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Cellulose microfibril production method

A technology of cellulose fibrils and cellulase, which is applied in the fields of green chemistry and biomass energy and materials, can solve the problems that limit the large-scale application of TEMPO chemical oxidation method, equipment blockage, wear and heat, and cannot be recycled and recycled. Reduced chemical consumption, improved production efficiency, and simple and convenient application

Inactive Publication Date: 2016-01-27
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the current method for producing MFC has the following disadvantages: although the energy consumption of producing MFC is significantly lower than that of NFC, it is still relatively large.
According to research reports, the power consumption of producing one ton of MFC products ranges from thousands to tens of thousands of kilowatt-hours; during large-scale and high-intensity production, equipment blockage, wear and heating are prominent
TEMPO chemical oxidation combined with mechanical treatment can significantly reduce energy consumption and equipment loss, but TEMPO oxidation has high requirements on the purity of raw materials; and TEMPO reagents are expensive and consume a large amount, which cannot be recycled; during oxidation, It is necessary to use sodium hypochlorite solution as an oxidant, and add sodium bromide or potassium bromide as an oxidation reaction aid
If the wastewater containing chlorine or bromine is discharged directly after production, it will seriously pollute the environment
Requires subsequent complex and costly water treatment
These problems limit the large-scale application of the TEMPO chemical oxidation method.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 200 grams of northern softwood chemical bleached pulp (Northernbleachedsoftwoodkraft, NBSK) pulp board was pre-soaked with 5 times the weight of distilled water for 60 minutes at room temperature (25° C.), and fully fluffed. Adjust the fiber concentration to 15% (w / w) and use a medium-concentration hydraulic disc refiner for refining. The pulp freeness was reduced to 200.

[0042] Use Na at a concentration of 0.2M 2 HPO 4 -NaH 2 PO 4 Buffer (pH=6.0) adjusted fiber concentration to 6% (w / w). The amount of mannanase added was 1.0×10 4 IU / kg dry pulp. The raw materials and the reaction solution were thoroughly mixed, and kept at 60° C. for 50 minutes.

[0043] The pulp suspension pretreated with hemicellulase was filtered and washed twice with water, and the fiber concentration was adjusted to 2% (w / w). Adjust the pH of the solution to 4 with dilute sulfuric acid. A solution containing an oxidizing agent (acid caroic acid oxidation solution) diluted by 0.5 times v...

Embodiment 2

[0046] 500 grams of sulfate bamboo pulp was adjusted to a fiber concentration of 15% (w / w) with water at room temperature (25° C.). Use a medium-consistency hydraulic disc refiner for beating until the freeness is reduced to 200. Use Na at a concentration of 0.3M 2 HPO 4 -NaH 2 PO 4 Buffer (pH=7.0) adjusted fiber concentration to 5% (w / w). The amount of xylanase added was 5.0×10 3 IU / kg dry pulp. The raw materials and the reaction solution were thoroughly mixed, and kept at 60° C. for 30 minutes.

[0047] The pulp suspension pretreated with hemicellulase was filtered and washed twice with water, and the fiber concentration was adjusted to 3% (w / w). Potassium hydroxide was used to adjust the pH of the solution to 9. A solution containing an oxidizing agent (basic potassium hydrogen persulfate oxidation solution) diluted by 0.5 times volume was added dropwise, and the weight ratio of potassium hydrogen persulfate to pulp dry weight was 1% (w / w). Simultaneously, mechanic...

Embodiment 3

[0051] 300 grams of bamboo mechanical pulp, with a freeness of 250 after refining with a disc refiner.

[0052] The fiber concentration was adjusted to 2% (w / w) using citric acid-sodium citrate buffer (pH = 5.5) at a concentration of 0.15M. Treatment with cellulase. The amount of cellulase added is 50 FPU / kg dry pulp. The raw materials and the reaction solution were thoroughly mixed, and kept at 55° C. for 60 minutes.

[0053] The pulp suspension pretreated with cellulase was filtered and washed twice with water, and the fiber concentration was adjusted to 3% (w / w). Potassium hydroxide was used to adjust the pH of the solution to 9. A solution containing an oxidizing agent (basic sodium peroxymonosulfate oxidizing solution) diluted by 0.5 times volume was added dropwise, and the weight ratio of sodium hydrogenmonomonosulfate to pulp dry weight was 1.5% (w / w). Simultaneously, mechanical stirring and mixing were carried out, the reaction temperature was 30° C., and the react...

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Abstract

The invention discloses a cellulose microfibril production method. The cellulose microfibril production method comprises the following steps of mechanically grinding the cellulose raw material into pulp, adding semi-cellulase and / or cellulase to perform enzyme pretreatment, using peroxy acid and one or more than two mixtures of metal salt of peroxy acid as an oxidizing liquid to oxide the enzyme-pretreated cellulose in water, and destroying a hydrogen bond network structure; mechanically dispersing or emulsifying the oxidized cellulose, so as to obtain the cellulose microfibril product. The cellulose microfibril production method has the advantages that by adopting the chemical oxidizing method of peroxy acid or peroxy acid salt, the -OH at the surface of cellulose can be efficiently oxidized and modified, one part of glycosidic bonds and hydrogen bonds can be destroyed, and the surface structure of the fiber can be loosened; the production cycle of post-processing can be shortened by the oxidized raw material, the mechanical energy consumption can be greatly reduced, and the cost is reduced; the operation is simple, and the cellulose microfibril production method is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the fields of green chemistry and biomass energy and materials. It specifically involves the use of green chemical methods to produce functional renewable biomaterials. Background technique [0002] Cellulose is an important natural structural component of plant tissue, supporting and protecting it. It has the advantages of wide distribution, huge reserves and renewable. Cellulose derived from plants is also an important raw material for the production of biomass fuel and biomass refining, and is widely used in pulp and paper making, textile and hydrolysis to produce fermented sugar and other fields. The basic structural unit of cellulose is a linear glucose chain formed by the connection of glucose through glycosidic bonds. Multiple glucose chains are stacked together to form fibrils. The fiber protofilaments are approximately 5 nm in diameter. The hydroxyl groups on the glucose units in the constituent cellulose protofil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B15/02C08B15/00D21C9/00
Inventor 田霄飞刘明友卢娴肖仙英
Owner SOUTH CHINA UNIV OF TECH
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