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A kind of long-chain perfluoropolyether surfactant and preparation method thereof

A technology of surfactants and perfluoropolyether, which is applied in chemical instruments and methods, fire prevention equipment, transportation and packaging, etc., can solve problems such as poor product purity, difficult product separation, and impact on fire extinguishing performance, and achieve good environmental protection effects , The equipment requirements are simple, and the effect of burning resistance is long

Active Publication Date: 2019-01-11
龙岩思康新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the synthesis cost of long-chain fluorocarbon surfactants in the industry is relatively high, and catalysts are required. It is difficult to separate the products in the later stage, and the purity of the products is not good, which affects the fire extinguishing performance.

Method used

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  • A kind of long-chain perfluoropolyether surfactant and preparation method thereof
  • A kind of long-chain perfluoropolyether surfactant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] Add 2.0 moles of perfluoropolyetheryl fluoride, with a molecular weight of 3000-4000, and 1 mole of isopropanol as a solvent, into a 20L reactor with reflux stirring and heating and heat preservation devices, and add 2.6 moles of N in batches under stirring. N dimethylpropylenediamine, and slowly heat up, the system temperature is 60 ° C, react for 6 hours, cool to room temperature, a small amount of hydrogen fluoride gas generated during the process is introduced into the lye pool from the upper port of the condenser tube for absorption; then treat the above-mentioned under reduced pressure at 100 ° C Product 2-4h, removal of solvent and diamide.

[0073] Column chromatography treatment: chromatography column, 100-200 mesh silica gel, the volume ratio of silica gel to product is 3:1-5:1, use 1,3 bis-trifluorotoluene as solvent for separation, and leave the required Components to obtain compound A, the yield is about 85%-90%, and the purity can reach more than 98%.

[...

Embodiment 2

[0076] As in Example 1, the difference is that the ammonolysis reaction solvent is dichloromethane, the temperature is 90 ° C, and the quaternization reaction is refluxed for 2 hours, which is designated as sample 2 and is ready for use.

Embodiment 3

[0078] As in Example 1, the difference is that the amount of N,N dimethylpropylenediamine in the ammonolysis reaction is 2.4 moles, the reaction temperature is 115 ° C, and the reaction is 7 hours. During the quaternization reaction, the amount of sodium chloroacetate is 2.6 moles. A 30% aqueous solution was refluxed for 2 hours, designated as sample 3, and set aside.

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Abstract

The invention relates to a long-chain perfluoropolyether surfactant and a preparation method thereof: firstly add perfluoropolyether acyl fluoride and a solvent into a reaction kettle, add diamide while stirring, heat the reaction kettle, and Cool to room temperature; then carry out decompression treatment and column chromatography purification, and finally add chloroacetate solution and water to compound A, heat and stir, and obtain long-chain perfluoropolyether surfactant after the reaction is completed. The preparation method of the long-chain perfluoropolyether surfactant described in the present invention is simple, the production process is stable, and it is easy to operate; the reaction conditions are mild, no catalyst is needed, the energy consumption is small, and the equipment requirements are simple; the conversion rate is high, and the production process has no toxic side effects. Product discharge, no pollution, has good environmental protection effect.

Description

technical field [0001] The invention relates to a surfactant, in particular to a long-chain perfluoropolyether surfactant and a preparation method thereof. Background technique [0002] Fluorosurfactants are the most active of the known surfactants. They have "three highs", "two phobias", namely high surface activity, high thermal stability, high chemical stability, and fluorocarbon chain segments are both hydrophobic and Oleophobic has a wide range of applications, such as ore flotation in industry, sugar refining, pharmaceuticals, and microbial factories. [0003] One of the applications of fluorocarbon surfactants is as an aqueous film-forming foam fire extinguishing agent, based on hydrocarbon surfactants and fluorocarbon surfactants, and can form a layer of water film foam on the surface of certain hydrocarbon liquids Extinguishing agent. The effect of ordinary carbon dioxide fire extinguishing agent is not obvious, especially in the case of large-scale fires such as ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/00A62D1/02C08G65/332C08G65/333B01F17/42C09K23/42
CPCA62D1/0085C08G65/3322C08G65/33306C09K23/007
Inventor 张伟刘彦军程思聪
Owner 龙岩思康新材料有限公司
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