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Method for preparing HCFC-244bb

A technology of tetrafluoropropane and trifluoropropene, which is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc., can solve the problems of poor reaction effect and complicated process, and achieve stable performance, simple process and good reaction effect of effect

Inactive Publication Date: 2014-11-12
XIAN MODERN CHEM RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chinese patent CN103180274 A has reported a kind of preparation method of HCFC-244bb, and this method uses ionic liquid [EMIM]Sb 2 f 11 As a catalyst, the reaction temperature is 85°C, and the reaction effect is poor: the conversion rate of HCFO-1233xf is only 16.7%, and the selectivity of HCFC-244bb is 92.6%
In addition, during the preparation process of the catalyst and the reaction process, chlorine gas must be introduced to ensure the pentavalent state of antimony, and the process is complicated.

Method used

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  • Method for preparing HCFC-244bb
  • Method for preparing HCFC-244bb

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] The liquid phase fluorination reaction was carried out in a stirred 200mL stainless steel autoclave. Add 15g of SbF to the reactor in sequence 5 , 10.1g [BMIM]BF 4 , then add 5g HF, stir for 4h, raise the temperature to 50°C, and keep the temperature constant for 1h.

[0013] Add 13g of HCFO-1233xf into the reactor, react at 50°C for 1 hour and then lower the temperature. The reaction product was analyzed by gas chromatography after being washed with water to remove acid, and the conversion rate of HCFO-1233xf was 95.3%, and the selectivity of HCFC-244bb was 99.1%.

Embodiment 2

[0015] The liquid phase fluorination reaction was carried out in a stirred 200mL stainless steel autoclave. Add 20.8g SbCl to the reactor successively 5 , slowly inject 30g HF for fluorination treatment, control the pressure within 0.20MPa during the treatment process, raise the temperature to 70°C, keep the temperature for 2h, add 10.1g [BMIM]BF 4 , constant temperature 4h.

[0016] Add 13g of HCFO-1233xf into the reactor, the reaction temperature is 70°C, and cool down after 3 hours of reaction. The reaction product was analyzed by gas chromatography after being washed with water to remove acid, and the conversion rate of HCFO-1233xf was 90.3%, and the selectivity of HCFC-244bb was 98.6%.

Embodiment 3～5

[0018] Examples 4-6 The method for preparing HCFC-244bb is the same as that of Example 1, except that the metal halide, the type of ionic liquid and the reaction temperature are changed. The reaction results are shown in Table 2.

[0019] Table 2

[0020]

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Abstract

The invention discloses a method for preparing HCFC-244bb. According to the method, 2-chloro-3, 3, 3-trifluoropropene is used as raw materials. The method comprises the following steps that, a metal halide and an ionic liquid are used as a catalyst, and fluorination is conducted on 2-chloro-3, 3, 3-trifluoropropene and a hydrogen fluoride solution, so that HCFC-244bb is prepared, wherein the metalhalide is antimony pentafluoride or antimony pentachloride or tantalum pentafluoride or tantalum pentachloride or niobium pentafluoride or niobium pentachloride, the general formula of ionic liquid is X+A-, X+ is positive ions of C1-C8 alkyl substitution type double-alkyl imidazole, pyridine and quaternary ammonium salt, A- is negative ions of tetrafluroborate negative ions or hexafluorophosphatenegative ions, the molar ratio between the metal halide and the ionic liquid is 1-3:1, the molar ratio between hydrogen fluoride and 2-chloro-3, 3, 3-trifluoropropene ranges is 1.1-10:1, and the reaction temperature ranges from 20 DEG C to 70 DEG C. The method for preparing HCFC-244bb has the advantages that the reaction temperature is low, the conversion rate is high, the selectivity is high, and chlorine is not needed in the reaction process. The method is used for preparation of HCFC-244bb.

Description

technical field [0001] The present invention relates to a kind of preparation method of 2-chloro-1,1,1,2-tetrafluoropropane (HCFC-244bb), especially relate to metal halide and ionic liquid as catalyst, 2-chloro-3,3,3 - Liquid-phase fluorination of trifluoropropene (HCFO-1233xf) with hydrogen fluoride to prepare 2-chloro-1,1,1,2-tetrafluoropropane. Background technique [0002] HCFC-244bb is one of the important intermediate products in the synthesis of 2,3,3,3-tetrafluoropropene (HFO-1234yf). The ozone depletion potential of HFO-1234yf is zero, and the greenhouse effect potential is 4. It has excellent environmental performance, physical properties and chemical properties, and is ideal for 1,1,1,2-tetrafluoroethane (HFC-134a) Substitute, can be widely used as refrigerator refrigerant, fire extinguishing agent, heat transfer medium, propellant, foaming agent, polymer monomer and electric cycle working fluid, etc. [0003] Chinese patent CN103180274 A has reported a kind of ...

Claims

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Application Information

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IPC IPC(8): C07C19/10C07C17/087
Inventor 韩升吕剑曾纪珺唐晓博亢建平张伟马辉郝志军杨志强
Owner XIAN MODERN CHEM RES INST
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