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Preparation method for special fluoroether oligomer

An oligomer and fluoroether technology, which is applied in the field of preparation of special fluoroether oligomers, can solve the problems of poor emulsion stability, low temperature resistance and easy brittle cracking, and environmental pollution of perfluorooctanoic acid.

Inactive Publication Date: 2015-12-02
江苏梅兰化工有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the surface activity of this fluoroether oligomer liquid is lower than that of perfluorooctanoic acid commonly used in fluoropolymer emulsion polymerization, and the emulsion stability is poor. However, due to the environmental pollution caused by perfluorooctanoic acid, it is urgent to find alternatives to perfluorooctanoic acid
In addition, the surface oil repellency of this kind of fluoroether oligomer is not as good as that of traditional three-proof fluoropolymer, and its surface tension performance still needs to be improved
In addition, the low temperature resistance of traditional fluorine rubber is not good. Taking fluorine rubber as an example, its low temperature resistance is generally as low as minus 30 degrees and it is easy to be brittle. This is not enough for the development of aerospace materials and needs to be improved.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1 (preparation of low molecular weight 300~1500 fluoroether oligomers)

[0022] In a photochemical reaction kettle with an internal volume of about 10 liters, nitrogen exhaust and dehumidification are first used, the jacket temperature is reduced to minus 70 degrees, and then 9.9 kilograms of fluorine-containing monomer A (90% hexafluoro Propylene, 10% tetrafluoroethylene), 0.1 kg of fluorine-containing monomer B: perfluoropropenyl methyl ether CF2=CFCF2-O-CF3, at this time, the mixed fluorine-containing monomer is basically liquefied, and the stirring is started, and the ultraviolet light is turned on The power of the lamp is about 300 watts. Oxygen (about 3.5 liters / minute) and difluorodichloromethane (about 0.45 liters / minute) are introduced into the bottom of the kettle, and the temperature in the kettle is controlled at about minus 35 to minus 40 degrees Celsius. After about 8 hours of reaction, the stirring was stopped, the unreacted monomers were disch...

Embodiment 2

[0023] Embodiment 2 (preparation of low molecular weight 300~1500 fluoroether oligomers)

[0024] In a photochemical reaction kettle with an internal volume of about 10 liters, nitrogen exhaust and dehumidification are first used, the jacket temperature is reduced to minus 70 degrees, and then 9.5 kilograms of fluorine-containing monomer A (80% hexafluoro Propylene, 20% tetrafluoroethylene), 0.5 kg of fluorine-containing monomer B: perfluoropropenyl propyl ether CF2=CFCF2-O-C3F7, at this time, the mixed fluorine-containing monomer is basically completely liquefied, stirring is started, and ultraviolet light is turned on The power of the lamp is about 300 watts. Oxygen (about 3.6 liters / minute) and trifluorobromomethane (about 0.41 liters / minute) are introduced into the bottom of the kettle, and the temperature in the kettle is controlled at about minus 35 to minus 40 degrees Celsius. After about 8 hours of reaction, the stirring was stopped, the unreacted monomers were dischar...

Embodiment 3

[0025]Embodiment 3 (preparation of low molecular weight 300~1500 fluoroether oligomers)

[0026] In a photochemical reaction kettle with an internal volume of about 10 liters, nitrogen exhaust and dehumidification are first used, the jacket temperature is reduced to minus 70 degrees, and then 8.0 kilograms of fluorine-containing monomer A (99% hexafluoro Propylene, 1% tetrafluoroethylene), 2.0 kg of fluorine-containing monomer B: perfluoropropenyl ethyl ether CF2=CFCF2-O-C2F5, at this time, the mixed fluorine-containing monomer is basically liquefied, and the stirring is started, and the ultraviolet light is turned on The power of the lamp is about 300 watts. Oxygen (about 3.9 liters / minute) and trifluorochloromethane (about 0.43 liters / minute) are introduced into the bottom of the kettle, and the temperature in the kettle is controlled at about minus 30 to minus 40 degrees Celsius. After about 8 hours of reaction, the stirring was stopped, the unreacted monomers were discharg...

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Abstract

The invention discloses a preparation method for a special fluoroether oligomer which is obtained by carrying out a photochemical polymerization reaction on a special fluorine-containing monomer mixture. The obtained fluoroether oligomer has many previously unimagined valuable applications. The fluoroether oligomer with the average molecular weight of 300-1500, the viscosity of about 1-20 cPs at 25 DEG C and the acidic value of about 70-100 is suitable for being used as a fluoroether surfactant and further can be used as a perfluoro caprylic acid substituent. The fluoroether oligomer with the average molecular weight over 1500 and the viscosity of about 20-500 cPs at 25 DEG C is further suitable for important applications of being processed as fluoroether oil and high-temperature-resistant lubricating oil and the like. The products or mixture thereof can be further used as an auxiliary for a polymerization process of special fluororubber, particularly low-temperature fluororubber. The low-temperature resistance can reach (-40) DEG C, so that the special fluoroether oligomer can be further accepted in markets of space flight and aviation and automobile industry.

Description

technical field [0001] The invention relates to a preparation method of a special fluoroether oligomer, in particular to a preparation method and application of the special fluoroether oligomer and its derived fluoroether surfactant, fluoroether oil and special fluororubber. Background technique [0002] Fluoroether oils, especially fluoroether oligomers, have excellent physical surface properties, low temperature resistance and chemical stability, and are widely used in chemical materials, mechanical seals, high temperature resistance lubrication, aerospace military industry, new materials and other fields. Applications. Fluorine-containing monomers and oxygen are exposed to light or radiation at sub-zero temperatures, and then treated with end groups to obtain fluorine-containing materials with excellent surface properties. Due to their special properties, this material has become a high-end application of fluorine-containing functional materials , such as chemical additi...

Claims

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Application Information

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IPC IPC(8): C08F214/28C08F214/26C08F216/14C08F2/48C08F8/12C08F8/22C08F8/00C08F214/22C08L27/20C08L27/16B01F17/52C07C51/04C09K23/52
Inventor 钱厚琴吴慧生
Owner 江苏梅兰化工有限公司
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