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Method for producing 1-chlorine-3,3,3-triflupropylene

A technology of trifluoropropene and pentachloropropane is applied in the field of gas-phase fluorination reaction to obtain 1-chloro-3, which can solve the problems of high reaction temperature, low yield of HCFC-1233zd, and fast carbon formation rate on the surface of catalyst.

Active Publication Date: 2007-09-05
ZHEJIANG FLUORINE CHEM NEW MATERIAL
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  • Abstract
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AI Technical Summary

Problems solved by technology

However, the reaction temperature is higher, resulting in a faster rate of carbon formation on the surface of the catalyst.
[0005] In the above-mentioned preparation method of HCFC-1233zd, there are respectively the problems of high reaction temperature and low yield of HCFC-1233zd

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 10.97g SnCl 4 Dissolve in 100ml of distilled water acidified with hydrochloric acid to make an impregnation solution, and then add 100g 3 The carrier is placed in the immersion solution, and after immersing for 5 hours, the water is evaporated on a rotary evaporator at 60°C to obtain Sn with a tin content of 5% 4+ / AlF 3 Fluorination catalyst. Before the reaction, hydrogen fluoride was separately introduced in advance to fluorinate the catalyst.

[0023] Add 50ml of 5% Sn to a carbon steel pipe with an inner diameter of 38mm 4+ / AlF 3 The catalyst was heated to 150°C in a nitrogen stream. Stop the nitrogen flow, and feed HF and HCC-240fa to react, control the molar ratio of HF to HCC-240fa to 8:1, and the contact time is 5 seconds. After 20 hours of reaction, the reaction product is washed with water and alkali to remove HCl and HF. , The conversion rate of HCC-240fa and the selectivity of HCFC-1233zd were analyzed by gas chromatography. The results are shown in Table 1.

Embodiment 2

[0025] The same operation as in Example 1, except that the reaction temperature was changed to 100°C, and the reaction results are shown in Table 1.

Embodiment 3

[0027] The same operation as in Example 1, except that the reaction temperature was changed to 180°C, and the reaction results are shown in Table 1.

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PUM

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Abstract

A process for preparing 1-Cl-3,3,3-trifluoropropene (HCFC-1233zd) features the catalytic gas-phase fluorinating reaction between HF and 1,1,1,3,3-pentapropane (HCC-240fa) at 100-200 deg.C. Its catalyst is also disclosed.

Description

Technical field [0001] The present invention relates to a preparation method of 1-chloro-3,3,3-trifluoropropene (HCFC-1233zd), in particular to a method for preparing hydrogen fluoride and 1,1,1,3,3-pentachloropropane (HCC- 240fa) as a raw material, a method for preparing 1-chloro-3,3,3-trifluoropropene by gas-phase fluorination in the presence of a fluorination catalyst. Background technique [0002] 1-Chloro-3,3,3-trifluoropropene is a raw material for the production of 1,1,1,3,3-pentafluoropropane (HFC-245fa). In addition, it is also used for the production of polymers Fluorine-containing monomers and the introduction of CF into organics 3 The raw material for the structural block of the group. [0003] Japanese patent JP9194404 discloses a kind of Cr 2 O 3 / Al 2 O 3 As a catalyst, it is a method to synthesize HCFC-1233zd by fluorinating HCC-240fa in the gas phase at 150℃~300℃. In this method, the yield of HCFC-1233zd is less than 90%, and the yield of HCFC-1233zd decreases as...

Claims

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Application Information

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IPC IPC(8): C07C19/10C07C17/20B01J27/135B01J27/138
Inventor 吕剑张伟王博寇联岗马洋博杜咏梅
Owner ZHEJIANG FLUORINE CHEM NEW MATERIAL
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