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Preparation method of trans-1, 2-dichloro-3, 3, 3-trifluoropropene

A technology of trifluoropropene and pentachloropropene is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc., and can solve the problems of low selectivity, unclear stereo configuration, low reaction conversion rate, etc.

Active Publication Date: 2016-07-13
XIAN MODERN CHEM RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this chlorofluorination reaction, the reaction raw material 1,1,1-trifluoropropene is not easy to obtain, and the content of HCFO-1223xd produced varies in the range of 0% to 20.2%, the selectivity is low, the conversion rate is low, and it is not clear stereo configuration
[0005] At present, there are few methods for preparing HCFO-1223xd disclosed, and there are generally low reaction conversion rate and low selectivity. More importantly, the product is a mixture of cis and trans isomers or an undefined stereo configuration. A public report on the one-way preparation of tran-HCFO-1223xd

Method used

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  • Preparation method of trans-1, 2-dichloro-3, 3, 3-trifluoropropene

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Experimental program
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Embodiment 1

[0031] Catalyst preparation: according to a certain proportion, weigh Al(NO 3 ) 2 9H 2 O, Mg(NO 3 ) 2 ·6H 2 O and Cr(NO 3 ) 2 9H 2O, dissolved in deionized water, under the condition of constant stirring, dropwise add ammonia water with a mass fraction of 10%, adjust the pH control to about 7-9, about 5h, centrifuge after washing, and then dry at 120°C , then calcined at 200°C for 1 hour, raised to 320°C at 5°C / min, fired for 2 hours, raised to 400°C at 10°C / min, fired for 4 hours, and finally activated by hydrogen fluoride at 200°C-380°C.

[0032] In a fixed-bed tubular reactor with an internal diameter of 38 mm, 50 ml of the above-mentioned Mg-Al-Cr composite catalyst was loaded, wherein the molar ratio of Mg, Al, and Cr was 2:1:7, and the catalyst was dried at 200 ℃, N 2 and 1,1,1,2,2,3-hexachloropropane (HCC-230ab), react under atmospheric pressure (normal pressure), the molar ratio of the two is 5:1, the contact time is 5 seconds, the reaction product After wash...

Embodiment 2～5

[0038] Embodiment 2~5 prepares 1,1,2,3,3-pentachloropropene according to the same preparation method in embodiment 1, difference is that the reaction temperature in embodiment 1 is 200 ℃, and embodiment 2~5 The reaction temperatures were 120°C, 150°C, 240°C, and 280°C in sequence, and the results are shown in Table 1.

[0039] Table 1

[0040]

[0041]

Embodiment 6～8

[0043] Examples 6-8 Prepare 1,1,2,3,3-pentachloropropene according to the same method as in Example 1, except that the molar ratio of Mg, Al, and Cr in the catalyst in Example 1 is 2:1 : 7, while in Examples 6-8, the molar ratios of the three are 1: 1: 8, 2: 2: 6, 2: 3: 5, and the reaction results are shown in Table 2.

[0044] Table 2

[0045]

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PUM

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Abstract

The invention discloses a preparation method of trans-1, 2-dichloro-3, 3, 3-trifluoropropene. The method comprises the following steps: a, 1,1,1,2,2,3-hexachloropropane and / or 1,1,1,2,3,3-hexachloropropane are reacted with the existence of diluent gas and a catalyst, a gas-phase reaction is carried out for removing hydrogen chloride, and 1,1,2,3,3-pentachloropropene is produced; b. a liquid phase fluoridation reaction is carried out between 1,1,2,3,3-pentachloropropene and hydrogen fluoride with the existence of a liquid phase fluorination catalyst, or a gas phase fluorination reaction is carried out between 1,1,2,3,3-pentachloropropene and hydrogen fluoride with the existence of a gas phase fluorination catalyst; c. washing, alkali washing and drying are carried out for reaction products in the step b, and trans-1, 2-dichloro-3, 3, 3-trifluoropropene is obtained by rectification in a condition with normal pressure. The method has the characteristics of high reaction selectivity, high conversion rate and high stereoselectivity, and is mainly used for preparing trans-1, 2-dichloro-3, 3, 3-trifluoropropene.

Description

technical field [0001] The invention relates to a preparation method of hydrochlorofluoroolefins, in particular to a preparation method of trans-1,2-dichloro-3,3,3-trifluoropropene (tran-HCFO-1223xd). Background technique [0002] Because fully halogenated chlorofluorocarbons (CFCs) pose serious hazards to the Earth's ozone layer, the fluorocarbon industry has shifted to developing safer alternatives containing fewer or no chlorine substitutions, such as hydrochlorofluoroolefins (HCFOs), hydrogen Fluorocarbons (HFCs), Hydrofluoroolefins (HFOs). Trans-1,2-dichloro-3,3,3-trifluoropropene (HCFO-1223xd), as one of HCFOs, can be used as raw materials and intermediates for the preparation of various fluorocarbons, such as cis-1, 1,1,4,4,4-hexafluoro-2-butene (cis-HCFO-1336), 1,1,1,3,3-pentafluoropropane (HFC-245fa), 2,3,3, 3-Tetrafluoropropene (HFO-1234yf), can also be used to introduce CF into fluorine-containing functional materials 3 The raw material of group structure block...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/18C07C17/35
Inventor 马辉吕剑李凤仙王博万洪赵波秦越郝志军杜咏梅韩升
Owner XIAN MODERN CHEM RES INST
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