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Method for preparing 2-chloro-3,3,3-trifluoropropene by gas-phase fluorination

A gas-phase fluorination and trifluoropropene technology, applied in the field of preparing HCFO-1233xf, can solve the problems of low reaction yield and many reaction steps, etc.

Active Publication Date: 2014-05-14
山东华安近代环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] U.S. Patent US20070197842 discloses a method for preparing HCFO-1233xf using 2,3-dichloropropene as a raw material. The reaction steps of the method are three steps. First, 2,3-dichloropropene reacts with chlorine to generate 1,1,2, 2,3-Pentachloropropane, then 1,1,2,2,3-Pentachloropropane is dehydrochlorinated with a strong base to give 1,1,2,3-Tetrachloropropene, and finally 1,1,2,3 - Tetrachloropropene and hydrogen fluoride are mixed and filled with FeCl through the upper layer 3 The lower layer of / C catalyst is filled with Cr 2 o 3 Catalyst reactor, gas phase fluorination reaction to produce HCFO-1233xf, the reaction yield is 85%, but this method has many reaction steps and the reaction yield is low

Method used

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Examples

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Effect test

preparation example Construction

[0013] Preparation of fluorination catalyst:

[0014] Calcium oxalate and gamma ferric hydroxide are uniformly mixed according to their mass ratio of 40:60, pressed and molded to obtain a catalyst precursor, and after roasting at 380°C, fluorinated with hydrogen fluoride gas at 350°C to obtain a fluorination catalyst. The gamma ferric hydroxide used in the present invention can be obtained by the following method: dissolve the soluble salt of ferric iron in water, add a precipitating agent at 50-60°C, control the pH of the solution between 7.0-7.5, and precipitate After filtering, washing and drying, gamma ferric hydroxide is obtained; the soluble salt of ferric iron mentioned above can be ferric nitrate, ferric sulfate, ferric chloride or ferric oxalate, preferably ferric nitrate; precipitating agent can be ammonia, sodium hydroxide, carbonic acid Sodium, sodium bicarbonate or ammonia water, preferably ammonia water.

[0015] The temperature for the fluorination treatment of...

Embodiment 1

[0019] In a nickel tube fixed-bed tubular reactor with an internal diameter of 38mm, 60ml of the above-mentioned calcium fluoride-based fluorination catalyst is charged, and HF and HCFC-1231 are introduced to react, and the molar ratio of HF / HCFC-1231 is controlled to be 15:1, the contact time is 10 seconds, the reaction temperature is 200°C, after 20 hours of reaction, the reaction product is washed with water and alkali to remove HCl and HF, and the conversion rate of HCFC-1231 is 100% by gas chromatography analysis. HCFO-1233xf The selectivity is 99.0%.

Embodiment 2

[0021] The operation is basically the same as in Example 1, except that the reaction temperature is changed to 160° C., and 60 ml of the calcium fluoride-based fluorination catalyst prepared above is loaded into a nickel tube fixed-bed tubular reactor with an inner diameter of 38 mm. , feed HF and HCFC-1231 to react, control the molar ratio of HF / HCFC-1231 to 15:1, the contact time is 10 seconds, the reaction temperature is 160°C, after 20 hours of reaction, the reaction product is washed with water and alkali to remove HCl and HF, the conversion rate of HCFC-1231 was 96% by gas chromatography analysis, and the selectivity of HCFO-1233xf was 96.0%.

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Abstract

The invention discloses a method for preparing 2-chloro-3,3,3-trifluoropropene by gas-phase fluorination, which comprises the following steps: introducing hydrogen fluoride and reacting hydrogen fluoride with 1,1,2-trichloro-3-fluoropropene (HCFC-1231) serving as a raw material in the presence of a fluorination catalyst, wherein the reaction conditions include a contact time of 2 to 20 seconds and a reaction temperature of 160 to 240 DEG C, and the molar ratio of hydrogen fluoride to the organic material is (5-30):1. The precursor of the fluorination catalyst used in the invention comprises the following components in percentage by mass: 40 percent of calcium oxalate and 60 percent of gamma iron hydroxide. The fluorination catalyst can be obtained by a method which comprises: mixing the precursor of the fluorination catalyst uniformly; subjecting the mixture to press forming; roasting at 380 DEG C; fluorinating at 350 DEG C by using hydrogen fluoride gas; and thus, obtaining the fluorination catalyst. The method is mainly used for preparing 2-chloro-3,3,3-trifluoropropene.

Description

technical field [0001] The invention relates to a method for preparing 2-chloro-3,3,3-trifluoropropene by gas-phase fluorination, in particular to a one-step gas-phase fluorination of 1,1,2-trifluoropropene under the catalysis of a fluorination catalyst. Method for preparing HCFO-1233xf from chloro-3-fluoropropene (HCFC-1231). Background technique [0002] 2-Chloro-3,3,3-trifluoropropene (HCFO-1233xf) is a raw material used in the production of 2,3,3,3-tetrafluoropropene (HFO-1234yf), and it is also used in the production of Fluorinated monomers of polymers and introduction of CF into organic matter 3 The structural block raw material of the group. [0003] U.S. Patent US20070197842 discloses a method for preparing HCFO-1233xf using 2,3-dichloropropene as a raw material. The reaction steps of the method are three steps. First, 2,3-dichloropropene reacts with chlorine to generate 1,1,2, 2,3-Pentachloropropane, then 1,1,2,2,3-Pentachloropropane is dehydrochlorinated with a ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C21/18C07C17/20
Inventor 吕剑秦越毛伟王博寇联岗刘波张伟韩升马辉
Owner 山东华安近代环保科技有限公司