A kind of preparation method of synthesizing chlorinated hydrocarbon
A technology for chlorinated hydrocarbons and olefins, applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc. Selective, continuous production is easy to operate and easy to operate
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preparation example Construction
[0023] A kind of preparation method of synthesizing chlorinated hydrocarbon of the present invention comprises the following steps:
[0024] (1) Mix carbon tetrachloride, ferric chloride and cocatalyst evenly, and preheat the above mixture to a temperature of 100-140°C with a preheater, wherein the molar ratio of carbon tetrachloride and olefin is 1-10: 1. Preferably, the molar ratio of carbon tetrachloride to olefin is 1.5 to 5:1, and the mass percentage of ferric trichloride to carbon tetrachloride is 0.5 to 10%. Preferably, ferric trichloride accounts for The mass percent of carbon is 1-6%, the mass percent of the cocatalyst accounting for carbon tetrachloride is 0.5~10%, preferably, the mass percent of the cocatalyst accounting for carbon tetrachloride is 1~5%, and the cocatalyst is phosphoric acid ester Phosphite or phosphite, preferably, the cocatalyst of phosphate or phosphite is one of trimethyl phosphate, triethyl phosphate, tributyl phosphate, tributyl phosphite or t...
Embodiment 1
[0031] The telomerization reactor in this example adopts an adiabatic tubular glass reactor with a pipe diameter of Ф20×2.5 mm and a length of 1 meter. Firstly, a composite metal annular filler is placed in the reactor, and the catalyst filling amount is 90% of the reactor volume. , wherein the content of each component in the composite metal is as follows: iron is 95%, nickel is 4.2%, and chromium is 0.8%. 198.4 grams of carbon tetrachloride, 5.9 grams of ferric chloride and 7.1 grams of tributyl phosphate are fully mixed, and preheated to 120 ° C by a preheater, and the preheated raw materials and 40.1 grams of vinyl chloride enter the tubular reaction In the reactor, under the conditions of reaction pressure 0.5MPa, reaction temperature 115°C, and residence time 30 minutes, telomerization reaction was carried out, the reaction product was collected by cold trap, and the composition of the product was determined by GC, wherein the conversion rate of vinyl chloride was 100%, H...
Embodiment 2
[0036] Reactor and main catalyst are carried out according to embodiment 1, at first in reactor, pack composite metal annular packing, catalyst filling amount is 85% of reactor volume. 203.6 grams of carbon tetrachloride, 8.1 grams of ferric chloride and 12.5 grams of triethyl phosphate are fully mixed, and preheated to 110 ° C by a preheater, the above-mentioned raw materials after preheating and 45.4 grams of vinyl chloride enter the tubular reaction In the reactor, under the conditions of reaction pressure 0.4MPa, reaction temperature 100°C, and residence time 35 minutes, telomerization reaction was carried out, the reaction product was collected by cold trap, and the composition of the product was determined by GC, wherein the conversion rate of vinyl chloride was 99.4%, HCC -240fa selectivity was 98.1%.
[0037] The reaction product collected by the above-mentioned cold trap first passes through the flash tower, and the pressure and temperature of the flash tower are resp...
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Abstract
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