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A method for grafting and modifying cellulose using supercritical carbon dioxide as a solvent

A technology of grafting modification and carbon dioxide, applied in the field of polymer chemistry, to achieve high accessibility, favorable mass and heat transfer performance, and simplified post-treatment process

Inactive Publication Date: 2019-03-29
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, in the prior art, there is no method of using regenerated cellulose airgel as a matrix and using supercritical carbon dioxide as a green solvent and product purification solvent to carry out graft modification of cellulose

Method used

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  • A method for grafting and modifying cellulose using supercritical carbon dioxide as a solvent
  • A method for grafting and modifying cellulose using supercritical carbon dioxide as a solvent
  • A method for grafting and modifying cellulose using supercritical carbon dioxide as a solvent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] (1) Microcrystalline cellulose adopts the method for dissolving at low temperature to prepare a clear and transparent cellulose solution with a mass fraction of 4%;

[0055] (2) Add 2ml of the cellulose solution into a 12-hole bacterial culture plate, and let it stand for 36 hours at a gel temperature of 30° C. to prepare a cellulose gel;

[0056] (3) Repeatedly soaking the obtained cellulose gel with deionized water until the aqueous solution is neutral to obtain regenerated cellulose hydrogel;

[0057] (4) Repeatedly soak the regenerated cellulose hydrogel with 5% glycerol solution for 24 hours, plasticize the regenerated cellulose hydrogel, soak the plasticized hydrogel in liquid nitrogen ( -170°C) for 1-2 minutes, and then carry out vacuum freeze-drying for 12 hours to obtain regenerated cellulose airgel; during vacuum freeze-drying, the drying temperature is -20°C--55°C, and the vacuum degree during drying is 5-50Pa .

[0058] Comparative example one of embodimen...

Embodiment 2

[0070] (1) Place the regenerated cellulose airgel prepared in Example 1 in a vacuum oven at 40°C and dry for 48 hours;

[0071] (2) Add a certain proportion of regenerated cellulose airgel, lactide, and stannous octoate into the dried high-pressure reactor; after the sealing work is done, enter atmospheric carbon dioxide for gas replacement, and drain the reactor Inner air; the amount of regenerated cellulose airgel is 12.5% ​​of the mass of lactide, and the amount of stannous octoate is 1% of the mass of lactide;

[0072] (3) After the gas replacement is completed, at room temperature T 0 A certain amount of high-pressure carbon dioxide is passed into the reactor under the condition that the pressure is P 0 , P 0 is given by the preset reaction pressure P 1 and preset reaction temperature T 1 by formula Calculated; the carbon dioxide reaches a supercritical state by raising the temperature of the reactor, and then reacts; the reaction temperature T 1 =120°C, reaction p...

Embodiment 3

[0093] (1) Place the regenerated cellulose airgel prepared in Example 1 in a vacuum oven at 40°C and dry for 48 hours;

[0094] (2) Add a certain proportion of regenerated cellulose airgel, lactide, and stannous octoate into the dried high-pressure reactor; after the sealing work is done, enter atmospheric carbon dioxide for gas replacement, and drain the reactor Inner air; the amount of regenerated cellulose airgel is 25% of the mass of lactide, and the amount of stannous octoate is 1% of the mass of lactide;

[0095] (3) After the gas replacement is completed, at room temperature T 0 A certain amount of high-pressure carbon dioxide is passed into the reactor under the condition that the pressure is P 0 ;P 0 is given by the reaction pressure P 1 and reaction temperature T 1 by formula Calculated; by raising the temperature of the reactor to make it reach a supercritical state, and then react; the reaction temperature T 1 =120°C, reaction pressure P 1 =22MPa, the react...

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Abstract

The invention relates to a cellulose graft modification method by using supercritical carbon dioxide as a green solvent, belonging to the field of high polymer chemistry. The cellulose graft modification method comprises the following steps: preparing a regenerated cellulose aerogel from cellulose, putting the regenerated cellulose aerogel, a grafting monomer and a catalyst in a supercritical carbon dioxide environment, and carrying out grafting reaction to obtain a regenerated cellulose aerogel grafting product, wherein the reaction temperature of the grafting reaction is 50-120 DEG C, the reaction pressure is 8-30 MPa, the stirring rate is 50-400 rpm, the reaction time is 1-48 hours, the regenerated cellulose aerogel accounts for 1-40 wt% of the grafting monomer, and the catalyst accounts for 0.14-3 wt% of the grafting monomer. The swelling and plastification actions of the supercritical carbon dioxide on the cellulose aerogel increase the accessibility of the regenerated cellulose aerogel, and enhance the dispersion and permeation of the monomers and the like in the regenerated cellulose aerogel.

Description

technical field [0001] The invention relates to a method for grafting and modifying cellulose by using supercritical carbon dioxide as a green solvent, and belongs to the field of polymer chemistry. Background technique [0002] With the rapid development of industrial production technology, environmental problems have become more and more serious. It has become a trend of technological development to use natural renewable resources instead of non-renewable fossil energy to prepare environmentally friendly green degradable products. Cellulose is a kind of natural polymer that has been studied more at present, but due to the strong hydrogen bond, the accessibility of cellulose is low, and it is difficult for small molecule reagents to penetrate into it, so it is difficult to dissolve and not melt, which also limits Application of cellulose in industrial production. By grafting and modifying cellulose, the physical and chemical properties of cellulose can be greatly improved,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J9/40C08J9/28C08L1/04
CPCC08J9/28C08J9/405C08J2201/0484C08J2205/026C08J2301/04Y02P20/54Y02P20/584
Inventor 杨鸣波王捍卿刘正英杨伟喻鹏
Owner SICHUAN UNIV
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