One-pot method for synthesizing surface treating agent

A surface treatment agent, pot cooking technology, applied in chemical instruments and methods, chemical/physical processes, coatings, etc., can solve the problems of complex synthesis route, irritating raw materials, poor chemical activity of perfluoroalkyl ethylene, etc. The effect of good process safety and mild reaction conditions

Pending Publication Date: 2020-05-08
苏州东杏表面技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, perfluoroalkylsiloxane-based compounds are mainly synthesized by hydrogen-silicon reaction of perfluoroalkylethylene and silane compounds, such as Chinese patent CN102070662A, using perfluoroalkylethylene iodide as raw material, in the presence of noble metal catalysts, continuous Add trichlorosilane dropwise for reaction to obtain intermediate product; then add high boiling point solvent, react by continuously dropping methanol or ethanol, and rectify under reduced pressure to obtain the target product. The main disadvantage is that the perfluoroalkylethylene in the reactant Poor chemical activity, this type of reaction usually needs to be carried out under the action of noble metal catalyst at high temperature and high pressure, and the raw materials are irritating and corrosive
[0004] At the same time, in order to achieve better anti-fouling and wear-resistant effects, it is necessary to prepare perfluoroalkyl siloxane compounds with longer carbon chains, but the synthesis of long-chain perfluorocarbons and their derivatives is more difficult
[0005] In comparison, long-chain perfluoropolyether is easy to obtain, but when it reacts with silane compounds, it is usually synthesized by hydrogen-silicon reaction, such as Chinese patent CN102666759A, the synthetic route adopted is more complicated, first Synthesize the perfluoropolyether compound, then connect the propylene group to the carbon chain, and finally connect the propylene group and the silane compound to the end of the silane compound under the action of the noble metal catalyst, and then obtain the fluorine-containing polyether siloxane through alcohol exchange reaction base compound
The whole synthetic route is more complicated, and also uses irritating and corrosive reactants, which is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Dissolve 20 grams of raw material perfluoropolyether acid (157FS, molecular weight 4000) in 80 grams of perfluorohexane, place it in a 250 ml flask, control the temperature at 70 ° C, and carry out reflux stirring, and add 2 gram of oxalyl chloride, and nitrogen gas was kept flowing through the reaction flask, and the reaction was continued for 2 hours. Continue to add 0.9 g of aminopropyltrimethoxysilane, and continue to reflux for 2 hours under the protection of nitrogen flow to obtain the product.

Embodiment 2

[0022] Dissolve 20 grams of the raw material perfluoropolyether acid (157FS, molecular weight 2500) in 80 grams of perfluorohexane, place it in a 250 ml flask, control the temperature at 70 ° C, and carry out reflux stirring, and add 2 drops dropwise under nitrogen protection. gram of oxalyl chloride, and nitrogen gas was kept flowing through the reaction flask, and the reaction was continued for 2 hours. Continue to add 1.5 g of aminopropyltrimethoxysilane, and continue to reflux for 2 hours under the protection of nitrogen flow to obtain the product.

Embodiment 3

[0024] Dissolve 20 grams of the raw material perfluoropolyether acid (157FS, molecular weight 7000) in 80 grams of perfluorohexane, place it in a 250 ml flask, control the temperature at 70 ° C, and carry out reflux stirring, and add 2 gram of oxalyl chloride, and nitrogen gas was kept flowing through the reaction flask, and the reaction was continued for 2 hours. Continue to add 0.5 g of aminopropyltrimethoxysilane, and continue to reflux for 2 hours under the protection of nitrogen flow to obtain the product.

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PUM

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Abstract

The invention discloses a one-pot method for synthesizing a surface treating agent, and belongs to the technical field of surface treating agent preparation. The method comprises the following steps:dissolving carboxylic acid containing a perfluoropolyether chain in a fluorine-containing solvent, adding an acylating chlorination reagent under the protection of nitrogen, and continuously adding aminopropyltrialkoxysilane to react after the acylating chlorination reaction is finished, thereby finally obtaining the product. The compound can be applied to surface treatment of glass, polymers, ceramics and metals to form a layer of wear-resistant and antifouling surface film. The one-pot method for preparing the surface treating agent has the advantages of mild reaction conditions, no need ofexpensive catalysts and good process safety.

Description

technical field [0001] The invention belongs to the technical field of preparation of surface treatment agents, in particular to a method for synthesizing surface treatment agents in one pot. Background technique [0002] The fluorine-containing siloxane compound can react with the hydroxyl groups on the surface of the substrate to form a film with amphiphobic properties (neither lipophilic nor hydrophilic), which can prevent dirt such as moisture or oil from adhering, And it increases the surface sliding property, thereby improving the surface wear resistance. It is a surface layer with anti-fouling and wear-resistant properties. It has been widely used in lenses, mobile phones and tablet computer displays. [0003] At present, perfluoroalkylsiloxane-based compounds are mainly synthesized by hydrogen-silicon reaction of perfluoroalkylethylene and silane compounds, such as Chinese patent CN102070662A, using perfluoroalkylethylene iodide as raw material, in the presence of no...

Claims

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Application Information

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IPC IPC(8): C08G65/336C08G65/331C08G65/326C08G65/338B01F17/54C09D171/00C03C17/30C09K23/54
CPCC08G65/336C08G65/331C08G65/326C08G65/338C09D171/00C03C17/30C09K23/00
Inventor 许波连何丽蓉王兴张黎斌张俊江
Owner 苏州东杏表面技术有限公司
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