Perfluoro alkyl alkane preparation method

A technology of perfluoroalkyl alkanes and perfluoroalkyl iodides, which is applied in the field of preparation of perfluoroalkyl alkanes, can solve the problems of unfavorable industrial production, non-recyclable reuse, and increased production costs, and achieve low production costs, The effect of mild reaction conditions and continuous operation process

Inactive Publication Date: 2012-09-12
锦州恒通氟化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problems of this method are: 1) the amount of catalyst used is large and cannot be recycled and reused, which increases the production cost; 2) the raw material acetic acid used is a corrosive and irritating substance, which is not conducive to production operations; 3) The reaction is carried out in two steps and cannot be operated continuously, which is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 346g perfluorobutyl iodide (1mol), 84g (1mol) n-hexene, 2.4g (0.01mol) into a 1L high-pressure stainless steel reactor with electric stirrer, thermocouple, cooling coil, and shaft seal cooling water Benzoyl peroxide and 21.2g (0.001mol) with a particle size of 3.2mm and a carrier of Al 2 o 3 , The effective content is 0.5wt% Pd catalyst. The reactor is sealed and vacuumed, and replaced with high-purity nitrogen three times to make the oxygen content in the reactor less than 10ppm. Start stirring, heat to 70°C to initiate the reaction, then control the reaction temperature at 90°C for 1 hour, continue to feed hydrogen for catalytic hydrogenation reaction, keep the system pressure at 0.5 MPa ~ 0.6 MPa, until the pressure does not change anymore, the reaction time is 3 hours, After the reaction, at a system pressure of -0.098MPa to -0.097MPa and a heating temperature of 80°C to 85°C, vacuum distillation and purification were carried out to obtain 302g of colorless an...

Embodiment 2

[0019] Add 446g perfluorohexyl iodide (1mol), 112g (1mol) n-octene, 2.5g (0.015mol) to a 1L high-pressure stainless steel reactor with electric stirrer, thermocouple, cooling coil, and shaft seal cooling water Azobisisobutyronitrile and 31.8g (0.0015mol) with a particle size of 3.2mm and a carrier of Al 2 o 3 , The effective content is 0.5wt% Pd catalyst. The reactor is sealed and vacuumed, and replaced with high-purity nitrogen three times to make the oxygen content in the reactor less than 10ppm. Start stirring, heat to 60°C to initiate the reaction, then control the reaction temperature to react at 80°C for 1 hour, continue to feed hydrogen for catalytic hydrogenation reaction, keep the system pressure at 0.5MPa ~ 0.6MPa, until the pressure does not change anymore, the reaction time is 4h, After the reaction, at a system pressure of -0.099MPa to -0.098MPa and a heating temperature of 90°C to 95°C, vacuum distillation and purification were carried out to obtain 427g of col...

Embodiment 3

[0021] Add 546g perfluorooctyl iodide (1mol), 140g (1mol) n-decene, 4.3g (0.02mol) ) tert-butyl peroxy-2-ethylhexanoate and 42.4g (0.002mol) with a particle size of 3.2mm and a carrier of Al 2 o 3 , The effective content is 0.5wt% Pd catalyst. The reactor is sealed and vacuumed, and replaced with high-purity nitrogen three times to make the oxygen content in the reactor less than 10ppm. Start stirring, heat to 90°C to initiate the reaction, then control the reaction temperature at 110°C for 1 hour, continue to feed hydrogen for catalytic hydrogenation reaction, keep the system pressure at 0.5 MPa ~ 0.6 MPa, until the pressure does not change anymore, the reaction time is 5 hours, After the reaction, at a system pressure of -0.1MPa to -0.099MPa and a heating temperature of 105°C to 110°C, vacuum distillation and purification were carried out to obtain 558g of white solid perfluorooctyldecane with a purity of 99.1% and a yield of 98.8%.

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Abstract

A perfluoro alkyl alkane preparation method comprises the following steps of: using perfluoroalkyl iodide and alkene as oligomers, performing addition reaction at 80-110 DEG C in the presence of an organic peroxide and a noble metal catalyst, blowing hydrogen in and continuously carrying out a catalytic hydrogenation reaction after the addition reaction, and performing underpressure distillation and purification after the reaction to prepare perfluoro alkyl alkane. The preparation method provided by the invention has the following advantages: the raw materials are safe and easily available; reaction condition is mild; the operation process is continuous and simple; the technology has good security; and the yield of the prepared perfluoro alkyl alkane is 98.2%-98.9% and its purity is 99.1%-99.5%. The invention is beneficial to industrial production.

Description

technical field [0001] The invention relates to a method for preparing perfluoroalkyl alkanes. Background technique [0002] Perfluoroalkyl alkanes, the general structural formula is F(CF 2 ) n (CH 2 ) m H, is an alkane compound in which a part of the hydrogen atoms in the aliphatic hydrocarbon chain are replaced by fluorine atoms. In practical applications, liquid perfluoroalkyl alkanes with shorter chain lengths are used as important active ingredients of fluorinated lubricating oil additives, while solid perfluoroalkyl alkanes with longer chain lengths are used as various fluorine-containing The main constituent of wax. [0003] At present, the preparation method of perfluoroalkyl alkanes is: first, the addition reaction is carried out by the addition of perfluoroalkyl halides and olefins, and then the reduction reaction is realized in two steps. The method cannot be operated continuously and is unfavorable for industrialized production. [0004] The patent of CN10...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/08C07C17/23
Inventor 魏潇魏奇谷峰
Owner 锦州恒通氟化学有限公司
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