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Method for preparing nano crystal cellulose by dissociating ZnCl2

A technology of nano-crystal and cellulose, which is applied in the field of preparation of nano-crystal cellulose, which can solve the problems of difficult control of cellulose degradation, generation of a large amount of acid waste liquid, and large corrosion of equipment, so as to achieve good mechanical strength and low corrosion of equipment , the effect of little degradation damage

Active Publication Date: 2012-11-07
FUJIAN AGRI & FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the preparation of nanocrystalline cellulose reported in the literature mainly adopts strong acid hydrolysis such as sulfuric acid, which is not easy to control the degradation degree of cellulose, and is more corrosive to equipment, and the post-treatment will produce a large amount of acid waste liquid, which will cause great environmental pollution.

Method used

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  • Method for preparing nano crystal cellulose by dissociating ZnCl2
  • Method for preparing nano crystal cellulose by dissociating ZnCl2

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Effect test

Embodiment 1

[0027] Take by weighing 3g microcrystalline cellulose, add to 30g mass fraction 65%ZnCl ２ In the solvent, 80 ° C oil bath for 1 hour, and at the same time high-speed dispersion homogeneous, the homogeneous speed is 12000 rpm, to obtain transparent cellulose / ZnCl 2 solution. Add 90ml of 0.5% hydrochloric acid to the cellulose / ZnCl 2 In the solution, the cellulose is precipitated, centrifuged and separated, and the upper layer of ZnCl is removed. ２ , acid solution, remove the cellulose jelly in the lower layer and perform centrifugation and elution with water for 5 times, remove the dissociated cellulose jelly in the crystallization area of ​​the lower layer and ultrasonicate at 50°C (ultrasonic frequency is 40KHz) for 2 hours, that is Nanocrystalline cellulose is obtained. It can be seen from the observation of the transmission electron microscope that the nanocrystalline microelements prepared by this method have a network structure, with a diameter of about 20-30nm and a...

Embodiment 2

[0029] Weigh 1g chemical pulp, add to 30g mass fraction 65%ZnCl ２ In the solvent, 80 ° C oil bath for 3 hours, at the same time, high-speed dispersion and homogeneity, the homogenization speed is 12000 rpm, to obtain transparent cellulose / ZnCl 2 solution. Add 105ml of 0.5% hydrochloric acid to the cellulose / ZnCl 2 In the solution, the cellulose is precipitated, centrifuged and separated, and the upper layer of ZnCl is removed. ２ , acid solution, remove the cellulose jelly in the lower layer and perform 8 times of centrifugation and elution with water, remove the dissociated cellulose in the crystallization area of ​​the lower layer and ultrasonicate at 80°C (ultrasonic frequency is 60KHz) for 4 hours to obtain nanocrystals cellulose.

Embodiment 3

[0031] Weigh 1g absorbent cotton, add to 30g mass fraction 65%ZnCl ２ In the solvent, 100 ° C oil bath for 4 hours, at the same time, high-speed dispersion and homogeneity, the homogenization speed is 8000 rpm, to obtain transparent cellulose / ZnCl 2 solution. Add 105ml of 0.5% hydrochloric acid to the cellulose / ZnCl 2 In the solution, the cellulose is precipitated, centrifuged and separated, and the upper layer of ZnCl is removed. ２ , acid solution, remove the lower layer of cellulose jelly, and then centrifuge and elute with water for 6 times, remove the dissociated cellulose in the crystallization area of ​​the lower layer and ultrasonicate at 80°C (ultrasonic frequency is 60KHz) for 4 hours to obtain nanocrystals cellulose.

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Abstract

The invention discloses a method for preparing nano crystal cellulose by dissociating ZnCl2. The method comprises the following steps of: (1) adding a cellulose raw material to a ZnCl2 solution to form a suspension; (2) homogenizing and dispersing the suspension at a high speed under a heating condition to obtain a transparent cellulose / ZnCl2 solution; (3) adding diluted acid to the cellulose / ZnCl2 solution, and controlling the pH value of the solution to be smaller than 5 to ensure that the cellulose is separated out, centrifuging and layering; removing the upper-layer solution; and taking the lower-layer cellulose jelly and carrying out ultrasonic dispersion treatment or wet grinding to prepare the nano crystal cellulose. In the invention, the adopted ZnCl2 has the advantages of green color, stability, low price, easiness of recovery, recycling capability, and the like; moreover, the method has the advantages of moderate reaction condition, small degradation injury to the cellulose,small equipment corrosivity, simpleness of operation and high yield; and the obtained nano crystal cellulose has a reticulate structure and good mechanical strength and is beneficial to being appliedto composite materials.

Description

technical field [0001] The invention relates to a preparation method of nanocrystalline cellulose, in particular to a method using ZnCl ２ A method of preparing nanocrystalline cellulose after dissociating the crystalline regions of the cellulose. Background technique [0002] Cellulose is the most abundant, renewable and biodegradable natural polymer in the world, and nature can provide about 100 billion tons of cellulose every year. The use of its performance improvement and high added value has become a research hotspot at home and abroad. Cellulose can be degraded by acid hydrolysis, enzyme treatment and mechanical method to produce nanocrystalline cellulose. Nanocrystalline cellulose has many excellent properties, such as high purity, high degree of polymerization, high crystallinity, high hydrophilicity, high Young's modulus, high strength, ultrafine structure and high transparency, etc. In view of the Excellent performance, it has good potential applications in fine...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B15/08
Inventor 黄彪欧文陈学榕唐丽荣林雯怡陈燕丹戴达松李素琼
Owner FUJIAN AGRI & FORESTRY UNIV
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