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Cellulose dissolving agent and application of cellulose dissolving agent in aspect of cellulose esterification modification

A technology of cellulose dissolution and cellulose solution, which is applied in the production of bulk chemicals, etc., can solve the problems of high viscosity of cellulose solution, long esterification reaction time, and low product substitution degree, and achieve low reaction temperature and low product substitution degree. High uniformity, yield and purity

Inactive Publication Date: 2015-07-22
BEIJING FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These two ionic liquids are more suitable for esterification modification reactions, but the disadvantages are that the dissolution time is relatively long and the viscosity of the cellulose solution is large.
At present, the method introduced in the literature about modifying cellulose with aromatic acid esterification agent not only takes too long for the esterification reaction time, but also has an extremely low degree of substitution of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Embodiment 1: dissolving agent and the method for dissolving cellulose thereof

[0041] 1. Dissolving agent composition: 2g BMIMAc, 4g TBAA, 12g DMAc.

[0042] 2. The method of dissolving cellulose

[0043] 1) Weigh 20g of pulp cellulose, put it in 800ml of deionized water, soak it for 6 hours, take it out and filter it with suction to remove most of the moisture in the pulp cellulose, dry it in a drying oven at 55°C for 24 hours, and set aside ;

[0044]2) Preparation of cellulose solution: Weigh BMIMAc, TBAA, DMAc according to the proportion, add them into a three-necked flask and stir evenly, mix at 50°C, and then accurately weigh 1.08g of pulp board cellulose (fiber The molar number of plain glucose units is 6.67mmol), and after stirring for 1 hour, a cellulose solution with a mass fraction of 6% (pulp plate cellulose mass / dissolving agent mass=6%) can be obtained, to obtain final product.

Embodiment 2

[0045] Embodiment 2: cellulose esterification reaction

[0046] 1. Accurately measure 8.8ml of tripropylamine and 6.2ml of DMAc and mix them homogeneously and then add them to the 6% cellulose solution prepared in Example 1 (the molar number of cellulose glucose units in the solution is 1.08g / 162g mol -1 =6.67mmol), after the temperature was adjusted to 8°C by an ice-water bath, a mixed solution of 6.36g p-toluenesulfonyl chloride (33.30mmol) and 4.2ml DMAc was added dropwise, so that the molar ratio of p-toluenesulfonyl chloride and cellulose glucose unit was 5.0 : 1, 12 hours of reaction.

[0047] 2. Pour the reaction mixture into 500ml deionized water / ethanol solution (6:4 by volume) for precipitation, filter with suction, wash the filter cake repeatedly with a large amount of deionized water, and place it in a vacuum drying oven at 55°C Let dry for 24 hours. 3.74 g of cellulose p-toluenesulfonate was obtained, the degree of substitution was 2.2, the yield was 89.9%, and ...

Embodiment 3

[0048] Embodiment 3: dissolving agent and the method for dissolving cellulose thereof

[0049] 1. Dissolving agent composition: 2g BMIMAc, 6g TBAA, 18g DMAc.

[0050] 2. The method of dissolving cellulose

[0051] 1) Weigh 20g of pulp cellulose, put it in 800ml of deionized water, soak it for 6 hours, take it out and filter it with suction to remove most of the moisture in the pulp cellulose, and dry it in a drying oven at 55°C for 24 hours for later use .

[0052] 2) Preparation of cellulose solution: Weigh 1-butyl-3-methylimidazolium acetate, tetrabutylammonium acetate and N,N'-dimethylacetamide according to the ratio, add them to a three-necked flask and stir Evenly, mix at 50°C, then accurately weigh 1.56g of the processed pulp sheet cellulose according to step 1 (the number of cellulose glucose units is 1.56g / 162g·mol -1 =9.63mmol), and stirred for 1 hour to obtain a cellulose solution with a mass fraction of 6% (pulp board cellulose mass / dissolving agent mass=6%), to ...

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Abstract

The invention relates to a cellulose dissolving agent and application of the cellulose dissolving agent in the aspect of cellulose esterification modification. The cellulose dissolving agent is prepared from the following constituents: 1-butyl-3-methylimidazolium acetate, ammonium tetrabutyl acetate and N,N'-dimethylacetamide. According to the invention, in the novel solvent, a homogeneous phase modification method is conducted to enable paratoluensulfony chloride to directly react with pulp board cellulose dissolved by the cellulose dissolving agent, the intermediate reaction step can be avoided, the reaction conditions can be controlled to regulate the degree of substitution of the pulp board cellulose on toluenesulfonate; the process is simple, the production cost is low, and the high purity is achieved.

Description

technical field [0001] The present invention relates to an esterification modification method for pulp board cellulose, in particular, it relates to the reaction of efficiently preparing high-substituted cellulose p-toluenesulfonate through low-temperature esterification reaction in a homogeneous solvent system, The invention belongs to the technical field of modification of natural polymer cellulose materials. Background technique [0002] Cellulose p-toluenesulfonate is an important cellulose derivative, which is often used in selective esterification, determination of substituent distribution of cellulose derivatives and as an intermediate in the synthesis of new cellulose derivatives. The heterogeneous synthesis of cellulose p-toluenesulfonate not only has long reaction time, high material ratio, many side reactions and poor product solubility. Compared with the heterogeneous process, the tosylation reaction time of cellulose is relatively short, the product has a high ...

Claims

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Application Information

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IPC IPC(8): C08J3/09C08L1/02C08B3/14C08B3/22
CPCY02P20/54
Inventor 张力平于永启苗娇娇姜泽明
Owner BEIJING FORESTRY UNIVERSITY
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