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A kind of preparation method of microcrystalline cellulose

A technology of microcrystalline cellulose and plant fiber is applied in the field of preparation of polymer compounds, which can solve the problems of yield and environmental protection need to be improved, and achieve the effects of saving consumption, reducing power consumption, and reducing the discharge of three wastes.

Active Publication Date: 2016-08-24
湖州展望天明药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] CN103526624B (2015-1-7) discloses a kind of production method of microcrystalline cellulose, but this method still needs to be improved in yield especially environmental protection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Acid hydrolysis: Mix plant fibers and concentrated hydrochloric acid in a rotary reactor at a mass ratio of 1:1, and acidify at 70°C for 0.8 hours to obtain an acidolysis solution with a mass fraction of concentrated hydrochloric acid of 28%; plant fibers are wood, pulp, straw or bamboo;

[0037] (2) Neutralization: add ammonia water accounting for 0.01 times the weight of the plant fiber to the acid solution, then add reverse osmosis water until the pH value is 6, and raise the temperature to 70°C to obtain a neutralization solution;

[0038] (3) Press filter washing: pump the neutralizing solution into the plate and frame filter press, wash with beating water until the chloride is less than 35mg / L, and obtain a wet material;

[0039] (4) Drying: Dry the wet material in a flash dryer, control the inlet air temperature to 130°C, and the outlet air temperature to 70°C, then pulverize and sieve to obtain microcrystalline cellulose.

Embodiment 2

[0041] (1) Acid hydrolysis: Mix plant fiber and concentrated hydrochloric acid in a rotary reactor at a mass ratio of 1: 1.5, and acidify at 100°C for 1.5 hours to obtain an acid hydrolysis solution. The mass fraction of concentrated hydrochloric acid is greater than or equal to 28%; the plant fiber is wood , pulp, straw or bamboo.

[0042] (2) Neutralization: add ammonia water accounting for 0.05 times the weight of the plant fiber to the acid solution, then add beating water until the pH value is 7, and raise the temperature to 100°C to obtain a neutralization solution; the beating water is reverse osmosis water;

[0043](3) Press filter washing: pump the neutralizing solution into the plate and frame filter press, wash with beating water until the chloride is less than 35mg / L, and obtain a wet material;

[0044] (4) Drying: Dry the wet material in a flash dryer, control the inlet air temperature to 140°C, and the outlet air temperature to 80°C, then pulverize and sieve to o...

Embodiment 3

[0046] (1) Acid hydrolysis: Mix plant fiber and concentrated hydrochloric acid in a rotary reactor at a mass ratio of 1:1.3, and acidolyze at 80°C for 1 hour to obtain an acidolysis solution, with a mass fraction of concentrated hydrochloric acid of 30%;

[0047] (2) Neutralization: add ammonia water accounting for 0.03 times the weight of plant fibers to the acid solution, then add beating water accounting for 10 times the weight of plant fibers until the pH value is 6.5, and heat up to 90°C to obtain a neutralizing solution;

[0048] (3) Press filter washing: pump the neutralizing solution into the plate and frame filter press, wash with beating water until the chloride is less than 35mg / L, and obtain a wet material;

[0049] (4) Drying: Dry the wet material in a flash dryer, control the inlet air temperature to 135°C, and the outlet air temperature to 75°C, then pulverize and sieve to obtain microcrystalline cellulose.

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Abstract

The invention relates to a preparation method of a high-molecular compound, and in particular relates to a preparation method of microcrystalline cellulose. The method sequentially comprises the following steps: (1) in a step of acidolysis, plant fibers are mixed with concentrated hydrochloric acid in a rotary reactor in a mass ratio of 1:1-1.5, a mixture is subjected to acidolysis for 0.8-1.5 hours at the temperature of 70-100 DEG C to obtain an acidolysis liquid, and the mass fraction of the concentrated hydrochloric acid is more than or equal to 28 percent; (2) in a neutralizing step, ammonia water of which the weight is 0.01-0.05 times that of the plant fibers is added into the acidolysis liquid, pulping water is added until a pH value is 6-7, and raising the temperature to be between 70 and 100 DEG C to obtain a neutralizing liquid; the pulping water is reverse osmosis water; (3) in a filter pressing and washing step, the neutralizing liquid is pumped into a plate-and-frame filter press and washed by using the pulping water until chloride is less than 35 mg / L to obtain a wet material; and (4) in a drying step, the wet material is put into a flash distillation dryer to be dried, an air inlet temperature is controlled to be between 130 and 140 DEG C, an air outlet temperature is controlled to be between 70 and 80 DEG C, and then, the wet material is pulverized and screened to obtain the microcrystalline cellulose. The method is energy-saving, environmental-friendly, and low in production cost.

Description

technical field [0001] The invention relates to a preparation method of a polymer compound, in particular to a preparation method of microcrystalline cellulose. Background technique [0002] Microcrystalline cellulose (Microcrystalline cellulose, MCC) is a free-flowing extremely fine short rod-shaped or powder-like porous particle that is hydrolyzed by dilute acid to the limiting degree of polymerization (LOOP) of natural cellulose. The color is white or nearly white. Smelly and tasteless, the particle size is generally 20-80 Lm, and the limiting degree of polymerization (LODP) is 15-375; it is not fibrous and has strong fluidity. Insoluble in water, dilute acids, organic solvents and oils, partially soluble and swelling in dilute alkaline solutions, and has high reactivity in the process of carboxymethylation, acetylation and esterification. Due to its special properties such as low degree of polymerization and large specific surface area, microcrystalline cellulose is wid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B15/00
Inventor 金晓明张晓波
Owner 湖州展望天明药业有限公司
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