Microcrystalline cellulose production method

A technology of microcrystalline cellulose and a production method, which is applied in the field of extraction of natural components of plants, can solve the problems of low purity of microcrystalline cellulose products, difficult waste liquid treatment and high cost of raw materials, and achieves easy recovery and reuse, environmental friendliness, The effect of improving purity

Inactive Publication Date: 2017-05-31

广州市楹晟生物科技有限公司

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Problems solved by technology

[0008] Aiming at the problems of the prior art microcrystalline cellulose production process, such as high cost of raw materials, large amount of acid used, difficulty in waste liquid treatment, low purity of microcrystalline cellulose products, etc., the pres...

Abstract

The invention provides a microcrystalline cellulose production method. Plant fiber raw materials are pre-treated by organic solvents or organic solvent water solution to obtain pre-treated plant fiber raw materials and pretreatment liquid; the organic solvents or organic solvent water solution serve as digestion solvents, catalysts are added, the pre-treated plant fiber raw materials are digested and subjected to solid-liquid separation to obtain digestion liquor and fibers; the obtained fibers serve as raw materials and are bleached, washed, dried and crushed to prepare microcrystalline cellulose. The microcrystalline cellulose production method is less in strong acid usage, low in raw material cost and simple in production waste liquid treatment, and the microcrystalline cellulose is high in purity and yield.

Technology Topic

SolventPre treatment +8

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Experimental program(16)
Comparison scheme(4)

Example Embodiment

[0096] Example 1

[0097] A method for producing microcrystalline cellulose, the method comprising the following steps:

[0098] (1) Use 10 times the benzene-ethanol mixture of absolutely dry plant fiber raw materials, in which the volume ratio of benzene to ethanol is 2:1, and the pressure is 1×10 5 Pa, the temperature is 80 ℃, 50g bagasse (moisture content 12%) with a particle size greater than 60 mesh pore size is pretreated for 50 minutes; the pretreatment liquid obtained after pretreatment is at 0.8×10 5 At a pressure of Pa and a temperature of 70°C, the benzene-ethanol mixture is recovered by concentration under reduced pressure;

[0099] (2) An aqueous acetic acid solution (concentration 95% by weight) with a total mass of 12 times the mass of the absolute dry plant fiber material is used as a cooking agent, and 4% hydrochloric acid of the mass of the absolute dry plant fiber material is used as a catalyst. 5 Steam for 180 minutes at a pressure of Pa and a temperature of 100°C, and filter to obtain a cooking liquid;

[0100] (3) Use hydrogen peroxide to bleach the fiber obtained in step (2), then wash the bleached fiber with water 50 times that of the dry plant fiber raw material, and then vacuum dry the washed fiber, and finally use Grinding and pulverizing to pulverize the fibers to the required particle size to obtain microcrystalline cellulose.

[0101] The purity of the prepared microcrystalline cellulose was 83%, and the yield was 83.7%.

Example Embodiment

[0102] Example 2

[0103] A method for producing microcrystalline cellulose, the method comprising the following steps:

[0104] (1) Use 15 times the benzene-ethanol mixture of absolutely dry plant fiber raw materials, in which the volume ratio of benzene to ethanol is 0.2:1, and the pressure is 1.5×10 5 Pa, at a temperature of 70℃, pretreat 50g bagasse (moisture content 12%) with a particle size greater than 60 mesh pore size for 120min; the pretreatment solution obtained after pretreatment is at 0.8×10 5 At a pressure of Pa and a temperature of 70°C, the benzene-ethanol mixture is recovered by concentration under reduced pressure;

[0105] (2) Use an aqueous solution of mixed acid of acetic acid and n-butyric acid with a total mass of 15 times the mass of the dry plant fiber raw material as a cooking agent, and take the mass of the organic acid aqueous solution as 100% by weight, in which the acetic acid content is 65%. The acid content is 24%, the organic acid aqueous solution and polyacrylic acid with 1% of the total mass of polyacrylic acid are used as additives, and 3% of the mass of the dry plant fiber raw materials is used as a catalyst. 5 Steam for 240 min under Pa pressure and 120°C temperature, filter to obtain cooking liquor;

[0106] (3) Use sodium hydroxide to bleach the fiber obtained in step (2), then wash the bleached fiber with 0.5 times the water of the dry plant fiber raw material, and then spray the washed fiber, and finally The fiber is crushed to the required particle size by extrusion crushing to obtain microcrystalline cellulose.

[0107] The purity of the prepared microcrystalline cellulose was 86.3%, and the yield was 84.2%.

Example Embodiment

[0108] Example 3

[0109] A method for producing microcrystalline cellulose, the method comprising the following steps:

[0110] (1) Use 20 times the benzene-ethanol mixture of absolutely dry plant fiber raw materials, in which the volume ratio of benzene to ethanol is 5:1, and the pressure is 2×10 5 Pa, at a temperature of 90℃, pretreat 50g bagasse (moisture content 12%) with a particle size greater than 60 mesh pore size for 180 minutes; the pretreatment solution obtained after pretreatment is at 0.8×10 5 At a pressure of Pa and a temperature of 70°C, the benzene-ethanol mixture is recovered by concentration under reduced pressure;

[0111] (2) Use an aqueous solution of mixed acid of acetic acid and isobutyric acid with a total mass of 20 times the mass of the dry plant fiber raw material as a cooking agent, and take the mass of the organic acid aqueous solution as 100% by weight, in which the acetic acid content is 70%. The content of butyric acid is 15%, polyacrylic acid with 5% of the total mass of organic acid aqueous solution and polyacrylic acid is used as an additive, and hydrochloric acid with 5% of the mass of dry plant fiber raw materials is used as a catalyst. 5 Steam it for 300 minutes at a pressure of Pa and a temperature of 150°C, and filter to obtain a cooking liquid;

[0112] (3) Use hydrogen peroxide and sodium hydroxide to bleach the fibers obtained in step (2), and then use 25 times the water of the dry plant fiber raw materials to wash the bleached fibers, and then wash the washed fibers Vacuum drying, and finally grinding and pulverizing the fiber to the required particle size to obtain microcrystalline cellulose.

[0113] The purity of the prepared microcrystalline cellulose was 89.7%, and the yield was 85.0%.

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Classification and recommendation of technical efficacy words

high purity
easy to recycle

Microcrystalline cellulose production method

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