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Method for preparing nano-crystalline cellulose by ionic liquid-sulfuric acid system and regulating and controlling morphology of nano-crystalline cellulose

The technology of nanocellulose and ionic liquid is applied in the field of preparation of nanocellulose and its shape regulation, which can solve the problems of equipment corrosion, complicated reaction steps and high acid concentration, so as to improve the yield, improve the reaction accessibility, The effect of reducing acid concentration

Inactive Publication Date: 2021-09-24
SOUTHWEST UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reaction steps of acid hydrolysis to prepare CNC are relatively complicated and there are problems such as high acid concentration and corrosion of equipment, which increases production costs and is prone to environmental problems.
In addition, there are still problems such as low yield and difficult control of cellulose structure in the preparation of CNC by acid hydrolysis.

Method used

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  • Method for preparing nano-crystalline cellulose by ionic liquid-sulfuric acid system and regulating and controlling morphology of nano-crystalline cellulose
  • Method for preparing nano-crystalline cellulose by ionic liquid-sulfuric acid system and regulating and controlling morphology of nano-crystalline cellulose

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Mix microcrystalline cellulose and ionic liquid 1-butyl-3-methylimidazolium chloride (BMIMCl) at a ratio of 1:30 (w / w), then stir and heat in an oil bath at 90 °C for 2 h to make It swells and partially dissolves. Continue to add sulfuric acid solution (10%) at a ratio of 1:1 (w / w) to the ionic liquid for mixing, sonicate (300 W, 30 min), then continue heating and hydrolysis (90°C, 3 h), add 3 times the volume The reaction was terminated with distilled water, and then centrifuged and washed with distilled water for 3 times (5000 rpm, 5 min) to collect the samples, dialyzed in distilled water until the dialysate was neutral, and the nanocellulose suspension was obtained.

Embodiment 2

[0026] Mix microcrystalline cellulose and ionic liquid 1-butyl-3-methylimidazolium chloride (BMIMCl) at a ratio of 1:30 (w / w), then stir and heat in an oil bath at 90 °C for 2 h to make It swells and partially dissolves. Continue to add sulfuric acid solution (20%) at a ratio of 1:1 (w / w) to the ionic liquid for mixing, sonicate (300 W, 30 min), then continue heating and hydrolysis (90°C, 3 h), add 4 times the volume The reaction was terminated with distilled water, and then centrifuged and washed with distilled water for 3 times (5000 rpm, 5 min) to collect the samples, dialyzed in distilled water until the dialysate was neutral, and the nanocellulose suspension was obtained.

Embodiment 3

[0028] Mix microcrystalline cellulose and ionic liquid 1-butyl-3-methylimidazolium chloride (BMIMCl) at a ratio of 1:30 (w / w), then stir and heat in an oil bath at 90 °C for 2 h to make It swells and partially dissolves. Continue to add sulfuric acid solution (30%) at a ratio of 1:1 (w / w) to the ionic liquid for mixing, sonicate (300 W, 30 min), then continue heating and hydrolysis (90°C, 3 h), add 5 times the volume Distilled water was used to terminate the reaction, and then centrifuged and washed with distilled water for 4 times (6000 rpm, 10 min) to collect the samples, and dialyzed in distilled water until the dialysate was neutral to obtain nanocellulose suspension.

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PUM

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Abstract

The invention belongs to the technical field of preparation of nano-crystalline cellulose, and particularly relates to a method for preparing nano-crystalline cellulose by an ionic liquid-sulfuric acid system and regulating and controlling the shape of the nano-crystalline cellulose. The method specifically comprises the following steps: dissolving (or swelling) microcrystalline cellulose in an ionic liquid, then adding a sulfuric acid solution with a certain concentration, regenerating and hydrolyzing under the assistance of ultrasonic waves, and further performing centrifuging and dialyzing to obtain the nano cellulose. The method disclosed by the invention is simple, convenient and rapid to operate, the acid concentration required by acid hydrolysis can be reduced and the yield can be improved through swelling (dissolving) treatment of the ionic liquid, meanwhile, the morphology of the nanocellulose can be synergistically regulated and controlled, and the preparation approach and the application potential of the nanocellulose are widened.

Description

technical field [0001] The invention belongs to the field of nanocellulose, and in particular relates to a method for preparing nanocellulose and regulating its shape. Background technique [0002] Nanocellulose refers to ultrafine cellulose with a diameter of about 1 to 100 nm, which is mainly derived from wood, cotton and other agricultural processing wastes such as straw, straw, bagasse, etc. It has a unique nanostructure, a wide range of sources, and is degradable. , good stability, good biocompatibility, low thermal expansion coefficient, easy modification and large specific surface area and other characteristics, it has been widely used in materials, medicine, food and other fields, and has become a functional nanomaterial with great potential. Nanocellulose mainly includes cellulose nanocrystals (Cellulose Nanocrystals, CNC), cellulose nanofibrils (Cellulose Nanofibrils, CNF) and bacterial nanocellulose (Bacterial Cellulose, BC). Among them, CNC is mainly synthesized...

Claims

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Application Information

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IPC IPC(8): C08J3/09C08L1/04B82Y40/00
CPCC08J3/096B82Y40/00C08J2301/04
Inventor 戴宏杰张书敏张宇昊
Owner SOUTHWEST UNIVERSITY
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