Method for synthesizing perfluoropolyether from perfluoropolyether peroxide

A technology of perfluoropolyether peroxide and perfluoropolyether, which is applied in the field of organic chemistry, can solve the problems of reducing the production efficiency of perfluoropolyether, the difficulty of handling small molecules, and increasing the production cost, etc., and achieve the refinement of product application fields , Good economic value, low cost effect

Active Publication Date: 2014-04-16
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The small molecules of such products have low value and cannot be used in lubricants, vacuum pump oils, and surfactants, which greatly reduces the production efficiency...

Method used

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  • Method for synthesizing perfluoropolyether from perfluoropolyether peroxide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Perfluoropolyether peroxide prepared by photooxidative polymerization: Rf-O-O-Rf, wherein Rf can be a mixture of any possible situation in the following formula:

[0033] A-O-(-C(T f ) (OCF 3 ) CF 2 -O) m (G f -O-O) n -(CF 2 O) p -(CF 2 OO) q -.

[0034] Self-made 5L stainless steel reaction kettle, built-in stirring, cooling coil, ultraviolet lamp, the measured peroxide value is 9.2×10 -2 Add 2kg of perfluoropolyether peroxide prepared by mmol / g photooxidative polymerization and 1.2kg of trifluorotrichloroethane into the reaction kettle, turn on the ultraviolet lamp (wavelength 365nm), when the temperature rises to 80°C, Slowly feed hexafluoropropylene intermittently, the temperature is controlled at about 100 ° C ~ 105 ° C, the pressure is 1 MPa, a total of 40 g of hexafluoro propylene is added, and 20 g is introduced per hour. After passing through the hexafluoro propylene, react for another 3 hours, then cool down and discharge . The peroxide value of th...

Embodiment 2

[0037] Self-made 5L stainless steel reaction kettle, built-in stirring, cooling coil, ultraviolet lamp, the measured peroxide value is 9.2×10 -2 Add 2kg of perfluoropolyether peroxide prepared by mmol / g photooxidative polymerization and 1.3kg of trifluorotrichloroethane into the reaction kettle, turn on the ultraviolet lamp (wavelength 365nm), when the temperature rises to 80°C, Slowly feed tetrafluoroethylene intermittently, the temperature is controlled at about 100°C to 105°C, the pressure is 1MPa, 30g of tetrafluoroethylene is added accumulatively, and 20g of tetrafluoroethylene is introduced per hour. . The peroxide value of the reacted product was measured to be 0.96×10 -6 mmol / g, the product is subjected to vacuum fractionation, and the fractions are shown in the table below.

Embodiment 3

[0039] Self-made 5L stainless steel reaction kettle, built-in stirring, cooling coil, ultraviolet lamp, the measured peroxide value is 9.2×10 -2 Add 2kg of perfluoropolyether peroxide prepared by mmol / g photooxidative polymerization into the reaction kettle, turn on the ultraviolet lamp (wavelength 365nm), and when the temperature rises to 80°C, intermittently and slowly pass tetrafluoroethylene into the kettle, The temperature is controlled at about 110°C to 120°C, the pressure is 1.2MPa, 30g of tetrafluoroethylene is added accumulatively, and 20g of tetrafluoroethylene is controlled to be introduced per hour. After passing through the tetrafluoroethylene, react for another 3 hours, and then cool down and discharge the material. The peroxide value of the reacted product was measured to be 0.53×10 -6 mmol / g, the product is subjected to vacuum fractionation, and the fractions are shown in Table 1 below.

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Abstract

The invention relates to a method for synthesizing perfluoropolyether from perfluoropolyether peroxide. The method is characterized by comprising the following steps of placing the perfluoropolyether peroxide prepared by a photo-oxidation method in an inert fluorine-containing solvent, introducing perfluoroolefine under an ultraviolet irradiation condition, and reacting the perfluoroolefine with the peroxide to form a stable perfluoropolyether compound. According to the method, reaction conditions comprise ultraviolet irradiation and pressure of more than 1.0MPa, and are mild, and the perfluoropolyether compound is easy to industrially produce; the synthesized perfluoropolyether compound has peroxide value of lower than 2*10<-6>mmol/g and molecular weight of more than 1,500; components with different molecular weights can be further obtained by a reduced pressure fractionation method, so that the application fields of the product are detailed, and high economic value is created.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and in particular relates to a synthesis method of perfluoropolyether. Background technique [0002] Perfluoropolyether (PFPE) is a special kind of high molecular perfluoropolymer, and there are only three elements of C, F and O in the molecule. Compared with hydrocarbon lubricants, PFPE lubricants have basically similar molecular structures, but fluorine atoms in the molecule replace hydrogen atoms, thereby replacing C-H bonds in hydrocarbons with stronger C-F bonds, and the presence of C-O and C-C strong covalent bonds , and the neutrality of PFPE molecules make PFPE have high chemical stability and oxidation stability as well as good chemical inertness and insulating properties. In addition, PFPE has shear stability, biological inertness, low surface energy, good lubricity, and good comprehensive properties such as compatibility with plastics, elastomers, and metal materials, making it an ext...

Claims

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Application Information

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IPC IPC(8): C08F283/06
Inventor 张鸣张建新李斌杨旭仓彭孝凤
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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