A kind of method of selective synthesis hexafluoropropylene oxide oligomer

A hexafluoropropylene oxide and selective technology, which is applied in the field of selective synthesis of hexafluoropropylene oxide oligomers, can solve the problems of low reaction temperature, long reaction time, restricted use and the like, and achieves environmentally friendly and low-cost Effect

Active Publication Date: 2021-07-09
湖南有色郴州氟化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of this patented method are: long reaction time, low reaction temperature as low as -20°C to -30°C, high catalyst production cost, low conversion rate of raw materials and mixture of trimers and tetramers. Body selectivity is not high
These unfavorable factors limit the use of this inventive technology

Method used

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  • A kind of method of selective synthesis hexafluoropropylene oxide oligomer
  • A kind of method of selective synthesis hexafluoropropylene oxide oligomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Weigh 2.33g (0.04mol) of anhydrous potassium fluoride, 17.8g of tetraethylene glycol dimethyl ether and 7.27g (0.04mol) of P, P-diisopropoxyphosphonamide, and add them to a 500mL 316L In a reaction kettle, stir and cool to 0°C under a sealed environment. Open the feed valve to feed 200g (1.2mol) of hexafluoropropylene oxide gas into the reactor, and stabilize the reaction temperature at 40±5°C by regulating the temperature of the cooling liquid and controlling the intake rate; To room temperature, discharge, and liquid separation to obtain 192.85 g of crude product of hexafluoropropylene dimer in the lower layer of colorless transparent oil phase, the content of dimer is 86.54%, and the content of trimer and tetramer is 13.46%.

[0048] The product in this example is carried out structural identification (19F-NMR), the result is as follows figure 1 as shown, figure 1 It is the fluorine spectrum of the product in Example 1 of the present invention. Depend on figure 1...

Embodiment 2

[0050] Take by weighing 11.65g (0.2mol) anhydrous potassium fluoride, 89.00g tetraethylene glycol dimethyl ether and 39.96g (0.2mol) P-isopropoxy-P-phenylphosphonamide, add to In a 2000mL 316L reaction kettle, stir in a sealed environment and cool to -10°C. Open the feed valve to feed 1000g (6.0mol) of hexafluoropropylene oxide gas into the reactor, and stabilize the reaction temperature at 50±5°C by regulating the temperature of the cooling liquid and controlling the intake velocity; to room temperature, discharge, and liquid separation to obtain 993.35 g of crude product of hexafluoropropylene dimer in the lower colorless transparent oil phase, the content of dimer is 85.94%, and the content of trimer and tetramer is 14.06%.

Embodiment 3

[0052] Weigh 2.07g (0.02mol) of anhydrous zinc fluoride, 17.8g of tetraethylene glycol dimethyl ether and 7.27g (0.04mol) of P, P-diisopropoxyphosphonamide, and add it to a 500mL 316L In a reaction kettle, stir and cool to 0°C under a sealed environment. Open the feed valve to feed 200g (1.2mol) of hexafluoropropylene oxide gas into the reactor, and stabilize the reaction temperature at 40±5°C by regulating the temperature of the cooling liquid and controlling the intake rate; To room temperature, discharge, liquid separation to obtain 195.09 g of crude hexafluoropropylene trimer in the lower layer of colorless transparent oil phase, the content of trimer is 84.59%, and the content of dimer and tetramer is 15.41%.

[0053] The product in this example is carried out structural identification (19F-NMR), the result is as follows figure 2 as shown, figure 2 It is the fluorine spectrum of the product in Example 3 of the present invention. Depend on figure 2 It can be seen th...

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Abstract

The invention provides a method for selectively synthesizing hexafluoropropylene oxide oligomers, comprising the following steps: A) adding phosphonamide, metal fluoride salt and organic solvent into a reaction device, and stirring in an airtight manner; the metal fluoride The salt is a monovalent metal fluoride salt or a divalent metal fluoride salt, and the monovalent metal fluoride salt is one or more of lithium fluoride, sodium fluoride, potassium fluoride, rubidium fluoride and cesium fluoride kind, the divalent metal fluoride salt is one or more of zinc fluoride, barium fluoride and magnesium fluoride; B) passing hexafluoropropylene oxide into the reaction device for reaction to obtain Hexafluoropropylene oxide dimer or hexafluoropropylene oxide trimer. The invention has low raw material cost, does not need low temperature and dry environment, and is environmentally friendly, and can selectively synthesize hexafluoropropylene oxide dimer or trimer with a content of more than 80%.

Description

technical field [0001] The invention belongs to the technical field of organic fluorine fine chemicals, in particular to a method for selectively synthesizing hexafluoropropylene oxide oligomers. Background technique [0002] Hexafluoropropylene oxide oligomer is an important intermediate in the material industry. The C-F bond energy in the molecule is relatively large, and the shielding of the main chain makes it have very high chemical inertness, thermal stability, oxidation resistance, and mechanical stability. , Radiation resistance, corrosion resistance. [0003] Hexafluoropropylene oxide dimer is used to prepare perfluoro-n-propyl vinyl ether (PPVE), which is an important fluorine-containing monomer. A small amount of PPVE is added to the polymerization of tetrafluoroethylene to prepare soluble polytetrafluoroethylene Ethylene (PFA), this kind of polytetrafluoroethylene not only retains the characteristics of the original tetrafluoroethylene, but also overcomes the sh...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/58C07C59/135
CPCC07C51/58C07C59/135
Inventor 王刚李军彭智敏刘斌李志鹏苏万里张振华
Owner 湖南有色郴州氟化学有限公司
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