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Method for preparing micro-fibre corn stalks by 1-butyl-3-methimidazole chloride-LiBr-DMF (dimethylformamide) system

A technology of methylimidazole chloride salt and corn stalks, which is applied in chemical instruments and methods, pharmaceutical formulas, and fiber chemical characteristics, can solve the problems of difficult separation of plant fiber cells, poor product performance, and high cost of modification, and achieve Value-added utilization, high sulfonation efficiency, and simple preparation method

Active Publication Date: 2017-12-22
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

[0041] A method for preparing microfibrillated fibers with a high degree of sulfonation by using corn stalks as raw materials, comprising the following steps:

[0042] (1) Crush corn stalks into grass powder with a mesh size below 20, and vacuum-dry at a vacuum degree of -0.09 MPa, a temperature of 30° C., and a time of 8.0 hours until the moisture content is less than 2.0 wt%.

[0043](2) prepare 1-butyl-3-methylimidazolium chloride salt-LiBr-DMF composite solvent system, solvent composition is: the content of 1-butyl-3-methylimidazolium chloride salt is 9.0wt%, LiBr content is 2.0wt%, DMF content is 89.0wt%.

[0044] (3) Perform high-shear sulfonation treatment in the solvent system, add 1.4g / g corn stalk sulfur trioxide pyridine complex (CAS number: 26412-87-3), add 40g corn stalks (concentration 6.0wt%) ), high-shear sulfonation treatment was carried out for 40 minutes at a temperature of 30° C. and a dispersion speed of 16,000 rpm.

[0045] (4) After the sulfonation tre...

Embodiment 2

[0050] A method for preparing microfibrillated fibers with a high degree of sulfonation by using corn stalks as raw materials, comprising the following steps:

[0051] (1) Crush corn stalks into grass powder below 20 meshes, and vacuum-dry at a vacuum degree of -0.08 MPa, a temperature of 45° C., and a time of 7.5 hours until the moisture content is less than 2.0 wt%.

[0052] (2) prepare 1-butyl-3-methylimidazolium chloride salt-LiBr-DMF composite solvent system, solvent composition is: the content of 1-butyl-3-methylimidazolium chloride salt is 4.5wt%, LiBr content is 1.5wt%, DMF content is 94.0wt%.

[0053] (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 7.0wt%) ), high-shear sulfonation treatment was carried out for 180 min at a temperature of 60° C. and a dispersion speed of 14,000 rpm.

[0054] (4) After the sulfonation treatment, the...

Embodiment 3

[0060] A method for preparing microfibrillated fibers with a high degree of sulfonation by using corn stalks as raw materials, comprising the following steps:

[0061] (1) Crush corn stalks into grass powder below 20 meshes, and vacuum-dry at a vacuum degree of -0.07 MPa, a temperature of 50° C., and a time of 6.0 hours until the moisture content is less than 2.0 wt%.

[0062] (2) prepare 1-butyl-3-methylimidazolium chloride salt-LiBr-DMF composite solvent system, solvent composition is: the content of 1-butyl-3-methylimidazolium chloride salt is 12.0wt%, LiBr content is 3.0wt%, DMF content is 85.0wt%.

[0063] (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 60g corn stalks (concentration 3.0wt%) ), high-shear sulfonation treatment was carried out at a temperature of 70°C and a dispersion speed of 12000rpm for 80min.

[0064] (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-LiBr-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-LiBr-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, so as 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 with LiBr, so that the cohesive force of a raw material is weakened, and the sulphonating modifying efficiency of sulphur trioxide-pyridine complex is improved. According to 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 relates to the field of plant fiber processing and modification methods, in particular to a high-shear method using corn stalks as a raw material in a 1-butyl-3-methylimidazolium chloride salt-LiBr-DMF (dimethylformamide) solvent system Process for preparing microfibrillated fibers with a high degree of sulfonation. Background technique [0002] As a renewable natural polymer material, lignocellulose is renewable and has a large output. The global annual output is as high as 1.0×1010 tons, and it is carbon neutral. It has become the best choice for the oil industry substitute. my country is a large agricultural country, and the output of agricultural waste resources such as corn stalks, rice straw, and wheat straw is large every year. Their efficient transformation and utilization are of great significance for increasing agricultural income, reducing dependence on oil resources, developing new functional materials, reducing environmental ...

Claims

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Application Information

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