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Preparation method for acetic acid octanoic acid cellulose ester

A technology of cellulose ester and cellulose, which is applied in the field of preparation of cellulose acetate octanoate, can solve the problems of incomplete solid-phase reaction and long reaction time, and achieve the advantages of improved freeze-thaw stability, obvious viscosity drop, and short time-consuming Effect

Inactive Publication Date: 2018-01-05
福建鸿燕化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method does not use a catalyst to activate the esterification agent, and the esterification reaction of this method is carried out in a ball mill without microwave heating, so this method also has the disadvantages of long reaction time and incomplete solid phase reaction. question

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A preparation method of cellulose acetate caprylate, it comprises the following steps:

[0033] (1) Weigh 20g of acetic anhydride, 20g of n-octanoic acid and 0.5g of catalyst concentrated sulfuric acid, and mix and pre-react the three at 90°C for 1 hour to obtain a co-reactant;

[0034] (2) Put the cellulose into a mechanical activation reactor for pretreatment, control the ball milling speed to 350r / min, the ball milling temperature to 50°C, and the ball milling time to 60min to obtain the treated cellulose.

[0035] (3) Weigh 81g of cellulose treated in step (2), mix it with the co-reactant obtained in step (1), put it into a microwave reactor for reaction, control the microwave power to 300W, and the microwave time to 5min, to obtain Crude cellulose acetate octanoate;

[0036] (4) The crude cellulose acetate octanoate obtained in step (3) is washed, filtered under reduced pressure, and dried in an oven at 40-60° C. to obtain the cellulose acetate octanoate product. ...

Embodiment 2

[0039] A preparation method of cellulose acetate caprylate, it comprises the following steps:

[0040] (1) Weigh 20g of acetic anhydride, 30g of n-octanoic acid and 1g of catalyst concentrated hydrochloric acid, and mix and pre-react the three at 80°C for 1 hour to obtain a co-reactant;

[0041] (2) Put the cellulose into a mechanical activation reactor for pretreatment, control the ball milling speed to 300r / min, the ball milling temperature to 60°C, and the ball milling time to 90min to obtain the treated cellulose.

[0042](3) Weigh 102g of cellulose treated in step (2), mix it with the co-reactant obtained in step (1), put it into a microwave reactor for reaction, control the microwave power to 350W, and the microwave time to 10min, to obtain Crude cellulose acetate octanoate;

[0043] (4) The crude cellulose acetate octanoate obtained in step (3) is washed, filtered under reduced pressure, and dried in an oven at 40-60° C. to obtain the cellulose acetate octanoate produc...

Embodiment 3

[0046] A preparation method of cellulose acetate caprylate, it comprises the following steps:

[0047] (1) Weigh 20g of acetic anhydride, 40g of n-octanoic acid and 1g of catalyst nitric acid, and mix and pre-react the three at 70°C for 80min to obtain a co-reactant;

[0048] (2) Put the cellulose into a mechanical activation reactor for pretreatment, control the ball milling at 400r / min, the ball milling temperature at 70°C, and the ball milling time for 50min to obtain the treated cellulose.

[0049] (3) Weigh 183g of cellulose treated in step (2), mix it with the co-reactant obtained in step (1), put it into a microwave reactor for reaction, the microwave power is 400W, and the microwave time is 5min to obtain acetic acid Crude cellulose caprylate;

[0050] (4) The crude cellulose acetate octanoate obtained in step (3) is washed, filtered under reduced pressure, and dried in an oven at 40-60° C. to obtain the cellulose acetate octanoate product.

[0051] The degree of sub...

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PUM

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Abstract

The invention discloses a preparation method for acetic acid octanoic acid cellulose ester, and relates to the technical field of cellulose modification. The preparation method comprises the followingsteps: carrying out mixing reaction on acetic anhydride, n-caprylic acid and catalyst to obtain coreaction agent; carrying out mechanical activation preprocessing on cellulose; putting the obtained coreaction agent and the processed cellulose into microwave reaction equipment to react to obtain the crude product of the acetic acid octanoic acid cellulose ester; carrying out post-processing on theobtained crude product of the acetic acid octanoic acid cellulose ester to obtain an acetic acid octanoic acid cellulose ester product. The preparation method has the advantages of short reaction time and high reaction efficiency, and the preparation process of the cellulose ester is shortened to 1-2h from 5-10h of a traditional liquid phase method. The prepared acetic acid octanoic acid cellulose ester is high in substitution degree, and the cellulose ester with the high substitution degree is prepared under a condition of short microwave time.

Description

technical field [0001] The invention relates to the technical field of cellulose modification, in particular to a preparation method of cellulose acetate octanoate. Background technique [0002] With the rapid development of the human economy, non-renewable resources such as petroleum on the earth are increasingly depleted, and the research on finding renewable resources to replace part of petroleum resources has become a topic of common concern to scholars at home and abroad. Cellulose is the most abundant natural renewable resource in nature and an inexhaustible natural polymer raw material. However, the molecular structure of cellulose is complex, there are crystalline regions and amorphous regions, and the molecules in the crystalline regions are tightly arranged, making it difficult for water, enzymes and chemical reagents to enter, and the reactivity is extremely low, so it must be modified. Cellulose esters Hydrogenation is one of the important cellulose modification...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B3/16C08B1/02
Inventor 陆享鸿陆享旗袁宜恩
Owner 福建鸿燕化工有限公司
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