Preparation method of optical cellulose triacetate

A cellulose triacetate, optical-grade technology, applied in the field of polymer chemistry, can solve problems such as insufficient viscosity, long dissolution time, uneven particles, etc., and achieve the effect of improving solubility, increasing degree of substitution, and fast dissolution

Active Publication Date: 2014-12-03
XIAN NORTH HUIAN CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the defects of existing cellulose triacetate, such as high ash content, high acidity, uneven particles, too long dissolution time, and insufficient viscosity, the purpose of the present invention is to provide a preparation method of optical grade cellulose triacetate, The method can reduce the ash content and acetic acid content of cellulose triacetate, improve the mechanical properties and optical properties of the cellulose triacetate film; and the obtained cellulose triacetate particles are uniform, dissolve quickly and have low viscosity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The degree of polymerization is 1200 refined cotton is pulverized with a refined cotton pulverizer, and the pulverized refined cotton is passed through a 20-mesh standard sieve;

[0036] The pulverized refined cotton is dried at 60°C, and the water content is below 5%;

[0037] At 20°C, add 1.5 parts by weight of glacial acetic acid to 1 part by weight of dried refined cotton, and activate it for 1 hour under stirring;

[0038] Under stirring, add 3.5 parts by weight of acetic anhydride, 0.005 parts by weight of 98% concentrated sulfuric acid and 4 parts by weight of glacial acetic acid to esterify for 3.5 hours, the esterification temperature is 45 ° C, and then add 0.016 parts by weight of Mass concentration is 2% magnesium acetate aqueous solution, react at 45 ℃ for 1 hour; Add 5 parts by weight of glacial acetic acid with a mass concentration of 90%, 0.05 parts by weight of hydrogen peroxide with a mass concentration of 30%, react at 45 ℃ After 1 hour, filter throu...

Embodiment 2

[0045] The refined cotton with a degree of polymerization of 1200 is pulverized with a refined cotton pulverizer, and the pulverized refined cotton is passed through a 20-mesh standard sieve;

[0046] The pulverized refined cotton is dried at 60°C, and the water content is below 5%;

[0047]At 25°C, add 2 parts by weight of glacial acetic acid to 1 part by weight of dried refined cotton, and activate it for 0.5 h under stirring;

[0048] Under stirring, add 3.6 parts by weight of acetic anhydride, 0.006 parts by weight of 98% concentrated sulfuric acid and 7 parts by weight of glacial acetic acid for 3 hours, the esterification temperature is 53 ° C, and then add 0.015 parts by weight of Mass concentration is 5% magnesium acetate aqueous solution, react at 53 ℃ for 0.5 hours; add 4.8 parts by weight of glacial acetic acid with a mass concentration of 90%, 0.04 parts by weight of hydrogen peroxide with a mass concentration of 30%, and react at 50 ℃ After 0.5 hour, filter throu...

Embodiment 3

[0054] The refined cotton with a polymerization degree of 1310 is pulverized with a refined cotton pulverizer, and the pulverized refined cotton is passed through a 20-mesh standard sieve;

[0055] The pulverized refined cotton is dried at 60°C, and the water content is below 5%;

[0056] At 30°C, add 2.5 parts by weight of glacial acetic acid to 1 part by weight of dried refined cotton, and activate it for 0.5 h under stirring;

[0057] Under stirring, add 4 parts by weight of acetic anhydride, 0.007 parts by weight of 98% concentrated sulfuric acid and 6 parts by weight of glacial acetic acid for esterification for 3 hours, the esterification temperature is 55 ° C, and then add 0.017 parts by weight of Mass concentration is 6% magnesium acetate aqueous solution, react at 55 ℃ for 0.5 hours; add 5.5 parts by weight of glacial acetic acid with a mass concentration of 90%, 0.03 parts by weight of hydrogen peroxide with a mass concentration of 30%, and react at 50 ℃ After 0.5 h...

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Abstract

The invention discloses a preparation method of optical cellulose triacetate, belonging to the technical field of high polymer chemistry. The method comprises the following steps of: (1) crushing of the refined cotton; (2) drying of the refined cotton; (3) activation; (4) esterification; (5) neutralization; (6) dilution and bleaching; (7) filtering, precipitation, wet crushing and washing; (8) drying; and (9) granulation. The method disclosed by the invention can reduce the ash content and acetic acid content of the cellulose triacetate and improve the mechanical properties and optical characteristics of a cellulose triacetate membrane; and the prepared cellulose triacetate has uniform particles and low viscosity and can be quickly dissolved.

Description

technical field [0001] The invention relates to a preparation method of optical-grade cellulose triacetate, belonging to the technical field of polymer chemistry. Background technique [0002] Cellulose acetate (Cellulose Acetate referred to as CA) is a cellulose acetate obtained by acetylating refined natural cellulose and acetic anhydride. Cellulose triacetate can be hydrolyzed to obtain cellulose diacetate and cellulose acetate ester. The degree of esterification is between 0 and 1, and the amount of combined acetic acid is 29.4%, which is called cellulose acetate (CMA for short); the degree of esterification is between 1 and 2, and the amount of combined acetic acid is 30.0~48.8 % is called cellulose diacetate (CDA for short); the degree of esterification is 2.5~3, and the amount of combined acetic acid is 57.5~62.5% is called cellulose triacetate (CTA for short); [0003] Cellulose triacetate film has excellent physical and mechanical properties (abrasion resistance a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B3/06
Inventor 赵双徐向前杨艳婷赵磊孙登林安忠维刘长增
Owner XIAN NORTH HUIAN CHEM IND CO LTD
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