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Perfluoroalkyl quaternary ammonium salt and preparation method thereof

A technology of perfluoroalkyl quaternary ammonium salt and hydrocarbyl quaternary ammonium salt, which is applied in the field of perfluoroalkyl quaternary ammonium salt and its preparation, and can solve the problem of shortage of fluorine-containing quaternary ammonium salt products, expensive raw materials of fluorine-containing quaternary ammonium salt, and biodegradation low critical micelle concentration, excellent rewetting performance, and good anti-yellowing ability

Inactive Publication Date: 2013-09-18
GUANGZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, fluorine-containing quaternary ammonium salt surfactants have problems such as expensive raw materials and poor biodegradability. Therefore, improvement in the raw material preparation process is still needed
There has not been a lot of research on the development of products such as fluorine-containing monomers, fluorine-containing alkyl halides and fluorine-containing quaternary ammonium salt surface agents, the integration of the fluorine-containing product industry chain, and cost reduction. The shortage of quaternary ammonium products

Method used

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  • Perfluoroalkyl quaternary ammonium salt and preparation method thereof
  • Perfluoroalkyl quaternary ammonium salt and preparation method thereof
  • Perfluoroalkyl quaternary ammonium salt and preparation method thereof

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Embodiment 1

[0022] The preparation method of embodiment 1 perfluoroalkyl quaternary ammonium salt

[0023] Weigh 0.02mol of perfluorohexylethyl iodide and 0.01mol of MDEA into a 50ml two-necked flask with a rotor, then add 8ml of n-butanol, place on a magnetic stirrer and stir evenly, then install a reflux condenser. Slowly raise the temperature to 90°C, and reflux for 48 hours. After cooling, the excess solvent and unreacted raw materials were evaporated by vacuum filtration, and the obtained substance was purified by chromatographic column and dried in vacuum at 50°C. The conversion rate reached 94.51%. The reaction equation is as follows:

[0024]

Embodiment 2

[0025] The preparation method of embodiment 2 perfluoroalkyl quaternary ammonium salts

[0026] Weigh 0.03mol of perfluorohexylethyl iodide and 0.01mol of MDEA into a 50ml two-necked flask with a rotor, then add 8ml of n-butanol, place on a magnetic stirrer and stir evenly, then install a reflux condenser. Slowly raise the temperature to 90°C, and reflux for 48 hours. After cooling, the excess solvent and unreacted raw materials were evaporated by vacuum filtration, and the obtained substance was purified by chromatographic column and dried in vacuum at 50°C. The conversion rate reached 95%.

[0027] The qualitative analysis of embodiment 3 embodiment 1 gained products

[0028] Identification of quaternary ammonium salts: Since bromophenol blue is insoluble in chloroform but soluble in water, it can react with cationic surfactants to form a blue complex that is soluble in chloroform, so the blue is transferred from the water phase to the chloroform layer. After adding the a...

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Abstract

The invention discloses perfluoroalkyl quaternary ammonium salt and a preparation method thereof. The structural formual of perfluoroalkyl quaternary ammonium salt is as shown in the specification. The preparation method comprises the following step: directly performing quaterisation on perfluorohexyl ethyl iodide and N-methyldiethanolamine to prepare perfluoroalkyl quaternary ammonium salt. According to the invention, MDEA and perfluorohexyl ethyl iodide are used as main raw materials to synthesize a novel perfluoroalkyl quaternary ammonium salt surfactant. The perfluoroalkyl quaternary ammonium salt surfactant has excellent performances such as surface tension and low critical micelle concentration. Performance comparison test shows that the perfluoroalkyl quaternary ammonium salt surfactant has re-wettability superior to re-wettabilities of EQ and D1821, and the anti-yellowing performance is superior to that of D1821 but inferior to that of EQ. The surfactant yet has good anti-yellowing performance. The perfluoroalkyl quaternary ammonium salt surfactant can be a good flexibilizer and has good development prospect.

Description

technical field [0001] The invention relates to a fluorine-containing quaternary ammonium salt surfactant, in particular to a perfluoroalkyl quaternary ammonium salt and a preparation method thereof. Background technique [0002] The fluorine-containing quaternary ammonium salt surfactant is to replace the H atom on the hydrocarbon group of the common hydrocarbon quaternary ammonium salt surfactant with an F atom to become an F-C chain, and the hydrophobic group after the substitution is a substituted fluorocarbon chain . Fluorinated quaternary ammonium surfactants can be divided into perfluorinated fluorinated quaternary ammonium surfactants and semi-fluorinated fluorinated quaternary ammonium surfactants according to the degree of fluorination. If all the H atoms in the C-H chain are replaced by F atoms, such a fluorosurfactant is called a perfluorinated fluorosurfactant; while the F atoms in the C-H chain are partially replaced by the H in the compound, it is called a se...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C215/40C07C213/08B01F17/18C09K23/18
Inventor 郑成徐运欢林璟聂旭春毛桃嫣张文涌黄武欢
Owner GUANGZHOU UNIVERSITY