Method of gas phase synthesis of 1,1,1,4,4,4-hexafluoropropylene-2-chlorine-2-butene

A gas-phase synthesis and butene technology, applied in halogen substitution preparation, organic chemistry, etc., can solve the problems of expensive raw materials, difficult separation, low selectivity, etc., to achieve improved yield and selectivity, rich sources of raw materials, and safe operation high effect

Active Publication Date: 2016-01-06
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of the first method is very low, and there are many by-products, the selectivity is low, and the separation is difficult
The second method uses noble metal rhodium as a catalyst, and the raw material is relatively expensive, and it is not easy to obtain, and the yield is also low

Method used

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  • Method of gas phase synthesis of 1,1,1,4,4,4-hexafluoropropylene-2-chlorine-2-butene

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Put a certain amount of catalyst AlF into a stainless steel gas phase reactor made of 316L material and a pipe diameter φ of 10mm 3 , raising the temperature to 240 °C. Add hexachloro-1,3-butadiene and HF respectively into the steam heater to vaporize them. Add the steam of hexachloro-1,3-butadiene into the meteorological reactor with a metering pump, and the flow rate is 20ml / min; add the HF vapor into the fixed bed with a metering pump, and the flow rate is 160ml / min (that is, hexachloro-1, The molar ratio of 3-butadiene to HF is 1:8), and the residence time of the reaction is 1s. The product is introduced into a condenser to be condensed and purified by rectification. The yield of 1,1,1,4,4,4-hexafluoro-2-chloro-2-butene was 82.5% and the selectivity was 90.7%.

Embodiment 2

[0027] Put a certain amount of catalyst AlF into a stainless steel gas phase reactor made of 316L material and a pipe diameter φ of 10mm 3 , raising the temperature to 320 °C. Add hexachloro-1,3-butadiene and HF respectively into the steam heater to vaporize them. Add the steam of hexachloro-1,3-butadiene into the fixed bed with a metering pump, and the flow rate is 20ml / min; add the HF vapor into the fixed bed with a metering pump, and the flow rate is 160ml / min (that is, hexachloro-1,3 - The molar ratio of butadiene to HF is 1:8), and the residence time of the reaction is 2.5s. The product is introduced into a condenser to be condensed and purified by rectification. The yield of 1,1,1,4,4,4-hexafluoro-2-chloro-2-butene was 84.2%, and the conversion was 92%.

Embodiment 3

[0029] Put a certain amount of catalyst SbF into a stainless steel gas phase reactor made of 316L material and a pipe diameter φ of 10mm 3 , raising the temperature to 400 °C. Add hexachloro-1,3-butadiene and HF respectively into the steam heater to vaporize them. Add the steam of hexachloro-1,3-butadiene into the fixed bed with a metering pump, and the flow rate is 20ml / min; add the HF vapor into the fixed bed with a metering pump, and the flow rate is 200ml / min (that is, hexachloro-1,3 - The molar ratio of butadiene to HF is 1:10), and the residence time of the reaction is 4s. The product is introduced into a condenser to be condensed and purified by rectification. The yield of 1,1,1,4,4,4-hexafluoro-2-chloro-2-butene was 85.8%, and the conversion was 95.5%.

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Abstract

The invention discloses a method of gas phase synthesis of 1,1,1,4,4,4-hexafluoropropylene-2-chlorine-2-butene. Gas-phase hexachloro-1,3-butadiene and gas-phase hydrofluoric acid serve as main materials, under the action of one or more mixtures of catalysts of AlF3, CrF3, ZnF2, SbF3 and SbF5, the gas-phase hexachloro-1,3-butadiene and the gas-phase hydrofluoric acid are introduced into a gas-phase reactor made of 316L stainless steel, continuous gaseous phase fluorination is conducted, the reaction temperature is controlled to range from 220 DEG C to 820 DEG C, the retention time of a reaction ranges from 0.1 s to 10 s, the molar ratio of hexachloro-1,3-butadiene to the hydrofluoric acid is 1 to 6-14, and a target product 1,1,1,4,4,4-hexafluoropropylene-2-chlorine-2-butene is obtained by conducting cooling, purification and rectification on a product obtained through a reaction. The method of the gas phase synthesis of the 1,1,1,4,4,4-hexafluoropropylene-2-chlorine-2-butene has the advantages of being simple in process, low in cost, high in yield, capable of achieving continuous production, suitable for industrial production and the like.

Description

technical field [0001] The invention relates to a gas phase synthesis method of 1,1,1,4,4,4-hexafluoro-2-chloro-2-butene, which belongs to the technical field of organic fluorine chemical industry. Background technique [0002] 1,1,1,4,4,4-hexafluoro-2-chloro-2-butene, the molecular formula is CF 3 CCl=CHCF 3 , is a very important organic fluorine-containing compound, under the conditions of catalytic hydrogenation and alkali elution to remove HCl, an important chemical product hexafluoro-2-butene can be synthesized, and the ODP value of hexafluoro-2-butene is 0. The GWP value is very low, it is the fourth generation of new foaming agent and refrigerant, and has a good market prospect. In addition, 1,1,1,4,4,4-hexafluoro-2-chloro-2-butene can also be used to synthesize trifluoroacetic acid and the like. [0003] There are not many reports on the synthesis of 1,1,1,4,4,4-hexafluoro-2-chloro-2-butene in existing patents and literatures. There are several methods: [0004]...

Claims

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Application Information

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IPC IPC(8): C07C17/21C07C21/18
Inventor 周强朱宏宇王树华王宗令罗孟飞方伟
Owner JUHUA GROUP TECH CENT
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