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Method for preparing cellulose nano crystal by using acidic eutectic solvent through hydrolysis

A low eutectic solvent and nanocrystal technology, applied in the field of preparation of natural polymer materials, can solve the problems of complicated overall steps, low yield, low thermal stability of products, etc. The effect of speed increase

Active Publication Date: 2020-08-18
TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method solves the problems of low yield and low thermal stability of the product caused by the acid method to prepare cellulose nanocrystals, but the overall steps are cumbersome

Method used

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  • Method for preparing cellulose nano crystal by using acidic eutectic solvent through hydrolysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 40g of oxalic acid dihydrate and 45g of choline chloride into a 250mL three-necked flask at 25°C, and add 5g of distilled water to it, then heat it with an oil bath, raise the temperature to 55°C, and stir mechanically for 10min at a speed of 100 r / min to form a deep eutectic solvent, then add 5 g of sulfuric acid with a mass concentration of 98% to the there-necked flask, stir for 5 min, then add 1 g of bleached eucalyptus pulp, continue stirring for 1 h at 55 ° C, and use 300 g of 90 Dilute the reaction mixture with distilled water at ℃, then centrifuge at a speed of 10000r / min for 5min while it is hot, pour out the supernatant and keep the precipitate, then disperse the obtained precipitate with 100g of distilled water, and centrifuge at a speed of 10000r / min for 5min , repeating the process of centrifugal washing with distilled water three times, and freeze-drying the solid obtained after washing, the yield of cellulose nanocrystals was 76.3%. The temperature at...

Embodiment 2

[0020] Add 40g of oxalic acid dihydrate and 50g of choline chloride into a 250mL three-necked flask at 25°C, add 5g of distilled water into it, then heat it with an oil bath, raise the temperature to 45°C, stir mechanically for 10min, and the stirring speed is 300r / min to form a deep eutectic solvent, then add 10g of sulfuric acid with a mass concentration of 98% to the there-necked flask, stir for 5min, then add 10g of dissolving slurry, continue to stir at 45°C for 2h, and use 700g of 60°C distilled water to dissolve the reaction Dilute the mixture, then centrifuge at 10000r / min for 5min while it is hot, pour out the supernatant and keep the precipitate, then disperse the obtained precipitate with 800 g of distilled water, then centrifuge at 10000r / min for 5min, repeat this process The washing process was centrifuged with distilled water for 5 times, and the solid obtained after washing was freeze-dried, and the yield of the obtained nanocellulose crystal was 71.5%. The tem...

Embodiment 3

[0022] Add 40g of oxalic acid dihydrate and 40g of choline chloride into a 250mL three-necked flask at 30°C, add 10g of distilled water into it, then heat it with an oil bath, raise the temperature to 60°C, stir mechanically for 5min, and the stirring speed is 200 r / min to form a deep eutectic solvent, then add 10g of sulfuric acid with a mass concentration of 98% to the there-necked flask, stir for 5min, then add 3g of cotton pulp, continue to stir at 60°C for 1h, and use 300g of 65°C distilled water to Dilute the reaction mixture, then centrifuge at a speed of 8000r / min for 5min while it is hot, pour out the supernatant and keep the precipitate, then disperse the precipitate with 600g of distilled water, then centrifuge at a speed of 8000r / min for 5min, repeat this process The process of washing with distilled water was centrifuged for 5 times, and the solid obtained after washing was spray-dried, and the yield of the obtained nanocellulose crystal was 68%. The temperature a...

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Abstract

The invention relates to a method for preparing a cellulose nano crystal by using an acidic eutectic solvent through hydrolysis, and belongs to the field of natural polymer material preparation. The cellulose nano crystal is prepared through hydrolysis of 1 to 10 parts by mass of cellulose slurry, wherein the hydrolysis is catalyzed by an acidic eutectic system composed of 40 parts by mass of oxalic acid dihydrate, 40-50 parts by mass of choline chloride, 5-10 parts by mass of distilled water and 5-10 parts by mass of sulfuric acid, the reaction time is 1-5 hours, and the reaction temperatureis 45-55 DEG C. The reaction conditions are mild, and the operation is simple. The cellulose nano crystal is prepared in one step by utilizing an acidic eutectic solvent, and the steps of machining treatment and the like are omitted. The prepared cellulose nano crystal has good thermal stability and good dispersion stability in water.

Description

technical field [0001] The invention relates to the field of preparation of natural polymer materials, in particular to a method for preparing cellulose nanocrystals by hydrolyzing an acidic deep eutectic solvent. Background technique [0002] Cellulose is one of the most abundant natural polymers in nature. It has been used as a material for thousands of years. Today, due to its rich sources and excellent performance, it is still widely used in papermaking, construction, textiles and other fields. use. Cellulose nanocrystals (CNC), also known as nanocrystalline cellulose and cellulose nanowhiskers, are highly crystalline products obtained by selectively hydrolyzing or oxidatively degrading the amorphous regions of cellulose with acids, enzymes or oxidants while retaining the crystalline regions. Nanomaterials are usually less than 100nm in diameter and 50-2000nm in length, mainly in two shapes: rod-like and spherical. CNC has excellent characteristics such as high specifi...

Claims

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Application Information

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IPC IPC(8): C08B15/02
CPCC08B15/02
Inventor 解洪祥司传领张筱仪成德华孙琳伊晴陈佳宁邬清魏鹏鹏尹茂辉
Owner TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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