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A kind of method for improving 1-allyl-3-methylimidazolium chloride dissolving cellulose performance

A methylimidazolium chloride salt and cellulose-dissolving technology, which is applied in the field of improving the cellulose-dissolving performance of 1-allyl-3-methylimidazolium chloride salt, can solve the problems of high-efficiency conversion and deep processing, long dissolution time, and solubility Low-level problems, to achieve the effect of increasing the concentration and ability of dissolution, reducing the dissolution time, and reducing the dissolution temperature

Active Publication Date: 2018-01-12
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The conversion of fiber resources into chemicals, materials and biofuels has received extensive attention, but plant fibers are difficult to dissolve in most solvents due to the high degree of polymerization, high hydrophobicity, highly ordered structure and extensive hydrogen bond network structure , which seriously hinders its efficient transformation and deep processing
To improve cellulose conversion efficiency, some cellulose solvent systems have been developed, including N,N-dimethylacetamide / lithium chloride (DMAc / LiCl), N,N-dimethylformamide / nitrogen tetroxide ( DMF / N2O4), N-methyl-N-oxymorpholine (NMMO), dimethylsulfoxide / tetrabutylammonium fluoride (DMSO / TBAF) and molten salt hydrates (such as LiClO4·3H2O, LiSCN· 2H2O), but these solvent systems more or less have the following disadvantages: strong toxicity, high cost, difficult solvent recycling and instability during use, etc.
At present, the research on 1-allyl-3-methylimidazolium chloride salt focuses on the dissolution and modification of cellulose, but the solubility of 1-allyl-3-methylimidazolium chloride salt to cellulose is not very good. Well, the dissolution temperature is high, the solubility is low, and the dissolution time is long; in addition, during the dissolution process, the thermal degradation of 1-allyl-3-methylimidazolium chloride salt is serious

Method used

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  • A kind of method for improving 1-allyl-3-methylimidazolium chloride dissolving cellulose performance

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0025] A method for improving the cellulose-dissolving performance of 1-allyl-3-methylimidazolium chloride salt, vacuum-drying microcrystalline cellulose with an average degree of polymerization of 265 at 50°C until the water content is less than 0.8%, adding to 1 -Allyl-3-methylimidazolium chloride salt, and then add solid acid-sulfonic acid ion exchange resin; stir at a temperature of 80°C and a mechanical stirring speed of 500rpm for 30min to completely dissolve. Wherein, the concentration of microcrystalline cellulose is 3wt%, the concentration of solid acid is 2.0wt%, the particle size of solid acid is 300 microns, and the resin exchange capacity is 4.2 eq / kg.

[0026] In the prior art, 1-allyl-3-methylimidazolium chloride salt dissolves microcrystalline cellulose (the average degree of polymerization is 265), the concentration of microcrystalline cellulose is 3 wt%, the temperature is 80°C, and the stirring speed is 500 rpm , the time required for microcrystalline cellul...

Embodiment 2

[0029] A method for improving the cellulose-dissolving performance of 1-allyl-3-methylimidazolium chloride salt, vacuum-drying cotton fibers with an average degree of polymerization of 2180 at 40°C until the water content is less than 0.8%, adding to 1-ene Propyl-3-methylimidazolium chloride, and then add solid acid-sulfonic acid ion exchange resin; dissolve at a temperature of 115°C and a mechanical stirring speed of 200rpm for 120min. Wherein, the quality of cotton fiber is 18wt% of 1-allyl-3-methylimidazolium chloride salt quality, the concentration of solid acid is 4.0wt%, the particle diameter of solid acid is 200 microns, and resin exchange capacity is 4.3 eq / kg.

[0030] In this example, the solubility of cotton fiber is 60.2%.

[0031] However, in the prior art, 1-allyl-3-methylimidazolium chloride salt dissolves cotton fibers (the average degree of polymerization is 2180), and the quality of cotton fiber is 100% of that of 1-allyl-3-methylimidazolium chloride salt. ...

Embodiment 3

[0034] A method for improving the performance of 1-allyl-3-methylimidazolium chloride salt dissolving cellulose, vacuum-drying eucalyptus wood dissolving pulp fibers with an average degree of polymerization of 520 at 30°C until the water content is less than 1%, adding to 1-allyl-3-methylimidazolium chloride salt, and then add solid acid-sulfonic acid ion exchange resin; at a temperature of 110°C, stir at a mechanical stirring speed of 800rpm for 90min to completely dissolve. Among them, the concentration of eucalyptus wood dissolving pulp fiber is 10wt%, the concentration of solid acid is 1.0wt%, the particle size of solid acid is 300 microns, and the resin exchange capacity is 4.5 eq / kg. The dissolved 1-allyl-3-methylimidazolium chloride salt is recovered by the solvent system and continues to be reused in the dissolution system. After 5 cycles of use, the recovery rate of 1-allyl-3-methylimidazolium chloride salt is was 97%, and the loss rate was 3.0%.

[0035] In the prio...

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Abstract

The invention discloses a method for improving the capability of 1-allyl-3-methylimidazole chloride to dissolve cellulose and belongs to the field of cellulose dissolution methods. The method includes: drying cellulose to less than 1% in water content, adding 1-allyl-3-methylimidazole chloride, adding a solid acid, and stirring and dissolving at 60-120 DEG C. Anions in the solid acid and cations of the 1-allyl-3-methylimidazole chloride act on hydroxyls of cellulose molecules, hydrogen bonds in and between the cellulose molecules are destroyed to great extent, and the capability of an ionic liquid to dissolve the cellulose is improved. Ineffective degradation of the ionic liquid of the 1-allyl-3-methylimidazole chloride during cellulose dissolution is effectively restrained, the structure of the ionic liquid is stabilized, steam pressure is zero, repeatability is available, and greenness is achieved; the solid acid is free of pollution, easy to recycle and reusable, reducing cost.

Description

technical field [0001] The invention relates to the field of cellulose dissolving methods, in particular to a method for improving the performance of 1-allyl-3-methylimidazolium chloride salt in dissolving cellulose. Background technique [0002] Cellulose is the most abundant natural polymer resource on the earth. It has the advantages of renewability, biodegradability and homogeneity. It has become an important raw material for traditional industries such as pulp and paper, textile, polymer materials and medicine. With the depletion of traditional non-renewable resources such as oil and coal on the earth, the sustainable development of energy and materials is imminent. Therefore, how to efficiently develop and utilize renewable resources such as cellulose has become an important problem in the sustainable development strategy of the world today. [0003] The conversion of fiber resources into chemicals, materials and biofuels has received extensive attention, but plant fi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/09
CPCC08J3/096C08J2301/02C08J2301/04
Inventor 庞志强董翠华孟亚会
Owner GUANGXI UNIV
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