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A two-step method for obtaining cellulose-rich materials from straw using ionic liquids

An ionic liquid and cellulose technology, applied in fiber raw material processing, textile and papermaking, etc., can solve the problems of high reaction pressure, long time, and reduce the crystallinity of cellulose, and achieve mild reaction conditions, low production cost, and high crystallinity. reduced effect

Active Publication Date: 2016-10-05
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the field of straw pretreatment, the traditional method is to use acid or alkali solution to soak the biomass for a long time to remove lignin or hemicellulose, but the waste liquid produced by these methods is serious to the environment, and it is difficult to Reduce the crystallinity of cellulose
In addition, steam explosion (such as water vapor, ammonia vapor and ozone), microwave radiation and other methods are also widely used in biomass pretreatment. The disadvantages are high reaction pressure, high equipment requirements, high energy consumption, and changes in cellulose crystallinity. Small, not conducive to the subsequent conversion of cellulose
[0005] Although the reported amino acid ionic liquid (patent CN102533907 A) and degradable ionic liquid (patent CN103031762 A) can achieve the pretreatment of rice and corn stalks to a certain extent, but the implementation temperature is 50 ° C ~ 130 ° C, 100 ° C Between ~180°C, the processing time is several hours or even several days, and the high reaction temperature and long time make the ionic liquid used partially decompose, thereby reducing the service life of the ionic liquid
It is difficult to completely dissolve straw and enrich cellulose in a short time by using functionalized ionic liquid alone to treat straw

Method used

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  • A two-step method for obtaining cellulose-rich materials from straw using ionic liquids
  • A two-step method for obtaining cellulose-rich materials from straw using ionic liquids
  • A two-step method for obtaining cellulose-rich materials from straw using ionic liquids

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh about 1.0964g of straw powder after washing with neutral detergent, add it into 20mL 50wt% choline hydroxide (ChOH) aqueous solution, stir at room temperature for 3h, centrifuge the residue and supernatant, and then use the residue 60 mL of distilled water was washed three times, filtered and dried to obtain a residue of 0.5218 g, and the dissolution rate of the straw in the solution reached 47.59%. The content of hemicellulose in the analysis residue component was 31.22%, the content of cellulose was 56.71%, that is, the content of cellulose was 87.93%, and the content of lignin was 12.07%.

[0021] Weigh about 0.5000g of the above residue, add it to 10.0028g 1-ethyl-3-methylimidazole dimethyl phosphate ([Emim][DMP]) ionic liquid, heat to 130°C and magnetically stir for 5-10min to complete the reaction Dissolve, no residue remains, and the dissolution rate reaches 100%. After stopping the reaction, cool to normal temperature, add 10mL DMSO to dilute the reaction...

Embodiment 2

[0023] Weigh about 1.0964g of straw powder after washing with neutral detergent, add it into 20mL 50wt% choline hydroxide (ChOH) aqueous solution, stir at room temperature for 3h, centrifuge the residue and supernatant, and then use the residue 60 mL of distilled water was washed three times, filtered and dried to obtain a residue of 0.5218 g, and the dissolution rate of the straw in the solution reached 47.59%. The content of hemicellulose in the analysis residue component was 31.22%, the content of cellulose was 56.71%, that is, the content of cellulose was 87.93%, and the content of lignin was 12.07%.

[0024] Weigh about 0.5022g of the above residue, add it to 10.0244g of 1-ethyl-3-methylimidazole acetic acid ([Emim][OAc]) ionic liquid, heat to 130°C and magnetically stir for 30min to dissolve completely, and no residue remains , the dissolution rate reaches 100%. After the reaction was stopped, it was cooled to room temperature, and 10 mL of DMSO was added to dilute the ...

Embodiment 3

[0026] Weigh about 1.0964g of straw powder after washing with neutral detergent, add it into 20mL 50wt% choline hydroxide (ChOH) aqueous solution, stir at room temperature for 3h, centrifuge the residue and supernatant, and then use the residue 60 mL of distilled water was washed three times, filtered and dried to obtain a residue of 0.5218 g, and the dissolution rate of the straw in the solution reached 47.59%. The content of hemicellulose in the analysis residue component was 31.22%, the content of cellulose was 56.71%, that is, the content of cellulose was 87.93%, and the content of lignin was 12.07%.

[0027] Weigh about 0.5000 g of the above residue, add it into 9.8572 g of 1-ethyl-3-methylimidazolium chloride salt ([Emim]Cl) ionic liquid, heat to 130°C and magnetically stir for 50 minutes to completely dissolve and no residue remains. The dissolution rate reaches 100%. After the reaction was stopped, it was cooled to room temperature, and 10 mL of DMSO was added to dilu...

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Abstract

The invention relates to a new method for obtaining a cellulose-rich material by quickly dissolving straws at low temperature by two steps by utilizing A and B ionic liquids. The new method is characterized by soaking the straws in an A ionic liquid aqueous solution at low temperature for a short time to obtain part of lignin-free insoluble residues in the first step, and completely dissolving the remaining residues in the B ionic liquid in a short time in the second step to obtain the cellulose-rich material which has changed cellulose crystal form and obviously reduced degree of crystallinity and is beneficial for subsequent conversion. Compared with other pretreatment methods, the method has the beneficial effects that the solution temperature is relatively low, the time is short, the method is convenient and simple to operate, and high-yield 5-hydroxymethyl furfural can be obtained through catalytic conversion of the obtained cellulose-rich material. Not only can corrosion of instruments caused by traditional acid-alkali pretreatment methods be avoided but also the pretreatment energy consumption is reduced to a greater extent. The environment-friendly low-energy-consumption treatment mode can help achieve effective pretreatment of the straws, and has great significance in solving the problem of biomass resource utilization.

Description

technical field [0001] The invention relates to a method for rapidly obtaining a cellulose-rich material whose crystal form is changed and crystallinity is obviously reduced from straw by using two types of ionic liquids A and B in two steps at low temperature. Background technique [0002] Biomass straw is one of the most common lignocellulosic materials. The annual output of straw in my country reaches more than 700 million tons. Incineration in situ not only wastes resources, but also causes serious environmental pollution. The limitation of petrochemical energy and the environmental pollution problems caused by it have also promoted the vigorous development of biomass conversion and utilization at some levels. Chemicals or intermediates derived from biomass, such as levulinic acid and 5-hydroxymethylfurfural, are widely used in chemical production, providing more and wider space for biomass utilization. The main components of straw are cellulose, hemicellulose and ligni...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D21C5/00
Inventor 吕兴梅徐俊丽张锁江周清辛加余何宏艳徐婷婷
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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