Tubular continuous method for preparing cyclopropanecarboxylic acid
A cyclopropane, tubular technology, applied in the field of tubular continuous synthesis of cyclopropane, can solve the problems of little practical application value, unstable product quality, and high equipment requirements, and achieve easy automatic control and suppression of harmful impurities The production, the effect of large production capacity
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Embodiment 1
[0021] The method for tubular continuous preparation of cyclopropanecarboxylic acid is carried out successively in the first reactor, the tubular reactor and the second reactor:
[0022] Input γ-butyrolactone at 45L / h into the 1500L first reaction kettle with an overflow at 2 / 3 of the height, and continuously add γ-butyrolactone, methanol and thionyl chloride in a molar ratio of 1:2.5:1.2 In the first reactor, the reaction temperature is controlled at 0°C, and the material in the reactor overflows from the overflow port and flows into a water tank with a temperature of 65°C for heat preservation and degassing. Then reclaim the unreacted methanol in recovery tower distillation, control and reclaim the liquid level in the methanol tower kettle at 2 / 3 place, the reaction solution and toluene that flow out recovery tower kettle are input water washing tower with 150L / h flow rate simultaneously, the water in water washing tower The flow rate is 150L / h. The organic phase output fro...
Embodiment 2
[0027] The method for tubular continuous preparation of cyclopropanecarboxylic acid is carried out successively in the first reactor, the tubular reactor and the second reactor:
[0028]Input γ-butyrolactone at 90L / h into the 2500L first reaction kettle with an overflow at 2 / 3 of the height, and continuously add γ-butyrolactone, methanol and thionyl chloride in a molar ratio of 1:2.0:1.05 In the first reactor, the reaction temperature is controlled at -5°C, and the material in the reactor overflows from the overflow port and flows into a water tank with a temperature of 80°C for heat preservation and degassing. Then reclaim the unreacted methanol in recovery tower distillation, control and reclaim the liquid level in the methanol tower kettle at 2 / 3 place, the reaction liquid and toluene that flow out recovery tower kettle are input into water wash tower with 750L / h flow rate simultaneously, the water in water wash tower The flow rate is 450L / h. The organic phase output from ...
Embodiment 3
[0033] The method for tubular continuous preparation of cyclopropanecarboxylic acid is carried out successively in the first reactor, the tubular reactor and the second reactor:
[0034] γ-butyrolactone is input at 45L / h into the 1500L first reaction kettle with an overflow at 2 / 3 of the height, and the molar ratio of γ-butyrolactone, isopropanol and thionyl chloride is 1:2.5:1.2 Continuously feed into the first reactor, the reaction temperature is controlled at 5°C, and the material in the reactor overflows from the overflow port and flows into a water tank with a temperature of 60°C for heat preservation and degassing. Then reclaim unreacted isopropanol in recovery tower distillation, control reclaims the liquid level in the isopropanol tower still at 2 / 3 place, the reaction liquid and benzene that flow out recovery tower still are input water-washing tower with 150L / h flow rate simultaneously, The flow rate of water in the water washing tower is 150L / h. The organic phase t...
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