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N doped activated carbon-supported Pd-Fe catalyst for synthesizing diphenylcarbinol through catalytic hydrogenation of diphenyl ketone and application thereof

A technology of iron catalyst and benzophenone, which is applied in the direction of physical/chemical process catalysts, preparation of organic compounds, preparation of hydroxyl compounds, etc., can solve the problems of unrealizable benzyl alcohol process, low production capacity, and many wastes, etc., and achieve maintenance Target product selectivity, content reduction, high catalytic activity effect

Active Publication Date: 2018-12-21
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The earliest production process of diphenylmethanol was zinc powder reduction, and then developed into aluminum powder reduction. These two methods have many wastes, low production capacity, poor quality and high energy consumption.
[0004] The catalytic hydrogenation process is a green synthesis process, but when benzophenone is hydrogenated to synthesize benzphenyl alcohol, it is often prone to excessive hydrogenation to form diphenylmethane, and the process of catalytic hydrogenation to synthesize benzphenyl alcohol has not been realized in industry

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0029] Take by weighing 10g activated carbon (particle size is 150 orders, specific surface area is 1800m 2 / g, pore volume is 0.8ml / g), under argon atmosphere, feed ammonia gas at 800 ℃, ammonia flow rate 2L / h, process 15h, obtain 10g nitrogen-doped activated carbon (particle size is 150 orders, specific surface area 1800m 2 / g, pore volume is 0.8ml / g, N content is 2.0wt%). Configure 8ml containing H 2 PdCl 4 and FeCl 3 The mixed solution (the quality of Pd in ​​the mixed solution is 0.5g, and the quality of Fe is 0.2g); the mixed solution is added dropwise to the above-mentioned nitrogen-doped activated carbon, and stirred evenly. The impregnated catalyst was vacuum dried at 20°C for 20 h. The dried catalyst was heated in H 2 Reduction was carried out at 40° C. for 10 h under the atmosphere to obtain a palladium-iron catalyst supported on nitrogen-doped activated carbon.

Embodiment 3

[0031] Take by weighing 10g activated carbon (particle size is 300 mesh, specific surface area is 1200m 2 / g, pore volume is 0.3ml / g), under helium atmosphere, feed ammonia gas at 1200 ℃, ammonia flow rate 5L / h, process 5h, obtain 10g nitrogen-doped activated carbon (particle size is 300 order, specific surface area is 1200m 2 / g, pore volume is 0.3ml / g, N content is 6.0wt%). Configure 3ml containing Pd(NO 3 ) 2 and FeCl 3 The mixed solution (the quality of Pd in ​​the mixed solution is 0.2g, and the quality of Fe is 0.2g); the mixed solution is added dropwise to the above-mentioned nitrogen-doped activated carbon, and stirred evenly. The impregnated catalyst was vacuum-dried at 30 °C for 4 h. The dried catalyst was heated in H 2 Reduction was carried out at 80° C. for 3 h under atmosphere to obtain a palladium-iron catalyst supported on nitrogen-doped activated carbon.

Embodiment 4

[0033] Take by weighing 10g activated carbon (particle size is 600 mesh, specific surface area is 1500m 2 / g, pore volume is 0.5ml / g) mixed with 0.6g urea evenly, and treated at 600°C for 20h under nitrogen atmosphere to obtain 10g nitrogen-doped activated carbon (particle size is 600 mesh, specific surface area is 1500m 2 / g, pore volume is 0.5ml / g, N content is 1.0wt%). Configure 5ml containing Pd(NO 3 )2 and Fe(NO 3 ) 3 The mixed solution (the quality of Pd in ​​the mixed solution is 0.3g, and the quality of Fe is 0.3g); the mixed solution is added dropwise to nitrogen-doped activated carbon, and stirred evenly. The impregnated catalyst was vacuum-dried at 30 °C for 8 h. The dried catalyst was heated in H 2 Reduction was carried out at 70° C. for 5 h under atmosphere to obtain a palladium-iron catalyst supported on nitrogen-doped activated carbon.

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Abstract

The invention discloses an N doped activated carbon-supported Pd-Fe catalyst for synthesizing diphenylcarbinol through catalytic hydrogenation of diphenyl ketone and application thereof. The N doped activated carbon-supported Pd-Fe catalyst is prepared from an N doped activated carbon carrier and active components Pd and Fe supported on the surface of the carrier, wherein the support capacity of Pd is 1 to 5 weight percent, and the support capacity of Fe is 1 to 5 weight percent; the granularity of N doped activated carbon is 100 to 1000 meshes, the specific surface area is 600 to 2000 m<2> / g,and the pore volume is 0.3 to 0.8 ml / g; an N element in the N doped activated carbon is directly doped in an activated carbon skeleton or between activated carbon and is connected by N-C bonds, wherein the N content is 0.5 to 10 weight percent. The invention provides the application of the N doped activated carbon-supported Pd-Fe catalyst in synthesizing the diphenylcarbinol through the catalytichydrogenation of the diphenyl ketone. High catalytic activity, high product selectivity, high catalytic hydrogenation reaction speed and high stability are expressed.

Description

(1) Technical field [0001] The invention relates to a nitrogen-doped activated carbon-supported palladium-iron catalyst used for catalytic hydrogenation of benzophenone to synthesize diphenylmethanol and an application thereof. (2) Background technology [0002] Diphenylmethanol, also known as α-phenylbenzyl alcohol, is an important organic intermediate, mainly used in the synthesis of diphenhydramine (antihistamine), dimenhydrinate (antihistamine, Chengyunning) , cyclizine (antihistamine), diphenylraline (antihistamine), benzotropine (anticholinergic), modafinil (antidepressant), cinnarizine (vasodilator), Synthesis of drfenib (central nervous system stimulant) and other drugs. [0003] The synthesis of benzhydryl alcohol is mainly obtained through the reduction of benzophenone. The earliest production process of diphenylmethanol was zinc powder reduction, and then developed into aluminum powder reduction. These two methods have many wastes, low production capacity, poor ...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J35/02C07C29/145C07C33/24
CPCC07C29/145B01J27/24B01J35/50B01J35/40C07C33/24
Inventor 张群峰黄伟民马磊卢春山丰枫李小年
Owner ZHEJIANG UNIV OF TECH
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