Method for preparing e-1,1,1,4,4,4-hexafluoro-2-butene by gas phase fluorination

A technology of gas-phase fluorination and tetrafluorobutatriene, which is applied in organic chemical methods, chemical instruments and methods, preparation of halogenated hydrocarbons, etc., can solve problems such as low yield per pass, environmental pollution, low yield per pass, etc. Achieve long service life, high activity, high yield per pass

Active Publication Date: 2021-07-16
泉州宇极新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The product 1,1,1,4,4,4-hexafluoro-2-butene of the above technical route is Z-1,1,1,4,4,4-hexafluoro-2-butene and E-1 , the mixture of 1,1,4,4,4-hexafluoro-2-butene mainly has the following defects: (1) The above-mentioned routes all involve liquid phase reactions, and a large amount of solvents and solid reagents will be used to enter KF and zinc powder etc., will produce a large amount of waste liquid and waste solid, which will seriously pollute the environment; (2) Route 4 has serious corrosion and pollution problems, in which the liquid phase system composed of antimony pentachloride or titanium tetrachloride and HF is harmful to the equipment and equipment The corrosiveness is extremely strong, and the pollution produced is also extremely serious; (3) The per-pass yield of E-1,1,1,4,4,4-hexafluoro-2-butene is low, although at 1,1 ,1,4,4,4-hexafluoro-2-butene in the mixed product, compared with Z-1,1,1,4,4,4-hexafluoro-2-butene, E-1, The proportion of 1,1,4,4,4-hexafluoro-2-butene is a higher configuration, but for example: route one, 1,2-dichloro-1,1,4,4,4-five The yield of 1,1,1,4,4,4-hexafluoro-2-butene from fluorobutane is 89.6%, 2-chloro-1,1,1,4,4,4-hexafluorobutene The yield of 1,1,1,4,4,4,4-hexafluoro-2-butene with alkane as raw material is 82.5%, and 1,1,1,4,4,4-hexafluoro-2-butene in route two Yield is 54.6%, and routes three to four routes are longer, and its one-way yield is not high
Thus, it can be inferred that the single-pass yield of E-1,1,1,4,4,4-hexafluoro-2-butene in the above technical route is not high

Method used

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  • Method for preparing e-1,1,1,4,4,4-hexafluoro-2-butene by gas phase fluorination

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Embodiment 1

[0038] Preparation of fluorination catalyst: According to the percentage composition of tungsten and cobalt elements of 90% and 10%, tungsten trichloride and cobalt nitrate are dissolved in water, concentrated ammonia water is added dropwise for precipitation, the pH value is adjusted to 7.5, and then aged 24 hours, washed with water, filtered, dried in an oven at 120°C for 15 hours, crushed the obtained solid, and pressed into tablets to obtain a catalyst precursor. Put 10 mL of the catalyst precursor into a Monel with an inner diameter of 1 / 2 inch and a length of 30 cm Tubular reactor made of material, filled with nitrogen and baked at 350°C for 12 hours, nitrogen space velocity is 200h -1 , and then lower the temperature to 300°C, and at the same time pass a mixed gas composed of hydrogen fluoride and nitrogen with a mass ratio of 1:2, and the total space velocity of the gas is 220h -1 , activate for 12 hours, stop the above mixed gas, and prepare the tungsten-based catalys...

Embodiment 2

[0052] A tubular reactor made of Inconium alloy with an inner diameter of 1 / 2 inch and a length of 30 cm was filled with 10 mL of the catalyst prepared in Example 1. The reaction conditions are as follows: the reaction temperature is 350°C, the ratio of tetrafluorobutatriene to hydrogen fluoride is 1:20, the contact time is 20s, and the reaction pressure is 0.1MPa. After running for 10 hours, the reaction product was washed with water, washed with alkali and dried, and the gas phase organic phase was taken for GC analysis. The reaction results are: the conversion rate of tetrafluorobutatriene is 95.4%, the selectivity of E-1,1,1,4,4,4-hexafluoro-2-butene is 99.6%, Z-1,1, The selectivity to 1,4,4,4-hexafluoro-2-butene was 0.4%.

Embodiment 3

[0054] A tubular reactor made of Inconium alloy with an inner diameter of 1 / 2 inch and a length of 30 cm was filled with 10 mL of the catalyst prepared in Example 1. The reaction conditions are as follows: the reaction temperature is 400°C, the ratio of tetrafluorobutatriene to hydrogen fluoride is 1:20, the contact time is 20s, and the reaction pressure is 0.1MPa. After running for 10 hours, the reaction product was washed with water, washed with alkali and dried, and the gas phase organic phase was taken for GC analysis. The reaction results are: the conversion rate of tetrafluorobutatriene is 100%, the selectivity of E-1,1,1,4,4,4-hexafluoro-2-butene is 99.2%, Z-1,1, The selectivity to 1,4,4,4-hexafluoro-2-butene was 0.8%.

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Abstract

The invention discloses a method for preparing E-1,1,1,4,4,4-hexafluoro-2-butene by gas-phase fluorination, namely: in the presence of a fluorination catalyst, tetrafluorobutatriene or tetrafluorobutatriene Chloroprene, fluorinated with hydrogen fluoride to give E-1,1,1,4,4,4-hexafluoro-2-butene. The invention is mainly used for producing E-1,1,1,4,4,4-hexafluoro-2-butene with high efficiency and continuous circulation.

Description

technical field [0001] The invention relates to a method for preparing E-1,1,1,4,4,4-hexafluoro-2-butene in the gas phase, in particular to a method for tetrafluorobutatriene or tetrachlorobutene in the presence of a fluorination catalyst Catalytic fluorination of butatriene with hydrogen fluoride to obtain E-1,1,1,4,4,4-hexafluoro-2-butene. Background technique [0002] Up to now, the synthesis routes of 1,1,1,4,4,4-hexafluoro-2-butene mainly include the following types: [0003] Route 1: U.S. Patent US5463150 reports that in sulfolane solvent, 190 ° C, 1,2-dichloro-1,1,4,4,4-pentafluorobutane or 2-chloro-1,1,1,4, The liquid-phase fluorination of 4,4-hexafluorobutane with KF gave 1,1,1,4,4,4-hexafluoro-2-butene in yields of 89.6% and 82.5%, respectively. [0004] Route 2: US Patent US5516951 reports the coupling of 1,1-dichloro-3,3,3-trifluoroethane with copper powder and diethylamine to obtain 1,1,1,4,4,4-hexafluoro -2-butene, its conversion rate is as high as 62%, and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/087C07C17/21B01J23/888B01J23/882B01J23/86B01J23/30C07C21/18B01J27/132B01J27/138
CPCB01J23/30B01J23/864B01J23/882B01J23/888B01J27/132B01J27/138C07B2200/09C07C17/087C07C17/21C07C21/18
Inventor 张呈平张妮庆飞要郭勤
Owner 泉州宇极新材料科技有限公司
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