Method for preparing phenylhydrazine
A technology for phenylhydrazine and phenol, applied in the field of preparing phenylhydrazine, can solve the problems of many reaction steps, easy decomposition and high cost, and achieve the effects of less by-products and wastes, mild reaction conditions and low production cost
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Embodiment 1
[0012] Put 188g of phenol, 166.7g of hydrazine hydrate with a content of 90% and 37.6g of HD-8 macroporous resin into a four-neck flask equipped with stirring, thermometer and rectification column, start stirring, and heat up to 110°C-120°C. Extract water vapor at the rectification column top temperature of 98°C to 100°C, take samples for analysis after 6 to 8 hours of reaction, end the reaction when the phenol content in the reaction liquid is lower than 0.3%, and then recover excess hydrazine hydrate by vacuum distillation, hydration After the recovery of hydrazine, the HD-8 macroporous resin was separated with a centrifugal filter device, and the remaining liquid was washed with an appropriate amount of sodium carbonate solution and pure water to obtain 199.2 g of phenylhydrazine.
Embodiment 2
[0014] Put 188g of phenol, 184.2g of hydrazine hydrate with a content of 95% and 56.4g of HD-8 macroporous resin into a four-necked flask equipped with a stirring, thermometer and rectification column, start stirring, and heat up to 110°C to 120°C. Extract water vapor at the rectification column top temperature of 98°C to 100°C, take samples for analysis after 6 to 8 hours of reaction, end the reaction when the phenol content in the reaction liquid is lower than 0.3%, and then recover excess hydrazine hydrate by vacuum distillation, hydration After the recovery of hydrazine, the HD-8 macroporous resin was separated with a centrifugal filter device, and the remaining liquid was washed with an appropriate amount of sodium carbonate solution and pure water to obtain 206.3 g of phenylhydrazine.
Embodiment 3
[0016] Put 188g of phenol, 202g of hydrazine hydrate with a content of 99%, and 18.8g of HD-8 macroporous resin into a four-necked flask equipped with a stirring, thermometer and rectification column, start stirring, and heat up to 110°C to 120°C. The rectification column top temperature is 98 ℃ ~ 100 ℃ to extract water vapor, after 6 ~ 8 hours of reaction, sampling analysis, when the content of phenol in the reaction liquid is less than 0.3%, the reaction is ended, and then the excess hydrazine hydrate is recovered by vacuum distillation, hydrazine hydrate After recovery, the HD-8 macroporous resin was separated with a centrifugal filter device, and the remaining liquid was washed with an appropriate amount of sodium carbonate solution and pure water to obtain 201.8 g of phenylhydrazine.
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