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Perfluoropolyether phosphate compound, preparation method and application thereof

A technology for perfluoropolyether phosphate esters and compounds, which is applied in the fields of phosphorus organic compounds, chemical instruments and methods, compounds of elements of Group 5/15 of the periodic table, etc., can solve the problems of polluting the environment, cumbersome steps and complicated operations, To achieve the effect of less environmental pollution

Active Publication Date: 2019-07-05
RUYUAN DONGYANG LIGHT FLUORIDE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional coating solution for coating has the following defects: first, it needs to be compounded with various additives during use, the operation is complicated and the steps are cumbersome; second, the film layer and metal body formed during use The adhesion is weak, it is easy to detach, the film structure is not dense enough, and the protection efficiency for metal is low; third, some coating liquids will produce wastewater during production and use, causing environmental pollution

Method used

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  • Perfluoropolyether phosphate compound, preparation method and application thereof
  • Perfluoropolyether phosphate compound, preparation method and application thereof
  • Perfluoropolyether phosphate compound, preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0045] In an anhydrous, oxygen-free nitrogen atmosphere, mix 10g of phosphorus oxychloride, 18.02g of 1,4-tere-phenylenedimethanol, and 100mL of tetrahydrofuran, stir and raise the temperature to 35°C, maintain this temperature for 9 hours, add 1mL of deionized water to continue the stirring reaction 1 h, during which the temperature remained constant. After the reaction was over, distillation under reduced pressure gave 13.18 g of intermediates with a yield of 83.05%.

[0046] Under anhydrous and oxygen-free nitrogen atmosphere, 10g of the intermediate (41.10mmol), 66g of perfluoropolyetheryl fluoride (n=6, Mn=1328g / mol), 100mL of trifluorotrichloroethane and 3mL of triethylamine were mixed, Stir and heat up to 25°C, maintain this temperature for 8 hours, and purify the crude product by distillation under reduced pressure to obtain a perfluoropolyether phosphoric acid ester compound (wherein the molar ratio of the perfluoropolyether phosphoric acid monoester compound to the p...

Embodiment 2

[0048]In an anhydrous, oxygen-free nitrogen atmosphere, mix 5g of phosphorus oxychloride, 9.01g of 1,4-tere-phenylenedimethanol, and 50mL of dichloromethane, stir and raise the temperature to 25°C, maintain this temperature for 9h, add 1mL of deionized water to continue The reaction was stirred for 1 h, during which the temperature was kept constant. After the end of the reaction, distillation under reduced pressure yielded 6.21g of intermediates with a yield of 80.65%.

[0049] Under anhydrous and oxygen-free nitrogen atmosphere, mix 5g of the intermediate (21.2mmol), 40g of perfluoropolyether fluoride (n=8, Mn=1660g / mol), 100mL of tetrahydrofuran, and 3mL of triethylamine, stir and heat up to 25°C , maintain this temperature for 8 hours, and purify the crude product by distillation under reduced pressure to obtain a perfluoropolyether phosphoric acid ester compound (wherein the molar ratio of the perfluoropolyether phosphoric acid monoester compound to the perfluoropolyether...

Embodiment 3

[0051] In an anhydrous, oxygen-free nitrogen atmosphere, mix 10g of phosphorus oxychloride, 18.02g of 1,4-tere-phenylenedimethanol, and 100mL of carbon tetrachloride, stir and raise the temperature to 25°C, maintain this temperature for 9 hours, and add 1mL of deionized water Continue to stir the reaction for 1 h, during which the temperature remains constant. After the end of the reaction, distillation under reduced pressure yielded 12.80g of intermediates with a yield of 83.95%.

[0052] Under anhydrous and oxygen-free nitrogen atmosphere, mix 10g of the intermediate (42.78mmol), 110g of perfluoropolyetheryl fluoride (n=12, Mn=2324g / mol), 100mL of tetraethylene glycol dimethyl ether, and 3mL of triethylamine , stirred and heated up to 25°C, maintained at this temperature for 8 hours, and the crude product was purified by distillation under reduced pressure to obtain a perfluoropolyether phosphoric acid ester compound (wherein, the moles of the perfluoropolyether phosphoric a...

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Abstract

The invention discloses a perfluoropolyether phosphate compound, a preparation method and application thereof. The structure of the compound is shown as formula (I), and the preparation method includes: first subjecting a phosphatizing reagent and 1, 4-benzenedimethanol to reaction in a solvent to obtain an intermediate, and then reacting the intermediate with perfluoropolyether acyl fluoride in asolvent in the presence of an acid-binding agent to obtain the perfluoropolyether phosphate compound. When used as a surface protective agent for treating metal and metal oxide substrates, the perfluoropolyether phosphate compound prepared according to the invention can endow the substrates with excellent waterproof, oil-proof, antifouling, friction-resistant, anti-corrosion and other characteristics, and the compound has little environmental pollution during preparation and use, thus meeting the requirements of green and environmental protection.

Description

technical field [0001] The invention relates to the technical field of metal surface treatment agents, in particular to a perfluoropolyether phosphate compound, its preparation method and its application as a metal protective agent. Background technique [0002] After the metal surface is damaged, corroded or worn, it will cause equipment damage, pipeline leakage, product pollution, etc., resulting in vicious accidents such as combustion or explosion, and serious waste of resources and energy. In addition, with the development of cutting-edge science and modern industry, various industrial sectors increasingly require mechanical equipment to operate stably for a long time under extreme working conditions, which puts forward higher requirements for the performance of mechanical equipment surface protection materials. Require. Therefore, the development of metal surface protection materials is of great significance. [0003] At present, metal surfaces are generally protected...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09C08G65/00C09D171/00C09D5/08
CPCC07F9/094C08G65/00C09D171/00C09D5/08Y02E60/10
Inventor 李义涛贾渊侯琴卿阳峰刘群方程珍
Owner RUYUAN DONGYANG LIGHT FLUORIDE CO LTD
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