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Preparation method of cellulose acetate propionate

A technology of cellulose acetate propionate and acetic acid, which is applied in the field of cellulose modification, can solve the problems of insignificant effect of crystal breaking zone, difficult esterification and unevenness, etc., and achieves good effect of crystal breaking zone and uniform esterification degree. , The effect of stable product performance

Active Publication Date: 2013-05-08
CHANGMAO BIOCHEMICAL ENG CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The present invention uses the mixture of acetic anhydride and propionic anhydride to activate the cellulose, which solves the problem in the prior art that the effect of the crystal-breaking region is not obvious after activation with acid, which leads to difficult and uneven esterification.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 10gAl 2 o 3 The carrier was placed in 20 mL of 10% Zr(NO 3 ) 4 Soak in solution, add NH 3 ·H 2 O to adjust pH=8~10, let stand, filter, wash, dry, and use 0.5mol / L H 2 SO 4 The solution was impregnated for 20 hours, filtered, dried, and calcined at 600°C for 3 hours to obtain a solid superacid catalyst SO 4 2- -ZrO 2 -Al 2 o 3 .

[0023] Take 10g of cellulose, activate it in 55g of acetic anhydride at 80°C for 1 hour, then add 25g of solvent acetic acid and 25g of propionic acid, the above SO 4 2- -ZrO 2 -Al 2 o 3 Catalyst 0.05g, esterification reaction at 90°C for 0.5 hours, adding 17g of waste acid water, hydrolysis at 60°C for 2 hours, precipitation, filtration, washing, and drying to obtain the product, which can be reused. In this embodiment, the content of acetyl group is 53.0%, and the content of propionyl group is 0.1%.

Embodiment 2

[0025] Mix tetraisopropyl titanate, acetic acid, and 2-butanol in a mass ratio of 1:0.1:5, stir, add water until a gel is formed, let stand, dry, grind, and use 0.5mol / L H 2 SO 4 The solution was soaked for 20 hours, filtered, dried, and calcined at 550°C for 4 hours to obtain a solid superacid catalyst SO 4 2- -TiO 2 .

[0026] Take 10g of cellulose, activate it at 60°C for 2 hours in a mixture of 30g of acetic anhydride and 30g of propionic anhydride, then add 20g of acetic acid, 20g of propionic acid, the above SO 4 2- -TiO 2 Catalyst 0.1g, esterification at 60°C for 2 hours, adding 20g of waste acid water, hydrolysis at 80°C for 1 hour, precipitation, filtration, washing, and drying to obtain the product, which can be reused. In this example, the acetyl content is 28.9%, and the propionyl content is 24.6%.

Embodiment 3

[0028] According to the preparation method of catalyst in embodiment 1, Zr(NO 3 ) 4 Change to TiCl 4 Preparation of solid superacid catalyst SO 4 2- -TiO 2 -Al 2 o 3 .

[0029] Take 10g of cellulose, activate it at 90°C for 0.5 hours in a mixture of 30g of acetic anhydride and 20g of propionic anhydride, then add 25g of acetic acid, 25g of propionic acid, the above SO 42- -TiO 2 -Al 2 o 3 Catalyst 0.08g, esterification at 30°C for 8 hours, adding 16g of waste acid water, hydrolysis at 60°C for 2 hours, precipitation, filtration, washing, and drying to obtain the product, which can be reused. In this embodiment, the acetyl content is 26.4%, and the propionyl content is 21.3%.

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Abstract

The invention relates to a preparation method of cellulose acetate propionate, belonging to technical field of cellulose modification. The preparation method of cellulose acetate propionate comprises the following steps of: taking cellulose as a raw material, activating by a mixed solution of acetic anhydride and propionic anhydride, adding acetic acid and propionic acid solvents and a solid super acidic catalyst for esterification, after esterification, filtering to remove the catalyst, adding waste acid water for hydrolyzing, settling out by waste acid water, and finally obtaining the cellulose acetate propionate by steps of filtering, washing, drying and the like. The production process is simple to operate, the solid super acidic catalyst substitutes the concentrated sulfuric acid catalyst and can be cyclically used for many times, thus alleviating the problem of serious corrosion of the original process equipment. The waste acid water generated in the reaction process only contains acetic acid and propionic acid without sulfuric acid and can be fully recovered and cyclically used, thus decreasing the tension in environmental protection, realizing zero discharge and greatly reducing the production cost. The cellulose acetate propionate prepared by the method has fine toughness, heat stability and compatibility, thus being extensively used.

Description

technical field [0001] The invention relates to the technical field of cellulose modification, in particular to a method for preparing cellulose acetate propionate (CAP for short), which can produce a series of cellulose acetate propionate fibers with different acetyl and propionyl contents white. Background technique [0002] Cellulose acetate propionate is a white solid with excellent toughness, thermal stability and compatibility. It is widely used in auto parts, tool handles, radio and TV parts, steering wheels, films, filter membranes, radio transistors, toys, walls Floor tiles, coatings, spinning and other industries. [0003] The preparation method of existing cellulose acetate propionate is basically carried out according to the following steps: activate cellulose with acid, use concentrated sulfuric acid as a catalyst, carry out esterification in the mixed solution of acid and acid anhydride, and then through hydrolysis, precipitation, washing, Drying and other pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B3/16
Inventor 冷一欣王宁芮新生黄春香李园园
Owner CHANGMAO BIOCHEMICAL ENG CO LTD
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