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Preparation method of fluoride anti-fingerprint agent

A technology of anti-fingerprint agent and perfluoroalkyl alcohol, which is applied in the field of preparation of fluorine-containing anti-fingerprint agent, can solve the problems of increased process cost and risk, strict process pipeline requirements, harsh reaction conditions, etc., to improve the safety of production process High chemical reactivity, high chemical reactivity, and simple operation

Inactive Publication Date: 2012-08-22
锦州恒通氟化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, fluorine-containing anti-fingerprint agents are mainly synthesized by the hydrosilylation reaction of perfluoroalkylethylene and silane compounds. The disadvantage is that due to the poor chemical activity of perfluoroalkylethylene in the reactants used, This type of reaction usually needs to be carried out in the presence of high temperature, high pressure and noble metal catalysts, which greatly reduces the safety of the production process and increases the production cost.
It has the following problems: 1. The precious metal catalyst chloroplatinic acid used is expensive, which increases the production cost; 2. The raw material trichlorosilane used is an irritating and corrosive substance, which has strict requirements on the process pipeline, which increases the process cost and danger; 3. The reaction conditions are harsh and need to be carried out under high temperature and pressure

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Under the protection of nitrogen, add 264g of perfluorobutyl alcohol and 271g of propyltriethoxysilane isocyanate to a 1L four-necked flask equipped with mechanical stirring, temperature measuring point, and reflux condenser, start stirring, and heat to 30℃~35℃, after reacting for 1h, under the system pressure -0.1MPa~-0.097MPa, heating temperature 100℃~110℃, the excess isocyanate propyltriethoxysilane was removed by vacuum distillation to obtain shallow 509 g of perfluorobutylethyl triethoxysilylpropyl isocyanate is a yellow transparent liquid, with a purity of 99.4% and a yield of 99.0% by gas chromatography. Dilute perfluorobutylethyl triethoxysilylpropyl isocyanate with 1,1,2,2-tetrafluoroethyl methyl ether to a 0.3% solution to obtain a fluorine-containing anti-fingerprint agent.

[0015] Soak the glass in the fluorine-containing anti-fingerprint agent for 5 minutes, then dry it naturally, and use a surface tensiometer to test the surface tension of the glass to be...

Embodiment 2

[0017] Under the protection of nitrogen, add 364g of perfluorohexyl alcohol and 271g of isocyanate propyltriethoxysilane into a 1L four-neck flask equipped with mechanical stirring, temperature measuring point, and reflux condenser, start stirring, and heat to 35 ℃~40℃, after 2 hours of reaction, under the system pressure -0.1MPa~-0.097MPa, heating temperature 100℃~110℃, excess isocyanate propyltriethoxysilane was removed by vacuum distillation to obtain light yellow 609 g of perfluorobutylethyl triethoxysilylpropyl isocyanate as a transparent liquid, with a purity of 99.3% and a yield of 98.9% by gas chromatography. Dilute perfluorobutylethyl triethoxysilylpropyl isocyanate with 1,1,2,2-tetrafluoroethyl methyl ether to a 0.3% solution to obtain a fluorine-containing anti-fingerprint agent.

[0018] Soak the glass in the fluorine-containing anti-fingerprint agent for 5 minutes, then dry it naturally, and use a surface tensiometer to test the surface tension of the glass to be ...

Embodiment 3

[0020] Under the protection of nitrogen, add 464g perfluorooctyl alcohol and 280g isocyanate ethyl triethoxysilane to a 1L four-necked flask equipped with mechanical stirring, temperature measuring point and reflux condenser, start stirring, and heat to 40℃~45℃, after reacting for 2 hours, under the system pressure -0.097MPa~-0.095MPa, heating temperature 90℃~100℃, the excess isocyanate ethyltriethoxysilane was removed by vacuum distillation to obtain shallow 694 g of perfluorooctylethyl triethoxysilylethyl isocyanate is a yellow transparent liquid, with a purity of 99.2% and a yield of 98.8% by gas chromatography. Dilute perfluorooctylethyl triethoxysilylethyl isocyanate with 1,1,2,2-tetrafluoroethyl methyl ether to a 0.2% solution to obtain a fluorine-containing anti-fingerprint agent.

[0021] Soak the glass in the fluorine-containing anti-fingerprint agent for 5 minutes, then dry it naturally, and use a surface tensiometer to test the surface tension of the glass to be 16....

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Abstract

The invention discloses a preparation method of a fluoride anti-fingerprint agent. Perfluor alkyl alcohol and carbimide alkyl trialkoxysilane are used as reaction substrates, and addition reaction is carried out to prepare a crude product; the superfluous carbimide alkyl trialkoxysilane is removed through reduced pressure distillation, and a fluoride anti-fingerprint agent concentrated solution is obtained; and the fluoride anti-fingerprint agent concentrated solution is diluted by 1,1,2,2- tetrafluoride ethyl methyl ether, and a final product that is the fluoride anti-fingerprint agent is obtained. The reaction condition of the method is mild, a noble metal catalyst is not needed, irritant and corrosive materials are not used, the process safety is good, the cost of production is low, and the method is conducive to industrial production.

Description

technical field [0001] The invention belongs to the field of fluorine-containing surfactants, in particular to a preparation method of a fluorine-containing anti-fingerprint agent. technical background [0002] The main component of fluorine-containing anti-fingerprint agent is fluorosilicon surfactant, and the main structure is F(CF 2 )nXSi(OR) 3 Through the silanization reaction, a dense fluorinated surface layer is formed on the surface of silicon-containing materials such as glass. Its extremely low surface tension makes it difficult for water and oil to be compatible, so that the treated glass products have an anti-fingerprint effect. Fluorine anti-fingerprint agent is mainly used on the surface of advanced glass products such as mobile phone screens and camera lenses. [0003] At present, fluorine-containing anti-fingerprint agents are mainly synthesized by the hydrosilylation reaction of perfluoroalkylethylene and silane compounds. The disadvantage is that due to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18B01F17/54C03C17/30C09K23/54
Inventor 杨华杰王忠华魏潇
Owner 锦州恒通氟化学有限公司
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