasticizers (triacetin, propylene glycol), lubricant (magnesium stearate), binding (polyvinylpyrrolidone, polyvinyl alcohol, gelatin) can be added, anti-7575
    statics (trioxide with polyoxidated chains), formers, fungicides, emulsifiers, agents of compatibility, sugars, collapse, small or proteins. These additives comprise only a few percent by weight of the coating.
    The active substances included in the Q compositions are various therapeutic or nutritional substances intended to be administered orally by ruminants, and in particular substances with an increased 5 solubility in water, usually exceeding 100 g / l. Lysine chlorohydrate can be used as active substance.
    The new products are spherical or cylindrical granules with an average diameter of 0.05-5 mm.
    The compositions can be obtained by applying known granulation techniques and a protective coating. 5Surface scrubbing is usually carried out by spraying a dispersion of mineral wool into an organic binder solution.
    The pre-coating of the surface-treated granules can be carried out using known techniques, for example, fluidized bed capsulation, dipping, or co-servicing.
    Various techniques can be used to effect the final coating.
    It is possible to carry out a final coating in a fluidized bed by macadam, adsorption in a liquid medium or by coacervation.
    It is also possible to coat the hydrophobic substance in the melt or in the solution by depositing the suspension with the pre-coated active substance into the melt or into the solution of the hydrophobic substance in an appropriate organic solvent, in which the pre-coated active substance is not soluble, on a flat or concave a disk having grooves and rotating at a certain speed when heated with hot air, usually from a temperature of 20 ° C to the temperature of solidification of the hydrophobic composition. The pre-coated active substance is dispersed in a hydrophobic composition, the weight of which is twice as large.
    five
    five
    An excess of the hydrophobic composition forms small particles that fall next to the disk while the particles of the coated active substance are further ejected. Separation of particles of the coated active substance and particles from the hydrophobic composition occurs systematically in the course of the method. In addition, excess hydrophobic composition can be recirculated.
    The surface treatment is carried out by spraying the granules of the dispersion of the mineral filler in a solution of the binder in an organic solvent (methylene chloride-methanol chloride 50-50).
    The precoating is carried out by treating the granules, pretreated in a boiling bed, with a solution in an organic solvent tetrahydrofuran, methylene chloride) of a precoat composition sensitive to changes in pH.
    The final coating is carried out by dispersing 50 g of pre-coated granules into 100 g of molten hydrophobic composition containing sometimes dispersed mineral filler, then pouring the dispersion into the center of a horizontal disk rotating at a speed of about 1500 rpm, which temperature is maintained above the melting point of the hydrophobic compositions. The granules roll off the disk, while the film is solidified by spontaneous cooling during the fall path. The salting out of the active substance contained in the obtained granules is determined by stirring a known amount of granules in a buffer medium maintained at a constant pH and at 40 ° C. The salting out rates of the sample at different pHs are compared.
    Resistance in the first chamber of the stomach is determined as follows.
    Weigh 200 mg of the test sample and place it in a nylon bag with a 300x300 µm empty space. The sachets are sealed by heat sealing and placed in the first gastric chamber of the fi xed ova. After 48 hours, the sachets are collected, washed and analyzed. The remaining active composition.
    Example 1 (comparative prototype). Methionine is precoated in the form of granules with an average diameter of 0.50-0.63 mm by means of a 2-vinylpyridine styrene copolymer so that the thickness of the precoat layer is about 8 microns.
    The granules thus obtained.
    is coated with a hydrophobic composition consisting of polyethylene with a small molecular weight (20), polyethylene wax (50) and paraffin, melt 5 at 60 ° C (30). Thus, granules with a methionine content of about 60% are obtained.
    The salting out test results are summarized in the table below. one.
    Example 2 (comparative) „
    The procedure is the same as in Example 1, but replacing methionine with lysine chlorohydrite.
    In example 1, methionine coated
    5, a two-layer system formed by a pH-sensitive copolymer coated with a hydrophobic substance leads to satisfactory results; lysine hydrochloride, covered by the same system, has no difference in behavior at pH 6 and at pH 2, i.e. these various results show the difficulty of properly coating lysine hydrochloride.
    Examples 3-14. Lysine hydrochloride containing 15% avicilli (Avicel - microcrystalline cellulose) in the form of granules with an average diameter of 0.8-1 mm is used.
    The granules are pretreated with zein (10 wt.% Granules) containing mineral fillers.
    Pre-coating (first
     the protective coating layer is carried out by means of a 2-vinyl-shdin-styrene copolymer (70-30) so that the pre-coating is 4 cores.
    The final coating is carried out by means of a composition consisting of a low molecular weight polyethylene (20), polyethylene wax (50), paraffin (30) - composition P, in known cases, containing
     Aerosil 300 - Q composition.
    The results of the salting out and durability tests in the first chamber of the burner are given in table. 2
    0
    0
    91
    Examples 15–16. Operate as in Examples 3-14, using lysine hydrochloride, containing 15% of Acercels in the form of granules with an average diameter of 0.8–1.0 mm.
    The surface treatment was carried out with the composition of ethylcellulose (10% by weight) and Aerosil 300 (10% by weight%)
    The precoat (first layer) is carried out by a pH-sensitive composition composed of 2- vinyl pyridin-styrene copolymer (70-30) and stearic acid, 20 to 80% by weight.
    The final coating (second layer) is carried out with the indicated composition P or composition Q.
    The results of testing for salting out and resistance in the first chamber of the stomach are given in table. 3
    Examples 17-19. Lysine hydrochloride is used, containing 15% avicilli in the form of granules with an average diameter of 0.8-1.0 mm.
    The granules are surface treated with a composition containing 10 wt.% Zeein core and 10 wt.% Kaolin core,
    The precoat composition is made up of 2-vinylpyridine-styrene copolymer (70-30). The precoat is about 4 wt.% Core (about 7 microns thick),
    The final coating is carried out with a composition formed of low molecular weight polyethylene (20), polyvax 500 (50), paraffin (30) and mineral filler. The content of the mineral filler is determined so that the viscosity of the molten mixture is the same in all tests.
    The test results on salting out and resistance in the first chamber of the stomach are given in table. four.
    For the composition of Example 19 salting out at pH 2 after 2 hours at 40 ° C is 92%.
    The results of Table 2 show that in Examples 3-14, the first coating layer is formed by a copolymer of 2-vinylpyridine with styrene and it does not contain an inorganic (mineral) filler.
    Without pretreatment of the core (examples 3 and 4), the results are unsatisfactory when the second coating layer contains or does not contain an inorganic filler, although



    0
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    ten
    a slight improvement is due to the addition of an inorganic filament to the second layer (example 4).
    When pre-treating the core with one zein (examples 5 and 6), a clear improvement occurs when the top coating layer contains an inorganic filler (Table 2, salting out percentage at pH 6 after 5 hours).
    With pretreatment with zein (examples) containing an inorganic filler, an even more significant improvement occurs when the topcoat layer contains an inorganic filler (examples 9, 11 and 13).
    The results of Table 3 show that in the examples the first layer of the coating does not contain an inorganic filler and is formed by a copolymer of 2-vinylpyridine-styrene and stearic acid, the core is pre-treated with ethyl cellulose associated with aerosil 300a
    The results are comparable, regardless of whether or not the topcoat layer contains an inorganic filler.
    权利要求:
    Claims (1)
    [1]
    Invention Formula
    five
    0
    five
    0
    five
    I. A method for obtaining ruminant feed pellets, comprising coating a core containing a biologically active substance with a protective sheath, characterized in that in order to increase the stability of the feed pellets in a medium with a JSS pH and release the biologically active substance at a pH of $ 3.5 , as a biologically active substance, lysine hydrochloride is used, which is mixed with microcrystalline cellulose with the formation of granules with a diameter of 0.8-1.0 mm, before coating the obtained coating with the protective sheath hydrophobic binder, zein or ethylcellulose with an inorganic filler — silica or calcium carbonate, or kaolin in a mass ratio of 10: 5–10 binder; and covered with two layers of protective sheath, the first of which is formed from a copolymer of nyl pyridystyrene, and the second applying a mixture of polyethylene, poly (poly) seal wax and paraffin, the first layer being 4% of the mass of sp1, the second layer is from the total thickness of the core and the first layer.
    } The method according to claim 1, that is, that the first layers of the protective shell are formed by mixing the copolymer 3 of vinylpyridine styrene with stearic acid, the melting point of which is above 60 ° C, in a weight ratio of 20:80, respectively.
    3. The method according to claim 1, I differ by the fact that the mixture of polyethylene, polyethylene wax and paraffin, constituting the second layer, is additionally mixed with silicon dioxide (aerosil) in an amount of 1-15% by weight of the composition of the second layer.
    Table 1
    In the presence of 0.6 /, tvn-80.
    In the presence of 0.5%,
    Aerosil
    300
    Levilit
    4 12
    53
    49 50
    Table 3
    Table 4
    78
    21 10
    43.0 + 9.8
    87.8 + 6.1 80.3 + 1.3
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    FR8615930A|FR2606597B1|1986-11-17|1986-11-17|NOVEL COMPOSITION FOR FEEDING RUMINANTS CONTAINING A BIOLOGICALLY ACTIVE SUBSTANCE AND PREPARATION THEREOF|
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