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Method for preparing ionic liquid containing cellulose triacetate through adopting bagasse cellulose as raw material

A technology of cellulose triacetate and ionic liquid is applied in the field of preparation of cellulose triacetate, which can solve the problems of demand and large cellulose acetate, and achieve the effects of saving energy consumption, uniform product properties and simple process

Inactive Publication Date: 2012-07-11
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

To solve the problem of large demand for cellulose acetate in my country

Method used

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  • Method for preparing ionic liquid containing cellulose triacetate through adopting bagasse cellulose as raw material
  • Method for preparing ionic liquid containing cellulose triacetate through adopting bagasse cellulose as raw material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh about 0.6g of bagasse cellulose and 14.4g of ionic liquid 1-allyl-3-methylimidazolium chloride (AMIMCl) into a round bottom flask, heat to 80°C in an oil bath, seal and vigorously stir mechanically for 4h. A clear and transparent cellulose solution was obtained, and the concentration of the cellulose solution was 4% (mass fraction). At the same time, acetic anhydride (about 0.735 ml) was added to the solution, so that the molar ratio of acetic anhydride to cellulose glucose unit was 10:1, the reaction temperature of acetylation was 100°C, and the reaction was carried out for 8 hours. After the reaction was completed, an aqueous solution 3 times the volume of the ionic liquid was added, and the product was repeatedly washed with water, then placed in a vacuum drying oven, and dried at 60°C for 24 hours; at the same time, the water in the washing liquid was removed by rotary evaporation to realize the recovery of the ionic liquid. After testing, the obtained cellulo...

Embodiment 2

[0027] Weigh about 0.6g of bagasse cellulose and 14.4g of ionic liquid 1-allyl-3-methylimidazolium chloride (AMIMCl), put them into a round bottom flask, heat to 80°C in an oil bath, seal and stir vigorously for 4h . A clear and transparent cellulose solution was obtained, and the concentration of the cellulose solution was 4% (mass fraction). Acetyl chloride (about 1.58ml) was added to the solution, so that the molar ratio of acetic anhydride to cellulose glucose unit was 8:1, the reaction temperature of acetylation was 100°C, and the reaction was carried out for 8 hours. The post-treatment of the reaction mixture and the recovery of the ionic liquid are basically the same as in Example 1, except that water 4 times the volume of the ionic liquid is added to the reaction mixture. After testing, the acetyl substitution degree of the product obtained is DS=2.98 .

Embodiment 3

[0029]Weigh about 0.6g of bagasse cellulose and 11.4g of ionic liquid 1-butyl-3-methylimidazolium chloride (BMIMCl) into a round bottom flask, heat to 90°C in an oil bath, seal and vigorously stir mechanically for 6h. A clear and transparent cellulose solution was obtained, and the concentration of the cellulose solution was 5% (mass fraction). Acetic anhydride (about 2.45ml) was added to the solution, so that the molar ratio of acetic anhydride to cellulose glucose unit was 10:1, the reaction temperature of acetylation was 120°C, and the reaction was carried out for 7 hours. The post-treatment of the reaction mixture and the recovery of the ionic liquid are basically the same as in Example 1, except that water 5 times the volume of the ionic liquid is added to the reaction mixture. After testing, the acetyl substitution degree of the product obtained is DS=2.99 .

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Abstract

The invention relates to the field of preparation of cellulose triacetate, and particularly relates to a method for preparing ionic liquid containing cellulose triacetate with through adopting bagasse cellulose as a raw material. The method comprises the steps as follows: firstly, the bagasse cellulose and the ionic liquid for dissolving the cellulose are mixed to generate a ionic liquid solution containing the cellulose; secondly, an acetylation reagent is added into the ionic liquid solution containing the cellulose to conduct homogeneous-phase acylation reaction to generate a reaction mixture containing the cellulose triacetate; thirdly, water is added into the reaction mixture to cause solid to subside; and fourthly, the filtered solid is dried to generate the cellulose triacetate. Compared with the conventional method for generating cellulose triacetate, the method has the advantages of adopting the ionic liquid as a solvent, avoiding any catalyst, and being simple in process, free of pollution, uniform in product property, controllable and the like; and the degree of substitution of the cellulose triacetate generated by the method ranges from 2.8 to 3.0.

Description

technical field [0001] The invention relates to the field of preparation of cellulose triacetate, in particular to a method for preparing ionic liquid of cellulose triacetate using bagasse cellulose as raw material. Background technique [0002] Cellulose triacetate refers to cellulose acetate products with an average degree of substitution between 2.8 and 3.0. Due to its excellent solubility and optical properties, it is mainly used in the manufacture of cellulose acetate filaments, films, semi-permeable membranes, photosensitive film and other materials. Widely used in textiles, aerospace, military industry and seawater desalination and other fields. [0003] The current technological routes for producing cellulose triacetate are all carried out in a heterogeneous system. It is prepared by using refined cotton linters or wood pulp as raw materials, using sulfuric acid as a catalyst, and undergoing steps such as crushing, activation, acetylation, hydrolysis, precipitation...

Claims

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Application Information

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IPC IPC(8): C08B3/06C08J3/09
Inventor 李会泉曹妍
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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