Preparation method of cationic hydroxyethyl cellulose ether

A technology of hydroxyethyl cellulose and hydroxyethylation, which is applied in the field of preparation of fine functional polymer materials, can solve the problems of high salt and monomer residues, high technical requirements for post-processing, and high material consumption, and achieves simplified process and post-processing. Treatment process, to achieve the effect of overall consumption reduction and production cost reduction

Inactive Publication Date: 2012-03-28
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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Problems solved by technology

[0004] In industrial production, the cationization reaction of cellulose generally adopts a heterogeneous reaction system. The heterogeneous reaction technology has better practical control and economic feasibility, but the efficiency is low (only 50%) and the material consumption is high. High salt and monomer residues in the product require high post-processing technology, which ultimately directly affects the application properties of the product
Therefore, the present invention aims at the low reaction efficiency and high material consumption in the current industrial cation production, which is not conducive to the realization of the goal of increasing efficiency, reducing consumption and saving energy, and develops a new process method for activated cationization reaction to improve reaction efficiency and simplify Post-processing process to achieve the purpose of overall consumption reduction, energy saving and emission reduction

Method used

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  • Preparation method of cationic hydroxyethyl cellulose ether
  • Preparation method of cationic hydroxyethyl cellulose ether
  • Preparation method of cationic hydroxyethyl cellulose ether

Examples

Experimental program
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Effect test

Embodiment 1

[0031] (1) Pretreatment: At normal temperature and pressure, add hydroxyethyl cellulose (industrial product, hydroxyethyl substitution degree DS is 1.6, 25°C, 1 part of a 2% aqueous solution with a viscosity of 400 mPa·s), and 0.75 part of a 25% sodium hydroxide solution, stirred and reacted at 25°C for 30 minutes to obtain a mixed solution A;

[0032] (2) Cationic reaction: adjust the temperature of solution A to 60°C, add 0.70 parts of 69% CTA aqueous solution, and react at constant temperature for 4 hours to obtain mixed solution B;

[0033] (3) Post-treatment: Liquid B is cooled to room temperature 30°C, adjusted to pH 7 with 10% hydrochloric acid by mass percentage, and filtered, and the filtrate is extracted for 4 hours with ethanol and isopropanol recovery liquid obtained through filtration, After drying, the cationized hydroxyethyl cellulose ether product is obtained.

[0034] (4) Calculation of degree of substitution DS and reaction efficiency Re:

[0035] Determine...

Embodiment 2～10

[0041] The basic operation process of Examples 2-10 is the same as that of Example 1, and the amount of each substance added and the reaction conditions are as shown in Table 1.

Embodiment 11～14

[0047] The basic operation process of Examples 11-14 is the same as that of Example 1, and the amount of each substance added and the reaction conditions are as shown in Table 2.

[0048] The reaction substance proportioning and condition of table 2 embodiment 11~14

[0049]

[0050]

[0051]According to the calculation method of cationic substitution degree and reaction efficiency given in the present invention, the results of cationic substitution degree and corresponding reaction efficiency of the products obtained in Examples 1-14 and Comparative Example A and Comparative Example B are shown in Table 3.

[0052] Table 3 Embodiment 1~14 and comparative examples A~B, DS and Re calculation result

[0053]

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Abstract

The invention discloses a preparation method of cationic hydroxyethyl cellulose ether. The method comprises the following steps: adding 1 part of hydroxyethyl cellulose, 0.6-0.8 part of 20-35wt% sodium hydroxide solution and 0-0.5 part of amine alkali coactivator in a mixed solution composed of 0-5 parts of absolute alcohol and 0-5 parts of isopropanol and stirring at 10-45 DEG C for 20-60 minutes to obtain liquid A; stirring the liquid A while controlling the temperature to 30-80 DEG C, adding 0.6-1.4 parts of cationic etherifying agent to react for 3-5h to obtain liquid B; cooling the liquid B to 25-35 DEG C, adjusting the pH value, filtering, extracting and drying to obtain the cationic hydroxyethyl cellulose ether. The cationic substitution degree of the method is 0.30-0.50, the cationic reaction efficiency is 42%-75%, the technological process does not require other intermediate links, the production cost is reduced and energy saving and emission reduction are realized in the production process.

Description

technical field [0001] The present invention relates to a preparation method of cationic hydroxyethyl cellulose ether, in particular to the cationic reaction of hydroxyethyl cellulose with cationic etherification agent to obtain cationic hydroxyethyl cellulose ether products with different degrees of substitution The process belongs to the field of preparation of fine functional polymer materials. Background technique [0002] Cationic hydroxyethyl cellulose ether is one of the important cellulose ether varieties. It is a general term for a series of cationic polymers obtained by cationizing hydroxyethyl cellulose with quaternary ammonium salts. It is also an important polysaccharide cationic surfactant. It has Excellent conditioning, moisturizing, film-forming, compounding stability and easy rinsing functions, as well as excellent water solubility, pH stability and biocompatibility, etc., are widely used in daily chemicals, fragrances, textiles, paper, Traditional technolo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B11/193
Inventor 陈玉放李伟
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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