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Preparation method of 2,3,3,3-tetrafluoropropene

A technology of trifluoropropene and propyne, which is applied in the direction of dehydrohalogenation preparation, organic chemistry, etc., and can solve the problem of low total reaction yield

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

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Problems solved by technology

But the reaction total yield of the synthetic method of this HCFC-1233xf is lower

Method used

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  • Preparation method of 2,3,3,3-tetrafluoropropene

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preparation example Construction

[0021] Catalyst preparation

[0022] 43.56g FeCl 3 Dissolved in 100ml of distilled water to make an impregnation solution, then 100g of CaF 2 The carrier is placed in the impregnation solution, and after immersion for 5 hours, the water is evaporated to dryness on a rotary evaporator at 60°C to obtain Fe 3+ / CaF 2 Fluorination catalyst precursors. Roast in a muffle furnace at 400°C for 8 hours, then put it into a tubular reactor, raise the temperature to 200°C, pass in hydrogen fluoride gas for fluorination for 1 hour, then raise the temperature to 350°C at a heating rate of 1°C / min, and continue the fluorination for 8 hours. A trivalent iron-supported catalyst was obtained.

Embodiment 1

[0023] Embodiment 1 Chlorine-propyne chlorination prepares 1,1,1,2,2-pentachloropropane

[0024] Dissolve 28.0g of monochloropropyne in 100ml of dichloromethane, add it to a 250ml three-necked flask equipped with a stirring bar, a thermometer and a reflux condenser, keep stirring at 0°C and feed in chlorine gas for reaction, and the chlorine gas controls the flow rate 1.5L / h, after 6 hours of chlorine gas, the chlorine gas was stopped, and the reaction was continued at room temperature for 12 hours, the reaction mixture was extracted with petroleum ether, and the fraction with a boiling point of 179-180°C was collected by distillation to obtain CCl with a yield of 92.0%. 3 CCl 2 CH 3 .

Embodiment 2

[0025] Embodiment 2 Chlorine-propyne chlorination prepares 1,1,1,2,2-pentachloropropane

[0026] Dissolve 28.0g of monochloropropyne in 100ml of dichloromethane, add it to a 250ml three-necked flask equipped with a stirring rod, a thermometer and a reflux condenser, and keep stirring at 60°C and pass in chlorine gas for reaction, and the chlorine gas controls the flow rate 1.5L / h, after 6 hours of chlorine gas, the chlorine gas was stopped, and the reaction was continued at room temperature for 12 hours, the reaction mixture was extracted with petroleum ether, and the fraction with a boiling point of 179-180°C was collected by distillation to obtain CCl with a yield of 96.0%. 3 CCl 2 CH 3 .

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Abstract

The invention discloses a preparation method of 2,3,3,3-tetrafluoropropene, comprising the following steps of: (1) dissolving monochloropropylene in dichloromethane, importing chlorine at reaction temperature of 0 to 60 DEG C for 6 h, then continuing the reaction at room temperature for 12 h, and extracting and distilling the reaction liquid to obtain 1,1,1,2,2-pentachloropropane; (2) placing catalyst SbC15 in an autoclave and cooling to -30 DEG C, after adding anhydrous hydrogen fluoride and the 1,1,1,2,2-pentachloropropane obtained in the step (1), heating to 80 DEG C while stirring with reaction pressure of 1.0 Mpa, keeping the reaction temperature at 80 DEG C and continuing the reaction for 8 h, carrying out water washing and alkali washing on the reaction mixture to remove HF (Hydrogen Fluoride), collecting a product with a cold trap, wherein the mole ratio of SbC15 to 1,1,1,2,2-pentachloropropane to HF is 1: 10: 200; and (3) flowing the product obtained in the step (2) into a dehydrohalogenation reactor in the presence of a ferric load type catalyst with contact time of 30 seconds and reaction temperature of 50 to 450 DEG C so as to obtain the 2,3,3,3-trifluoropropene. The invention is mainly used for preparing the 2,3,3,3-tetrafluoropropene.

Description

technical field [0001] The present invention relates to a kind of preparation method of 2,3,3,3-tetrafluoropropene (HFO-1234yf), especially to a kind of chloropropyne as raw material through chlorination, liquid phase fluorination and dehydrofluorination reaction to obtain Process for the preparation of 2,3,3,3-tetrafluoropropene. Background technique [0002] At present, 1,1,1,2-tetrafluoroethane (HFC-134a) is widely used as a refrigerant in mobile air-conditioning systems. Because of its greenhouse effect potential (GWP) of 1430, it will cause global warming and requires Develop new alternatives to suit the needs of the environment. [0003] 2,3,3,3-Tetrafluoropropene (HFO-1234yf), Ozone Depletion Potential (ODP) is zero, GWP is 4, atmospheric life is only 11 days, has excellent physical and chemical properties, it is considered as HFC-134a direct alternative to . [0004] Currently, there are various methods for preparing HFO-1234yf, for example, US2009240090 discloses...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C21/18C07C17/25
Inventor 王博吕剑张伟石磊李春迎谷玉杰郝志军毛伟封利民
Owner 山东华安近代环保科技有限公司