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Straight-chain polyperfluoroether compound with hydroxyl-containing terminal group and preparation method thereof

A polyperfluoroether and compound technology, which is applied in the field of linear perfluoropolyether compounds, can solve problems such as affecting the integrity of molecular arrangement, and achieve the effect of neat molecular structure, smooth compound, and good adaptability to high and low temperature changes.

Active Publication Date: 2020-09-15
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among the existing hydroxyl-terminated perfluoropolyether compounds, the molecular structure of most perfluoropolyethers contains branched chains. For example, CN102660012A discloses a preparation method for hydroxyl-terminated perfluoropolyether compounds. The perfluoropolyether carboxylic acid or ester of the chain will affect the integrity of the molecular arrangement during use

Method used

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  • Straight-chain polyperfluoroether compound with hydroxyl-containing terminal group and preparation method thereof
  • Straight-chain polyperfluoroether compound with hydroxyl-containing terminal group and preparation method thereof
  • Straight-chain polyperfluoroether compound with hydroxyl-containing terminal group and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0034] 1) Preparation of linear perfluoropolyetheryl fluoride

[0035] Add tetrafluoroethylene gas to the reactor, and feed oxygen into the reactor at the same time, control the volume ratio of tetrafluoroethylene and oxygen to 1:4, control the temperature of the reactor at -50°C, and carry out photooxidative polymerization under ultraviolet light Reaction, the reaction time is 28 hours, and the linear perfluoropolyether product whose terminal group is acid fluoride is obtained, the structural formula is shown in formula II, wherein m is 59, and n is 100.

[0036] 2) Esterification reaction of linear perfluoropolyetheryl fluoride

[0037] Taking triethylamine as the acid-binding agent, the volume ratio of triethylamine and the end group obtained in step 1) is a linear perfluoropolyether of acid fluoride is 2:1, and the product obtained in step 1) and ethanol are according to 1:1 The molar ratio of 4 was reacted at 60°C for 7 hours. After cooling to room temperature, the obtai...

Embodiment 2

[0041] 1) Preparation of linear perfluoropolyetheryl fluoride

[0042] Add tetrafluoroethylene gas to the reactor, and feed oxygen into the reactor at the same time, control the volume ratio of tetrafluoroethylene and oxygen to 1:3, control the temperature of the reactor at -40°C, and carry out photooxidative polymerization under ultraviolet light Reaction, the reaction time is 35 hours, and the linear perfluoropolyether product whose terminal group is acid fluoride is obtained, the structural formula is shown in formula II, wherein m is 130, and n is 62.

[0043] 2) Esterification reaction of linear perfluoropolyetheryl fluoride

[0044] Taking triethylamine as the acid-binding agent, the volume ratio of triethylamine and the end group obtained in step 1) is a linear perfluoropolyether of acid fluoride is 2:1, and the product obtained in step 1) and ethanol are according to 1:1 The molar ratio of 4 was reacted at 50°C for 11 hours. After cooling to room temperature, the obta...

Embodiment 3

[0048] 1) Preparation of linear perfluoropolyetheryl fluoride

[0049] Add tetrafluoroethylene gas to the reactor, and feed oxygen into the reactor at the same time, control the volume ratio of tetrafluoroethylene and oxygen to 1:6, control the temperature of the reactor at -70°C, and carry out photooxidative polymerization under ultraviolet light Reaction, the reaction time is 35 hours, and the linear perfluoropolyether product whose terminal group is acid fluoride is obtained, the structural formula is shown in formula II, wherein m is 200, and n is 38.

[0050]2) Esterification reaction of linear perfluoropolyetheryl fluoride

[0051] Taking triethylamine as the acid-binding agent, the volume ratio of triethylamine and the end group obtained in step 1) is a linear perfluoropolyether of acid fluoride is 4:1, and the product obtained in step 1) is mixed with methanol according to 1:1 The molar ratio of 3 was reacted at 70°C for 7 hours. After cooling to room temperature, the...

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Abstract

The invention provides a straight-chain polyperfluoroether compound with a hydroxyl-containing terminal group and a preparation method thereof. The compound does not contain a branched chain structure, the molecular structure is neater, the compound is smoother, meanwhile, the compound has better viscosity-temperature characteristics, and the application range is wider. The straight-chain polyperfluoroether compound with the terminal group containing the hydroxyl group has a structural formula I shown in the specification; in the structural formula I, m is greater than or equal to 1, and n isgreater than or equal to 1.

Description

technical field [0001] The invention relates to a straight-chain perfluoropolyether compound with a hydroxyl group at the end and a preparation method thereof. Background technique [0002] As a kind of special fluorine-containing compound, perfluoropolyether with terminal hydroxyl group is the key intermediate for the preparation of perfluoropolyether derivatives, which can be further converted into perfluoropolyether surfactants and fluoroether active monomers , used in coating ink, polymer emulsifier, plastic / rubber processing, cleaning agent and other fields. Among the existing hydroxyl-terminated perfluoropolyether compounds, the molecular structure of most perfluoropolyethers contains branched chains. For example, CN102660012A discloses a preparation method for hydroxyl-terminated perfluoropolyether compounds. The perfluoropolyether carboxylic acid or ester of the chain will affect the integrity of the molecular arrangement during use. Contents of the invention [...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/00
CPCC08G65/007
Inventor 赵恒曹春兰辛虎
Owner CHINA PETROLEUM & CHEM CORP
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