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Method for preparing nano cellulose from plant fibers

A technology of nano-cellulose and plant fiber, which is applied in the direction of pulping with acid acid/anhydride, washing/replacing pulp treatment liquid, etc., to shorten the process time, realize the effect of increasing the size and yield

Inactive Publication Date: 2017-12-08
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Recover residual acid and continue to add it in the pretreatment process

Method used

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  • Method for preparing nano cellulose from plant fibers
  • Method for preparing nano cellulose from plant fibers
  • Method for preparing nano cellulose from plant fibers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Weigh 10g of dry hardwood dissolving pulp fiber raw material into a three-necked flask, add 60ml of sulfuric acid with a mass concentration of 45%, put in a water bath at 55°C, pretreat for 20min, and then add 240ml of deionized water to terminate the reaction. Sulfuric acid was removed by centrifugal washing with deionized water for 4 times, and the washing liquid was collected, and unreacted sulfuric acid and cellulose-degraded sugar were collected by separation of sulfuric acid and carbohydrate nanofiltration separation membrane. The residual sulfuric acid in the pretreated solid obtained by centrifugation was neutralized with 0.1mol / L NaOH solution, adjusted to pH = 7, and then washed by centrifugation three times to remove the salt generated during the neutralization process. The concentration of the pretreated solid solution was adjusted to 5wt%. After a period of disc grinding, the disc grinding gap was 50 μm, and then a uniform and transparent nanocellulose suspe...

Embodiment 2

[0045] Weigh 10g of dry cotton pulp fiber raw material and place it in a three-necked flask, add 100ml of sulfuric acid with a mass concentration of 47%, put it in a water bath at 30°C, pretreat for 15min, and then add 600ml of deionized water to terminate the reaction. The sulfuric acid was removed by centrifugal washing with deionized water for 3 times, and the washing liquid was collected, and unreacted sulfuric acid and cellulose-degraded sugar were collected by separation of sulfuric acid and carbohydrate nanofiltration separation membrane. The residual sulfuric acid in the pretreated solid obtained by centrifugation was neutralized with 0.1mol / L KOH solution, adjusted to pH = 7, and then subjected to 2 centrifugal washings to remove the salt generated during the neutralization process. The concentration of the pretreated solid solution was adjusted to 10 wt%, and after a period of disc grinding, the disc grinding gap was 100 μm, and then a uniform and transparent nanocell...

Embodiment 3

[0047]Weigh 10g of absolute dry bleached bagasse pulp fiber raw material and place it in a three-necked flask, add 80ml of sulfuric acid with a mass concentration of 50%, put it in a water bath at 40°C, pretreat for 10min, and then add 400ml of deionized water to terminate the reaction. The sulfuric acid was removed by centrifugal washing with deionized water for 3 times, and the washing liquid was collected, and unreacted sulfuric acid and cellulose-degraded sugar were collected by separation of sulfuric acid and carbohydrate nanofiltration separation membrane. The residual sulfuric acid in the pretreated solid obtained by centrifugation was neutralized with ammonia water, adjusted to pH = 7, and then subjected to 3 times of centrifugal washing to remove the salt generated during the neutralization process. The concentration of the pretreated solid solution was adjusted to 15 wt%. After a period of disc grinding, the disc grinding gap was 75 μm, and then a uniform and transpar...

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Abstract

The invention discloses a method for preparing nano cellulose from plant fibers. The method comprises the following steps of adding sulfuric acid with mass concentration of 45%-55% into the plant fibers to perform pre-treating for 10-20 minutes at a temperature of 30-55 DEG C, wherein a massic volume ratio of the plant fibers to the sulfuric acid is 1g to (6-10) ml; after pre-treatment is ended, centrifugally washing to remove the sulfuric acid and collecting washing liquid, and separately recycling the sulfuric acid and carbohydrate in the washing liquid through a membrane separating method; neutralizing residual sulfuric acid in a pre-treated solid with alkaline to obtain a pre-treated solid, performing disc-milling on the pre-treated solid with a disc-milling gap of 50 mu m-100mu m, and performing high-pressure homogenizing to obtain nano cellulose suspension liquid; and performing freeze-drying or spray-drying on the suspension liquid to obtain the nano cellulose. Compared with a convention method of preparing the nano cellulose by acid hydrolysis, the method has the advantages of high yield and less time consumption, and provides a new idea for industrial production of the nano cellulose.

Description

technical field [0001] The invention belongs to the field of preparation of nanofibers, in particular to a method for preparing nanocellulose from plant fibers. Background technique [0002] Cellulose is a relatively abundant natural renewable biomass resource in nature, and its structure is a long-chain macromolecule composed of glucose units linked by β-1,4 glycosidic bonds. According to Muhlethaler's ultrastructural model, about 40 cellulose molecular chains are arranged in parallel through intermolecular hydrogen bonds to form crystalline fibrils with a diameter of about 3.5 nm. The metafibrils are connected by hydrogen bonds to form microfibers with a diameter of 15-25 nm. Theoretically, both the molecular chains of cellulose and the microfibers have infinite lengths, but the microfibers are not completely cellulose crystals, but are composed alternately of crystalline regions and amorphous regions. [0003] Nanocellulose obtained from natural cellulose has some excel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D21C3/04D21D1/30D21C9/02
CPCD21C3/04D21C9/02D21D1/30
Inventor 付时雨彭洋洋陈莉
Owner SOUTH CHINA UNIV OF TECH
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