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Process for preparing 1,1,1,3,3-pentachloro butane
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A technology for pentachlorobutane and chloropropene, which is applied in the field of preparation of saturated halogenated hydrocarbons, can solve the problems of a large number of reaction products decomposing, the products cannot be completely separated, and it is unfavorable for industrial amplification.
Active Publication Date: 2006-11-22
SINOCHEM LANTIAN +1
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However, due to the presence of a catalyst in the distillation process, the reaction product will be decomposed in large quantities, which is not conducive to industrial scale-up.
[0011] And in the patent WO9705089 it is mentioned that the material after the reaction is divided into two phases, and the phase containing the catalyst is reused after separation, but the product can not be completely separated in the two phases, and it is difficult to implement in an industrial device
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Embodiment 1
[0024] Add 600Kg carbon tetrachloride, 200Kg acetonitrile, 7Kg cuprous chloride, 6Kg tert-butylamine into a high-pressure enamel kettle, add 150Kg 2-chloropropene, stir and heat to 140°C, keep warm for 8 hours, cool to room temperature, and distill under reduced pressure Go out acetonitrile and unreacted carbon tetrachloride, obtain 440Kg product after washing and drying again. After analysis, the content of 1,1,1,3,3-pentachlorobutane (ie selectivity) is 98.8%, based on 2-chloropropene, the yield is 96.2%, and the selectivity is 98.8%.
[0025] Repeat above-mentioned test, solvent replaces acetonitrile with dimethyl sulfoxide, dimethylformamide, tert-butanol respectively, and the results are shown in Table 1:
[0026] solvent
Embodiment 2
[0028] Add 600Kg carbon tetrachloride, 200Kg acetonitrile, 7Kg cuprous chloride, 6Kg tert-butylamine into a high-pressure enamel kettle, add 150Kg 2-chloropropene, stir and heat to 130°C, keep warm for 8 hours, cool to room temperature, and distill under reduced pressure Go out acetonitrile and unreacted carbon tetrachloride, obtain 430Kg product after washing and drying, after analyzing 1,1,1,3, the content of 3-pentachlorobutane is 98.8%, taking 2-chloropropene as a benchmark, The yield was 93.9%.
Embodiment 3
[0030] Add 600Kg carbon tetrachloride, 200Kg acetonitrile, 7Kg cuprous chloride, 6Kg tert-butylamine into a high-pressure enamel kettle, add 150Kg 2-chloropropene, stir and heat to 130°C, keep warm for 6 hours, cool to room temperature, and distill under reduced pressure Go out acetonitrile and unreacted carbon tetrachloride, obtain 422Kg product after washing and drying, after analyzing 1,1,1,3, the content of 3-pentachlorobutane is 99.1%, taking 2-chloropropene as a benchmark, The yield was 92.5%.
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Abstract
The invention relates to a preparation method of 1,1,1,3,3-pentachlorobutane with high conversion rate, high selectivity, recyclable catalyst and materials. It is the addition of carbon tetrachloride and 2-chloropropene, and its main feature is that the method is carried out in the presence of solvents, copper salts and amines. In order to dissolve the catalyst, a solvent which is inert to the reactants and final product can be used in the telomerization reaction, the solvent can be dimethylsulfoxide, dimethylformamide, acetonitrile, tert-butanol.
Description
technical field [0001] The invention relates to a method for preparing saturated halogenated hydrocarbons, in particular to a method for preparing 1,1,1,3,3-pentachlorobutane. technical background [0002] 1,1,1,3,3-Pentachlorobutane is an intermediate for the preparation of 1,1,1,3,3-pentafluorobutane. 1,1,1,3,3-Pentafluorobutane is also known as HFC-365mfc, molecular formula CF 3 CH 2 CF 2 CH 3 , boiling point 40 ℃, colorless transparent liquid, non-toxic, its ozone depletion potential (ODP) is equal to zero. HFC-365mfc can replace HCFC-141b, CFC113, CFC11, etc. for polyurethane foaming and cleaning industries, and is a new type of environmentally friendly product. [0003] According to literature reports, the number of methods for preparing HFC-365mfc is small and generally involves the addition of chlorine precursors such as 2,2-difluoro-4,4,4-trichlorobutane or 2-bromo-2,4,4, 4-tetrachlorobutane or 1,1,1,3,3-pentachlorobutane fluorination. [0004] The HENNE grou...
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