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Perfluoropolyether preparation method and perfluoropolyether

A technology of perfluoropolyether and perfluoroalkyl alcohol, which is applied in the chemical industry, can solve the problems of toxic waste post-processing, low efficiency, and low yield, and achieve low production cost, simple preparation process, and high catalytic efficiency. Effect

Pending Publication Date: 2021-05-28
GUANGDONG UNIV OF PETROCHEMICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These methods have certain disadvantages such as low efficiency, low yield, toxic waste and complicated post-treatment.

Method used

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  • Perfluoropolyether preparation method and perfluoropolyether
  • Perfluoropolyether preparation method and perfluoropolyether
  • Perfluoropolyether preparation method and perfluoropolyether

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preparation example Construction

[0031] A method for preparing perfluoropolyether, comprising: weighing raw materials perfluoroalkyl alcohol, perfluoroalkylene oxide, and double metal cyanide catalyst; Fill with nitrogen, then add perfluoroalkyl alcohol and part of perfluoroalkylene oxide for the first time, stir for 10-60 minutes and then heat to 90-120°C. When the pressure in the reactor drops significantly, slowly add the remaining The perfluoroalkylene oxide is added at a rate to maintain the pressure in the reactor at 0.5MPa; after the addition is completed, wait until the pressure in the reactor is constant, and the reaction ends; the reaction product is refined to obtain perfluoropolyether. Further, in the preparation method of perfluoropolyether, preferably the perfluoroalkyl alcohol is the following compound: C 1 ~C 10 of perfluoroalkyl alcohols.

[0032] Further, in the preparation method of perfluoropolyether, preferably the perfluoroalkylene oxide is the following compound: C 2 ~C 22 perfluoro...

Embodiment 1

[0051] Embodiment 1, a kind of perfluoropolyether, is the compound of following structure:

[0052]

[0053] The preparation method of the above-mentioned perfluoropolyether: add 10 mg of multimetal cyanide catalysts Co[Fe(CN) to a 250mL autoclave 3 ] 3 2ZnCl 2 · 3LaCl 3 , evacuate for 10 minutes, replace with nitrogen three times, under nitrogen, add 20 mg of perfluoromethanol, 14.5 grams of perfluoroethylene oxide and 12.6 grams of perfluoropentylene oxide into the reaction kettle, stir for 10 minutes and heat to 90 ℃, when the pressure in the reactor drops significantly, add 140 grams of perfluoroethylene oxide and 120 grams of perfluoropentylene oxide at a rate of 0.3 g / min to maintain the pressure in the reactor at 0.5 MPa, continue After aging for 1 hour, the reaction was completed. The reaction product was filtered to obtain the product of Example 1.

Embodiment 2

[0054] Embodiment 2, a kind of perfluoropolyether, is the compound of following structure:

[0055]

[0056] The preparation method of the above-mentioned perfluoropolyether: add 50 mg of multimetal cyanide catalysts Ni[Fe(CN) to a 250mL autoclave 3 ] 2 ·5ZnCl 2 2CeCl 3 , evacuate for 30 minutes, replace with nitrogen three times, under nitrogen, add 100 mg of perfluorobutanol, 20 grams of perfluoropropylene oxide and 10 grams of perfluorodecane to the reaction kettle, stir for 60 minutes and heat to 120 ℃, when the pressure in the reactor drops significantly, add 180 grams of perfluoropropylene oxide and 170 grams of perfluorodecane at a rate of 0.5 g / min, maintain the pressure in the reactor at an atmospheric pressure, and continue aging After 1 hour, the reaction was over. The reaction product was filtered to obtain the product of Example 2.

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Abstract

The invention discloses a preparation method of perfluoropolyether and the perfluoropolyether. The preparation method comprises the steps of weighing raw materials including perfluoroalkyl alcohol, perfluoroalkylene oxide and a double-metal cyanide catalyst; firstly adding the double-metal cyanide catalyst into a reaction kettle, vacuumizing for 10-30 minutes, filling nitrogen, adding perfluoroalkyl alcohol and part of perfluoroalkylene oxide which is added for the first time, stirring for 10-60 minutes, heating to the temperature of 90-120 DEG C, and slowly adding the rest perfluoroalkylene oxide for the second time when the pressure in the reaction kettle is obviously reduced, wherein the pressure in the reaction kettle is maintained at 0.5 MPa according to the adding speed; after completely adding the perfluoroalkylene oxide, ending the reaction when the pressure in the reaction kettle is constant; and refining the reaction product to obtain the perfluoropolyether. According to the preparation method disclosed by the invention, the compound with the structure shown in the description is prepared through direct catalytic polymerization, the production efficiency is high, the yield is high, and no toxic waste is generated.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of perfluoropolyether and the perfluoropolyether. Background technique [0002] Perfluoropolyether has unique physical and chemical properties due to the C-F chemical bond, such as: odorless, non-toxic, non-irritating, good hand feeling, good chemical stability, low viscosity, good film-forming properties, etc., belonging to a unique class of liquid materials , Widely used in electronics, chemical industry, machinery, electrical, nuclear industry, aerospace and other fields. [0003] At present, perfluoropolyethers are mainly prepared by photochemical oxidation polymerization of special fluorine-containing monomer mixtures and anionic polymerization of perfluoroepoxides, and further treated with fluorine gas to form stable perfluoropolyethers. The catalysts used include: hypervalent fluorides of transition metals, anhydrous hydrogen flu...

Claims

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Application Information

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IPC IPC(8): C08G65/28
CPCC08G65/2639C08G65/2663Y02P20/584
Inventor 程亮张杰
Owner GUANGDONG UNIV OF PETROCHEMICAL TECH
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