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Preparation method of?bromofluoromethane

A technology of bromofluoromethane and CH3F, which is applied in the field of preparation of bromofluoromethane, can solve problems such as low yield of bromofluoromethane, high cost of raw materials, complicated process, etc., and achieve the effects of reducing production costs, high product yield, and good selectivity

Active Publication Date: 2014-04-30
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Currently reported bromofluoromethane synthesis technology has high cost of raw materials and complex process
[0004] As US5189229 uses tributyltin hydride to reduce dibromofluoromethane, although the yield is higher as 81.8%, the raw material tributyltin hydride is expensive, the production cost is high, and the process operation is complicated
[0005] EP0317125 uses sodium amalgam to reduce dibromofluoromethane, but the disadvantages are high raw material cost, complicated process and poor product selectivity
[0006] EP0503792 and EP0503793 respectively use high-valent metal fluorides and transition metal oxyfluorides to react with methylene bromide to synthesize bromofluoroalkanes. The disadvantage is that not only the yield of bromofluoromethane is low, but also the source of high-valent metal fluorides and transition metal oxyfluorides is difficult. complex process issues

Method used

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  • Preparation method of?bromofluoromethane

Examples

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Effect test

Embodiment 1

[0028] 1,1,2,2-Tetrafluoroethyl methyl ether at a liquid space velocity of 0.6h -1 Filled with 30ml of Mg-doped AlF 3 Catalyst (the doping amount of Mg is AlF 3 8% of the mass) in the 316L stainless steel U-shaped reactor ( ), a catalytic cracking reaction occurs at a temperature of 250 ° C, and the cracked gas produced is mainly difluoroacetyl fluoride and CH 3 F. Absorption of difluoroacetyl fluoride with ethanol in triethylamine gave CH with a purity of 96%. 3 F gas, then CH 3 F gas through anhydrous CaCl 2 Particles are dried, and after drying the CH 3 F and Br 2 Mixed and preheated at 150°C, then passed into a quartz reaction tube for thermal bromination reaction, CH 3 F and Br 2 The molar ratio is 1:1, the thermal bromination reaction temperature is 500°C, the reaction product is passed through the buffer bottle and then passed into NaOH and NaOH at 60°C 2 SO 3 Washing with aqueous solution to remove HBr and unreacted traces of Br 2 , then sampled and analyz...

Embodiment 2

[0030] 1,1,2,2-Tetrafluoroethyl methyl ether at a liquid space velocity of 0.4h -1 Filled with 30ml of AlF doped with Y 3 Catalyst (the doping amount of Y is AlF 3 4% of the mass) in the 316L stainless steel U-shaped reactor ( ), a catalytic cracking reaction occurs at a temperature of 280 ° C, and the cracked gas produced is mainly difluoroacetyl fluoride and CH 3 F. Absorption of difluoroacetyl fluoride with an aqueous solution of sodium hydroxide afforded CH with a purity of 97% 3 F gas, then CH 3 F gas is dried through molecular sieves, and the dried CH 3 F and Br 2 Mixed and preheated at 160°C, then passed into a quartz reaction tube for thermal bromination reaction, CH 3 F and Br 2 The molar ratio is 1:2, and the thermal bromination reaction temperature is 550°C. After the reaction product passed through the buffer bottle, it was passed through NaOH and NaOH at 60°C 2 SO 3 Washing with aqueous solution to remove HBr and unreacted traces of Br 2 , then sample...

Embodiment 3

[0032] 1,1,2,2-Tetrafluoroethyl methyl ether at a liquid space velocity of 0.6h -1 Filled with 30ml Na-doped AlF 3 Catalyst (the doping amount of Na is 1% of AlF3 mass) in the 316L stainless steel U-shaped reactor ( ), a catalytic cracking reaction occurs at a temperature of 270 ° C, and the cracked gas produced is mainly difluoroacetyl fluoride and CH 3 F. Absorption of difluoroacetyl fluoride with an aqueous solution of sodium hydroxide afforded CH with a purity of 97% 3 F gas, then CH 3 F gas is dried through a mixture of calcium oxide, molecular sieve and silica gel, and the dried CH3 F and Br 2 After mixing and preheating at 170°C, it is passed into a quartz reaction tube for thermal bromination reaction, CH 3 F and Br 2 The molar ratio is 1:3, and the thermal bromination reaction temperature is 600°C. After the reaction product passed through the buffer bottle, it was passed through NaOH and NaOH at 60°C 2 SO 3 Washing with aqueous solution to remove HBr and un...

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Abstract

The invention discloses a preparation method of bromofluoromethane. The method comprises the following steps: (1) subjecting 1,1,2,2-tetrafluoroethyl methyl ether to a catalytic cracking reaction in the presence of a catalyst, at the reaction temperature of 200-350 DEG C and the liquid space velocity at 0.3-0.8 / h, in order to obtain a reaction product containing CH3F, separating impurities in the reaction product and drying to obtain CH3F gas; and (2) mixing the CH3F gas obtained in the step (1) with Br2, preheating to 150-200 DEG C, and carrying out a thermal bromination reaction with reaction temperature of 400-800 DEG C, wherein a molar ratio of CH3F gas to Br2 is 1:0.8-5.5, separating impurities in the reaction products, removing water, cooling and distilling to obtain the bromofluoromethane product. The invention has the advantages of simple process, high yield, good selectivity and easy availability of raw materials.

Description

technical field [0001] The present invention relates to the preparation method of hydrobromocarbon, particularly a kind of preparation method of chlorofluoromethane. Background technique [0002] Bromofluoromethane (CH 2 BrF) is an important fluoromethylation reagent, which is more active than chlorofluoromethane when introducing a fluoromethyl group. It plays an important role in the synthesis of organic intermediates, fluorine-containing medicines, fluorine-containing pesticides and other chemicals. As we all know, it has Cephalosporins with broad-spectrum antibacterial activity have recently been found to have broader antibacterial activity after the introduction of fluoromethyl groups, especially for Pseudomonas aeruginosa; Ester, is an important cure for asthma drugs. [0003] Currently reported bromofluoromethane synthesis techniques have high raw material costs and complex processes. [0004] For example, in US5189229, the reduction of dibromofluoromethane with tri...

Claims

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Application Information

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IPC IPC(8): C07C19/14C07C17/10
Inventor 李宏峰周强王树华邓绍平
Owner JUHUA GROUP TECH CENT
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