• 专利附录
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    • 专利摘要:
    NEW METHOD FOR THE PRODUCTION OF MICROCELLULOSE The present invention is related to a process for the production of microcellulose, comprising the submission of fibrous cellulosic material to an acid hydrolysis procedure, at a temperature of at least 140 ° C and with a consistency of at least 8 % in relation to the dry weight of cellulose, in which the amount of acid added varies from 0.2 to 2%, preferably from 0.5 to 1.5%, in relation to the dry weight of cellulose.
    公开号:BR112012031250B1
    申请号:R112012031250-2
    申请日:2011-06-07
    公开日:2020-11-03
    发明作者:Dahl Olli；Vanhatalo Kari；Parviainen Kari；Svedman Mikael
    申请人:Aalto University Foundation Sr；
    IPC主号:
    专利说明:

    Field of the Invention
    The present invention relates to an improved process for preparing microcellulose by hydrolyzing weak acid from fibrous cellulosic material. Background of the Invention
    Microcellulose (also called stabilized Degree of Polymerization (DP) cellulose and microcrystalline cellulose) is a versatile product in several industrial applications, for example, in the field of food, pharmaceutical, cosmetic, paper and cardboard applications and in many other applications . Microcellulose can also be used in the production of microcellulose derivatives, such as, for example, cellulose / viscose, CMC, nanocellulose and various composite products.
    In addition, several methods have been proposed in the patent literature for the production of microcellulose.
    US Patent 2,978,446 describes the production of stabilized Grade Polymerization cellulose through acid hydrolysis and mechanical treatment. Cellulose is hydrolyzed by boiling in 2.5 N hydrochloric acid (HCl). The concentration of the acid is therefore 9% and the temperature is about 105 ° C. The consistency of the pulp and the amount of acid added are not specified. Hydrolyzed cellulose requires mechanical disintegration in an aqueous medium.
    US Patent 3,278,519 describes a similar method for producing stabilized Grade Polymerization cellulose by cellulose hydrolysis, either with 2.5 N HCl at 105 ° C or with HCl under 0.5% concentration at temperature 250 ° F (121 ° C). The consistency of the pulp and the amount of acid added are not specified.
    US Patent 3,954,727 discloses a method for producing microcrystalline cellulose by hydrolyzing cellulose with diluted sulfuric acid at a temperature ranging between 120 and 160 ° C. The diluted sulfuric acid to which cellulose is added has a concentration of 1% and the mass of acidic cellulose has a concentration of 5%. Thus, the pulp consistency is low and the amount of acid based on the dry weight of the cellulose is high.
    US Patent 7,037,405 describes a method in which a raw pulp material is brought into contact with acid and heated to a high temperature and then mechanically treated. A suitable concentration of acid is mentioned as being 1-5% of the mixture, an adequate pulp consistency as being 3-50%, an adequate temperature range as being 80-120 ° C and a suitable reaction time as being from 30 minutes to 4 hours. After acid hydrolysis, the pulp mixture is mechanically treated to disintegrate the fibers. Preferably, the step of the mechanical disintegration process provides for shearing the microcrystalline cellulose particles to micron size, ranging from about 1 - 10 microns in size. However, the process described in US Patent 7,037,405 is complicated to produce. Thus, the mechanical disintegration step is required after acid hydrolysis. This stage requires a high-cost refining unit in production, in addition to refining energy of 5-100 kWh / ton.
    US Patent 6,228,213 discloses a process for producing microcrystalline cellulose by adding an acidic solution to the cellulose and feeding the cellulose and acidic solution through an extruder, where the cellulose undergoes acid hydrolysis and forms microcrystalline cellulose. The temperature of the extrusion barrel during hydrolysis is 80 to 200 ° C. Due to the temperature of the extruder and the pressure created by the die or screw of the extruder, the cellulose fuses in the extruder, which allows a more intimate contact between the cellulose and the acid. The compression ratio of the extruder screw varies between 1.5: 1 and 3: 1, preferably about 3: 1. The disadvantages of using extruders are that they are expensive, maintenance costs are quite high and require a high input of mechanical energy, with an estimate of at least 100 kWh, typically at least 150 kWh, per ton of dry cellulose (heating energy input is excluded).
    US Patent 5,543,511 describes the production of Cellulose of Degree of Polymerization (DP) stabilized using partial hydrolysis with oxygen and / or carbon dioxide, under a temperature in the range of 100 - 200 ° C.
    US Patent 4,427,778 describes the production of stabilized Degree of Polymerization (DP) cellulose using enzymatic hydrolysis.
    Acid hydrolysis is also used in the production of dissolving pulp, for example, in cooking with acid bisulfite and as a pre-hydrolysis step in the Kraft process. Cooking with acid bisulfite is described, for example, in Rydholm SE's article, Pulping Processes, pages 649 to 672. US Patent 5,589,033 describes a Kraft process for pre-hydrolysis of cellulosic material containing lignin (ie, wood chips). wood), at a temperature of 100-160 ° C for soft woods and 120-180 ° C for hard woods, over a period of 10 to 200 minutes. Kraft-type alkaline neutralization and cooking follows the pre-hydrolysis step. The final product is a pulp with high-purity alpha-cellulose, which can be used as a dissolving pulp. The dissolving pulp has a fibrous structure with a fiber extension of, typically, 0.5 mm to 2.5 mm, depending on the wood raw material. Thus, the physical dimensions are much larger than that of microcellulose.
    In view of the processes described above for the production of microcellulose, there is a need for an even more efficient and economical process for its production. Summary of the Invention
    According to the present invention, it has surprisingly been discovered that a high quality microcellulose with narrow particle size distribution can be produced, from fibrous cellulosic material, by means of mild acid hydrolysis and with a high consistency of at least 8% , and high temperature of at least 140 ° C. The particle size distribution can be easily controlled by varying the conditions of mild acid hydrolysis. Brief Description of the Drawings - Figure 1 shows the particle size distribution curve of the microcellulose produced according to the present invention, at a temperature of 160 ° C and an acid dosage of 0.5%; Figure 2 shows the particle size distribution curve of the microcellulose produced according to the present invention, at a temperature of 175 ° C and an acid dosage of 0.5%; figure 3 shows the particle size distribution curve of the microcellulose produced according to the present invention, at a temperature of 140 ° C and an acid dosage of 0.5%; figure 4 shows the particle size distribution curve of the microcellulose produced according to the present invention, at a temperature of 140 ° C and an acid dosage of 1.5%; and - figure 5 shows the particle size distribution curve of the microcellulose produced at a temperature of 120 ° C and an acid dosage of 1.5%, which does not represent the present invention. Detailed Description of the Invention
    According to the present invention, there is provided a process for producing microcellulose, comprising subjecting a fibrous cellulosic material to an acid hydrolysis procedure, at a temperature of at least 140 ° C and with a consistency of at least 8% with respect to dry cellulose weight, wherein the amount of acid added is from 0.2 to 2%, preferably from 0.5 to 1.5%, with respect to the dry weight of cellulose.
    As used in this specification, the term "microcellulose" includes microcrystalline cellulose (MCC), but it also refers to similar products that are not entirely crystalline and that may contain some amorphous regions. The microcellulose of the present invention typically has a hemicellulose content of about 0 to 10%, preferably 0.5 to 7%, more preferably 1 to 5% by weight, as measured by typical carbohydrate analysis methods ("Determination of hemicelluloses and pectins in wood and pulp fibers by acid methanolysis and gas chromatography"; 1996, Nordic Pulp and Paper Research Journal, No. 4, 1996, pages 216-219).
    Suitable acids for hydrolysis include organic acids and inorganic acids. Organic acids can be, for example, formic acid or acetic acid. Preferred acids are mineral acids, such as sulfuric acid, hydrochloric acid, nitric acid, sodium bisulfate or sodium bisulfite. Also, mixtures of two or more of these acids can be used. A preferred mineral acid is sulfuric acid.
    Preferably, hydrolysis is carried out in a reactor without essential compression, where the reactor's compression ratio is preferably below 1.5: 1, more preferably below 1.2: 1.
    The temperature of the hydrolysis is preferably between 140 and 185 ° C, more preferably between 150 and 180 ° C, and most preferably between 155 and 175 ° C.
    The consistency of the cellulose material during hydrolysis is preferably 8 to 50%, more preferably 15 to 50%, even more preferably 20 to 50%, and even more preferably, 25 to 45%, with respect to dry weight of cellulose.
    The hydrolysis time is preferably 5 to 180 minutes, more preferably 15 to 150 minutes.
    Preferably, mechanical energy is provided during hydrolysis to ensure uniform chemical and temperature distribution, without substantial mechanical shearing and mechanical defibration of the cellulose matrix, preferably at most 20 kWh per dry ton of cellulose, more preferably, a maximum of 10 kWh per dry ton of cellulose, and more preferably, between 1 and 5 kWh per dry ton of cellulose.
    According to the invention, the fibrous cellulosic material and the acid are contacted with each other, preferably by means of mixing.
    After hydrolysis, the mixture obtained from microcellulose-hydrolyzate can, if necessary, be neutralized, or the microcellulose can be separated from the hydrolyzate. The separated microcellulose can be washed and the separated or washed microcellulose can be neutralized. Also, the acid hydrolyzate can be neutralized. Thus, for example, sodium carbonate, sodium bicarbonate, potassium hydroxide, magnesium hydroxide or sodium hydroxide can be used for neutralization procedures. The hydrolyzate is rich in hemicellulose hydrolysis products, such as xylose and glucose, and can be used in the production of ethanol.
    Also, it was observed that the microcellulose material with an average particle size of about 8-100 pm, preferably 10-60 pm, more preferably, 15-30 pm - as determined by the procedure that will be described later in the present description - it can be produced from fibrous cellulosic material, by means of mild acid hydrolysis, with a consistency of at least 8%, and at a temperature of at least 140 ° C, without a subsequent disintegration step. An essential feature of the present invention is the high consistency of the cellulosic material, which is preferably at least 20% based on the dry weight of the cellulose. The high consistency increases the concentration of chemicals, which provides a favorable effect with respect to the reaction speed. In addition, the heating requirement will be less.
    The fibrous cellulosic material used as a starting material in the process of the present invention can be any cellulosic material that can be hydrolyzed under specific conditions. The fibrous cellulosic material does not necessarily have to be a pure cellulosic material, so it can also contain other materials, such as, for example, lignin.
    The lignin content of the fibrous cellulosic starting material is preferably at most 5%, more preferably at most 2%, most preferably at most 1%.
    The fibrous cellulosic starting material typically has a hemicellulose content of about 3 to 15%, preferably 5 to 10% by weight, measured by typical methods of carbohydrate analysis ("Determination of hemicelluloses and pectins in wood and pulp fibers by acid methanolysis and gas chromatography "; 1996, Nordic Pulp and Paper Research Journal, No. 4, 1996, pages 216- 219).
    The fiber length of the fibrous cellulosic raw material is preferably 5-0.2 mm. For fibrous cellulosic materials of a different origin than wood, such as cotton, the fiber length can be greater than 5 mm.
    The fibrous cellulosic material can be derived from material originating from a wood plant, such as, for example, soft wood or hard wood.
    A preferred fibrous cellulosic material is a bleached or unbleached chemical pulp, such as Kraft pulp, soda-anthraquinone pulp (soda-AQ), sulfite pulp, neutral sulfite pulp, acid sulfite pulp, or solvent pulp organic. The pulp may be a softwood or hardwood pulp. The pulp can be a pulp obtained immediately after digestion or a pulp that has been delignified after digestion, or a pulp that has been delignified and bleached.
    A preferred delignified pulp is an O2 delignified pulp. A preferred pulp is a fully bleached pulp.
    According to the present invention, it is also possible to use fibrous cellulosic material obtained from lignocellulosic materials from plants other than wood, such as cotton, grass, bagasse, grain crop straw, flax, hemp, sisal, abaca , or bamboo. Typically, these materials are treated with an alkaline substance to break down the lignocellulosic material into cellulose, lignin and hemicellulose, followed by the separation of cellulose from the mixture. Some plant materials with a low lignin content, such as cotton linen or cotton fabrics, do not necessarily require treatment with an alkaline substance. The cited materials may contain more than 90% cotton fibers from the fibrous material.
    Fibrous cellulosic material, such as, for example, a chemical pulp, preferably has a lignin content below the Kappa number 40, preferably below the Kappa number 30, more preferably below the Kappa number 10.
    According to a preferred embodiment of the invention, the microcellulose produced has a narrow particle size distribution, wherein the average particle size (D50) is 10-60 pm, more preferably, 15-30 pm, and preferably, the particle size distribution (D90) is such that at least 90% by volume of the particles are below 100 µm in size. The particle size was determined by the procedure that will be described later in this specification, whose procedure includes ultrasonic treatment, which can cause disaggregation or disintegration of the sample.
    The microcellulose material obtained by the process of the invention typically has an average particle size between 8-100 pm, preferably between 10-60 pm, and more preferably, between 15-30 pm - as determined by the procedure that will be described later in this report - without any mechanical treatment. It is possible to refine the structure if a finer particle size is required. Therefore, the microcellulose material obtained from hydrolysis can, if desired, be refined to a smaller particle size, through the use of suitable devices, such as, for example, friction polishing devices, in which the refining is performed by means of grinding stones (for example, a Masuko grinder or polisher), high shear mixers or jet milling machines.
    An advantage of the process of the invention is that the purity of the final microcellulose is moderately high and that the product can be easily washed to remove low molecular weight carbohydrates. The cellulose purity of the washed microcellulose can be even greater than 97%.
    The yield of microcellulose production depends on hydrolysis conditions, such as temperature, amount of acid and hydrolysis time, as well as consistency. A typical yield is at least 80%, preferably at least 85% and the yield can still be 90% or more than that.
    According to the present invention, microcellulose can be produced in any suitable equipment, in which the cellulose-acid mixture is not subjected to any substantial compression, such as a vessel / reactor equipped with a helical mixer or conveyor. The latter can be a continuous vertical or semi-vertical type device, for example, M&D digesters, vertical helical digester / reactor type having a helical conveyor. The compression ratio, if any, is typically below 1.5: 1, more preferably below 1.2: 1. Other devices may include continuous blasting towers or continuous downflow digesters, for example, Kamyr type. Experimental Section
    The following examples for producing microcellulose describe the procedure according to the invention. The cooking experiments were carried out with an air bath digester, manufactured by Haato Oy. The air bath digester consists of six separate autoclave units, with a total volume of 2.5 liters. The units are heated with hot air. The air is heated with an electrical resistance and the heated air is circulated with the help of a fan.
    All cooking experiments were done as follows. The cellulose material, pulp or other type of material, was placed in an autoclave unit. The pulp in bale sheets was cut into square pieces with an edge of about 1-2 cm, before introduction into the autoclave unit. A fresh cellulose material, for example, unbleached pulp, was dried to a consistency of 45-50%, then homogenized in a Kenwood home mixer for 5 minutes, prior to introduction into the autoclave unit. An acidic solution was dosed after the cellulose material. First, the acid was previously mixed with deionized water and the aqueous acid solution was poured evenly into the pulp. The lid of the autoclave unit was closed and the unit was heated to 80 ° C. The preheating stage took about 20 minutes for each test. When the starting temperature of 80 ° C was reached, the actual heating stage began. The autoclave unit was heated in a controlled manner, with a heating speed of 2 ° C / min, until the target cooking temperature was reached. Thus, heating, for example, at 160 ° C took 40 minutes, and at 175 ° C, it took 47.5 minutes. The cooking time started when the target cooking temperature was reached. The temperature was maintained at the target temperature for the entire cooking time. When the cooking time was finished, the autoclave unit was immediately removed and cooled with cold water (temperature around 10 ° C).
    Then, the autoclave unit was opened and the cellulose mixture was placed inside a filter bag (90 mesh). The excess acid solution in the mixture was removed with a rotary dryer (manufactured by UPO - drying time of 2 min, speed of about 2800 rpm). The consistency after treatment in the rotary dryer was 45-50%. The cellulose material was then washed with 3 liters of deionized water, first, gently mixing the mixture for 5 minutes and drying the mixture with the rotary dryer, to obtain a consistency of 45-50%. The washing step with deionized water was repeated twice. The pH in the last (third) aqueous mixture was about 6-7, and the wash was considered to be finished.
    The washed cellulose material was weighed. Three samples were taken, each weighing about 20 g, combined and weighed. The combined samples were dried in an oven (105 ° C, 24 hours). Using the moisture value of the sample, the total amount of dry cellulose material (absolute) was calculated. The process yield was calculated using the amount of dry cellulose material from the washed product and the dry cellulose material from the start.
    The particle sizes of the cellulose products were determined by laser diffraction using the Mastersizer 2000 device (manufactured by Malvern Instruments Ltd), equipped with a Hydro 2000MU wet dispersion unit. The determinations were made according to the following procedure: - A sample of cellulosic material was dispersed in 500 mL of distilled water. The sample concentration was adjusted to obtain a 10% darkening. The pumping or stirring speed of the dispersion unit was adjusted to 1500 rpm. The sample was treated by ultrasonic means, for 60 seconds, before measuring the particle size. Particle sizes were measured in 3 sequential measurements, with 60-second intervals. The average value of the three measurements was calculated. A reference sample was measured each time, prior to the sample. The measurement time for each reference sample and for each sample was 5 seconds. The measurements were made using Fraunhofer parameters. More data for laser diffraction measurement principles are presented in application note MRK 561 of the Mastersizer 2000 device, (PiZet method development for laser diffraction measurements), provided by Malvern Instruments, and in accordance with ISO-13320-1 (1: 1999), Particle size analysis - Laser diffraction General Principles. Example 1 - Acid hydrolysis of fully bleached pulp, with 0.5% dosage or acid concentration (in relation to dry pulp), and cooking temperature of 160 ° C
    A series of experiments was carried out with a softly bleached softwood pulp. The pulp was presented in bale leaves (92.4% dry substance content). The procedure for experiment 1-1 is described below. All experiments were done in a similar way.
    Thus, 324.7 g of pieces of pulp (bale leaves, 92.4% dry substance content, 300 g of dry pulp) were placed inside an autoclave unit of an air bath digester. Then, 15.3 ml of sulfuric acid (cone. 1 mole / liter, amount of absolute sulfuric acid 1.50 g) and 660 ml of water were premixed and added to the pieces of pulp. The consistency of the mixture was 30%. The pulp sulfuric acid dosage or concentration (absolute dry pulp acid) was 0.5%.
    The autoclave unit was closed and heating started. The digester was first heated to 80 ° C in 20 minutes and then the heating stage was started. The mixture was heated at a speed of 2 ° C / min, at a temperature of 160 ° C. When the temperature reached 160 ° C, the cooking time started. After 30 minutes of cooking, the autoclave unit was immediately removed and cooled in a water bath. The water bath temperature was 10 ° C. The reaction product was transferred from the autoclave unit into a filter bag (90 mesh) and dried with a rotary dryer (manufactured by UPO, with a drying time of 2 minutes and a speed of about 2800 rpm), then washed according to the washing procedure mentioned above. The amount of washed material was 573.3 g. The material consistency was 47.2%. The amount of dry material was 270.6 g and the process yield was 90.2%. The parameters and results of Example 1 are shown in Table 1.Table 1

    The particle size distribution was determined using the Malvern Mastersizer 2000 device, using the Hydro 2000 MU dispersion unit. The particle size distribution curve for experiment 1-1 is shown in figure 1.
    The results of the experiments in Example 1 show that hydrolysis with a low acid concentration at a temperature of 160 ° C produces a homogeneous microcellulose of satisfactory quality, with an average particle size of about 20 pm, without any mechanical treatment. The yield is satisfactory, with a cooking time of 90 minutes or less, starting to decrease slightly with a cooking time above 90 minutes. Example 2 - Acid hydrolysis of fully bleached pulp, with 1.5% dosage or acid concentration and cooking temperature of 160 ° C.
    A series of hydrolysis experiments were carried out with fully bleached softwood pulp, with 10% humidity. The parameters and results of Example 2 are shown in Table 2.Table 2

    The particle size distribution curves were similar to the curves of Example 1. The results show that microcellulose with an average particle size below 20 pm can be produced without the need for mechanical treatment. The results show that with increasing cooking time, the particle size decreases slightly, but the yield decreases significantly. Compared to Example 1, the average particle sizes are smaller, but the yields are also smaller. Example 3 - Acid hydrolysis of fully bleached pulp, with dosage or acid concentration of 0.5% and cooking temperature of 175 ° C.
    A series of hydrolysis experiments were carried out with fully bleached softwood pulp, with 10% humidity. The parameters and results of Example 3 are shown in Table 3. The particle size distribution curve for Experiment 3-1 is shown in Figure 2.Table 3

    The results presented in Table 3 show that microcellulose with an average particle size of approximately 20 pm can be produced with satisfactory yield, with a cooking time of 30 minutes or less. A decrease in the process yield was observed with a cooking time of 90 minutes. Example 4 - Acid hydrolysis of fully bleached pulp, with 1.5% dosage or acid concentration and cooking temperature of 175 ° C.
    A series of hydrolysis experiments were carried out with fully bleached softwood pulp, with humidity of 101. The parameters and results of Example 4 are shown in Table 4.Table 4

    The results show that a microcellulose of satisfactory quality, with particle size below 20 pm can be produced in the cooking time of 15 minutes. The process yield starts to decrease depending on the reaction time. Short reaction times are advantageous under high cooking temperatures. Example 5 - Acid hydrolysis of fully bleached pulp, with cooking time of 90 minutes and cooking temperature of 140 ° C.
    Two hydrolysis experiments were carried out with fully bleached softwood pulp (10% humidity). The parameters and results of Example 5 are shown in Table 5. The particle size distribution curve for Experiment 5-1 is shown in figure 3, and the curve for Experiment 5-2 is shown in figure 4.Table 5

    The results show that at a temperature of 140 ° C, the sulfuric acid concentration of 1.5% is sufficient to provide a microcellulose of satisfactory quality, with a satisfactory process yield. The process yield is also satisfactory with an acid concentration of 0.5%, but the particle size distribution curve of Experiment 5-1 shows that there is a population of particles with a diameter above 100 pm present in the product. Example 6 - Acid hydrolysis of unbleached pine pulp, with 0.5% dosage or acid concentration and cooking temperature of 160 ° C.
    A series of hydrolysis experiments was carried out with soft wood pulp after the cooking stage. The parameters and results of Example 6 are shown in Table 6.Table 6

    The results show that a high quality microcellulose can be produced, using a freshly produced softwood pulp as raw material. The process yield was considered satisfactory in Experiments 6-1 and 6-2 and moderate in Experiment 6-3. The smallest average particle size is that shown in Experiment 6-3. Example 7 - Acid hydrolysis of unbleached soft wood pulp, with an acid concentration of 1.5% and cooking time of 30 minutes.
    Two hydrolysis experiments were carried out with unbleached softwood pulp. The parameters and results of Example 7 are shown in Table 7.Table 7

    The results show that the pulp of soft, unbleached wood is an adequate raw material for the production of microcellulose. The cooking time of 30 minutes is sufficient. Example 8 (Comparative) - Acid hydrolysis of fully bleached pulp, at a temperature of 120 ° C.
    A series of hydrolysis experiments were carried out with fully bleached softwood pulp (10% humidity). The parameters and results of Comparative Example 8 are shown in Table 8. The particle size distribution of Experiment 8-5 is shown in figure 5.Table 8

    The results show that when the pulp is cooked at a temperature of 120 ° C, even for long periods, the quality of the microcellulose is not very satisfactory. Above 10% of the particles have a particle size 10 greater than 100 pm, and therefore, a refining step is necessary to obtain sufficient material for microcellulose applications.
    权利要求:
    Claims (14)
    [0001]
    1. Process for the production of microcellulose, the process of which involves subjecting fibrous cellulosic material to an acid hydrolysis procedure, at a temperature of at least 140 ° C and with a consistency of 15 to 50% in relation to the dry weight of cellulose, where the amount of acid added varies from 0.2 to 2% in relation to the dry weight of cellulose, and in which hydrolysis is carried out in a reactor, characterized by the fact that the compression rate of said reactor is below 1.2 :1.
    [0002]
    Process according to claim 1, characterized in that the added acid is a mineral acid, preferably sulfuric acid, hydrochloric acid, nitric acid, sodium bisulfate or sodium bisulfite.
    [0003]
    Process according to either of claims 1 and 2, characterized in that the amount of acid added varies from 0.5 to 1.5% with respect to the dry weight of cellulose.
    [0004]
    Process according to any one of claims 1 to 3, characterized in that the temperature is between 140 and 185 ° C, preferably between 150 and 180 ° C, more preferably between 155 and 175 ° C.
    [0005]
    Process according to any one of claims 1 to 4, characterized in that the consistency of the cellulose is 20 to 50%, and preferably, 25 to 45% with respect to the dry weight of cellulose.
    [0006]
    Process according to any one of claims 1 to 5, characterized in that the hydrolysis time is 5 to 180 minutes, preferably 15 to 150 minutes.
    [0007]
    7. Process according to any one of claims 1 to 6, characterized by the fact that the entry of mechanical energy during hydrolysis is carried out to guarantee a uniform chemical and temperature distribution, without any mechanical cutting and defibration of the matrix. cellulose, preferably not more than 20 kWh per dry ton of cellulose, more preferably not more than 10 kWh per dry ton of cellulose, and even more preferably between 1 and 5 kWh per dry ton of cellulose.
    [0008]
    Process according to any one of claims 1 to 7, characterized in that the fibrous cellulosic material and the acid are mixed together.
    [0009]
    Process according to any one of claims 1 to 8, characterized in that the obtained microcellulose-hydrolyzate mixture is neutralized, or the microcellulose is separated from the hydrolyzate, the separated microcellulose being optionally washed and the microcellulose separated or washed being neutralized or the separated hydrolyzate being neutralized.
    [0010]
    Process according to any one of claims 1 to 9, characterized by the fact that the fibrous cellulosic material originates from a wood production plant, such as softwood or hardwood.
    [0011]
    Process according to any one of claims 1 to 10, characterized in that the fibrous cellulosic material comprises bleached or unbleached chemical pulp, such as Kraft pulp, soda-anthraquinone pulp (soda-AQ), sulfite pulp, neutral sulfite pulp, acid sulfite pulp, or organic solvent pulp.
    [0012]
    12. Process according to any one of claims 1 to 9, characterized in that the fibrous cellulosic material is derived from a production material other than wood, such as cotton, grass, bagasse, grain-growing straw , linen, hemp, sisal, abaca or bamboo.
    [0013]
    13. Process according to any one of claims 1 to 12, characterized in that the fibrous cellulosic material, such as chemical pulp, 10 has a lignin content below the number Kappa 40, preferably below the number Kappa 30 , more preferably, below the Kappa number 10.
    [0014]
    Process according to any one of claims 1 to 13, characterized in that the microcellulose produced has an average particle size of 8 - 100 pm, preferably 10 - 60 pm, and more preferably, the distribution the particle size is such that at least 90% by volume of the particles are below 100 µm in size.
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    法律状态:
    2018-04-10| B06F| Objections, documents and/or translations needed after an examination request according art. 34 industrial property law|
    2018-07-17| B25D| Requested change of name of applicant approved|Owner name: AALTO UNIVERSITY FOUNDATION SR. (FI) |
    2019-08-06| B06U| Preliminary requirement: requests with searches performed by other patent offices: suspension of the patent application procedure|
    2019-12-24| B06A| Notification to applicant to reply to the report for non-patentability or inadequacy of the application according art. 36 industrial patent law|
    2020-05-19| B09A| Decision: intention to grant|
    2020-11-03| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 07/06/2011, OBSERVADAS AS CONDICOES LEGAIS. |
    优先权:
    申请号 | 申请日 | 专利标题
    FI20105641A|FI126842B|2010-06-07|2010-06-07|A novel process for preparing microcellulose|
    FI20105641|2010-06-07|
    PCT/FI2011/050527|WO2011154601A1|2010-06-07|2011-06-07|A novel method to produce microcellulose|
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