Cellulose solvent, and preparation method and application thereof

A cellulose solvent and cellulose technology, applied in the production of bulk chemicals, etc., can solve problems such as hindering large-scale industrial production, high requirements for cellulose raw materials, and difficulty in realizing industrial application, etc. Dissolution effect, effect of shortening dissolving time

Active Publication Date: 2019-09-20
BEIJING FORESTRY UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the existing cellulose dissolving system has the following disadvantages: solvent systems such as sodium hydroxide / thiourea use alkaline solutions, which are difficult to meet environmental protection requirements, and require low temperature (-12°C) operation, high energy consumption, and are not conducive to industrialization. ;Although the alkyl ammonium hydroxide aqueous solution system can dissolve a large amount of cellulose, the dissolution conditions are harsh, and the requirements for cellulose raw materials are high, so it is difficult to realize industrial application; High, water-sensitive, and ionic liquids with excellent solubility are expensive, while ionic liquids with relatively low prices take a long time to dissolve, and cellulose will be severely degraded, which hinders large-scale industrial production

Method used

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  • Cellulose solvent, and preparation method and application thereof
  • Cellulose solvent, and preparation method and application thereof
  • Cellulose solvent, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Take 15.224g of organic base DBU and 45mL of n-hexane in a three-necked flask, pass nitrogen, and slowly add 7.206g of acrylic acid to the reaction system at a rate of 30 drops / min under magnetic stirring at 200rpm. During the addition, the temperature of the reaction system Control at 25°C, after the acrylic acid is completely added, continue to stir at 200rpm at room temperature for 8h, the non-imidazole ionic liquid is precipitated from n-hexane, after separation, the obtained high-purity non-imidazole ionic liquid is under the protection of argon, at 80°C After heating for 2h, the dry cellulose solvent [DBUH][CH 2 =CHCOO] (its structural formula sees figure 1 ). Weigh microcrystalline cellulose and add it to the above cellulose solvent, and continue to stir at 80° C. and 200 rpm until it cannot be dissolved, and a homogeneous solution in which microcrystalline cellulose is dissolved is obtained. After analysis, it can be obtained that the maximum solubility of Avi...

Embodiment 2

[0049] Take 13.702g of organic base DBU and 50mL of n-hexane in a three-necked flask, pass nitrogen gas, and slowly add 9.008g of methoxyacetic acid dropwise to the reaction system at a rate of 40 drops / min under magnetic stirring at 400rpm. The temperature of the system was controlled at 30°C. After the methoxyacetic acid was completely added, the stirring was continued at 400 rpm for 10 h at room temperature. The non-imidazole ionic liquid was precipitated from n-hexane. After separation, the obtained high-purity non-imidazole ionic liquid was Under protection, heating at 80°C for 2h, the dry cellulose solvent [DBUH][CH 3 OCH 2 COO] (its structural formula sees figure 1 ). Weigh microcrystalline cellulose and add it to the above cellulose solvent, and continue to stir at 80° C. and 200 rpm until it cannot be dissolved, and a homogeneous solution in which microcrystalline cellulose is dissolved is obtained. After analysis, the maximum solubility of microcrystalline cellulo...

Embodiment 3

[0051] Take 15.224g of organic base DBU and 50mL of ether in a three-necked flask, pass nitrogen gas, and slowly add 9.212g of thioglycolic acid dropwise to the reaction system at a rate of 40 drops / min under magnetic stirring at 300rpm. During the dropwise addition, the reaction system The temperature was controlled at 28°C. After the thioglycolic acid was completely added, the stirring was continued at 300 rpm at room temperature for 11 hours. The non-imidazole ionic liquid was precipitated from ether. After separation, the obtained high-purity non-imidazole ionic liquid was protected by nitrogen. Heating at 80°C for 2h, the dry cellulose solvent [DBUH][HSCH 2 COO] (its structural formula sees figure 1 ). Weigh microcrystalline cellulose and add it to the above cellulose solvent, and continue to stir at 80° C. and 200 rpm until it cannot be dissolved, and a homogeneous solution in which microcrystalline cellulose is dissolved is obtained. After analysis, the maximum solubi...

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Abstract

The invention relates to a cellulose solvent, and a preparation method and application thereof. The preparation method for the cellulose solvent comprises the following steps of: mixing an organic base having a heterobicycle in its chemical structure with an organic solvent, placing the formed mixture in a three-necked flask, introducing nitrogen, dropwise adding an acidic reagent to a reaction system under magnetic stirring, and allowing a temperature to be kept at 30 DEG C or below in the whole reaction process so as to obtain a transparent mixture; continuing stirring the mixture at room temperature to realize full reaction of the mixture, allowing non-imidazole ionic liquid to be precipitated from an organic phase, and carrying out separation to obtain the non-imidazole ionic liquid; and heating the non-imidazole ionic liquid under the protection of an inert gas so as to obtain the dried cellulose solvent. According to the invention, the dissolution effect of cellulose in the relatively-inexpensive non-imidazole ionic liquid is improved through the preparation and utilization of the non-imidazole ionic liquid cellulose solvent; and in particular, the maximum solubility of cellulose is increased, the dissolution time of cellulose is shortened, and the degradation rate of cellulose is remarkablely reduced.

Description

technical field [0001] The invention belongs to the technical field of cellulose solvents, in particular to a cellulose solvent and its preparation method and application. Background technique [0002] Cellulose, the most abundant biorenewable and biodegradable resource in nature, is one of the main components of plant cell walls and accounts for more than 50% of the plant kingdom's carbon content. Biomass-based materials such as films, silks, gels, and microspheres developed by using cellulose and its ester or ether derivatives are widely used in textiles, plastics, medicine, electrical engineering, architectural design, scientific research equipment, daily chemicals, and food additives. and other fields have broad application prospects. The preparation and application of cellulose-based products are closely related to their solubility properties. [0003] Cellulose is a linear polymer polysaccharide composed of D-glucopyranose groups connected by β-1,4 glycosidic bonds, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/09C08J5/18C08L1/04C08L1/02
CPCC08J3/096C08J5/18C08J2301/02C08J2301/04Y02P20/54
Inventor 许凤李鑫游婷婷张逊张学铭吴玉英
Owner BEIJING FORESTRY UNIVERSITY
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