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A kind of preparation method of acetyl butyryl cellulose

A technology of acetyl butyryl and cellulose, which is applied in the field of polymer chemistry, can solve the problems of non-conformity with green chemistry, difficulty in realizing industrialization, and low butyryl content, and achieve environmental protection and sustainable economic development. Environmental friendliness and low reaction temperature

Active Publication Date: 2018-01-09
中山大桥化工集团有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the acetyl butyryl cellulose developed in China, the content of butyryl is low and unstable, the consumption of raw materials is large, the cost is high, the reaction time is long, the reaction temperature is high, the controllability is poor, and the waste generated by the reaction is large, which is not easy to recycle. Does not conform to the concept of green chemistry and is difficult to realize industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Acetyl butyryl cellulose was prepared as follows:

[0036] (1) Put 10g of cotton pulp in a beaker, add 50g of acetic acid, seal it, soak it at room temperature for 0.5 days, and filter out excess acetic acid;

[0037] (2) Put the soaked cotton pulp, 40g of butyric anhydride, and 1g of catalyst in a three-necked flask equipped with a condenser and mechanical stirring, and stir at 70°C for 0.5h;

[0038] (3) Add 0.5g of catalyst, then add 20g of acetic anhydride, and continue to stir and react at 70°C for 0.5h;

[0039] (4) Add 0.5g catalyst and continue to stir and react at 70°C for 0.5h;

[0040] (5) Cool the product obtained in step (4) to room temperature, add 50 g of hexane into the flask under rapid stirring, and stir for 0.5 h to obtain a suspension;

[0041] (6) Filtrate the suspension, soak the obtained solid powder in 100g of 1wt% sodium bicarbonate solution for 1 hour, filter again, wash the product with deionized water until neutral, and finally dry, pulveri...

Embodiment 2

[0045] Acetyl butyryl cellulose was prepared as follows:

[0046] (1) Put 10g of wood pulp in a beaker, add 100g of acetic acid, seal it, soak it at room temperature for 2 days, and filter out excess acetic acid;

[0047] (2) Put the soaked wood pulp, 20g of butyric anhydride, and 2g of catalyst in a three-necked flask equipped with a condenser and mechanical stirring, and stir at 50°C for 1 hour;

[0048] (3) Add 1g of catalyst, then add 15g of acetic anhydride, and continue to stir and react at 50°C for 1h;

[0049] (4) Add 1g of catalyst and continue to stir and react at 50°C for 1h;

[0050] (5) Cool the product obtained in step (4) to room temperature, add 100 g of hexane into the flask under rapid stirring, and stir for 1 hour to obtain a suspension;

[0051] (6) Filtrate the suspension, soak the obtained solid powder in 200g of 0.5wt% sodium bicarbonate solution for 0.5h, filter again, wash the product with deionized water until neutral, and finally dry, pulverize, an...

Embodiment 3

[0055] Acetyl butyryl cellulose was prepared as follows:

[0056] (1) Put 10g of bamboo pulp in a beaker, add 60g of acetic acid, seal it, soak it at room temperature for 7 days, and filter out excess acetic acid;

[0057] (2) Put the soaked bamboo pulp, 60g of butyric anhydride, and 1.5g of catalyst in a three-necked flask equipped with a condenser and mechanical stirring, and stir at 60°C for 0.8h;

[0058] (3) Add 0.8g of catalyst, then add 30g of acetic anhydride, and continue to stir and react at 60°C for 1h;

[0059] (4) Add 0.7g catalyst and continue to stir and react at 60°C for 0.5h;

[0060] (5) Cool the product obtained in step (4) to room temperature, add 80 g of hexane into the flask under rapid stirring, and stir for 1 hour to obtain a suspension;

[0061] (6) Filtrate the suspension, soak the obtained solid powder in 150g of 1wt% sodium bicarbonate solution for 0.5h, filter again, wash the product with deionized water until neutral, and finally dry, pulverize, a...

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Abstract

The invention belongs to the technical field of polymer chemistry, and particularly relates to a method for preparing acetyl butyryl cellulose. The method comprises the following steps: soaking and activating cellulose with acetic acid; conducting a heat reaction on the activated cellulose, butyric anhydride and a catalyst; adding the catalyst and acetic anhydride; adding the catalyst; cooling to room temperature after the reaction is completed; adding hexane; and performing filtering, sodium bicarbonate solution soaking, deionized water washing, drying, grinding and other steps to obtain the acetyl butyryl cellulose. By adopting the method, the acetyl butyryl cellulose with high butyl content can be obtained, the content of butyryl can be 55 percent or more, and the product has stable quality; the catalyst is fractionally added, so that the degradability of cellulose is effectively reduced, and the average molecular weight of the product is high; excessive acetic anhydride, butyric anhydride, acetic acid and butyric acid can be recycled, so that environmental protection and sustainable development of economy can be favored.

Description

technical field [0001] The invention belongs to the technical field of polymer chemistry, and in particular relates to a preparation method of acetyl butyryl cellulose. Background technique [0002] With the progress of society, more and more synthetic polymer materials are used in daily life. Due to their non-biodegradability or long time for degradation, it has caused a non-negligible damage to the natural environment on which human beings depend. Negative effects, people urgently need to find new polymer materials. Natural polymer materials are renewable, and their development and application have gradually become a hotspot in scientific research and production. The hydrophilic nature of cellulose makes them incompatible with lipophilic resins, reducing the mechanical properties of the composites. Therefore, the modification of cellulose is particularly important, and acetyl butyryl cellulose is one of them. [0003] Acetyl butyryl cellulose is a modified cellulose pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B3/18C08B3/02C08B3/28
CPCC08B3/02C08B3/18C08B3/28
Inventor 王明晶刘欣王念贵刘玉娇张俐娜
Owner 中山大桥化工集团有限公司
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