Preparation method of high-molecular-weight cellulose acetate butyrate

A technology of acetic acid butyric acid and high molecular weight, which is applied in the field of preparation of high molecular weight cellulose acetate butyrate, can solve the problems of high cost, high metal content, high viscosity of reaction liquid, etc., reduce operating time, reduce waste water discharge, and reduce production cost effect

Active Publication Date: 2021-03-19
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN110642954A adopts the method of hydrogenolysis to remove the acyl group of cellulose acetate butyrate so as to obtain high hydroxyl content cellulose acetate butyrate, but this method needs to use noble metal palladium catalyst, the cost is higher, and high molecular weight cellulose acetate butyrate The viscosity of the reaction solution is high, and the separation and recovery of the solid catalyst is difficult, resulting in high metal content in the cellulose acetate butyrate product, so this method is not suitable for the preparation of high molecular weight cellulose acetate butyrate
[0005] In summary, in the current hydrolysis process of cellulose acetate butyrate, directly adding water or palladium-catalyzed hydrogenation is not conducive to the preparation of high molecular weight cellulose acetate butyrate. Therefore, it is necessary to find a new process to solve the existing problems. Various deficiencies in the technology

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Prepare cellulose acetate butyrate as follows:

[0040] (1) Use a pulverizer to pulverize the refined cotton, take 100g of the pulverized 100-200 mesh sieve, put it in a beaker, add 1000g of acetic acid, mix well, soak for 10h, and then centrifuge to remove part of the solution to obtain acetic acid content of 40.5 The activated cellulose powder 168g of wt%.

[0041](2) Weigh 55g of acetic anhydride, 600g of butyric anhydride, 200g of n-butyric acid, and 5g of concentrated sulfuric acid into a 3L jacketed glass kettle, then add the above-mentioned 168g of activated cellulose powder, stir and control the temperature at 20°C, and keep it warm for 10 hours, the esterification reaction solution was obtained.

[0042] (3) Add 4.3 g of sodium acetate into the esterification reaction solution, control the temperature at 20° C. under stirring, and stop the reaction after 20 minutes to obtain a neutralization reaction solution.

[0043] (4) Add 5 g of sodium triacetoxyborohydr...

Embodiment 2

[0046] Prepare cellulose acetate butyrate as follows:

[0047] (1) Use a pulverizer to pulverize the refined cotton, take 100g of the pulverized 100-200 mesh sieve, put it in a beaker, add 2500g of acetic acid, mix well, soak for 5h, and then centrifuge to remove part of the solution to obtain 60wt of acetic acid % activated cellulose powder 250g.

[0048] (2) Weigh 185g of acetic anhydride, 450g of butyric anhydride, 600g of n-butyric acid, and 25g of concentrated sulfuric acid into a 3L jacketed glass kettle, then add the above-mentioned 250g of activated cellulose powder, stir and control the temperature at 30°C, and keep it warm for 5 hours, the esterification reaction solution was obtained.

[0049] (3) Add 30.8 g of sodium acetate to the above-mentioned esterification reaction liquid, control the temperature at 30° C. under stirring, stop the reaction after 30 min, and obtain a neutralization reaction liquid.

[0050] (4) Add 12 g of sodium triacetoxyborohydride to the...

Embodiment 3

[0053] Prepare cellulose acetate butyrate as follows:

[0054] (1) Use a pulverizer to pulverize the refined cotton, take 100g of the pulverized 100-200 mesh sieve, put it in a beaker, add 4500g of acetic acid, mix well, soak for 1h, and then centrifuge to remove part of the solution to obtain acetic acid content of 51.5 206g of activated cellulose powder by wt%.

[0055] (2) Weigh 300g of acetic anhydride, 120g of butyric anhydride, 1000g of n-butyric acid, and 50g of concentrated sulfuric acid into a 3L jacketed glass kettle, then add the above-mentioned 206g of activated cellulose powder, control the temperature at 40°C under stirring, and keep it warm for 3h , to obtain an esterification reaction solution.

[0056] (3) Add 82 g of sodium acetate to the above-mentioned esterification reaction solution, control the temperature at 40° C. under stirring, and stop the reaction after 60 minutes to obtain a neutralization reaction solution.

[0057] (4) Add 30 g of sodium triac...

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Abstract

The invention discloses a preparation method of high-molecular-weight cellulose acetate butyrate, which comprises the steps of 1) conducting activation, specifically, soaking cellulose powder in acetic acid to obtain activated cellulose powder; 2) conducting esterification, specifically, enabling the activated cellulose powder to react with acetic anhydride and butyric anhydride under the condition of an acid catalyst to obtain an esterification reaction solution; 3) conducting neutralization, specifically, adding a neutralizer into the esterification reaction liquid to neutralize the acid catalyst into salt; and 4) conducting reduction, specifically, adding sodium triacetoxyborohydride into the neutralized esterification reaction solution to partially reduce the ester group into hydroxyl,thereby obtaining the high-molecular-weight cellulose acetate butyrate. The method avoids cellulose acetate butyrate glucose unit breakage and molecular degradation caused by hydrolysis by adding water, and also avoids the problems of difficult separation and high metal content caused by adding a heterogeneous catalyst.

Description

technical field [0001] The invention relates to cellulose acetate butyrate, in particular to a preparation method of high molecular weight cellulose acetate butyrate. Background technique [0002] Cellulose acetate butyrate (abbreviated as CAB) is a kind of cellulose mixed ester, which is mainly used in automobile paint, leather brightener, ink, wood paint, motorcycle paint, plastic, thermosetting powder coating, etc. In the car finish varnish, CAB plays an irreplaceable role. In the car primer, metal flakes such as aluminum powder should be used as pigments, and the metal flakes should be oriented parallel to the substrate; CAB is used in car refinish paint systems. It can shorten the drying time, resist cold cracking, and has good polishing performance. [0003] High molecular weight cellulose acetate butyrate has a high melting point and better alcohol resistance, and the thermoplastic film prepared by using it has higher strength and toughness and better mechanical prop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B3/18C08B3/22
CPCC08B3/18C08B3/22Y02P20/584
Inventor 崔乾余炎冰于冠群何金同刘超牟通黎源
Owner WANHUA CHEM GRP CO LTD
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