Process method for synthesizing and purifying 4-chlorobutyryl chloride
A technology of chlorobutyryl chloride and a process method, applied in the directions of acid halide preparation, chemical recovery, etc., can solve problems such as inability to guarantee product purity, difficult disposal of organic matter, pollution of surrounding environment, etc. good stability
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Embodiment 1
[0023] 1. Preparation of Mixed Catalyst
[0024] Mix 21.3kg of ZnO and 4.2Kg of CuO, add 44.3Kg of 98% concentrated sulfuric acid to react, cool the resulting reactant and dry it at 350°C to obtain the product;
[0025] 2. Add 1000kg of γ-butyrolactone and 50kg of newly prepared mixed catalyst to the reactor, stir, and at the same time, enter tap water into the jacket of the reactor to cool; slowly add 2000kg of thionyl chloride into the reactor from the elevated tank, and add After the completion, the hot water in the jacket was slowly heated to 50-80°C, kept for 5-7 hours for acylation reaction, and the excess thionyl chloride was recovered by negative pressure distillation. The liquid is ready for use; the catalyst in the lower layer can be recycled;
[0026] 3. Pump the supernatant liquid into the crude distillation still and distill under reduced pressure at -0.095MPa~-0.1MPa, accept the fractions in sections, and the fractions before 50°C are mainly thionyl chloride and...
Embodiment 2
[0030] 1. Mix 30.7kg ZnO and 7.5Kg CuO, add 60Kg 98% concentrated sulfuric acid to react, cool the obtained reactant and dry it at 400°C to obtain it;
[0031] 2. Add 1000kg of γ-butyrolactone and 70kg of newly prepared mixed catalyst to the reactor, stir, and at the same time enter tap water into the jacket of the reactor to cool; slowly add 2500kg of thionyl chloride into the reactor from the elevated tank, and add After the completion, the hot water in the jacket was slowly heated to 50-80°C, kept for 5-7 hours to carry out the acylation reaction, the excess thionyl chloride was recovered by negative pressure distillation, and the precipitation was carried out for 8-10 hours after cooling down to normal temperature, and the supernatant was taken The liquid is ready for use; the catalyst in the lower layer can be recycled;
[0032] 3. Pump the supernatant liquid into the crude distillation still and distill under reduced pressure at -0.095MPa~-0.1MPa, accept the fractions i...
Embodiment 3
[0036] 1. Mix 14.4kg ZnO and 4.7Kg CuO, add 37.9Kg 98% concentrated sulfuric acid for reaction, cool the obtained reactant and dry it at 320°C to obtain it;
[0037] 2. Add 1000kg of γ-butyrolactone and 30kg of mixed catalyst to the reactor, stir, and at the same time enter the tap water into the jacket of the reactor to cool; slowly add 1500kg of thionyl chloride into the reactor from the head tank, after the addition is completed Enter the hot water in the jacket and slowly raise the temperature to 50-80°C, keep it warm for 5-7 hours to carry out the acylation reaction, and recover the excess thionyl chloride by negative pressure distillation. After cooling down to normal temperature, it will precipitate for 8-10 hours. use; the lower catalyst can be recycled;
[0038] 3. Pump the supernatant liquid into the crude distillation still and distill under reduced pressure at -0.095MPa~-0.1MPa, accept the fractions in sections, and the fractions before 50°C are mainly thionyl chl...
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