Process of preparing hexafluoropropylene oligomer

A technology of hexafluoropropylene and oligomer is applied in the field of preparation of hexafluoropropylene oligomer to achieve the effects of less three wastes, good selectivity and improved selectivity

Inactive Publication Date: 2007-08-22
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

With activated carbon as the carrier, the conversion rate of hexafluoropropylene is relatively high, and the product contains slightly more perfluorononene, but the product contains a large amount of by-product C 9 f 16 ; When using nickel oxide as a carrier, although the single-pass conversion rate of hexafluoropropylene is slightly lower, the product is mainly perfluorohexene, up to 80% (US 4296265)

Method used

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  • Process of preparing hexafluoropropylene oligomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Measure 40mL of dimethyl sulfoxide into the autoclave, then add 2.5g of KF, 2.5g of N,N-xylaniline and 2.5g of polyethylene glycol 600 respectively, cover and seal, connect the vacuum device, remove The air in it was fed with nitrogen, and then vacuumized to make the pressure in the kettle zero, and the ventilation operation was carried out three times. Then feed hexafluoropropylene gas to make the pressure reach 0.6MPa, turn on the stirrer, 400 rpm, heat to 70°C, keep the pressure and temperature basically unchanged, and close the hexafluoropropylene inlet valve after 90 minutes. Continue to stir to normal pressure, blow nitrogen to 0.6MPa, react at 70°C for 30 minutes, stop stirring, and cool. Then the reactant was transferred to a 1L pear-shaped separatory funnel and left to stand overnight. After separation, the light yellow fluorocarbon in the lower layer was obtained, which was washed with water and dried. According to gas chromatography analysis, the mass conten...

Embodiment 2

[0029] The three-way catalyst was changed to 2.0g KF, 2.0g diethylamine and 2.0g polyethylene glycol nonylphenyl ether, and other reactions and post-treatment were the same as in Example 1. The mass content of perfluorohexene in the hexafluoropropylene oligomerization product is 1.4%, the mass content of perfluorononene is 93.2%, and the mass content of perfluorononene after rectification treatment is 99.5%.

Embodiment 3

[0031] The three-way catalyst was changed to 1.5g KF, 2.0g triethylamine and 2.5g polyethylene glycol nonylphenyl ether, and the reaction temperature was changed to 150°C. Other reaction conditions and post-treatment were the same as in Example 1. The mass content of perfluorohexene in the hexafluoropropylene oligomerization product is 1.1%, the mass content of perfluorononene is 93.2%, and the mass content of perfluorononene after rectification treatment is 99.6%.

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Abstract

The process of preparing hexafluoropropylene oligomer with hexafluoropropylene as material, alkali metal fluoride as main catalyst, organic base as co-catalyst and polyether as catalytic promoter includes two sections of pressurized oligomerization reaction in non-protonic polar solvent at 10-150 deg.c, with the weight ratio of main catalyst, co-catalyst, catalytic promoter and non-protonic polar solvent being 1 to 0.1-10 to 1-10 to 8-40. The first section of pressurized oligomerization reaction is performed in a pressure container with hexafluoropropylene gas pressure of 0.1-1.5 MPa, and the second section of pressurized oligomerization reaction is performed in inert gas of pressure 0.1-1.5 MPa. The present invention has the beneficial effects of high hexafluoropropylene converting rate, synergistic catalysis, high perfluoro nonylene selectivity, convenient solvent recovery, etc.

Description

(1) Technical field [0001] The invention relates to a preparation method of a hexafluoropropylene oligomer, in particular to a preparation method of a hexafluoropropylene oligomer with a perfluorononene mass content of more than 99%. (2) Background technology [0002] Perfluorononene is an important fluorine-containing organic intermediate obtained from the oligomerization of hexafluoropropylene, which can be used to derive many fluorine-containing surfactants. This type of surfactant has high activity, high heat resistance stability, high chemical inertness and water and oil repellency, making it suitable for use in coatings, washing, fire protection, metal anticorrosion, pigments, dyes, emulsifying dispersants, fiber leather treatment agents , electronics industry, petroleum products and other fields play a unique role. For example, the perfluoroalkyl ether produced by the reaction of hexafluoropropylene oligomer and phenol can be made into sulfonate fluorosurfactant if i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/269C07C21/18
Inventor 史鸿鑫项菊萍武宏科
Owner ZHEJIANG UNIV OF TECH
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