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A kind of preparation method of 2-chloro-3,3,3-trifluoropropene

A technology of trifluoropropene and trifluoropropane, which is applied in the field of preparation of 2-chloro-3,3,3-trifluoropropene, can solve the problem that the inhibition of catalyst deactivation cannot be well achieved, the requirement of HF water content is high, and the product Problems such as low selectivity, to achieve the effect of being conducive to product diffusion, reducing product coking, and simple process flow

Active Publication Date: 2022-04-12
常州新东化工发展有限公司
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  • Abstract
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  • Claims
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Problems solved by technology

[0003] There are many preparation methods for HCFO-1233xf, for example: CN109651077A uses a chromium-containing fluorination catalyst to catalyze the reaction of polyhalopropene and HF under gas phase conditions to prepare HCFO-1233xf. This method requires high water content in HF and uses a Chromium heavy metal catalysis, large pollution
WO2007079431 and WO2008054781 use 1,1,2,3-tetrachloropropene as a raw material to synthesize HCFO-1233xf by gas-phase fluorination under the action of a chromium catalyst. The catalyst is easily deactivated in this method, and 2-chloro-3,3,3 - The selectivity of trifluoropropene decreases gradually with the activity
US20090030247 uses 1,1,1,2,3-pentachloropropane and 2,3,3,3-tetrachloropropene as raw materials, adding amines, hydroquinones or other stabilizers to synthesize HCFO-1233xf by catalytic fluorination , the product selectivity of this method is low, and the purpose of suppressing catalyst deactivation cannot be well achieved

Method used

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  • A kind of preparation method of 2-chloro-3,3,3-trifluoropropene

Examples

Experimental program
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Effect test

Embodiment 1

[0033] The photochlorination reaction kettle is equipped with a light source of partial ultraviolet wavelength and 2,3-dichloro-1,1,1-trifluoropropane. The feed flow rate of the 2,3-dichloro-1,1,1-trifluoropropane absorption liquid at the top of the rectification tower to the light chlorination reactor is 10mol / h, and the 3,3,3-trifluoropropene is fed to the light chlorine The feed flow rate of the chemical reactor is 40.8mol / h, the feed flow rate of chlorine gas to the photochlorination reactor is 40mol / h, the reaction temperature is 45°C, and the reaction residence time is 0.5h.

[0034] After the reaction is completed, the molar fraction of each component in the photochlorination reactor is: 2,3-dichloro-1,1,1-trifluoropropane 0.997, 2,3,3-trichloro-1,1,1-tri Fluoropropane 0.001, 3,3,3-trifluoropropene 0.002, use the material pump to transport the material in the photochlorination reactor to the rectification tower at a liquid phase flow rate of 50.8mol / h, and 3,3, The fee...

Embodiment 2

[0038]The photochlorination reaction kettle is equipped with a light source of partial ultraviolet wavelength and 2,3-dichloro-1,1,1-trifluoropropane. The feed flow rate of the 2,3-dichloro-1,1,1-trifluoropropane absorption liquid at the top of the rectification tower to the light chlorination reactor is 10mol / h, and the 3,3,3-trifluoropropene is fed to the light chlorine The feed flow rate of the chemical reactor is 40.8mol / h, the feed flow rate of chlorine gas to the photochlorination reactor is 40mol / h, the reaction temperature is 35°C, and the reaction residence time is 5h.

[0039] After the reaction is completed, the molar fraction of each component in the chlorination reactor is: 2,3-dichloro-1,1,1-trifluoropropane 0.995, 2,3,3-trichloro-1,1,1-trifluoro Propane 0.002, 3,3,3-trifluoropropene 0.003, use the material pump to transport the material in the photochlorination reactor to the rectification tower at a liquid phase flow rate of 50.8mol / h, and transfer the 3,3,3 -...

Embodiment 3

[0043] The photochlorination reaction kettle is equipped with a light source of partial ultraviolet wavelength and 2,3-dichloro-1,1,1-trifluoropropane. The feed flow rate of the 2,3-dichloro-1,1,1-trifluoropropane absorption liquid at the top of the rectification tower to the light chlorination reactor is 10mol / h, and the 3,3,3-trifluoropropene is fed to the light chlorine The feed flow rate of the chemical reactor is 40.8mol / h, the feed flow rate of chlorine gas to the photochlorination reactor is 40mol / h, the reaction temperature is 75°C, and the reaction residence time is 0.5h.

[0044] After the reaction is completed, the molar fraction of each component in the chlorination reactor is: 2,3-dichloro-1,1,1-trifluoropropane 0.996, 2,3,3-trichloro-1,1,1-trifluoro Propane 0.001, 3,3,3-trifluoropropene 0.003, use the material pump to transport the material in the photochlorination reactor to the rectification tower at a liquid phase flow rate of 50.8mol / h, and transfer the 3,3,3...

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Abstract

The invention discloses a preparation method of 2-chloro-3,3,3-trifluoropropene, which mainly includes the following steps: (1) passing 3,3,3-trifluoropropene and chlorine gas into the ,3-dichloro-1,1,1-trifluoropropane in the light chlorination reactor; (2) the reactants in the photochlorination reactor in step (1) are continuously added to the rectification tower, and the tower still Obtain 2,3-dichloro-1,1,1-trifluoropropane; (3) use a metering pump to add 2,3-dichloro-1,1,1-trifluoropropane obtained in step (2) into gasification After being vaporized, it is mixed with oxygen-deficient nitrogen gas, and then enters a fixed-bed reactor equipped with a catalyst for gas-phase catalytic dehydrochlorination; (4) Pass the reaction gas from the fixed-bed reactor in step (3) through the primary cooler, The secondary cooler is condensed to obtain the material of crude 2-chloro-3,3,3-trifluoropropene, and the crude 2-chloro-3,3,3-trifluoropropene is purified by distillation. The invention has the advantages of high product selectivity, simple process and easy industrialization.

Description

technical field [0001] The invention relates to the technical field of synthesis of intermediates, in particular to a preparation method of 2-chloro-3,3,3-trifluoropropene. Background technique [0002] 2-Chloro-3,3,3-trifluoropropene (HCFO-1233xf) can be used as an intermediate for the preparation of various fluorocarbons, such as for the synthesis of HFC-245fa, HFO-1234yf, etc., and can also be used as a monomers of a polymer. [0003] There are many preparation methods for HCFO-1233xf, for example: CN109651077A uses a chromium-containing fluorination catalyst to catalyze the reaction of polyhalopropene and HF under gas phase conditions to prepare HCFO-1233xf. This method requires high water content in HF and uses Chromium is catalyzed by heavy metals, and the pollution is relatively large. WO2007079431 and WO2008054781 use 1,1,2,3-tetrachloropropene as a raw material to synthesize HCFO-1233xf by gas-phase fluorination under the action of a chromium catalyst. This method...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/25C07C21/18
CPCC07C17/25C07C17/04C07C21/18C07C19/10
Inventor 王顺利孙运林张驰朱成明马凯吴发明刘向超董亮陶文平
Owner 常州新东化工发展有限公司
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