Preparation method of cellulose acetate propionate mixed ester with high propionyl content

A technology of cellulose acetate propionate and high propionyl group, applied in the field of cellulose lipid derivatives, can solve the problems of inaccurate control of hydrolysis reaction, long esterification reaction time, corrosive process equipment, etc., to reduce corrosion and environment Effects of pollution, increased application, product performance stability

Inactive Publication Date: 2015-12-30
JIANGSU RUICHEN CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cellulose acetate butyrate butyryl content that this method prepares is higher, but there are following problems: 1. use the concentrated sulfuric acid as catalyzer in this preparation method, process equipment is had very strong corrosion, and use the concentrated sulfuric acid in a large amount, It will pollute the environment; 2. The esterification reaction time is long, and the hydrolysis reaction control is not precise enough; 3. The reaction stage needs to be cooled by an external jacket, which makes the production cost higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The preparation method of the high propionyl content cellulose acetate propionate mixed ester of the present embodiment specifically comprises the following steps:

[0032] (1) Weigh 650g of wood pulp, 2630g of propionic acid, 40g of acetic anhydride, 2070g of propionic anhydride, and 19.5g of catalyst. The catalyst is a mixture of liquid acid catalyst and heteropolyacid catalyst, of which 3.8g of liquid acid catalyst sulfuric acid, heteropolyacid catalyst h 3 PW 12 o 40 11.7g;

[0033] (2) Spray 650g of wood pulp with 325g of propionic acid, and then activate it at 25°C for 0.5h;

[0034] (3) Mix the remaining propionic acid with proportioned propionic anhydride, acetic anhydride, and catalyst, and cool the mixture to 3°C for use;

[0035] (4) Put the activated wood pulp in step (2) into the cooling liquid in step (3) within 5 minutes, fully stir without external cooling, and the reaction will naturally heat up, so that the temperature in the final esterification r...

Embodiment 2

[0040] The preparation method of the high propionyl content cellulose acetate propionate mixed ester of the present embodiment specifically comprises the following steps:

[0041] (1) Weigh 650g of wood pulp, 2630g of propionic acid, 40g of acetic anhydride, 2070g of propionic anhydride, and 52g of catalyst. The catalyst is a mixture of a liquid acid catalyst and a heteropolyacid catalyst. 3 PW 12 o 40 20.8g;

[0042] (2) Spray 650g of wood pulp with 1300g of propionic acid, and then activate it at 35°C for 3 hours;

[0043] (3) Mix the remaining propionic acid with proportioned propionic anhydride, acetic anhydride and catalyst, and cool the mixture to 10°C for use;

[0044] (4) Put the activated wood pulp in step (2) into the cooling liquid in step (3) within 8 minutes, fully stir without external cooling, and the reaction will naturally heat up, so that the temperature in the final esterification reaction system does not exceed 70°C , set the reaction time to 180min;

...

Embodiment 3

[0049] The preparation method of the high propionyl content cellulose acetate propionate mixed ester of the present embodiment specifically comprises the following steps:

[0050] (1) Weigh 650g of wood pulp, 2630g of propionic acid, 40g of acetic anhydride, 2070g of propionic anhydride, and 36g of catalyst. The catalyst is a mixture of liquid acid catalyst and heteropolyacid catalyst. 3 PW12 o 40 18g;

[0051] (2) Spray 650g of wood pulp with 650g of propionic acid, and then activate it at 30°C for 2 hours;

[0052] (3) Mix the remaining propionic acid with proportioned propionic anhydride, acetic anhydride, and catalyst, and cool the mixture to 5°C for use;

[0053] (4) Put the activated wood pulp in step (2) into the cooling liquid in step (3) within 6 minutes, fully stir without external cooling, and the reaction will naturally heat up, so that the temperature in the final esterification reaction system does not exceed 70°C , set the reaction time to 150min;

[0054] (...

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PUM

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Abstract

The invention relates to a preparation method of cellulose acetate propionate mixed ester with high propionyl content. Cellulose is prepared from the following components in parts by weight: 650g of wood pulp, 2630g of propionic acid, 40g of acetic anhydride, 2070g of propionic anhydride and 19.5-52g of a catalyst, wherein the ratio of a liquid acid catalyst to heteropolyacid catalyst is 4:6 to 6:4. The preparation method comprises the steps of activating, carrying out esterification reaction, mixing, adding a magnesium acetate solution, hydrolyzing and carrying out chromatography; and then, sequentially carrying out conventional filtration, washing and drying to obtain a finished product. The preparation method has the advantages that the finished product of cellulose acetate propionate, prepared by using the method, contains more than or equal to 46% of propionyl content and less than or equal to 2% of acetyl and is stable in performance; the catalyst is a mixture of liquid acid and heteropolyacid, so that the consumption of sulfuric acid is reduced, furthermore, corrosion to process equipment and environment pollution can be reduced, and the process safety can be improved; and meanwhile the heteropolyacid is additionally applied, so that the esterification reaction is accelerated, and hydrolysis reaction is more precise and controllable.

Description

technical field [0001] The invention belongs to the field of cellulose lipid derivatives, in particular to a kind of high propionyl content [0002] The preparation method of cellulose acetate propionate mixed ester. Background technique [0003] Cellulose acetate propionate (CAP for short) is a cellulose organic acid ester prepared by esterification of cellulose, acetic anhydride and propionic anhydride. CAP has excellent toughness, thermal stability and compatibility, and is widely used in auto parts, tool handles, radio and TV parts, steering wheels, films, filters, radio transistors, toys, wall and floor tiles, coatings, spinning and other industries . [0004] At present, the content of propionyl group in cellulose acetate propionate produced in China is relatively low and unstable. Chinese patent application number is: 201110009701.8 patent discloses a kind of preparation method of cellulose acetate propionate, this method uses cellulose as raw material, after activ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B3/16
Inventor 陈祥宋宇飞钱冬郭鹏程
Owner JIANGSU RUICHEN CHEM
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