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Method for preparing special fluoroether surfactant

A surfactant and fluoroether technology, which is applied in the field of preparation of special fluoroether surfactants, can solve problems such as poor low temperature resistance, insufficient aerospace materials, and environmental pollution of perfluorooctanoic acid, and achieve good low temperature resistance.

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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preparation example Construction

[0012]Optionally, the preparation method of the fluoroether surfactant includes: adding deionized water and a fluoroether oligomer with an average molecular weight of 300 to 1500 in a hydrolysis reactor, and the weight ratio is about (1:15) to ( 3:1), and stir to heat up, the temperature in the kettle is maintained at about 30~200°C, the unstable end groups of fluoroether oligomers (such as acid fluoride-COF, acid chloride-COCl, etc.) will be hydrolyzed into carboxylic acid end groups , the reaction time is about half an hour to 8 hours, and the preferred temperature in the kettle is maintained at 50~200°C; after the reaction, let the reaction solution stand and separate layers, suck out the upper aqueous solution, and then add about the same amount of clean deionized water to the hydrolysis kettle To clean the reactants, stir at room temperature for about half an hour, then suck out and remove the upper aqueous solution, repeat the cleaning method for 1 to 3 times, and dischar...

Embodiment 1

[0026] Embodiment 1 (preparation of low molecular weight 300~1500 fluoroether oligomers)

[0027] 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

[0028] Embodiment 2 (preparation of low molecular weight 300~1500 fluoroether oligomers)

[0029] 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 bromotrifluoromethane (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...

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Abstract

The invention discloses a method for preparing a special fluoroether surfactant. The method comprises the steps of adding deionized water and a fluoroether oligomer, of which the average molecular weight is 300-1,500, into a hydrolysis reaction kettle according to the weight ratio of about (1: 15) to (3: 1), carrying out stirring heating, maintaining the internal temperature of the kettle to be about 30-200 DEG C, hydrolyzing unstable terminal groups of the fluoroether oligomer into carboxylic acid terminal groups, carrying out reaction for half an hour to 8 hours, then, standing a reaction solution to carry out layering, removing an upper-layer aqueous solution through sucking, adding an approximately equal volume of clean deionized water into the hydrolysis kettle so as to clean reactants, carrying out stirring for about half an hour at normal temperature, then, removing an upper-layer aqueous solution through sucking, repeating the cleaning method for 1-3 times, and discharging the reactant, thereby preparing the fluoroether surfactant containing the carboxylic acid terminal groups.

Description

technical field [0001] The invention relates to a preparation method of a special fluoroether surfactant, in particular to a preparation method of a special fluoroether oligomer and a fluoroether surfactant derived therefrom. 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 additives, additives, surfactants, cosmetics, protective...

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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