Method for synthesizing fluorine-containing anti-fingerprint agent

An anti-fingerprint agent and solvent technology, applied in the coating and other directions, can solve the problems of increasing process cost and danger, harsh reaction conditions, harsh process conditions, etc., to improve the safety of the production process, facilitate industrial production, and avoid precious metals. The effect of catalyst

Inactive Publication Date: 2015-05-20
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

Its disadvantages are: 1. The cost of raw materials is high and difficult to obtain—perfluoropolyether as a raw material needs to be prepared by hexafluoropropylene oxide, which has poor production safety and harsh process conditions; 2. The preparation process is cumbersome and the yield is low, increasing Production cost; 3: The reaction conditions are harsh, noble metal catalysts are required, and the reaction time is too long
Its shortcoming is: 1. the noble metal catalyst chloroplatinic acid that uses is expensive, has increased production cost; 2. the raw material trichlorosilane that uses has irritating and corrosive substance, has strict requirements on process pipeline, has increased process cost and Danger; 3. The reaction conditions are harsh and need to be carried out under high temperature and high pressure

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Under the protection of nitrogen, add 380g of perfluoroalkyl ethyl methacrylate to a 1L four-necked flask equipped with mechanical stirring, temperature measuring point and reflux condenser, whose structural formula is: n=14, 10g 3-(methacryloyloxy)propyltrimethoxysilane, 8g methyl methacrylate, 1.6g dodecylmercaptan, 0.4g diisopropyl peroxydicarbonate, and 200 g methyl acetate. Start stirring to mix the reactants well, then heat to 30°C to initiate the reaction, control the reaction temperature to 30-40°C, and stop the reaction after 2 hours. The reaction solvent, methyl acetate, was distilled off under reduced pressure to obtain 391 g of a light yellow gel-like substance with a yield of 97.8%. Dilute the obtained product with hydrofluoroether HFE-254 to a solution with a mass percentage of 0.1%, to obtain the fluorine-containing anti-fingerprint agent A.

[0016] Soak the glass sheet in the fluorine-containing anti-fingerprint agent A for 1 minute, take ...

Embodiment 2

[0018] Under nitrogen protection, add 370g of perfluoroalkyl ethyl methacrylate to a 1L four-necked flask equipped with mechanical stirring, temperature measuring point, and reflux condenser, whose structural formula is: n=8, 24g 3-(methacryloyloxy)propyltrimethoxysilane, 4g methyl methacrylate, 1.6g dodecylmercaptan, 0.4g diisopropyl peroxydicarbonate, and 200 g of ethyl acetate. Start stirring to mix the reactants well, then heat to 30°C to initiate the reaction, control the reaction temperature to 30-40°C, and stop the reaction after 1.5 hours. Ethyl acetate, the reaction solvent, was distilled off under reduced pressure to obtain 389 g of a light yellow gel-like substance with a yield of 97.3%. Dilute the obtained product with hydrofluoroether HFE-374 to a solution of 0.1% by mass to obtain the fluorine-containing anti-fingerprint agent B.

[0019] Soak the glass piece in the fluorine-containing anti-fingerprint agent B for 1 minute, take it out, dry it naturall...

Embodiment 3

[0021] Under the protection of nitrogen, add 360g of perfluoroalkyl ethyl methacrylate to a 1L four-neck flask equipped with mechanical stirring, temperature measuring point, and reflux condenser. Its structural formula is: n=12, 38g 3-(methacryloyloxy)propyltrimethoxysilane, 1.6g dodecylmercaptan, 0.4g diisopropyl peroxydicarbonate, and 200g butyl acetate. Turn on the stirring to fully mix the reactants, heat to 30°C to initiate the reaction, control the reaction temperature to 30-40°C, and stop the reaction after 1 hour. The reaction solvent, butyl acetate, was distilled off under reduced pressure to obtain 392 g of a light yellow gel-like substance with a yield of 98.0%. Dilute the obtained product with hydrofluoroether HFE-347 to a solution of 0.1% by mass to obtain fluorine-containing anti-fingerprint agent C.

[0022] Soak the glass sheet in the fluorine-containing anti-fingerprint agent C for 1 minute, take it out, dry it naturally at room temperature for 30 m...

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PUM

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Abstract

The invention relates to a method for preparing a fluorine-containing anti-fingerprint agent. The method comprises the following steps of by adopting perfluoroalkyl ethyl methacrylate, 3-(methacryloxy)propyl trimethoxysilane and methyl methacrylate as reaction substrates, dodecyl mercaptan as a chain transfer agent and diisopropyl peroxydicarbonate as an initiator and in the presence of a solvent, initiating polymerization reaction for a reaction time of 1-2 hours, controlling the reaction temperature at 30-40 DEG C to prepare a crude product; carrying out reduced pressure distillation to remove the solvent to obtain a perfluoroalkyl silane compound; and diluting the perfluoroalkyl silane compound into a 0.1% (by mass concentration) solution with hydrofluoroether to obtain the finished product, namely, fluorine-containing anti-fingerprint agent. The method has the advantages of mild reaction conditions, no need of precious metal catalyst, safe and easily available raw materials, simple process, good safety and low production costs and is conducive to industrial production.

Description

technical field [0001] The invention belongs to the field of fluorine-containing surface protection materials, in particular to a synthesis method of a fluorine-containing anti-fingerprint agent. technical background [0002] The fluorine-containing anti-fingerprint agent with fluorinated silane compounds as the main component has been widely used on the surface of high-end glass products such as high-end mobile phone screens, digital camera lenses, and precision optical components. It has excellent waterproof, oil-proof and anti-fouling effects. "Three defenses" effect. There are two main types of fluorine-containing anti-fingerprint agents currently on the market, including perfluoropolyether silanes and perfluoroalkyl silanes. [0003] Among them, perfluoropolyether silane fluorine-containing anti-fingerprint agents are mainly synthesized by addition reaction of perfluoropolyether and silane compounds. Its disadvantages are: 1. The cost of raw materials is high and diff...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09D133/16C08F220/24C08F230/08C08F220/14C08F2/38
CPCC08F2/38C08F220/24C09D133/16C08F230/08C08F220/14
Inventor 魏奇王忠华谷峰
Owner 锦州恒通氟化学有限公司
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