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

A technology of trifluoropropene and gas phase fluorination, which is applied in the fields of dehydrohalogenation preparation, chemical instruments and methods, halogen substitution preparation, etc., and can solve the problems of many reaction steps and low yield of HCFO-1233xf

Active Publication Date: 2010-12-15
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. In the method, 2,3-dichloropropene reacts with chlorine gas to generate 1,1,2,2,3-pentachloro Propane, then 1,1,2,2,3-Pentachloropropane dehydrochlorination with a strong base to 1,1,2,3-Tetrachloropropene, finally 1,1,2,3-Tetrachloropropene and hydrogen fluoride Mixing through the top loading FeCl 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 highest yield is only 85%, but this method has many reaction steps, three steps of reaction steps, and the yield of HCFO-1233xf is low

Method used

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Examples

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Comparison scheme
Effect test

preparation example Construction

[0015] Preparation of fluorination catalyst

[0016] Dissolve ferric chloride in water, react with precipitant ammonia water at 50°C, adjust the pH value of the reaction solution in the range of 7.0 to 7.5, make it fully precipitate under stirring conditions, and put the formed ferric hydroxide slurry Hot filtration followed by overnight drying at 120°C for 12 hours yielded γ-Fe(OH) 3 .

[0017] Calcium carbonate and γ-Fe(OH) 3 Mix evenly at a mass ratio of 60:40, press into tablets to form a catalyst precursor. The catalyst precursor was calcined in a muffle furnace at 450°C for 8 hours, then loaded into a tubular reactor, heated to 300°C, fed with hydrogen fluoride gas for fluorination for 1 hour, then raised to 400°C at a heating rate of 1°C / min, and continued After fluorination for 8 hours, a calcium fluoride-based fluorination catalyst was obtained.

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 was charged, and HF and HCC-240ab were introduced to react, and the molar ratio of HF / HCC-240ab was controlled to be 15:1, the contact time is 10 seconds, the reaction temperature is 280 ° 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 HCC-240ab is 100% by gas chromatography analysis, and the conversion rate of HCFO-1233xf The selectivity was 94%.

Embodiment 2

[0021] The operation is basically the same as in Example 1, except that the reaction temperature is changed to 260° 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 HCC-240ab to react, control the molar ratio of HF / HCC-240ab to 15:1, contact time is 10 seconds, reaction temperature is 260°C, after reaction for 20 hours, the reaction product is washed with water and alkali to remove HCl and HF, the conversion rate of HCC-240ab was 96% by gas chromatography analysis, and the selectivity of HCFO-1233xf was 92%.

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Abstract

The invention discloses a method for preparing 2-chloro-3,3,3-trifluoropropene by gas-phase fluorination. In the method, 1,1,1,2,2-pentachlororopropane or 1,1,1,2,3-pentachlororopropane is used as a raw material, and the method comprises the following step of: in the presence of the action of a fluorinated catalyst, introducing hydrogen fluoride to react with the 1,1,1,2,2-pentachlororopropane orthe 1,1,1,2,3-pentachlororopropane, wherein the reaction condition comprises that the molar ratio of the hydrogen fluoride to an organic matter is (10-20):1, the contact time is 2-20 seconds, the reaction temperature is 260-300 DEG C, the precursors of the fluorinated catalyst comprise the following components in percentage by weight: 60 percent of calcium carbonate and 40 percent of gamma iron hydroxide, and the fluorinated catalyst can be prepared from the following method of: uniformly mixing the precursors of the fluorinated catalyst, press-molding, roasting at 450 DEG C, and then fluorinating by using hydrogen fluoride gas at 400 DEG C to prepare the fluorinated catalyst. The invention is mainly applied to preparing the 2-chloro-3,3,3-trifluoropropene.

Description

technical field [0001] The invention relates to a preparation method of 2-chloro-3,3,3-trifluoropropene (HCFO-1233xf), in particular to a one-step gas-phase fluorination of 1,1,1 under the catalysis of a fluorination catalyst. , 2,2-pentachloropropane (HCC-240ab) or 1,1,1,2,3-pentachloropropane (HCC-240db) the method for preparing HCFO-1233xf. 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. In the method, 2,3-dichloropropene reacts with chlorine gas to generate 1,1,2,2,3-pentachloro Propane, then 1,1,2,2,3-Pentachloropropane dehydrochlorination with a strong base to 1,1,2,3-...

Claims

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Application Information

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IPC IPC(8): C07C21/18C07C17/25C07C17/20B01J27/138
Inventor 吕剑王博曾纪珺李凤仙刘波杜咏梅秦越赵锋伟封利民
Owner 山东华安近代环保科技有限公司