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A kind of continuous preparation method of 1,1,1,2,3-pentachloropropane
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A technology of pentachloropropane and trichloropropene, which is applied in the field of preparation of chlorinated alkanes, can solve the problems of unfavorable environmental protection and industrial production application, low reaction selectivity, short catalyst life, etc., to avoid uneven heat exchange effect, The effect of high yield and low cost
Active Publication Date: 2021-12-14
JUHUA GROUP TECH CENT
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Disclosed is a kind of synthetic method of 1,1,1,2,3-pentachloropropane, this method is with trichloropropene or 1,1,1,3-tetrachloropropane as precursor, in oxychlorination catalyst (main Under the action of active component CuCl2), feed oxygen and HCl and make 1,1,1,2,3-pentachloropropane, the selectivity is lower than 82%
The reaction selectivity of this method is low and the life of the catalyst used is short, which is not conducive to environmental protection and industrial production application
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[0031] According to the required reaction molar ratio and residence time, set the flow rate of trichloropropene (1,1,3-trichloropropene or 3,3,3-trichloropropene or their mixture) and chlorine, and flow them to Input trichloropropene and chlorine gas into trichloropropene preheater and chlorine gas preheater, the temperature of trichloropropene preheater and chlorine gas preheater is set at 135~140 ℃, the preheated trichloropropene and chlorine gas enter micro The reaction is carried out in the channel reactor, and the reaction product is collected, cooled and rectified under reduced pressure (vacuum degree 0.099MPa), and the fraction at 76-78°C is collected to obtain 1,1,1,2,3-pentachloropropane product (purity 99.8%) . Sampling and analysis were taken from the outlet of the microchannel reactor. The experimental results of different reaction conditions are shown in Table 1.
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Abstract
The invention discloses a continuous preparation method of 1,1,1,2,3-pentachloropropane. The chlorine gas and trichloropropene are continuously fed into a microchannel preheater at a molar ratio of 0.5 to 1.5:1 for preheating. , and then the preheated materials are continuously passed into the microchannel reactor for reaction, the reaction time is 0.1-10s, the reaction temperature is 100-200°C, the reaction product is collected, cooled and rectified under reduced pressure to obtain 1,1 ,1,2,3‑Pentachloropropane products. The invention has the advantages of simple process, high production efficiency, safety and environmental protection, and easy industrialization.
Description
technical field [0001] The invention relates to a preparation method of chlorinated alkanes, in particular to a continuous preparation method of 1,1,1,2,3-pentachloropropane. Background technique [0002] 1,1,1,2,3-Pentachloropropane is an important intermediate for the preparation of 1,1,2,3-tetrachloropropene. At the same time, 1,1,2,3-tetrachloropropene is the main intermediate for the synthesis of a new generation of environmentally friendly refrigerant HFO-1234yf and the preparation of the pesticide herbicide "avencam". How to efficiently and environmentally friendly prepare 1,1,1,2,3-pentachloropropane is attracting widespread attention. At present, according to the different precursors of 1,1,1,2,3-pentachloropropane, there are mainly the following two routes: (1) using trichloropropene (including 1,1,3-trichloropropene or 3, 3,3-trichloropropene or their mixture) as the precursor for the preparation of 1,1,1,2,3-pentachloropropane by chlorination; (2) 1,1,1,3-tetra...
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