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Preparation method for Ni, Cu and Zn-loaded mesoporous MnO2 catalyst and 4, 4-dimethyl-1-(4-p-chlorophenyl)-3-pentanone

A technology of p-chlorophenyl and catalyst is applied in the field of preparation of mesoporous MnO2 catalyst and 4,4-dimethyl-1--3-pentanone, which can solve the problem that it is difficult to achieve quality and yield, and the reaction conditions are harsh. and other problems, to achieve the effect of improving industrial production efficiency, improving quality and good stability

Active Publication Date: 2015-10-28
JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The hydrogenation from intermediate 1 to intermediate 2 is a key step in the synthesis process. In the existing process, Raney nickel is often used as the hydrogenation catalyst, which needs to be reacted under high temperature and high pressure. The reaction conditions are harsh, and it is difficult to achieve the desired quality and yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1) Take SBA-15 to make a solution in n-hexane, and disperse it ultrasonically for 2 hours. 30% Mn(NO 3 ) 2 The solution was then continuously stirred at room temperature for 8 hours, filtered with suction, dried under vacuum and then calcined at 300°C for 4 hours. The obtained solid was stirred in sodium hydroxide solution for 10 hours, washed, dried, and ground to obtain mesoporous MnO 2 powder.

[0032] 2) Dissolve nickel nitrate, copper nitrate, and zinc nitrate in deionized water to make a metal salt solution with an overall concentration of 0.1mol / L, then mix it with the manganese dioxide powder obtained in step 1), and stir at room temperature After 12 hours, the obtained impregnating solution was dried at 80°C, and calcined at 300°C for 3 hours to obtain a block solid; the obtained block solid was ground through a 100-mesh sieve, and reduced by passing H2 in a tube furnace at 300°C After reacting for 3h, the mesoporous MnO supported by nickel, copper and zin...

Embodiment 2

[0034] 1) Take SBA-15 to make a solution in n-hexane, and disperse it ultrasonically for 2 hours. 50% Mn(NO 3 ) 2 The solution was then continuously stirred at room temperature for 12 hours, filtered with suction, dried in vacuum and calcined at 400° C. for 4 hours. The obtained solid was stirred in sodium hydroxide solution for 20 hours, washed, dried, and ground to obtain mesoporous MnO 2 powder.

[0035] 2) Dissolve nickel nitrate, copper nitrate, and zinc nitrate in deionized water to make a metal salt solution with an overall concentration of 0.3mol / L, then mix it with the manganese dioxide powder obtained in step 1), and stir at room temperature After 30 hours, the obtained impregnating solution was dried at 100°C, and calcined at 600°C for 6 hours to obtain a block solid; the obtained block solid was ground through a 100-mesh sieve, and reduced by H2 in a tube furnace at 500°C After 6h, the mesoporous MnO supported by Ni, Cu and Zn was obtained 2 catalyst. The mo...

Embodiment 3

[0037] 1) Take SBA-15 to make a solution in n-hexane, and ultrasonically disperse for 3 hours. 40% Mn(NO 3 ) 2 The solution was then continuously stirred at room temperature for 8 hours, filtered with suction, dried in vacuo and then calcined at 350° C. for 3 hours. The obtained solid was stirred in sodium hydroxide solution for 15 hours, washed, dried and ground to obtain mesoporous MnO 2 powder.

[0038]2) Dissolve nickel nitrate, copper nitrate, and zinc nitrate in deionized water to make a metal salt solution with an overall concentration of 0.2mol / L, then mix it with the manganese dioxide powder obtained in step 1), and stir at room temperature After 20 hours, the obtained impregnation solution was dried at 50°C and calcined at 500°C for 4 hours to obtain a block solid; the obtained block solid was ground through a 100-mesh sieve, and reduced by passing H2 in a tube furnace at 400°C After reacting for 4h, the mesoporous MnO supported by nickel, copper and zinc was ob...

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Abstract

The invention relates to a preparation method for a Ni, Cu and Zn-loaded mesoporous MnO2 catalyst and 4, 4-dimethyl-1-(4-p-chlorophenyl)-3-pentanone. The catalyst comprises a mesoporous MnO2 carrier, Ni, Cu and Zn, wherein Ni, Cu and Zn are loaded on the mesoporous MnO2 carrier. The molar ratio of Ni, Cu and Zn is 1:0.3-1:0.1-0.3. The mass ratio of the sum of Ni, Cu and Zn to the mesoporous MnO2 carrier is 1-3:10. The catalyst prepared through the above method is high in catalytic activity, low in cost, simple in preparation technology and long in service life. The catalyst is applied to the hydrogenation reaction of 4, 4-dimethyl-1-(4-p-chlorophenyl)-1-pentene-3-ketone for preparing 4, 4-dimethyl-1-(4-p-chlorophenyl)-3-pentanone. The yield and the purity are up to 99%.

Description

technical field [0001] The invention relates to a kind of mesoporous MnO supported by nickel, copper and zinc 2 Catalyst and preparation method of 4,4-dimethyl-1-(4-p-chlorophenyl)-3-pentanone. Background technique [0002] Tebuconazole is a sterol demethylation inhibitor and a highly effective fungicide for seed treatment or foliar spraying of various crops. It was first developed by Bayer Company. Its common name in English is tebuconazole. Its chemical structure is: [0003] . [0004] Tebuconazole has a wide bactericidal spectrum, not only has high activity, but also has a long duration. It is mainly used to prevent and control various fungal diseases on crops such as wheat, peanuts, vegetables, bananas, apples, and pears. In 2014, the global sales of tebuconazole exceeded US$800 million, ranking second only to azoxystrobin among all fungicide varieties. [0005] The relatively mature production process of tebuconazole is to use p-chlorobenzaldehyde and pinacolone...

Claims

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Application Information

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IPC IPC(8): B01J23/80B01J35/10C07C45/62C07C49/233
Inventor 顾怡周炜周彬胡春红秦鸿飞
Owner JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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