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Catalyst for synthesizing p-aminophenol by hydrogenation reduction of nitrobenzene and preparation method thereof

A technology for p-aminophenol and a catalyst is applied in the field of catalyst for preparing p-aminophenol by catalytic hydrogenation of nitrobenzene and the field of preparation thereof, which can solve the problems of poor PAP selectivity and the like, and achieves improved activity, high catalytic activity and catalytic stability, The effect of high specific surface

Active Publication Date: 2010-06-09
FUDAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Others such as Pt / nylon or Ni / HZSM-5 have better catalytic stability, but the selectivity of PAP is relatively poor

Method used

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  • Catalyst for synthesizing p-aminophenol by hydrogenation reduction of nitrobenzene and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Impregnate the chloroplatinic acid solution with 1% Pt in all silicon mesoporous zeolite MCM-41, MCM-48, SBA-12, SBA-15, MCF, HMS, or KIT-6 for 100-180 minutes , dry at 50-80°C, in an air atmosphere of 350°C, with a space velocity of 9 liters / (hour·gram), roast for 3 hours, switch to nitrogen at room temperature, and then pass through hydrogen for reduction. The reduction conditions are: temperature 450°C, space velocity 25 Liter / (hour·gram) for 3 hours. The hydrogenation reaction process of nitrobenzene is as follows: add catalyst, sulfuric acid, cetyltrimethylammonium bromide, and nitrobenzene into a four-neck flask, close the system, replace the air in the system with hydrogen for 3 times, and the reaction temperature 82°C, connected with a hydrogen meter, record the hydrogen consumption during the reaction, estimate the activity of the catalyst, suck out the supernatant liquid, and obtain the product after two times of steam distillation and acidity adjustment, and ...

Embodiment 2

[0021] Change the active species Ni to test the catalytic activity

[0022] Wet impregnation of 1% Ni chloride solution with all-silicon mesoporous zeolite SBA-15, impregnated for 100-180 minutes, dried at 70°C, and under air atmosphere of 350°C, the space velocity was 8 liters / (hour g ), roasted for 3 hours, switched to nitrogen at room temperature, and then reduced with hydrogen. The reduction conditions were: temperature 450 ° C, space velocity 22 liters / (hour·gram), and maintained for 3 hours. The hydrogenation reaction process of nitrobenzene is as follows: add catalyst, sulfuric acid, cetyltrimethylammonium bromide, and nitrobenzene into a four-neck flask, close the system, replace the air in the system with hydrogen for 3 times, and the reaction temperature 80°C, connected with a hydrogen meter, record the consumption of hydrogen during the reaction, estimate the activity of the catalyst, suck out the supernatant, and obtain the product after two times of steam distilla...

Embodiment 3

[0024] Changing Surfactants to Test Catalytic Activity for OP-10

[0025] Wet impregnation of all-silicon mesoporous zeolite SBA-15 with a chloroplatinic acid solution of 1% measured Pt, impregnated for 100-180 minutes, dried at 70°C, and under an air atmosphere of 350°C, the space velocity was 8 liters / (hour g ), roasted for 3 hours, switched to nitrogen at room temperature, and then reduced with hydrogen. The reduction conditions were: temperature 450 ° C, space velocity 22 liters / (hour·gram), and maintained for 3 hours. The hydrogenation reaction process of nitrobenzene is as follows: add the catalyst, sulfuric acid, OP-10, and nitrobenzene into the four-necked bottle, close the system, replace the air in the system with hydrogen for 3 times, the reaction temperature is 82 ° C, and the hydrogen meter Connected, record the consumption of hydrogen in the reaction process, estimate the activity of the catalyst, suck out the supernatant, and obtain the product through two steam...

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Abstract

The invention belongs to the technical field of catalysts, and in particular relates to a catalyst for synthesizing p-aminophenol by hydrogenation reduction of nitrobenzene and a preparation method thereof. The catalyst takes an all-silica mesoporous molecular sieve as a carrier and is prepared by loading active components, namely Pt and Ni, on the carrier. The preparation method for the catalyst comprises the following steps: impregnating the carrier by adopting a wet method, namely dripping solution of metal salts of the active components onto the carrier, baking the carrier in air and reducing the carrier with hydrogen to obtain the catalyst. The catalyst is used for catalytic hydrogenation of the nitrobenzene; and the intermediate product is rearranged in acidic aqueous solution to prepare the p-aminophenol, wherein the yield of the target product can reach over 75 percent. The preparation method for the catalyst is simple; and because the catalyst has relatively good stability and can be circulated for over 16 times, the catalyst has good industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a catalyst for preparing p-aminophenol by catalytic hydrogenation of nitrobenzene and a preparation method thereof. Background technique [0002] P-aminophenol (PAP) is a widely used fine chemical intermediate, mainly used in pharmaceutical, dyestuff and other related industries. The method for preparing p-aminophenol can be divided into nitrosation method, ammonolysis method, coupling reduction method, electrolytic reduction method, hydrogenation reduction and other methods. The raw materials involved include nitrobenzene, aniline, phenol, p-nitrochlorobenzene, p-nitrobenzene Nitrophenol, hydroquinone, etc. There are many chemical reducing agents used, such as iron powder, zinc powder, tin powder, sodium sulfide, ammonium sulfide, hydrogen gas, etc. However, there are two ideal methods that have been adopted by foreign industrial production, the electrolytic redu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/76B01J29/74C07C215/76C07C213/00
Inventor 钱林平徐新联
Owner FUDAN UNIV
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