Method for producing 1,1,3-trichloropropene by liquid-phase dehydrochlorination of 1,1,1,3-tetrachloropropane and recovering catalyst
A tetrachloropropane liquid, dehydrochlorination technology, applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, chemical recovery, etc., can solve the problem of easy decomposition, high processing cost, high energy consumption, etc. problems, to achieve the effects of reducing hazardous waste emissions, easy industrialization, and low process energy consumption
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Embodiment 1
[0025] Add 5.1 kg of 1,1,1,3-tetrachloropropane into a 5L glass reactor, and add iron p-toluenesulfonate according to the mass ratio of catalyst and 1,1,1,3-tetrachloropropane at 4.5:100 , start stirring, and heat the material to 80.4°C for dehydrochlorination, and the hydrogen chloride generated in the reaction is absorbed by water. The reaction was stopped after 0.5h. After the reaction solution was cooled to room temperature, sampling and analysis were carried out. The conversion rate of the raw material 1,1,1,3-tetrachloropropane was 90.3%, and the selectivity of the product 1,1,3-trichloropropene was 98.1%. High boil about 1.2%. The catalyst was extracted and recovered by adding ethylene glycol extractant at a mass ratio of 20:1 to the catalyst, and the extract was rectified under reduced pressure to obtain 1,1,3-trichloropropene with a purity of 99.8%, and the yield was 87%.
Embodiment 2
[0027] Add 5.1 kg of 1,1,1,3-tetrachloropropane into a 5L glass reactor, and add iron p-toluenesulfonate according to the mass ratio of catalyst and 1,1,1,3-tetrachloropropane at 0.05:100 , start stirring, and heat the material to 145°C for dehydrochlorination, and the hydrogen chloride generated in the reaction is absorbed by water. The reaction was stopped after 4.5 hours. After the reaction solution was cooled to room temperature, a sample was taken for analysis. The conversion rate of the raw material 1,1,1,3-tetrachloropropane was 87.9%, and the selectivity of the product 1,1,3-trichloropropene was 98.6%. High boiling about 0.8%. The catalyst was extracted and recovered by adding ethylene glycol extractant at a mass ratio of 80:1 to the catalyst, and the extract was rectified under reduced pressure to obtain 1,1,3-trichloropropene with a purity of 99.7%, and the yield was 85%.
Embodiment 3
[0029] Add 5.1 kg of 1,1,1,3-tetrachloropropane into a 5L glass reactor, and add iron p-toluenesulfonate according to the mass ratio of catalyst and 1,1,1,3-tetrachloropropane at 0.5:100 , start stirring, and heat the material to 110°C for dehydrochlorination, and the hydrogen chloride generated in the reaction is absorbed by water. The reaction was stopped after 3.0 hours. After the reaction solution was cooled to room temperature, a sample was taken for analysis. The conversion rate of the raw material 1,1,1,3-tetrachloropropane was 92.9%, and the selectivity of the product 1,1,3-trichloropropene was 98.3%. High boiling about 0.9%. Water extractant was added at a mass ratio of 50:1 to the catalyst to extract and recover the catalyst, and the extract was rectified under reduced pressure to obtain 1,1,3-trichloropropene with a purity of 99.8%, and the yield was 90%.
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