Method for preparing cellulose ester by using cellulose

A cellulose ester and cellulose technology, applied in the field of cellulose ester production from cellulose, can solve the problems of high cost of purification and recycling, high cost of solvent, high cost of raw materials, etc.

Active Publication Date: 2015-01-14
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method solves the problems of high cost of raw materials, high cost of solvent, and high cost of purification,

Method used

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  • Method for preparing cellulose ester by using cellulose
  • Method for preparing cellulose ester by using cellulose
  • Method for preparing cellulose ester by using cellulose

Examples

Experimental program
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Effect test

Embodiment 1

[0070] Weigh about 0.5g of corn stalk cellulose, and about 10g of a mixed solution composed of 1,8-diazabicyclo[5.4.0]undec-7-ene (DBU), methanol and DMSO (DMSO accounts for The mole fraction of the solution is 80%, DMSO is about 5.8g, DBU is about 2.8g, methanol is about 0.59g), put them into the autoclave together, cover the autoclave, and pass 0.5MPa of CO 2 , the temperature is at 80°C, sealed and vigorously stirred mechanically for 1 hour, and a one-pot reaction is carried out to dissolve the cellulose. A clear and transparent cellulose solution was obtained, and the concentration of the cellulose solution was 5% (mass fraction). Keep the temperature at 80°C, and add acetic anhydride (about 2.86g) to the solution at the same time, so that the molar ratio of acetic anhydride to the total hydroxyl groups in the cellulose solution is 1:1, and react for 5h. After the reaction was completed, the product was precipitated with 3 times the amount of water, and the solid product ...

Embodiment 2

[0072] Efficient recycling of solvents is an important special feature of this patent, which we illustrate through this example.

[0073] Weigh 0.5g of microcrystalline cellulose, weigh about 10g of the mixed solution composed of DBU, methanol and DMSO (the molar fraction of DMSO in the mixed solution is 80%, about 5.8g of DMSO, about 2.8g of DBU, and about 0.59g of methanol), Add together in the autoclave, cover the autoclave, pass 0.5MPa of CO 2 , the temperature is at 80°C, sealed and vigorously stirred mechanically for 1 hour, and a one-pot reaction is carried out to dissolve the cellulose. A clear and transparent cellulose solution was obtained, and the concentration of the cellulose solution was 5% (mass fraction). Keep the temperature at 80°C, and add acetic anhydride (about 2.86g) to the solution at the same time, so that the molar ratio of acetic anhydride to the total hydroxyl groups in the cellulose solution is 1:1, and react for 5h. After the reaction was complet...

Embodiment 3

[0076] Weigh about 0.5g of α-cellulose, weigh about 10g of a mixed solution composed of 1,1,3,3-tetramethylguanidine (TMG), methanol and DMSO (DMSO accounts for 80% of the molar fraction of the mixed solution, methanol About 0.63g), put into the autoclave together, cover the autoclave, pass 2MPa CO 2 , the temperature is at 60°C, sealed with strong mechanical stirring for 3 hours, and a one-pot reaction is carried out to dissolve the cellulose. A clear and transparent cellulose solution was obtained, and the concentration of the cellulose solution was 5% (mass fraction). Raise the temperature to 80°C, and at the same time add acetic anhydride (about 3.64g) to the solution so that the molar ratio of acetic anhydride to the total hydroxyl groups in the cellulose solution is 1.2:1, and react for 5 hours. After the reaction was completed, the product was precipitated with 4 times the amount of methanol, and the solid product was repeatedly washed with water and freeze-dried for 2...

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Abstract

The invention provides a method for preparing cellulose ester by using cellulose. The method comprises the following steps: 1, using cellulose as a raw material; 2, dissolving the cellulose in a CO2 switchable ionic compound or a CO2 switchable ionic compound and organic solvent mixed solvent to obtain a solution containing cellulose; 3, adding an acylation reagent into the cellulose solution to obtain a reaction mixture solution; 4, adding water or C1-C3 of lower fatty alcohol to the reaction mixture solution, and filtering the reaction mixture liquid containing water or the lower fatty alcohol; and 5, drying the solid obtained after the filtration to obtain the cellulose ester. The CO2 switchable ionic compound or the CO2 switchable ionic compound and organic solvent mixed solvent is used as a solvent, and the component of the switchable ionic compound also has a catalysis effect without any other catalysts. The method has the advantages of simple process, low solvent cost, convenient operation, solvent recyclability and the like.

Description

technical field [0001] The invention relates to a method for preparing cellulose acetate, cellulose propionate, cellulose butyrate, cellulose acetate propionate and cellulose acetate butyrate by using cellulose as a raw material, especially a method using Cellulose in CO 2 Switching ionic compounds or CO 2 The invention discloses a method for homogeneously preparing cellulose ester in a mixed solvent composed of a switch-type ionic compound and an organic solvent. Background technique [0002] Cellulose derivatives are the earliest natural polymer materials developed by humans. With the increasing shortage of non-renewable resources such as coal, oil, and natural gas, natural cellulose, as the most abundant renewable resource in nature, has attracted more and more attention. Natural polymer materials have the characteristics of biodegradability and bioabsorbability, and people's development and application of them emerge in endlessly. Cellulose esters are important deriv...

Claims

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Application Information

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IPC IPC(8): C08B3/00
Inventor 谢海波赵宗保杨云龙
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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