Clean production method of p-anisidine
A technology of p-aminoanisole and p-nitroanisole, which is applied in the field of clean production of p-aminoanisole, can solve the problems of increased methanol distillation volume, increased energy consumption, and high energy consumption, and achieves simple operation, Reduce high salt and high COD wastewater, high yield and high purity effect
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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 to carry out contact reaction. Finally, continue to heat up to 100-105° C. for heat preservation reaction, and reach the end of the reaction in about 6 hours, wherein the purity of p-nitroanisole is 97.2%.
[0023] Then the reaction product is filtered to obtain p-nitroanisole solution and filter cake. The filter cake is washed with methanol and dried to obtain sodium chloride, the content of which is more than 99%, reaching the industrial product standard. The resulting p-nitroanisole solution was distilled to remove about 300 g of methanol, then the material was...
Embodiment 2
[0026] 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 to carry out contact reaction. Finally, continue to heat up to 100-105° C. for heat preservation reaction, and reach the end of the reaction in about 6 hours, wherein the purity of p-nitroanisole is 97.5%.
[0027] Then the reaction product is filtered to obtain p-nitroanisole solution and filter cake. The filter cake is washed with methanol and dried to obtain sodium chloride, the content of which is more than 99%, reaching the industrial product standard. The obtained p-nitroanisole solution was distilled to distill out about 400g of methanol, then the material ...
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