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Preparation method of fluoro-ether carboxylic acid surfactant

A technology of surfactant and fluoroether carboxylic acid, which is applied in the field of preparation of fluoroether carboxylic acid surfactant, can solve problems such as the influence of processing and molding performance, and achieve the effect of eliminating residues

Inactive Publication Date: 2013-05-01
江苏梅兰化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, some researchers believe that the polymer particles obtained when the surfactant is polymerized with tetrafluoroethylene are not spherical, which will affect some processing properties.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Under normal pressure, add 150Kg of hexafluoropropylene into the reaction kettle at -40°C, turn on the ultraviolet lamp, adjust the frequency to 350nm, the intensity is 15kw, turn on the stirring, and feed oxygen into the reaction kettle (the flow rate is 12kg / h) and three Chlorofluoroethylene (flow rate: 5kg / h). After 3 hours of reaction, the material from the reactor is discharged to the middle tank to raise the temperature to recover hexafluoropropylene. Add 200kg of pure water to the hydrolysis kettle, turn on the UV lamp, adjust the frequency to 450nm, and the intensity is 25kw, start stirring, and add the fully recovered materials in the middle tank to the hydrolysis kettle at a rate of 8kg / min, and stop the reaction after 3 hours of reaction. The waste water in the hydrolysis kettle is discharged, and then 100 kg of pure water is added for washing, and the pure product of fluoroether carboxylic acid is obtained after washing three times.

Embodiment 2

[0012] Under normal pressure, add 450kg of hexafluoropropylene into the reaction kettle at -30°C, turn on the ultraviolet lamp, adjust the frequency to 350nm, the intensity is 20kw, turn on the stirring, and feed oxygen into the reaction kettle (the flow rate is 12kg / h) and three Chlorofluoroethylene (flow rate: 5kg / h). After 3 hours of reaction, the material from the reactor is discharged to the middle tank to raise the temperature to recover hexafluoropropylene. Add 200kg of pure water to the hydrolysis kettle, turn on the UV lamp, adjust the frequency to 450nm, and the intensity is 25kw, start stirring, and add the fully recovered materials in the middle tank to the hydrolysis kettle at a rate of 8kg / min, and stop the reaction after 3 hours of reaction. The waste water in the hydrolysis kettle is discharged, and then 100 kg of pure water is added for washing, and the pure product of fluoroether carboxylic acid is obtained after washing three times.

Embodiment 3

[0014] Under normal pressure, add 400kg of tetrafluoroethylene into the reaction kettle at -78°C, turn on the ultraviolet lamp, adjust the frequency to 350nm, the intensity is 10kw, start stirring, and feed oxygen into the reaction kettle (the flow rate is 12kg / h) and three Chlorofluoroethylene (flow rate: 5kg / h). After 3 hours of reaction, the material from the reactor is discharged to the middle tank to raise the temperature to recover hexafluoropropylene. Add 200kg of pure water to the hydrolysis kettle, turn on the UV lamp, adjust the frequency to 450nm, and the intensity is 25kw, start stirring, and add the fully recovered materials in the middle tank to the hydrolysis kettle at a rate of 8kg / min, and stop the reaction after 3 hours of reaction. The waste water in the hydrolysis kettle is discharged, and then 100 kg of pure water is added for washing, and the pure product of fluoroether carboxylic acid is obtained after washing three times.

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Abstract

The invention discloses a preparation method of a fluoro-ether carboxylic acid surfactant. A fluorine-containing olefin monomer, oxygen and a molecular weight regulator are initiated to carry out the photochemical reaction by ultraviolet light to generate fluoro-ether acyl chloride and fluoro-ether acyl fluoride at the temperature of -40 to -80 DEG C, fluoro-ether acyl chloride and fluoro-ether acyl fluoride are hydrolyzed under the radiation of ultraviolet light to generate fluoro-ether carboxylic acid, and the fluoro-ether carboxylic acid is washed and purified to obtain a fluoro-ether carboxylic acid finished product. Through the adoption of the preparation method, the completely nontoxic fluoro-ether carboxylic acid surfactant can be produced, and can serve as a dispersing agent to completely replace perfluoro caprylic acid during the fluorine-containing polymer production process.

Description

technical field [0001] The invention relates to a preparation method of a fluoroether carboxylic acid surfactant. Background technique [0002] As an excellent emulsifier for synthetic fluoropolymers, perfluorooctanoic acid has faced the fate of banning its use after causing serious pollution to the environment. However, the excellent properties of fluoropolymers are more and more widely used in the national economy. Therefore, how to find a surfactant that can replace PFOA in performance is an urgent and arduous task before us. At the Boao Forum in 2007, experts called on the organic fluorine industry to take the road of clean production, and the development of PFOA substitutes is imminent. It is currently known that DuPont's Zonyl-TBS (CF3CF2CF2CF2CF2CF2CH2CH2SO3) and trimer acid of perfluoropropylene oxide can be used in fluoropolymers, but Zonyl-TBS has a chain transfer effect and cannot be synthesized with higher molecular weight and ultra-high molecular weight. Fluo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/04
Inventor 李浩胡经宇钱厚琴
Owner 江苏梅兰化工有限公司
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