Method for synthesizing trans-1,1,1,4,4,4-hexafluoro-2-butene
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A technology of butene and trifluorobutane, applied in the field of synthesizing trans-1,1,1,4,4,4-hexafluoro-2-butene, which can solve the problem of high reaction temperature and no stability evaluation and other problems to achieve the effect of high catalytic activity and mild and controllable reaction conditions
Active Publication Date: 2019-04-02
XIAN MODERN CHEM RES INST
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[0003] Chinese patent CN 102884030 B reported that 3,3,3-trifluoropropene and carbon tetrachloride were used as raw materials to synthesize 1,1 ,1,3-Tetrachloro-4,4,4-trifluorobutane, then fluorinated Cr 2 o 3 As a catalyst, the reaction temperature is 250-260°C, and the gas-phase fluorination reaction synthesizes a mixture of HFO-1336mzz cis-trans structure, and the conversion rate of 1,1,1,3-tetrachloro-4,4,4-trifluorobutane is 98.9%, 1,1,1,4,4,4-hexafluoro-2-butene cis-trans configuration with an overall selectivity of 93.9%, no stability evaluation
The reaction temperature of this method is high, and the reaction has only been carried out for 20 hours, and the stability evaluation has not been carried out.
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Embodiment 1
[0029] With main catalyst copper bromide 11.17g (0.05mol), procatalyst p-fluoroaniline 5.56g (0.05mol), initiator azobisisobutyronitrile 6.81g (0.05mol) and CCl 4 770g (5mol) was added to a 1L stainless autoclave. Seal the autoclave, start stirring, and replace the air in the autoclave with nitrogen for three times. Then, 240.13 g of 3,3,3-trifluoropropene was added at one time, the temperature of the reactor was heated to 60° C., and the reaction was completed after 4 hours. After the autoclave was lowered to room temperature, the autoclave was unloaded and the material was taken out. A liquid sample was taken with a pipette and analyzed by chromatography. The conversion rate of 3,3,3-trifluoropropene was 97.5%, 1,1,1,3-tetrachloro-4,4,4-trifluorobutane The selectivity of 1,1,1,3-tetrachloro-4,4,4-trifluorobutane was 96.6%, and the yield of 1,1,1,3-tetrachloro-4,4,4-trifluorobutane was 94.2%.
Embodiment 2
[0031] Add 0.08mol of MgF to the beaker 2 Support, impregnated with AlCl by isometric impregnation 3 ·6H 2 O, AlCl 3 ·6H 2 O and MgF 2 The molar ratio is 0.05, dried in an oven at 100°C for 8h, and calcined in a muffle furnace at 450°C for 1h to make a catalyst 5Al / MgF 2 .
[0032] Measure 5mL of the catalyst prepared by the above steps and put it into the reaction tube. The time is 6s, the molar ratio of HF and 1,1,1,3-tetrachloro-4,4,4-trifluorobutane is 10:1, and the operation is 24h. After the reaction product is washed with water to remove acid and dried, the gas chromatography Analysis showed that the conversion rate of 1,1,1,3-tetrachloro-4,4,4-trifluorobutane was 100%, and the selectivity of E-HFO-1336mzz was 97.9%.
Embodiment 3
[0034] The operation process of embodiment 3 is similar to embodiment 1, and difference is that main catalyst is cupric chloride. The product was analyzed by chromatographic method, the conversion rate of 3,3,3-trifluoropropene was 96.5%, the selectivity of 1,1,1,3-tetrachloro-4,4,4-trifluorobutane was 95.8%, The selective yield of 1,1,1,3-tetrachloro-4,4,4-trifluorobutane was 92.2%.
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Abstract
The invention discloses a method for synthesizing trans-1,1,1,4,4,4-hexafluoro-2-butene. The method comprises the following steps: (a) in the presence of a telomerization catalyst, performing a reaction on 3,3,3-trifluoropropene and carbon tetrachloride to synthesize 1,1,1,3-tetrachloro-4,4,4-trifluorobutane, wherein the reaction temperature is 30-70 DEG C, and the reaction time is 1-10 h; and (b)under the action of a fluorination catalyst, performing gas phase fluorination on the 1,1,1,3-tetrachloro-4,4,4-trifluorobutane and HF to synthesize the trans-1,1,1,4,4,4-hexafluoro-2-butene, whereinthe reaction temperature is 200-300 DEG C, a molar ratio of the HF to the 1,1,1,3-tetrachloro-4,4,4-trifluorobutane is (5-50):1, the telomerization catalyst is composed of a main catalyst, a cocatalyst and an initiator, the main catalyst is a monovalent or divalent copper salt, the cocatalyst is an organic amine, and the initiator is p-hydroxyacetophenone or 1,1-azobis(cyanocyclohexane); and thefluorination catalyst is a supported catalyst with a composition of Nx / MgF2, N is an active component and selected from one of Al, Cu, Zn and Co, x is a molar ratio of N to MgF2, and a value of x satisfies the relationship of 0.05 <= x <= 0.15. The method provided by the invention is mainly used for synthesizing the trans-1,1,1,4,4,4-hexafluoro-2-butene.
Description
technical field [0001] The invention relates to a method for synthesizing trans-1,1,1,4,4,4-hexafluoro-2-butene, in particular to telomerization of 3,3,3-trifluoropropene and carbon tetrachloride Reaction, fluorination reaction to synthesize trans-1,1,1,4,4,4-hexafluoro-2-butene. Background technique [0002] As the problem of global warming has become increasingly serious in recent years, the third-generation blowing agent is facing to be eliminated or eliminated in advance. Cis-1,1,1,4,4,4-hexafluoro-2-butene (Z-HFO-1336mzz), as the fourth generation liquid blowing agent, has a good market prospect. Trans-1,1,1,4,4,4-hexafluoro-2-butene (E-HFO-1336mzz), as one of the important intermediates of Z-HFO-1336mzz, has important research and industrial Value. [0003] Chinese patent CN 102884030 B reported that 3,3,3-trifluoropropene and carbon tetrachloride were used as raw materials to synthesize 1,1 ,1,3-Tetrachloro-4,4,4-trifluorobutane, then fluorinated Cr 2 o 3 As a c...
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