Preparation method of low-propionyl-content cellulose acetate propionate mixed ester

A technology of cellulose acetate propionate and low propionyl group is applied in the field of cellulose lipid derivatives, and can solve the problems of rare cellulose acetate propionate mixed ester, inaccurate control of hydrolysis reaction, long esterification reaction time, etc. Reduce corrosion and environmental pollution, increase application, and stabilize product performance

Inactive Publication Date: 2016-01-20
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
[0006] In addition, cellulose acetate propionate mixed esters with low propionyl content are currently used in some specific chemical fields, but it is rare to produce cellulose acetate propionate mixed esters with low propionyl content

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The preparation method of the low propionyl content cellulose acetate propionate mixed ester of the present embodiment specifically comprises the following steps:

[0034] (1) Weigh 650g of wood pulp, 296g of propionic acid, 2250g of acetic acid, 118g of acetic anhydride, 2070g of propionic anhydride, and 19.5g of catalyst. Polyacid Catalyst H 3 PW 12 o 40 11.7g;

[0035] (2) Spray 650g of wood pulp with 325g of acetic acid, and then activate it at 25°C for 0.5h;

[0036] (3) Mix the remaining acetic acid with propionic acid, propionic anhydride, acetic anhydride and catalyst, and cool the mixture to -10°C for use;

[0037] (4) Put the solid wood pulp activated 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 reaction system does not exceed 50 ℃, the reaction time is set to 90min;

[0038] (5) Add 45g of magnesium acetat...

Embodiment 2

[0042] The preparation method of the low propionyl content cellulose acetate propionate mixed ester of the present embodiment specifically comprises the following steps:

[0043] (1) Weigh 650g of wood pulp, 296g of propionic acid, 2250g of acetic acid, 118g of acetic anhydride, 2070g of propionic anhydride, and 52g of catalyst. Acid Catalyst H 3 PW 12 o 40 20.8g;

[0044] (2) Spray 650g of wood pulp with 1300g of acetic acid, and then activate it at 35°C for 3 hours;

[0045] (3) Mix the remaining acetic acid with propionic acid, propionic anhydride, acetic anhydride and catalyst, and cool the mixture to 5°C for use;

[0046] (4) Put the solid wood pulp activated 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 50 ℃, the reaction time is set to 120min;

[0047] (5) Add 50g of magnesium acetate s...

Embodiment 3

[0051] The preparation method of the low propionyl content cellulose acetate propionate mixed ester of the present embodiment specifically comprises the following steps:

[0052] (1) Weigh 650g of wood pulp, 296g of propionic acid, 2250g of acetic acid, 118g of acetic anhydride, 2070g of propionic anhydride, and 36g of catalyst. The catalyst is a mixture of liquid acid catalyst and heteropolyacid catalyst. Catalyst H 3 PW 12 o 40 18g;

[0053] (2) Spray 650g of wood pulp with 650g of acetic acid, and then activate it at 30°C for 2 hours;

[0054] (3) Mix the remaining acetic acid with propionic acid, propionic anhydride, acetic anhydride and catalyst, and cool the mixture to 5°C for use;

[0055] (4) Put the solid wood pulp activated 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 50 ℃, the react...

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Abstract

The invention relates to a preparation method of low-propionyl-content cellulose acetate propionate mixed ester. Cellulose is prepared from, by weight, 650 g of wood pulp, 296 g of propionic acid, 2250 g of acetic acid, 118 g of acetic anhydride, 2070 g of propionic anhydride and 19.5-52 g of catalysts. The ratio of liquid acid catalysts to heteropolyacid catalyst is between 4 to 6 and 6 to 4. The preparation method includes the steps of conducting activating, the esterification reaction, mixing, magnesium acetate solution adding, hydrolysis and chromatography, sequentially conducting conventional filtering, washing and drying, and obtaining the finished product. The method has the advantages that the propionyl content of the obtained cellulose acetate propionate finished product is 15-20%, and the acetyl content is smaller than 22-30%; the mixture of liquid acid and heteropolyacid is selected for the catalysts, and therefore the sulfuric acid consumption is lowered, the corrosion to a technological device and the pollution to the environment can be reduced, and technological safety is improved; meanwhile, by adding heteropolyacid, the esterification reaction is accelerated, and the 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 the domestic production of cellulose acetate propionate is relatively unstable, and the Chinese patent application number is: 201110009701.8 patent discloses a kind of preparation method of cellulose acetate propionate, this method is raw material with cellulose, wit...

Claims

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Application Information

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IPC IPC(8): C08B3/16
Inventor 陈祥宋宇飞钱冬郭鹏程
Owner JIANGSU RUICHEN CHEM
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