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Cellulose acetate butyrate mixed ester with high butyryl content, and preparation method thereof

A technology of cellulose mixed ester and acetic acid butyric acid is applied in the preparation of cellulose acetate butyrate mixed ester and the field of cellulose acetate butyrate mixed ester, which can solve the problem of low cellulose efficiency, low butyryl content, long reaction time, etc. problem, to achieve the effect of less dosage, good effect and short preparation period

Inactive Publication Date: 2015-02-25
JIANGSU RUICHEN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the production of cellulose has low efficiency, low butyryl content, high reaction temperature and long reaction time

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A cellulose acetate butyrate mixed ester with high butyryl content comprises the following components: 600 kg of wood pulp, 980 kg of butyric acid, 2745 kg of butyric anhydride, 24 kg of acetic anhydride, and 30 kg of concentrated sulfuric acid catalyst.

[0029] The above method for preparing cellulose acetate butyrate mixed ester with high butyryl content is innovative in that it specifically comprises the following steps:

[0030] (1) The proportioned wood pulp is first sprayed with 370kg of butyric acid, and then activated at 25°C for 12 hours to become solid;

[0031] (2) Mix the remaining amount of butyric acid with the matching amount of butyric anhydride, acetic anhydride, and concentrated sulfuric acid catalyst, and cool the mixture to 3°C for use;

[0032] (3) Put the activated solid in step (1) into the cooling liquid of step (2) within 5 minutes, stir fully, adjust the cooling amount of the cooling liquid to control the reaction heating rate, so that the tem...

Embodiment 2

[0038] On the basis of embodiment 1, change the content of the concentrated sulfuric acid catalyst in the composition, specifically as follows: wood pulp 600kg, butyric acid 980kg, butyric anhydride 2745kg, acetic anhydride 24kg, 60kg concentrated sulfuric acid catalyst. Adopt the preparation method of embodiment 1 to prepare, obtain product.

[0039] In this example, cellulose acetate butyrate with a butyryl content of 52% and an acetyl content of 2.5% was obtained, and the product performance was stable.

Embodiment 3

[0041] On the basis of Example 1 or 2, using the ratio of raw materials in Example 1 or 2, the wood pulp in the raw material is pulverized to ensure that the length of the short fluff after pulverization is ≤ 1mm, and the hydrolysis reaction process is controlled before the start of the process. , Control the initial water content of the reaction system at 5% to 10%. Adopt the preparation method of embodiment 1 to prepare, obtain product.

[0042] In this example, cellulose acetate butyrate with a butyryl content of 52% and an acetyl content of 3% was obtained, and the product performance was stable.

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Abstract

The invention discloses cellulose acetate butyrate mixed ester with high butyryl content, and a preparation method thereof. The cellulose ester is prepared from the following components in parts by weight: 600 parts of wood pulp, 800-1200 parts of butyric acid, 2500-3500 parts of butyric anhydride, 20-40 parts of acetic anhydride, and concentrated sulfuric acid catalyst accounting for 5-10% of total weight parts of wood pulp. The preparation method comprises the following steps: activating, performing esterification reaction, mixing, adding magnesium acetate solution, hydrolyzing, performing chromatography, and then sequentially conventionally filtering, washing and drying to obtain a finished product. According to cellulose acetate butyrate mixed ester with high butyryl content, cellulose acetate butyrate with the butyryl content of 48-53% and acetyl content of less than or equal to 4% can be obtained after the combination according to specific formula and proportion, and the product is stable in performances. The preparation method is simple in steps, the preparation period is short, the preparation conditions are not strict and easily achieved, and especially, the activated solid is fed into a cooling liquid within 2-5min, so that the quality of products can be guaranteed while the fast follow-up reaction is guaranteed.

Description

technical field [0001] The invention relates to a cellulose acetate butyrate mixed ester with high butyryl content, and also relates to a preparation method of the cellulose acetate butyrate mixed ester with high butyryl content, belonging to the field of cellulose lipid derivatives. Background technique [0002] Cellulose acetate butyrate (abbreviated as CAB) is a cellulose organic acid ester obtained by esterification of cellulose, acetic anhydride and butyric anhydride. CAB is compatible with a variety of synthetic resins, has good flexibility, cold resistance, leveling, and color retention, and is anti-aging and non-yellowing. An important aid for the development of industry technology. [0003] At present, the content of butyryl in cellulose acetate butyrate produced in China is relatively low and unstable. Chinese patent application number is: the patent of 200810106426.X discloses a kind of method for preparing cellulose acetate propionate or cellulose acetate butyr...

Claims

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Application Information

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IPC IPC(8): C08B3/18
Inventor 陈祥张勇张杰钱冬郭鹏程
Owner JIANGSU RUICHEN CHEM
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