A kind of 1-butyl-3-methylimidazolium chloride salt-licl-dmf system prepares the method for microfiber corn stalk

A technology of methylimidazolium chloride and corn stalk, which is applied in chemical instruments and methods, pharmaceutical formulations, chemical characteristics of fibers, etc., can solve the problems of difficult to effectively separate plant fiber cells, poor reaction performance, and high modification costs, and achieves the realization of Value-added utilization, reduced degradation, and high sulfonation efficiency

Active Publication Date: 2019-07-05
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional plant fiber modification has poor reactivity due to its dense structure, and it is difficult to effectively separate plant fiber cells. The corresponding modification method needs to undergo multi-step chemical, biological or mechanical treatment, which leads to high cost of modification, heavy pollution, and poor product performance.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] A method for preparing microfibrillated fibers with a high degree of sulfonation by using corn stalks as raw materials, comprising the following steps:

[0044] (1) Crush corn stalks into grass powder with a mesh size of 20 or less, and vacuum-dry at a vacuum degree of -0.08 MPa, a temperature of 30° C., and a time of 8.0 hours until the moisture content is less than 2.0 wt%.

[0045] (2) prepare 1-butyl-3-methylimidazolium chloride salt-LiCl-DMF composite solvent system, solvent composition is: the content of 1-butyl-3-methylimidazolium chloride salt is 8.0wt%, LiCl content is 2.0wt%, DMF content is 90.0wt%.

[0046] (3) Perform high-shear sulfonation treatment in the solvent system, add 1.5g / g corn stalk sulfur trioxide pyridine complex (CAS number: 26412-87-3), add 40g corn stalks (concentration 4.0wt%) ), high-shear sulfonation treatment was carried out for 40 minutes at a temperature of 20° C. and a dispersion speed of 16,000 rpm.

[0047] (4) After the sulfonati...

Embodiment 2

[0052] A method for preparing microfibrillated fibers with a high degree of sulfonation by using corn stalks as raw materials, comprising the following steps:

[0053] (1) Crush corn stalks into grass powder below 20 meshes, and vacuum-dry at a vacuum degree of -0.07MPa, a temperature of 50°C, and a time of 7.0 hours until the moisture content is less than 2.0wt%.

[0054] (2) prepare 1-butyl-3-methylimidazolium chloride salt-LiCl-DMF composite solvent system, solvent composition is: the content of 1-butyl-3-methylimidazolium chloride salt is 4.0wt%, LiCl content is 1.0wt%, DMF content is 95.0wt%.

[0055] (3) Perform high-shear sulfonation treatment in the solvent system, add 2.5g / g corn stalk sulfur trioxide pyridine complex (CAS number: 26412-87-3), add 200g corn stalks (concentration 3.0wt%) ), high-shear sulfonation treatment was carried out for 180 min at a temperature of 50° C. and a dispersion speed of 14,000 rpm.

[0056] (4) After the sulfonation treatment, the cor...

Embodiment 3

[0062] A method for preparing microfibrillated fibers with a high degree of sulfonation by using corn stalks as raw materials, comprising the following steps:

[0063] (1) Crush corn stalks into grass powder below 20 meshes, and vacuum-dry at a vacuum degree of -0.09 MPa, a temperature of 30° C., and a time of 6.0 hours until the moisture content is less than 2.0 wt%.

[0064] (2) prepare 1-butyl-3-methylimidazolium chloride salt-LiCl-DMF composite solvent system, solvent composition is: the content of 1-butyl-3-methylimidazolium chloride salt is 10.0wt%, LiCl content is 1.5wt%, DMF content is 88.5wt%.

[0065] (3) Perform high-shear sulfonation treatment in the solvent system, add 0.8g / g corn stalk sulfur trioxide pyridine complex (CAS number: 26412-87-3), add 50g corn stalks (concentration 7.0wt%) ), high-shear sulfonation treatment was carried out at a temperature of 70°C and a dispersion speed of 12000rpm for 90min.

[0066] (4) After the sulfonation treatment, the corn ...

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Abstract

The invention discloses a method for preparing micro-fibre corn stalks by a 1-butyl-3-methimidazole chloride-LiCl-DMF (dimethylformamide) system. The method comprises the following steps: crushing and drying corn stalks; performing high-shear sulphonating treatment at a certain temperature by taking a 1-butyl-3-methimidazole chloride-LiCl-DMF compound system as a solvent and adding a pyridine sulphur trioxide compound; filtering, washing and performing vacuum drying on a material which is subjected to the sulphonating treatment to obtain the micro-fibre corn stalks with high sulphonation degree. According to the method, the corn stalk fibres can be effectively swelled and free hydroxyls can be released by combining 1-butyl-3-methimidazole chloride and LiCl, so that the cohesive force of a raw material is weakened, and the sulphonating modifying efficiency of sulphur trioxide-pyridine complex is improved. By the method, the degradation of hemicellulose and lignin components of the corn stalks can be reduced remarkably; a modifying process is simple and feasible; the modified products of micro-fibres are high in yield and sulphonation degree and large in specific surface area; value-added utilization of agricultural waste is realized; moreover, a modifying liquid is easy to recycle and utilize.

Description

technical field [0001] The invention belongs to the field of plant fiber processing and modification methods, in particular to a high-shear method using corn stalks as raw materials in a 1-butyl-3-methylimidazolium chloride salt-LiCl-DMF (dimethylformamide) solvent system Process for preparing microfibrillated fibers with a high degree of sulfonation. Background technique [0002] Plant fiber is one of the most abundant renewable resources on the earth, containing huge biomass energy. The main components of biomass resources are cellulose, hemicellulose and lignin. Cellulose is the main component of plant cell walls; hemicellulose acts as a molecular adhesive between cellulose and lignin; lignin has a network structure to connect cells, and acts as a supporting framework to surround and reinforce cellulose and hemicellulose. At present, the global energy shortage, atmospheric greenhouse effect and tight oil supply have promoted the research of biomass refining. [0003] P...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08H8/00D01F9/00B01J20/24B01J20/30C02F1/28A61K36/899A61P31/12C02F101/20
CPCA61K36/899B01J20/24C02F1/286C02F2101/20C08H8/00D01F9/00
Inventor 庞志强陈嘉川杨桂花
Owner QILU UNIV OF TECH
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