Clean production method of paranitroanisole
A p-nitroanisole and clean production technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of large amount of by-products, large amount of waste water, environmental pollution, etc., and achieve improvement Yield, the effect of achieving zero emissions
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Embodiment 1
[0022] Add 204.4g of p-nitrochlorobenzene and 200g of methanol into a 1000mL autoclave, close the autoclave, slowly raise the temperature until the p-nitrochlorobenzene is basically dissolved, start stirring and continue to heat up to 80°C, and then start to oxidize 460mL of hydrogen Sodium methanol solution (the content of sodium hydroxide is 125g / L) is added in batches to p-nitrochlorinated benzyl alcohol solution for contact reaction, the dropping process is controlled as follows: add 150mL dropwise for about 1 hour; then continue to heat up to 85°C About 230 mL was added dropwise in about 2 hours; then the temperature was raised to 90-95°C, and the remaining sodium hydroxide methanol solution was added dropwise in about 1 hour. Finally, continue to heat up to 100-105° C. for heat preservation reaction, and reach the end of the reaction in about 6 hours.
[0023] Then the obtained reaction product mixture is distilled to obtain gaseous methanol and a distillation substrate,...
Embodiment 2
[0027] Add 204.4g of p-nitrochlorobenzene and 115g of methanol into a 1000mL autoclave, close the autoclave, slowly raise the temperature until the p-nitrochlorobenzene is basically dissolved, start stirring and continue to heat up to 80°C, and then start to oxidize 430mL of hydrogen Sodium methanol solution (the content of sodium hydroxide is 155g / L) is added in batches to p-nitrochlorinated benzyl alcohol solution for contact reaction. The dropping process is controlled as follows: add 150mL dropwise for about 1 hour; then continue to heat up to 85°C Add 200 mL dropwise in about 2 hours; then raise the temperature to 90-95°C, and add the remaining methanolic sodium hydroxide solution dropwise in about 1 hour. Finally, continue to raise the temperature to 100-105° C. and keep it warm for the reaction, and reach the end of the reaction in about 4.5 hours.
[0028] Then the obtained reaction product mixture is distilled to obtain gaseous methanol and distillation bottoms, where...
Embodiment 3
[0032] Add 204.4g of p-nitrochlorobenzene and 150g of methanol into a 1000mL autoclave, close the autoclave, slowly raise the temperature until the p-nitrochlorobenzene is basically dissolved, start stirring and continue to heat up to 80°C, and then start to oxidize 440mL of hydrogen Sodium methanol solution (the content of sodium hydroxide is 140g / L) is added in batches to p-nitrochlorinated benzyl alcohol solution for contact reaction, the dropping process is controlled as follows: add 150mL dropwise for about 1 hour; then continue to heat up to 85°C Add 200 mL dropwise in about 2 hours; then raise the temperature to 90-95°C, and add the remaining methanolic sodium hydroxide solution dropwise in about 1 hour. Finally, continue to heat up to 100-105° C. for heat preservation reaction, and reach the end of the reaction in about 5 hours.
[0033] Then the obtained reaction product mixture is distilled to obtain gaseous methanol and distillation bottoms, wherein, the gaseous met...
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