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Preparation method of high-stability carboxymethyl hydroxyethyl cellulose

A carboxymethyl hydroxyethyl, high-stability technology, applied in the field of cellulose production, can solve problems such as poor high-temperature stability, and achieve the effect of improving stability and storage performance

Inactive Publication Date: 2021-02-26
泸州北方纤维素有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention provides a kind of preparation method of high-stability carboxymethyl hydroxyethyl cellulose for overcoming the stability of the carboxymethyl hydroxyethyl cellulose produced by the existing technology, especially the poor high temperature stability, which comprises the following step:

Method used

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  • Preparation method of high-stability carboxymethyl hydroxyethyl cellulose

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preparation example Construction

[0041] Concrete, the preparation method of high stability carboxymethyl hydroxyethyl cellulose comprises the following steps:

[0042] A, sodium hydroxide and the mixed solvent of organic solvent-water are mixed, carry out alkali;

[0043]B. After alkalization, cool down, add refined cotton, and alkalization;

[0044] C, after alkalization finishes, add etherifying agent chloroacetic acid, heat up and carry out the etherification reaction of the first stage;

[0045] D, after the first stage etherification reaction finishes, cool, add acid to adjust the alkali concentration of the system to 10~20wt%;

[0046] E, then add etherification agent oxirane, heat up and carry out the second stage etherification reaction;

[0047] F. After the second-stage etherification reaction, cool down, add acid to neutralize the system until the pH of the system is 6.0-7.0, and then separate, wash, cross-link and dry to obtain high-stability carboxymethyl hydroxyethyl cellulose.

[0048] In st...

Embodiment 1

[0059] A. Add 3.0kg of caustic soda and 20kg of mixed solvent (3.0kg of water and 17.0kg of pure isopropanol) to a 50L reactor, stir and heat up to 55°C, and keep warm for 1.5h;

[0060] B. Cool down to 10-25°C, add 2.0kg of cotton powder, evacuate and replace 5 times, fill with nitrogen 0.15MPa, and alkalize at 20°C for 1.5h;

[0061] C. Add 2.0kg of chloroacetic acid solution (dissolve 1.2kg of chloroacetic acid in 0.8kg of isopropanol), raise the temperature for 30min to 65°C, keep the temperature for 1h, and carry out the first stage etherification reaction;

[0062] D. After the first stage etherification reaction is finished, cool down to 35° C., add 2.18 kg of glacial acetic acid for neutralization, and adjust the alkali concentration of the system to 12.03 wt %;

[0063] E. Then add 2.1kg etherification agent ethylene oxide, fill with nitrogen gas 0.20MPa, heat up for 35min to 80°C, keep warm for 3.0h, and carry out the second stage etherification reaction;

[0064] F...

Embodiment 2

[0066] A, add caustic soda 2.85kg, 18kg mixed solvent (3.6kg water and 14.4kg pure isopropanol) in the 50L reactor, stir and heat up to 70 ℃, heat preservation alkali 1h;

[0067] B. Cool down to 10-25°C, add 2.0kg of cotton powder, vacuumize and replace 4 times, fill with nitrogen gas 0.20MPa, and alkalize at 25°C for 2.5h;

[0068] C. Add 2.9kg of chloroacetic acid solution (dissolve 1.6kg of chloroacetic acid in 1.3kg of isopropanol), heat up for 35min to 60°C, keep warm for 2h, and carry out the first stage etherification reaction;

[0069] D. After the etherification reaction in the first stage is finished, cool down to 35° C., add 0.9 kg of glacial acetic acid for neutralization, and adjust the alkali concentration of the system to 17.67 wt %;

[0070] E. Then add 1.8kg etherification agent ethylene oxide, fill with nitrogen gas 0.30MPa, raise the temperature for 40min to 92°C, keep the temperature for 1.5h, and carry out the second stage etherification reaction;

[007...

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Abstract

The invention discloses a preparation method of high-stability carboxymethyl hydroxyethyl cellulose, and belongs to the technical field of cellulose production. In order to solve the problem of poor viscosity stability of carboxymethyl hydroxyethyl cellulose, the invention provides a preparation method of high-stability carboxymethyl hydroxyethyl cellulose, which comprises the following steps: cellulose activation reaction, first-stage etherification reaction, partial neutralization, second-stage etherification reaction, neutralization, washing, crosslinking and drying. Carboxymethylation reaction and hydroxyethylation reaction are carried out under different alkali concentration conditions, so that the uniformity of hydroxyl substitution at 2, 3 and 6 sites of glucose units is improved, the uniformity of the product is improved, and the stability of the viscosity of CMHEC under the conditions of normal temperature and high temperature is remarkably improved. And the application fieldof the CMHEC is expanded.

Description

technical field [0001] The invention belongs to the technical field of cellulose production, and in particular relates to a preparation method of high-stability carboxymethyl hydroxyethyl cellulose. Background technique [0002] Carboxymethyl hydroxyethyl cellulose (CMHEC) contains both carboxymethyl ions and hydroxyethyl nonionic cellulose mixed ethers in the cellulose molecular chain. It has both ionic cellulose and nonionic cellulose ethers. Features, good solubility, enzymolysis resistance, temperature resistance, salt tolerance and acid and alkali resistance, can effectively solve some complex problems in the drilling industry, such as the infringement of various minerals Na, Ca, chloride, etc. . [0003] CN200410012892.3 discloses a carboxymethyl hydroxyethyl cellulose production process, the process is: refined cotton powder through alkalization, carboxymethylation reaction, solid-liquid separation, secondary addition of alkali and alkalization, hydroxyethyl chemica...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B11/193
CPCC08B11/193
Inventor 周能武吕玉山高汕杨利芬
Owner 泸州北方纤维素有限公司
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