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A method for improving 1-butyl-3-methylimidazolium chloride salt 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-butyl-3-methylimidazolium chloride salt, can solve the problem that the cellulose dissolving performance is not very good, which hinders efficient conversion and deep Processing, solvents are difficult to recycle, etc., to achieve the effect of improving solubility, increasing solubility concentration and ability, and reducing dissolution time

Inactive Publication Date: 2018-01-12
QILU UNIV OF TECH
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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-butyl-3-methylimidazolium chloride concentrates on the dissolution and modification of cellulose, but the solubility of 1-butyl-3-methylimidazolium chloride to cellulose is not very good. 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-butyl-3-methylimidazolium chloride is serious

Method used

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  • A method for improving 1-butyl-3-methylimidazolium chloride salt dissolving cellulose performance

Examples

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Effect test

Embodiment 1

[0027] A method for improving the cellulose dissolving performance of 1-butyl-3-methylimidazole chloride salt. The microcrystalline cellulose with an average degree of polymerization of 230 is vacuum dried at 50°C until the water content is less than 0.5%. 99.0% of 1-butyl-3-methylimidazole chloride salt, and then add solid acid-sulfonic acid ion exchange resin; at a temperature of 80 ℃, mechanical stirring speed 500rpm stirring for 25min to completely dissolve. Among them, the concentration of microcrystalline cellulose is 3 wt%, the concentration of solid acid is 2.0 wt%, the particle size of solid acid is 300 microns, and the resin exchange capacity is 4.2 eq / kg.

[0028] In the prior art, 1-butyl-3-methylimidazole chloride salt dissolves microcrystalline cellulose (average degree of polymerization is 230), the microcrystalline cellulose concentration is 3 wt%, the temperature is 80°C, and the stirring speed is 500 rpm. The time required for the complete dissolution of microcr...

Embodiment 2

[0031] A method for improving the cellulose dissolving performance of 1-butyl-3-methylimidazole chloride salt, vacuum drying cotton fiber with an average degree of polymerization of 2180 at 40°C, until the moisture content is less than 0.8%, and adding to the purity of 98.0% The solid acid-sulfonic acid ion exchange resin is added to the 1-butyl-3-methylimidazole chloride salt; the temperature is 120°C and the mechanical stirring speed is 200rpm for 120min to dissolve. Among them, the mass of cotton fiber is 20wt% of the mass of 1-butyl-3-methylimidazole chloride, the concentration of solid acid is 4.0wt%, the particle size of solid acid is 200 microns, and the resin exchange capacity is 4.3 eq / kg .

[0032] In this example, the solubility of cotton fiber is 56.1%.

[0033] In the prior art, 1-butyl-3-methylimidazole chloride salt dissolves cotton fiber (average degree of polymerization is 2180), and the mass of cotton fiber is 20wt% of the mass of 1-butyl-3-methylimidazole chlori...

Embodiment 3

[0036] A method for improving the cellulose dissolving performance of 1-butyl-3-methylimidazole chloride salt. The eucalyptus wood dissolving pulp fiber with an average degree of polymerization of 560 is vacuum dried at 30°C to a water content of less than 1%, and then added to 1 -Butyl-3-methylimidazole chloride salt, and then add solid acid-sulfonic acid ion exchange resin; at a temperature of 110°C, a mechanical stirring speed of 800rpm, stirring for 90min, completely dissolved. Among them, the concentration of eucalyptus dissolving pulp fiber is 10 wt%, the concentration of solid acid is 1.0 wt%, the particle size of solid acid is 300 microns, and the resin exchange capacity is 4.5 eq / kg. The dissolved 1-butyl-3-methylimidazole chloride salt is recovered by the solvent system and is reused in the dissolution system. After 5 cycles of use, the recovery rate of 1-butyl-3-methylimidazole chloride salt is 96.8 %, the loss rate is 3.2%.

[0037] In the prior art, 1-butyl-3-methyl...

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Abstract

The invention discloses a method for improving the cellulose dissolution performance of 1-butyl-3-methylimidazole chlorine salt and belongs to the field of cellulose dissolution methods.After cellulose is dried till the water content is smaller than 1%, cellulose is added to 1-butyl-3-methylimidazole chlorine salt, then solid acid is added, and the mixture is stirred at the temperature of 60-120 DEG C to be dissolved.Positive ions of solid acid and negative ions of 1-butyl-3-methylimidazole chlorine salt act on hydroxyl of cellulose molecules, hydrogen bonds in the cellulose molecules and between the molecules are damaged massively, and therefore the capacity of ionic liquid to cellulose dissolution is improved.Ineffective degradation of the 1-butyl-3-methylimidazole chlorine salt ionic liquid in the cellulose dissolution process is effectively restrained, and the ionic liquid is simple in structure, zero in vapor pressure, capable of being recycled repeatedly and environmentally friendly; solid acid is free of pollution, recovery is easy, recycling can be conducted, and the cost is reduced.

Description

Technical field [0001] The invention relates to the field of cellulose dissolution methods, in particular to a method for improving the cellulose dissolution performance of 1-butyl-3-methylimidazole chloride. 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 pulping and papermaking, textiles, polymer materials and medicine. With the increasing 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] Fiber resources conversion chemicals, materials and biofuels have received extensive attention, but due to high d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/09C08L1/04C08L1/02
CPCC08J3/096C08J2301/02C08J2301/04
Inventor 庞志强董翠华孟亚会
Owner QILU UNIV OF TECH
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