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Method for separating cellulose and lignin from plant fiber raw material by utilizing ion liquid

An ionic liquid and plant fiber technology, which is applied in fiber raw material processing, textile and papermaking, etc., can solve the problems of low solubility of plant raw materials, inability to obtain effects, low extraction rate of lignin and cellulose, etc., and achieve strong industrial application prospects. , The effect of low production cost and shortened processing time

Inactive Publication Date: 2012-09-19
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

None of the above involves the cellulose purification process and the lignin extraction method;
[0005] The 2005 patent (application number: PCT / FI2004 / 000476) disclosed a method for dissolving lignocellulosic raw materials with ionic liquids, but did not effectively separate and regenerate lignin or cellulose
[0006] In the patent whose application number is 200910012002.1, it is mentioned that a mixture of imidazole compounds and water is used as a solvent to dissolve and separate plant materials. During the separation and extraction of lignin and cellulose, it was found that water was added to the ionic liquid as a solvent, which had a low dissolving ability for plant materials, so that the extraction rate of lignin and cellulose was very low; at the same time, according to the patent The dissolution time given can not achieve good results
Therefore, carry out experiment by the condition that this patent gives, can not obtain good effect
[0007] In addition, when only ionic liquids are used to dissolve plant materials, due to the high viscosity of ionic liquids, it is difficult to achieve solid-liquid separation through filtration after the reaction, which brings great difficulties to subsequent separation operations. Therefore, in order to To overcome the above-mentioned problems, the inventors of the present invention have carried out experimental investigations on the screening of diluents, the reasonable mass ratio of diluents and ionic liquids, and the impact on subsequent separation operations of lignin and cellulose

Method used

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  • Method for separating cellulose and lignin from plant fiber raw material by utilizing ion liquid
  • Method for separating cellulose and lignin from plant fiber raw material by utilizing ion liquid
  • Method for separating cellulose and lignin from plant fiber raw material by utilizing ion liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Weigh about 0.5 g of pine sawdust, 50.0 g of a mixed solution of ionic liquid 1-allyl-3-methylimidazolium chloride (AmimCl) and DMSO (mass ratio 6:1), put them into a round bottom flask, and heat with microwave to 110°C with vigorous mechanical stirring for 2 hours. After the reaction is finished, use a 300-mesh stainless steel filter to filter and separate, and add water to the filtrate to separate out cellulose and lignin. The mixture was washed 8 times with DMSO / water solution (1:1v), filtered and separated with 200-mesh nylon filter cloth to obtain pine wood cellulose and washing liquid containing lignin. Put pine wood cellulose into a vacuum drying oven and dry at 60°C for 24 hours to obtain cellulose products; recover DMSO / water from the washing liquid by rotary evaporation under reduced pressure to obtain DMSO / water, and separate lignin products at the same time. After testing, the dissolution rate of raw materials in ionic liquid is 36%, the purity of cellulose...

Embodiment 2

[0053] Weigh about 0.5 g of pine sawdust, 50.0 g of a mixed solution of ionic liquid 1-ethyl-3-methylimidazolium acetate (EmimAc) and DMSO (mass ratio 9:1), put them into a round-bottomed flask, and microwave to 100°C with vigorous mechanical stirring for 2 hours. After the reaction is over, use a 400-mesh stainless steel filter screen to filter and separate. The post-treatment of the reaction mixture and the recovery of the ionic liquid are basically the same as in Example 1. The nylon filter cloth is 300 mesh. After testing, the dissolution rate of the raw material in the ionic liquid is 35%, the cellulose purity in the extract is 83%, the cellulose extraction rate can reach 59%, and the lignin purity is 80%.

Embodiment 3

[0055] Weigh about 1.5 g of pine sawdust, 50.0 g of a mixed solution (mass ratio 5:1) of ionic liquid 1-butyl-3-methylimidazolium chloride (BmimCl) and DMSO, put them into a round bottom flask, and heat to 100 ° C, strong mechanical stirring for 3h. After the reaction, use a 280-mesh stainless steel filter to filter and separate. The post-treatment of the reaction mixture and the recovery of the ionic liquid are basically the same as in Example 1. The nylon filter cloth is 280 mesh. After testing, the dissolution rate of the raw material in the ionic liquid is The purity of cellulose in the extract is 85%, the extraction rate of cellulose can reach 62%, and the purity of lignin is 80%.

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Abstract

The invention relates to the field of treatment of plant fibers and particularly relates to a method for separating cellulose and lignin from a plant fiber raw material by utilizing ion liquid. According to the invention, the method comprises the following steps of: 1) mixing DMSO (Dimethylsulfoxide) and the ion liquid according to a mass ratio of 1: 4-9 to be used as a solvent, and adding the plant fiber raw material; 2) dissolving at 80 to 140 DEG C for 4-48 hours to obtain a reaction mixed liquid; 3) filtering and separating the reaction mixed liquid by a stainless steel filter screen or a nylon filter cloth, adding water into the obtained filtrate, and depositing a mixed extract of the cellulose and the lignin; 4) washing and extracting a mixed extract of the cellulose and the lignin by a water / DMSO mixed solvent, and filtering to obtain mixed liquid of a cellulose solid and lignin / DMSO / water; 5) drying the cellulose solid to obtain a cellulose product; and 6) decompressing and distilling the mixed liquid of the cellulose / DMSO / water to obtain a cellulose product. The method, provided by the invention, is simple, feasible and high in purity of the obtained cellulose.

Description

technical field [0001] The invention relates to the field of plant fiber treatment, in particular, the invention relates to a method for separating cellulose and lignin from plant fiber raw materials by using ionic liquid. Background technique [0002] With the increasingly serious consumption of fossil resources and environmental pollution, as well as the gradual enhancement of the concept of sustainable development and environmental protection awareness, the research and development of products and related processes prepared from renewable biomass resources have attracted more and more attention from the world. The potential amount of woody biomass is very sufficient. The plant fiber raw material produced by photosynthesis is about 180 billion tons per year, which is equivalent to 10 times the total annual energy consumption in the world. Therefore, it is imperative to replace fossil resources with woody biomass resources. . The main components of plant fiber raw material...

Claims

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Application Information

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IPC IPC(8): D21C5/00C08H7/00
Inventor 李会泉王学静曹妍唐清
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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