Cellulose acetate butyrate and preparation method thereof

A technology of acetic acid butyric acid and cellulose, applied in the field of cellulose lipid derivatives, can solve the problems of affecting product performance, shortening the service life of reaction devices, increasing production costs, etc., achieving low cost, improving activation efficiency, and reducing corrosion. Effect

Active Publication Date: 2020-05-19
JIANGSU RUICHEN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] But all use concentrated sulfuric acid as catalyzer in the prior art, and the cellulose acetate butyrate that it obtains contains a small amount of sulfuric acid ester, affects the performance of product, for example white latex paint wall turns yellow after a long time; In the cellulose process, the presence of concentrated sulfuric acid accelerates the corrosion of equipment and shortens the service life of the reaction device, thereby increasing production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] A kind of cellulose acetate butyrate with high butyryl content and preparation method thereof, described preparation method, comprises the following steps:

[0042] S1. Cellulose pretreatment: According to the mass ratio of 1:8, mix refined cotton with 5% phosphoric acid by mass, ball mill, filter, and rinse until the pH of the filtrate is 6.5-7 to obtain fibers with a particle size of 10 μm Prime 1;

[0043] S2. Cellulose activation: according to the mass ratio of 0.3:1, mix the cellulose 1 obtained in step S1 with butyric acid, mix well and transfer to a digestion tank, put the digestion tank into a microwave digestion reaction container, seal and vacuumize , filled with nitrogen, and digested with a microwave digestion instrument to obtain a digestion solution;

[0044] The output power of the microwave digestion is 500W, and the automatic heating program is as follows: the temperature is raised to 120°C within 2 minutes, kept at 120°C for 10 minutes, and the progra...

Embodiment 2

[0050] A preparation method of cellulose acetate butyrate with high butyryl content, comprising the following steps:

[0051] S1. Cellulose pretreatment: according to the mass ratio of 1:10, mix refined cotton with 3% phosphoric acid by mass, ball mill, filter, and rinse until the pH of the filtrate is 6.5-7 to obtain fibers with a particle size of 30 μm Prime 1;

[0052] S2. Cellulose activation: according to the mass ratio of 0.5:1, mix the cellulose 1 obtained in step S1 with butyric acid, mix well and transfer to a digestion tank, put the digestion tank into a microwave digestion reaction container, seal and vacuumize , filled with nitrogen, and digested with a microwave digestion instrument to obtain a digestion solution;

[0053] The output power of the microwave digestion is 500W, and the automatic heating program is as follows: the temperature is raised to 120°C within 4 minutes, and the temperature is kept at 120°C for 12 minutes. After the sample is cooled to 40°C, ...

Embodiment 3

[0059] A preparation method of cellulose acetate butyrate with high butyryl content, comprising the following steps:

[0060] S1. Cellulose pretreatment: According to the mass ratio of 1:9, mix refined cotton with 4% phosphoric acid by mass, ball mill, filter, and rinse until the pH of the filtrate is 6.5-7 to obtain fibers with a particle size of 20 μm Prime 1;

[0061] S2. Cellulose activation: according to the mass ratio of 0.4:1, mix the cellulose 1 obtained in step S1 with butyric acid, mix well and transfer to a digestion tank, put the digestion tank into a microwave digestion reaction container, seal and vacuumize , filled with nitrogen, and digested with a microwave digestion instrument to obtain a digestion solution;

[0062] The output power of the microwave digestion is 500W, and the automatic heating program is as follows: the temperature is raised to 120°C within 3 minutes, and the temperature is kept at 120°C for 11 minutes. After the sample is cooled to 40°C, t...

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Abstract

The invention discloses cellulose acetate butyrate and a preparation method thereof. The preparation method comprises the following steps that S1, cellulose pretreatment: mixing cellulose and phosphoric acid are mixed and performing ball milling, filtration and leaching to obtain cellulose 1; S2, cellulose activation: mixing the cellulose 1 obtained in the step S1 with butyric acid, and carrying out microwave digestion to obtain a digestion solution; S3, esterification reaction: sequentially adding butyric anhydride, acetic anhydride and a catalyst into the digestion solution obtained in the step S2, mixing the components, and carrying out esterification reaction to obtain a crude product; and S4, product precipitation and purification: carrying out precipitation, filtration, washing and drying on the crude product obtained in the step S3 to obtain the cellulose acetate butyrate. The method is high in yield and low in cost, the prepared cellulose acetate butyrate is high in butyryl content and good in performance and stability, meanwhile, cyclic utilization of waste water is achieved in the production process, and environmental pollution is reduced.

Description

technical field [0001] The invention belongs to the field of cellulose lipid derivatives, in particular to cellulose acetate butyrate with high butyryl content and a preparation method thereof. Background technique [0002] Cellulose acetate butyrate (abbreviated as CAB) is a cellulose organic acid ester prepared 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. It is ideal for contemporary automotive paints, motorcycle paints, furniture paints, inks, and pens. An important aid for the development of industry technology. [0003] At present, the preparation method of CAB is basically carried out according to the following steps: activate cellulose with acid, use concentrated sulfuric acid as a catalyst, carry out esterification in a mixed solution of acid and anhydride, and then go through proc...

Claims

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Application Information

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IPC IPC(8): C08B3/18
CPCC08B3/18
Inventor 陈祥张勇郭鹏程钱建强
Owner JIANGSU RUICHEN CHEM
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