Method for efficiently preparing cellulose acetate through catalyzing waste biomass by organic solvents

A technology of cellulose acetate and waste biomass, which is applied in the field of chemical industry, can solve problems such as difficult separation of products and complex processing methods, and achieve the effects of alleviating environmental pollution, convenient separation of products, and low energy consumption

Inactive Publication Date: 2015-12-09
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the above-mentioned technical problems in the prior art, the present invention provides a method for efficiently preparing cellulose acetate from waste biomass catalyzed by an organic solvent, and the method for preparing cellulose acetate solves the problems in the prior art The technical problems of complex process and difficult product separation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 1g of dried biomass into a 250ml small flask, slowly add 12ml of a mixture of formic acid and water with a volume ratio of 1:1, gently shake the small flask to mix evenly, and then add 0.05% hydrochloric acid (accounting for the solvent system) ) as a catalyst, heated in an oil bath at 40°C for 0.5 hours, suction filtered the pretreatment solution, and washed the solid residue with 40°C hot hydrochloric acid aqueous solution and deionized water in turn to obtain cellulose. Then take 1g of dry cellulose and pour it into a 250ml three-necked flask, add 0.7g of acetic acid and acetic anhydride with a mass ratio of 1:20, a mass fraction of 0.02% sulfuric acid (accounting for biomass dry weight) and 4ml of dichloromethane. The acetylation reaction was carried out by heating in an oil bath at 50°C for 2 hours, suction filtration, and rotary evaporation of the filtrate to obtain cellulose acetate. Cellulose acetate (dry biomass).

Embodiment 2

[0026] Take 2g of dry biomass into a 250ml small flask, slowly add 30ml of a mixture of formic acid and water with a volume ratio of 4:1, gently shake the small flask to mix evenly, and then add 0.08% (accounting for the solvent system) of Using hydrochloric acid as a catalyst, heating in an oil bath at 130°C for 1.5 hours, suction filtration of the pretreatment solution, and successively washing the solid residue with a 50°C hot aqueous sulfuric acid solution and deionized water to obtain cellulose. Then take 1.4g of dry cellulose and pour it into a 250ml three-necked flask, add 1.4g of acetic acid and acetic anhydride in a mass ratio of 1:16, a mass fraction of 0.12% sulfuric acid (accounting for biomass dry weight) and 9ml of dichloromethane. The acetylation reaction was carried out by heating in an oil bath at 110 °C for 5 hours, suction filtration, and rotary evaporation of the filtrate to obtain cellulose acetate. Cellulose acetate (dry biomass).

Embodiment 3

[0028] Take 3g of dried biomass into a 250ml small flask, slowly add 50ml of a mixture of formic acid and water with a volume ratio of 7:1, gently shake the small flask to mix evenly, and then add 0.1% hydrochloric acid (accounting for the solvent system) ) as a catalyst, heated in an oil bath at 100 °C for 2.5 hours, suction filtered the pretreatment solution, and washed the solid residue with hot phosphoric acid aqueous solution at 55 °C and deionized water in turn to obtain cellulose. Then take 1.8g of dry cellulose and pour it into a 250ml three-necked flask, add 2.1g of acetic acid and acetic anhydride in a mass ratio of 1:12, a mass fraction of 0.22% sulfuric acid (accounting for biomass dry weight) and 14ml of dichloromethane. The acetylation reaction was carried out by heating in an oil bath at 90 °C for 4 hours, suction filtration, and rotary evaporation of the filtrate to obtain cellulose acetate. Cellulose acetate (dry biomass).

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Abstract

The invention provides a method for efficiently preparing cellulose acetate through catalyzing waste biomass by organic solvents. According to the method, dry biomass powder is poured into a reaction vessel; then, a mixed solution of methanoic acid and water is added into the reaction vessel; after the materials are uniformly mixed, hydrochloric acid is added to be used as catalysts; under the condition of 40 to 150 DEG C, oil bath heating and stirring are carried out; pre-treatment liquid is subjected to suction filtration; a hot acid water solution and deionized water are used for sequentially washing solid residue, and the cellulose can be obtained; the dry cellulose powder is poured into another reaction vessel; a mixed solution of acetic acid and acetic anhydride, concentrated sulfuric acid and methylene dichloride are added; oil bath heating is performed under the condition being 50 to 120 DEG C; suction filtration, rotary distillation, rotary distillation product washing, extraction filtering and solid residue vacuum drying are performed; the cellulose acetate is obtained. The method has the advantages that a great amount of cellulose in the waste biomass in the nature can be converted into high-added-value cellulose acetate, and the yield reaches 18.25 percent to 50.16 percent.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to cellulose acetate, in particular to a method for efficiently preparing cellulose acetate by catalyzing waste biomass with an organic solvent. Background technique [0002] Cellulose is the main structural component of plant cell walls. Generally, the content in wood is 40%~50%. It is the oldest and most abundant natural polymer on the earth, and it is the most precious and inexhaustible human Natural renewable resources, with highly ordered crystal structure and degree of polymerization, linked together with hemicellulose and lignin with different binding forces. The surface pore structure of cellulose and the protective effect of lignin and hemicellulose on cellulose make it difficult to degrade biomass. The degradation of any type of component must be restricted by other components. Therefore, pretreatment of biomass raw materials It is a necessary means to degrade the network st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B3/06
Inventor 韩生陈红艳曹磊昌蔺华林薛原马鹏余焓于飞卢德力蒋继波李原婷邱丰裴素鹏祝俊何忠义熊丽萍陈凯绯孙赛楠常兴李勇
Owner SHANGHAI INST OF TECH
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