Method for high-selectivity preparation of 3,4-dichloroaniline
A dichloroaniline and high-selectivity technology, which is applied in the field of high-selectivity catalytic hydrogenation preparation 3, can solve the problems of low catalyst application times and high cost, and achieve the effects of low cost, reduced corrosion and high selectivity
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Embodiment 1
[0025] Add 64 g of 3,4-dichloronitrobenzene and 0.16 g of 3% Pt (water content 59.98%) catalyst containing additives into a stainless steel autoclave, close the autoclave, replace the air in the autoclave with nitrogen three times, and then Replace the nitrogen in the kettle with hydrogen three times and maintain a certain pressure in the kettle. Heat up to 85°C under stirring, maintain the reaction pressure at 1.75MPa, close the hydrogen valve after the reaction is over, let the gas out, open the autoclave to discharge, keep warm at about 75°C to filter out the catalyst, and use gas chromatography to analyze the reduction product, 3,4-dichloronitro The conversion rate of benzene is 100%, the selectivity of 3,4-dichloroaniline is 99.6%, and the dechlorination rate is 0.19%.
Embodiment 2
[0027] The catalyst was changed, and the influence of the Pt catalyst without promoters on the hydrogenation of 3,4-dichloronitrobenzene was investigated.
[0028] Add 64 g of 3,4-dichloronitrobenzene and 0.16 g of 3% Pt (water content 59.78%) catalyst into a stainless steel autoclave, seal the autoclave, replace the air in the autoclave with nitrogen three times, and then replace the autoclave with hydrogen Inner nitrogen three times and maintain a certain pressure in the kettle. Heat up to 85°C under stirring, maintain the reaction pressure at 1.75MPa, close the hydrogen valve after the reaction is over, let the gas out, open the autoclave to discharge, keep warm at about 75°C to filter out the catalyst, and use gas chromatography to analyze the reduction product, 3,4-dichloronitro The conversion rate of benzene is 100%, the selectivity of 3,4-dichloroaniline is 99.0%, and the dechlorination rate is 0.27%.
Embodiment 3
[0030] Increase the amount of catalyst to investigate the effect of catalyst amount on the hydrogenation of 3,4-dichloronitrobenzene.
[0031] 64 g of 3,4-dichloronitrobenzene and 0.18 g of 3% Pt (water content 59.98%) catalyst containing additives were added to a stainless steel autoclave, the autoclave was sealed, and the air in the autoclave was replaced with nitrogen for three times, and then Replace the nitrogen in the kettle with hydrogen three times and maintain a certain pressure in the kettle. Heat up to 85°C under stirring, maintain the reaction pressure at 1.75MPa, close the hydrogen valve after the reaction is over, let the gas out, open the autoclave to discharge, keep warm at about 75°C to filter out the catalyst, and use gas chromatography to analyze the reduction product, 3,4-dichloronitro The conversion rate of benzene is 100%, the selectivity of 3,4-dichloroaniline is 99.5%, and the dechlorination rate is 0.20%.
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