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Cellulose triacetate and preparation method thereof

A technology of cellulose triacetate and cotton fiber, applied in the production of bulk chemicals, etc., which can solve problems such as difficulties in industrial application, industrialization of corrosion equipment, and the preparation process of undisclosed perfluorinated sulfonic acid-loaded solid superacid catalysts, etc. Achieve the effect of avoiding severe corrosion of equipment, avoiding environmental pollution problems, and realizing industrial utilization

Active Publication Date: 2022-02-22
JIANGSU RUICHEN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention uses perfluorinated sulfonic acid-supported solid superacid catalyst, which can recover the catalyst in subsequent steps. The catalyst or catalyst residue has little influence on acetylation, hydrolysis and subsequent processing steps, reducing the difficulty of post-processing , but the invention does not disclose the specific preparation process of perfluorinated sulfonic acid-supported solid superacid catalyst, but according to the preparation of the material known in the prior art, such as patent CN201511029289.0, the whole is relatively complicated and industrialized Difficult to apply
[0005] In view of the problems of catalyst pollution, equipment corrosion and industrialization difficulties existing in the prior art, it is urgent to find a kind of cellulose triacetate and its preparation method which is environmentally friendly, resource-saving and relatively simple and can be promoted in industrialization, and then prepared Cellulose triacetate with better performance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A preparation method of cellulose triacetate, comprising the following steps:

[0036] (1) Activation: After mixing 50 parts of cotton fiber A with 200 parts of glacial acetic acid and 1 part of catalyst, the reaction was activated at 25°C to obtain a homogenate;

[0037] (2) Acetylation: add 550 parts of acetyl chloride and 8 parts of catalyst to the homogenate, stir, heat up to 55°C, keep warm to make it fully react, after cooling down, filter to obtain solution A;

[0038] (3) Hydrolysis and post-treatment: add excess acetic acid to solution A, separate out a white precipitate, filter, wash, and dry to obtain cellulose triacetate;

[0039] Wherein, the catalyst is a solid acid catalyst, and the raw material of the catalyst specifically includes cotton fiber B, a sulfuric acid solution with a mass fraction of 15%, and a mixed solution of ferric chloride and ferric citrate. The specific preparation method of the catalyst includes: S1: making 5g cotton Fiber B was soak...

Embodiment 2

[0041] A preparation method of cellulose triacetate, comprising the following steps:

[0042] (1) Activation: After mixing 80 parts of cotton fiber A with 400 parts of glacial acetic acid and 2 parts of catalyst, the reaction was activated at 30°C to obtain a homogenate;

[0043] (2) Acetylation: Add 850 parts of acetic anhydride and 10 parts of catalyst to the homogenate, stir, heat up to 55°C, keep warm to make it react fully, and filter to obtain solution A after cooling down;

[0044] (3) Hydrolysis and post-treatment: add excess acetic acid to solution A, separate out a white precipitate, filter, wash, and dry to obtain cellulose triacetate;

[0045] Wherein, the catalyst is a solid acid catalyst, and the raw material of the catalyst specifically includes cotton fiber B, a sulfuric acid solution with a mass fraction of 20%, and a mixed solution of ferric chloride and ferric citrate. The specific preparation method of the catalyst includes: S1: making 10g cotton Fiber B w...

Embodiment 3

[0047] A preparation method of cellulose triacetate, comprising the following steps:

[0048] (1) Activation: After mixing 65 parts of cotton fiber A with 300 parts of glacial acetic acid and 1.6 parts of catalyst, the reaction was activated at 28°C to obtain a homogenate;

[0049] (2) Acetylation: Add 680 parts of acetyl chloride and 9 parts of catalyst to the homogenate, stir, heat up to 55°C, keep warm to make it fully react, and filter to obtain solution A after cooling down;

[0050] (3) Hydrolysis and post-treatment: add excess acetic acid to solution A, separate out a white precipitate, filter, wash, and dry to obtain cellulose triacetate;

[0051] Wherein, the catalyst is a solid acid catalyst, and the raw materials of the catalyst specifically include cotton fiber B, a sulfuric acid solution with a mass fraction of 18%, and a mixed solution of ferric chloride and ferric citrate. The specific preparation method of the catalyst includes: S1: making 8g cotton Fiber B wa...

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Abstract

The invention provides cellulose triacetate and a preparation method thereof, and relates to the field of cellulose preparation. The preparation method of the cellulose triacetate specifically comprises the steps of 1, conducting activation, specifically, mixing cotton fiber A with glacial acetic acid and a catalyst, then conducting reaction activation, and obtaining homogenate; (2) conducting acetylation, specifically, adding an acetylation reagent and a catalyst into the homogenate, stirring, heating, keeping the temperature for reaction, cooling, and filtering to obtain a solution A; and (3) conducting hydrolysis and post-treatment, specifically, adding excessive acetic acid into the solution A, separating out white precipitate, and then filtering, washing and drying to obtain cellulose triacetate, wherein the catalyst is a solid acid catalyst, and the raw materials of the catalyst specifically comprise cotton fibers B, a sulfuric acid solution and a mixed solution of ferric chloride and ferric citrate. The method is simple, feasible, environmentally friendly and capable of saving resources, and the prepared cellulose triacetate is excellent in overall performance and can be applied to membrane materials.

Description

technical field [0001] The invention relates to the field of cellulose preparation, in particular to cellulose triacetate and a preparation method thereof. Background technique [0002] Cellulose triacetate is usually obtained by activation and acetylation of cellulose. It has excellent thermoplasticity, ease of processing, optical properties and mechanical properties, and has a wide range of applications, including plastics, aerospace and reverse osmosis membranes. At present, the preparation methods of cellulose triacetate include homogeneous method and heterogeneous method, the former includes glacial acetic acid method, dichloromethane method and other solvent methods (such as ionic liquid, LiCl / DMAC solution), while the latter includes heterogeneous Phase solvent method and heterogeneous non-solvent method. At present, the most common method in the industry is the glacial acetic acid method, which usually uses cellulose as a raw material and uses a catalyst to prepare ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B3/06C08J5/18C08L1/12
CPCC08B3/06C08J5/18C08J2301/12Y02P20/54
Inventor 陈祥张勇杨旭忠郭鹏程
Owner JIANGSU RUICHEN CHEM