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Method of synthesizing sodium p-perfluorous nonenoxybenzenesulfonate

A technology of sodium oxybenzenesulfonate and sodium hydroxybenzenesulfonate, which is applied in the field of synthesis of sodium perfluorononoxybenzenesulfonate, can solve the problems of high product quality, many waste acids, and many process steps, and achieve The effect of short process route and mild reaction conditions

Inactive Publication Date: 2007-09-12
JUHUA GROUP TECH CENT +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problems of many process steps, complex sulfonation process, and many waste acids in the prior art, the present invention provides a simple process route, few steps, mild reaction conditions, avoiding the use of dangerous substance oleum, and improving product quality. Not less than the synthetic method of perfluoronon(enyl)oxybenzene sulfonate sodium of traditional multi-step method

Method used

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  • Method of synthesizing sodium p-perfluorous nonenoxybenzenesulfonate
  • Method of synthesizing sodium p-perfluorous nonenoxybenzenesulfonate
  • Method of synthesizing sodium p-perfluorous nonenoxybenzenesulfonate

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Effect test

Embodiment 1

[0021] Add 21g of sodium p-hydroxybenzenesulfonate and 150ml of DMF into a 250ml four-necked glass flask, stir and raise the temperature to 20°C. After dissolving, add 45g of hexafluoropropylene trimer, reflux the system with a condenser tube, and add 14g of triethylamine dropwise. The dropwise addition was completed in about half an hour, and the reaction was continued at the temperature for 3 hours. After cooling, it was poured into 400ml of water, salted out with NaCl, filtered and dried to obtain the product.

Embodiment 2

[0023] Add 21g of sodium p-hydroxybenzenesulfonate into a 250ml four-neck glass flask, fully dissolve it in tetrahydrofuran, stir and raise the temperature to 30°C, after the sodium hydroxybenzenesulfonate is dissolved, add 45g of hexafluoropropylene trimer, and use a condenser tube to Reflux, add 10 g of dimethylamine dropwise, the dropwise addition is completed in about half an hour, continue to maintain the temperature for 3 hours, after cooling, pour into 400ml of water, salt out with NaCl, filter and dry to obtain the product.

Embodiment 3

[0025] Add 21g of sodium p-hydroxybenzenesulfonate into a 250ml four-necked glass flask, fully dissolve it in dimethyl sulfite, stir and raise the temperature to 30°C, after the sodium hydroxybenzenesulfonate is dissolved, add 45g of hexafluoropropylene trimer, and the system Use a condenser to reflux, add 20 g of diamylamine dropwise, and the dropwise addition is completed in about half an hour. Continue to maintain the temperature for 3 hours. After cooling, pour into 400ml of water, salt out with NaCl, filter and dry to obtain the product.

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Abstract

This invention discloses a method for synthesizing perfluorinated azelaic(en) sybthesis of benzene sodium sulfophenylate including: solving hexafluoropropylene trimer in a polarity solvent, adding p-hydroxybenzoic sodium sulfophenylate reacting the hexafluoropropylene trimer completely and adding a catalyst to control the reaction temperature to get a rough product of perfluorinated azelaic(en) sybthesis of benzene sodium sulfophenylate, which is separated from the solution.

Description

technical field [0001] The invention relates to a method for synthesizing sodium perfluoronon(enyl)oxybenzenesulfonate. Background technique [0002] Sodium perfluoronon(enyl)oxybenzenesulfonate is a fluorocarbon surfactant with low surface tension and critical micelle concentration, acid and alkali resistance, and can still maintain good surface activity in strong acid and strong alkali , mainly used in fluoroprotein fire extinguishing agent, nickel plating brightener, metal etchant, detergent, leveling agent for color film and as dispersant for polymerization in the resin polymerization process, widely used in oil fields, fire protection, leather, Electroplating, papermaking and other fields. [0003] Regarding the synthetic method of perfluorononyloxybenzenesulfonate sodium, the patents (JP51011084 and JP57164199) applied by Japan Shin Nitto Chemical and Japan NEOSKK Company, its synthetic process route is: perfluorononylphenyl ether uses hair Sulfonated with nicotinic ...

Claims

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Application Information

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IPC IPC(8): C07C309/42
Inventor 雷志刚王树华
Owner JUHUA GROUP TECH CENT
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