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A technology for pentafluorobutane and pentachlorobutane, which is applied in 1 field, can solve problems such as poor mass transfer and heat transfer effects, and achieve the effects of accelerating the reaction speed, increasing the reaction temperature and increasing the reaction speed.
Active Publication Date: 2013-08-28
XIAN MODERN CHEM RES INST
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Problems solved by technology
Poor mass and heat transfer in the absence of agitation and low reaction temperatures
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Embodiment 1
[0026] The temperature of the low temperature reaction zone (1) of the liquid phase fluorination reactor is controlled at 90°C, the temperature of the low temperature reaction zone (1) is controlled at 140°C, and the HF entering the liquid phase fluorination reactor is mixed with 1, 1, 1, 3 , the molar ratio of 3-pentachlorobutane is 15:1, the reaction pressure is 1.5MPa, and the catalyst is SbCl 5 . The composition of the organic matter in the lower layer of the phase separator (8) is analyzed by gas chromatography, and the selectivity of HFC-365mfc is 93.3%, and the others are 6.7%.
Embodiment 2
[0028]The temperature of the low temperature reaction zone (1) of the liquid phase fluorination reactor is controlled at 60°C, the temperature of the low temperature reaction zone (1) is controlled at 90°C, and the HF entering the liquid phase fluorination reactor is mixed with 1, 1, 1, 3 , the molar ratio of 3-pentachlorobutane is 15:1, the reaction pressure is 1.0MPa, and the catalyst is SbCl 5 . The composition of the organic matter in the lower layer of the phase separator (8) is analyzed by gas chromatography, and the selectivity of HFC-365mfc is 92.5%, and the others are 7.5%.
Embodiment 3
[0030] The temperature of the low temperature reaction zone (1) of the liquid phase fluorination reactor is controlled at 90°C, the temperature of the low temperature reaction zone (1) is controlled at 110°C, the HF entering the liquid phase fluorination reactor is mixed with 1, 1, 1, 3 , the molar ratio of 3-pentachlorobutane is 6:1, the reaction pressure is 1.2MPa, and the catalyst is SnCl 4 . The composition of the organic matter in the lower layer of the phase separator (8) was analyzed by gas chromatography, and the selectivity of HFC-365mfc was 90.1%, and the others were 9.9%.
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Abstract
The invention provides a preparation method of 1,1,1,3,3-pentafluorobutane, which comprises the following step of reacting 1,1,1,3,3,-pentachlorobutane with HF (Hydrogen Fluoride) in a liquid-phase fluorination reactor provided with a low-temperature reaction zone (1) and a high-temperature reaction zone (2) in the presence of a liquid-phase fluorination catalyst. The reaction conditions are as follows: the mol ratio of the HF to the 1,1,1,3,3,-pentachlorobutane is 6-15:1, the reaction pressure is 1.0-1.5 MPa, the reaction temperature of the low-temperature reaction zone is 60-90 DEG C, the reaction temperature of the high-temperature reaction zone is 90-140 DEG C, wherein the liquid-phase fluorination catalyst is antimony pentachloride or tin tetrachloride; the 1,1,1,3,3,-pentachlorobutane enters the low-temperature reaction zone (1) of the liquid-phase fluorination reactor; the fresh HF enters the high-temperature reaction zone (2) of the liquid-phase fluorination reactor and then enters a reaction system; and the circulating HF enters the low temperature reaction zone (1) and the high-temperature reaction zone (2) of the liquid-phase fluorination reactor simultaneously. The invention is used for the preparation of the 1,1,1,3,3-pentafluorobutane.
Description
technical field [0001] The present invention relates to a kind of preparation method of 1,1,1,3,3-pentafluorobutane (HFC-365mfc), especially relate to a kind of preparation method with hydrogen fluoride and 1,1,1,3,3-pentachlorobutane ( HCC-360jfa) is used as raw material, and the preparation method of 1,1,1,3,3-pentafluorobutane is synthesized by liquid phase fluorination reaction. Background technique [0002] HFC-365mfc is a fluorinated hydrocarbon compound that is safe for the atmospheric ozone layer and is currently mainly used as a blowing agent for trifluorochloromethane (CFC-11) and 1,1,1-dichlorofluoroethane (HCFC-141b) In addition, it is also widely used as a solvent, propellant, fire extinguishing agent and dry etchant. [0003] At present, using HCC-360jfa as a raw material to obtain HFC-365mfc through fluorination is the main method for preparing HFC-365mfc in industry. US5917098 discloses a method for preparing HFC-365mfc by intermittent liquid-phase fluorina...
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