Method of preparing clubbed nano-cellulose

A nanocellulose, rod-shaped technology, applied in fiber raw material processing, textiles and papermaking, etc., can solve the problems of low aspect ratio and limit the application of composite materials, and achieve high aspect ratio, high frequency and power stability, and reactivity. improved effect

Inactive Publication Date: 2009-08-19
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, the products obtained by the domestically disclosed nanocellulose preparation methods are all granular and have low aspect ratio, which limits its application in the field of composite materials.

Method used

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  • Method of preparing clubbed nano-cellulose
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  • Method of preparing clubbed nano-cellulose

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Disperse 10 grams of cotton fiber in 200 grams of sulfuric acid aqueous solution with a concentration of 60% by mass, and carry out single-mode microwave radiation hydrolysis at a temperature of 45°C. The single-mode microwave radiation power is 100w, and the radiation time is 5 minutes to obtain a hydrolyzed solution Add distilled water to the obtained hydrolyzate to dilute the hydrolyzate to 10 times the volume, then centrifuge the diluted hydrolyzate at 10,000rpm for 3 times; get the precipitate and dialyze for 3 days, and the molecular weight cut-off of the dialysis membrane used After dialysis, it is filtered through a filter membrane with a pore size of 0.45 microns, and the filtrate is dispersed by 200w ultrasonic waves for 35 minutes to obtain a stable rod-shaped nanocellulose suspension, wherein the nanocellulose has a diameter of 5-10 nanometers and a length of 100-300 Nano.

Embodiment 2

[0024] Disperse 10 grams of wood pulp fibers in 150 grams of sulfuric acid aqueous solution with a mass concentration of 50%, and carry out single-mode microwave radiation hydrolysis at a temperature of 50°C. The single-mode microwave radiation power is 10w, and the radiation time is 60 minutes. The obtained hydrolysis Distilled water was added to the solution to dilute the hydrolyzate to 10 times the volume, and then the diluted hydrolyzate was centrifuged at 12000rpm for 5 times, and the precipitate was dialyzed for 3 days. The molecular weight cut-off of the dialysis membrane used was 12000; after dialysis Filtrate with a filter membrane with a pore size of 0.45 microns, and the filtrate is dispersed by 200w ultrasonic waves for 30 minutes to obtain a stable rod-shaped nanocellulose suspension, wherein the nanocellulose has a diameter of 5-20 nanometers and a length of 100-300 nanometers.

Embodiment 3

[0026] Disperse 10 grams of microcrystalline cellulose in 100 grams of sulfuric acid aqueous solution with a mass concentration of 65%, and carry out single-mode microwave radiation hydrolysis at a temperature of 40 ° C. The single-mode microwave radiation power is 20w, and the radiation time is 20 minutes; the obtained Distilled water was added to the hydrolyzate to dilute the hydrolyzate to 10 times the volume. The diluted hydrolyzate was centrifuged 4 times at 11,000 rpm, and the precipitate was dialyzed for 3 days. The molecular weight cut-off of the dialysis membrane used was 14,000; Filtrate through a 0.45 micron filter membrane, and the filtrate is dispersed by 200w ultrasonic waves for 25 minutes to obtain a stable rod-shaped nanocellulose suspension, wherein the nanocellulose has a diameter of 10-20 nanometers and a length of 100-300 nanometers.

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Abstract

The invention discloses a method for preparing nano-rod cellulose, which comprises the following steps: dispersing fiber raw material into sulphuric acid water solution of which mass concentration is 50 to 65 percent, hydrolyzing the fiber raw material by single-mode microwave radiation for 5 to 60 minutes at a temperature of between 20 and 50 DEG C and at the microwave radiation power of 10 to 100 watts, then adding distilled water into hydrolysis solution and diluting the hydrolysis solution to have 10 times of volume, and obtaining stable nano-rod cellulose suspension through post treatment processes such as centrifugal separation, dialysis, filter, ultrasonic dispersion and the like of the diluent, so as to obtain the nano-rod cellulose of which width is about 10 nanometers and length is about 200 to 300 nanometers.

Description

1. Technical field [0001] The invention belongs to the field of preparation of nanometer materials, in particular to a preparation method of rod-shaped nanocellulose. 2. Background technology [0002] Due to the needs of sustainable development and environmental protection, in the past few decades, biodegradable materials based on natural renewable resources have attracted more and more attention from researchers and manufacturers at home and abroad, and nanocellulose has also been Applied to the research of polymer composite materials. Compared with other nanofillers, the advantages of nanocellulose are cheap, easy to obtain, renewable, biocompatible, simple to prepare, chemically or physically modified, etc., and rod-shaped nanocellulose has high mechanical strength. Its crystal structure is highly ordered, which can significantly change the electrical, optical, magnetic, insulating and even superconducting properties of materials. [0003] The chemical structure of cell...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D21C5/00
Inventor 王丹商士斌宋湛谦刘鹤
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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