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Preparation method of medium-viscosity cellulose acetate butyrate

A technology of acetic acid butyric acid and cellulose ester, which is applied in the field of cellulose ester derivatives, can solve the problems of high cost, limited wide application, complex modification process operation, and unsatisfactory protection, and achieve stable product quality indicators and reliable Strong controllability and environment-friendly effect

Active Publication Date: 2014-04-09
JIANGSU RUICHEN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The cellulose acetate butyrate obtained by the above-mentioned prior art is white powder or solid. When dissolving, a large amount of solvent is needed to achieve the film-forming function. Solvent volatilization and emission are not good for environmental protection , Secondly, the coating is soft, the scratch resistance is poor, and the protection is not ideal
Therefore, Tan Zhuohua ([M] Guangdong University of Technology, 2008) modified it by solution polymerization to obtain acrylate-grafted butyl acetate cellulose, but the modification process is complicated and the high cost limits its wide application. application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Prepare medium viscosity cellulose acetate butyrate as follows:

[0034] 1) Put 5.75g of pulverized wood pulp in the activator, spray 3.5g of acetic acid and 2.3g of butyric acid on the wood pulp evenly, activate it at room temperature for 1 hour and wait for esterification;

[0035] 2) Mix 20.2g of butyric anhydride, 1.3g of acetic anhydride, 1.56g of butyric acid, and 0.13g of concentrated sulfuric acid and cool to -20°C;

[0036] 3) Put the activated wood pulp into the cooled mixed solution in step 2), keep the system temperature at 65°C, and esterify for 30min; then add 0.25g of magnesium acetate aqueous solution with a mass fraction of 30% to neutralize 40% Then, 11.5g of 67% acetic acid aqueous solution was added, the temperature of the control system was 60°C, and the hydrolysis time was 2h; after the hydrolysis, 0.38g of 30% magnesium acetate aqueous solution was added to neutralize the remaining 60% concentrated sulfuric acid, then add 150g of water to carry o...

Embodiment 2

[0038] Prepare medium viscosity cellulose acetate butyrate as follows:

[0039] 1) Put 5.75g of pulverized wood pulp in the activator, spray 1.44g of acetic acid and 1.44g of butyric acid on the wood pulp evenly, activate it at room temperature for 2 hours and wait for esterification;

[0040] 2) Mix 26g butyric anhydride, 1.3g acetic anhydride, 1.04g butyric acid and 0.2g concentrated sulfuric acid and cool to -20°C;

[0041] 3) Put the activated wood pulp into the cooled mixed solution in step 2), keep the temperature of the system at 60°C, and esterify for 30 minutes; then add 0.58 g of an aqueous solution of magnesium acetate with a mass fraction of 30% to neutralize 60% Then, 11.5g of 67% acetic acid aqueous solution was added, the temperature of the control system was 60°C, and the hydrolysis time was 2h; after the hydrolysis, 0.39g of 30% magnesium acetate aqueous solution was added to neutralize the system. The remaining 40% concentrated sulfuric acid is then added to...

Embodiment 3

[0043] Prepare medium viscosity cellulose acetate butyrate as follows:

[0044] 1) Put 5.75g of pulverized wood pulp in the activator, spray 1.6g of acetic acid and 1.28g of butyric acid on the wood pulp evenly, activate it at room temperature for 2 hours and wait for esterification;

[0045] 2) Mix 13g butyric anhydride, 1.3g acetic anhydride, 1.56g butyric acid and 0.2g concentrated sulfuric acid and cool to -20°C;

[0046] 3) Put the activated wood pulp into the cooled mixed solution in step 2), keep the temperature of the system at 55°C, and esterify for 180 minutes; then add 0.48 g of an aqueous solution of magnesium acetate with a mass fraction of 30% to neutralize 50 % concentrated sulfuric acid; then add 11.5 g of acetic acid aqueous solution with a mass fraction of 67%, control the temperature of the system to 65 °C, and the hydrolysis time is 2 h; after the hydrolysis is completed, add 0.48 g of a 30% mass fraction of magnesium acetate aqueous solution to neutralize ...

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Abstract

The invention discloses a preparation method of medium-viscosity cellulose acetate butyrate. The preparation method comprises the following steps of pulverizing wood pulp; uniformly spraying a mixture of acetic acid and butyric acid into the pulverized wood pulp, and activating for 1h to 6h at the normal temperature; cooling a mixture of acetic anhydride, butyric anhydride, butyric acid and a liquid acid catalyst to minus 5 DEG C to minus 20 DEG C for standby use; slowly throwing the activated wood pulp into the well-cooled mixture, and maintaining the temperature to be less than or equal to 65 DEG C; adding magnesium acetate solution into the reacted system, and adding 200 to 500 parts by weight of acetic acid with the mass percentage of 50 to 70 percent for hydrolysis, wherein the system temperature is controlled at 60 to 70 DEG C, and the hydrolysis time is 2h to 5h; continuing adding magnesium acetate to neutralize the liquid acid catalyst, and adding the material into water for chromatographic solid-liquid separation; washing the separated CAB (cellulose acetate butyrate) solids with water until the acid value is less than 300ppm, and drying the CAB solids to obtain the CBA finished product. Through the method, a method for preparing medium / high-viscosity CAB is developed, and the content of butyryl in CAB is 36 to 40 percent; the power viscosity is 400cps to 1000cps.

Description

technical field [0001] The invention belongs to the field of cellulose ester derivatives, in particular to a method for synthesizing and preparing medium-viscosity cellulose acetate butyrate. Background technique [0002] Cellulose acetate butyrate, also known as cellulose acetate butyrate, the English name is Cellulose acetate butyrate or cellaburate, referred to as CAB. The CAS registry number is 9004-36-8. [0003] Cellulose acetate butyrate has excellent moisture resistance, UV resistance, cold resistance, flexibility, transparency, electrical insulation and other properties, and has good compatibility with resins and high boiling point plasticizers, and can be used to make high transparency, weather resistance Good plastic base, film and leveling agent of various coatings, film-forming substances, etc. Such as production film base, aerial photographic film base, film, oilfield gas and other pipelines, tool handles, glass lamps for automobiles and airplanes, undergrou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B3/18C08B3/24C08B3/28
Inventor 陈祥张勇张杰郭鹏程钱冬
Owner JIANGSU RUICHEN CHEM
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