Method for preparing benzhydrol by hydrogenation of benzophenone

A technology of benzophenone and benzphenyl alcohol, which is applied in the field of hydrogenation of benzophenone to produce benzphenyl alcohol, can solve the problems of unfavorable large-scale industrial production separation, difficult industrial application, expensive catalyst, etc., and achieve easy large-scale industrialization Effects on production, sintering inhibition, excellent conversion and selectivity

Pending Publication Date: 2020-06-05
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this series of reaction systems uses noble metal Pd as the main active component, the catalyst is expensive, and it is not easy to realize industrial application.
In addition, a large amount of basic protective agent needs to be added to the reaction system to achieve excellent catalytic effect, which is not conducive to large-scale industrial production of separation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Mix 4.3 g of copper nitrate, concentrated ammonia water, and deionized water at room temperature to prepare a mixture with a pH of 9.5 to 12.5, add 5.75 g of powdered aluminum oxide to it, and stir for 12 hours at room temperature. The temperature rises to 120°C, and the pH value of the mixed solution is monitored in real time until it drops to 6-7. Filter and wash with deionized water. The obtained solid sample was dried in an oven at 100°C for 6 hours, and then transferred to a muffle furnace for calcination at 650°C for 3 hours to obtain a catalyst Cu / Al 2 O 3 .

[0030] Take 0.1g of the above catalyst and place it in a connected high-temperature reduction furnace to reduce the catalyst. The reduction temperature is 350℃, the reduction time is 1h, the reduction pressure is 0.3MPa, the reducing gas is hydrogen, and the gas space velocity is 3000h. -1 . After the reduction, the temperature was lowered to room temperature and switched to nitrogen. Under the protection of ...

Embodiment 2

[0032] Mix 4.3 g of copper nitrate, concentrated ammonia water, and deionized water at room temperature to prepare a mixture with a pH of 9.5 to 12.5, add 5.75 powdered aluminum oxide to it, and stir for 12 hours at room temperature. The temperature rises to 120°C, and the pH value of the mixed solution is monitored in real time until it drops to 6-7. Filter and wash with deionized water. The obtained solid sample was dried in an oven at 100°C for 6 hours, and then transferred to a muffle furnace for calcination at 650°C for 3 hours to obtain a catalyst Cu / Al 2 O 3 .

[0033] Weigh the 2.0 g sample prepared above, immerse it in an equal volume of the aqueous solution containing palladium nitrate for 36 hours, and dry it in an oven at 100°C for 6 hours. Then transfer to a muffle furnace for calcination at 650°C for 6 hours. The component in the obtained catalyst is Cu-Pd / Al 2 O 3 .

[0034] Take 0.1g of the above catalyst and place it in a connected high-temperature reduction fur...

Embodiment 3

[0036] Mix 4.3 g of copper nitrate, concentrated ammonia water, and deionized water at room temperature to prepare a mixture with a pH of 9.5 to 12.5, add 5.75 g of powdered aluminum oxide to it, and stir for 12 hours at room temperature. The temperature rises to 120°C, and the pH value of the mixed solution is monitored in real time until it drops to 6-7. Filter and wash with deionized water. The obtained solid sample was dried in an oven at 100°C for 6 hours, and then transferred to a muffle furnace for calcination at 650°C for 3 hours to obtain a catalyst Cu / Al 2 O 3 .

[0037] Weigh the 2.0 g sample prepared above, immerse it in an equal volume of an aqueous solution containing magnesium nitrate for 36 hours, and dry it in an oven at 100°C for 6 hours. Then transfer to a muffle furnace for calcination at 650°C for 6 hours. The component in the obtained catalyst is Cu-Mg / Al 2 O 3 .

[0038] Take 0.1g of the above catalyst and place it in a connected high-temperature reduction...

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PUM

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Abstract

The invention discloses a method for preparing benzhydrol by hydrogenation of benzophenone, which adopts a supported heterogeneous catalyst, and comprises the following components in percentage by mass: 0.1-60% of a main active component, 0-15% of an assistant and the balance of a carrier, wherein the main active component is one or more of Cu, Ni and Co, the assistant is one or more simple substances of Pd, Pt, Ru, Rh, Ir, Au, Re, Al, B, Cr, Mg, Mn, La, Ag, Li, Zn and Ce, or oxides, and the carrier is one or more of activated carbon, silicon oxide, aluminum oxide, titanium oxide, a molecularsieve, diatomite and zirconium oxide. According to the invention, a cheap metal is used as a main active component, so that the cost of the catalyst is reduced, a protective agent is not required to be added in the benzhydrol preparation process, an excellent conversion rate and selectivity can be achieved under mild conditions, the catalyst preparation method is simple, and large-scale industrialproduction is easy to realize.

Description

Technical field [0001] The invention relates to a method for preparing benzophenone by hydrogenation of benzophenone, and belongs to the technical field of chemical synthesis. Background technique [0002] Benzyl alcohol, also known as α-phenylbenzyl alcohol, is an important organic intermediate, which is widely used in pharmaceutical synthesis, such as the synthesis of diphenhydramine, diphenyllaline, cyclizine, and dimenhydrinate (Antihistamines), benzotropine (anticholinergic drugs), cephalosporin antibiotics (anti-inflammatory drugs), cinnarizine (vasodilators), adrafenib (central nervous system stimulants), etc. [0003] At present, benzyl alcohol is mainly prepared by benzophenone reduction, including three processes: [0004] (1) Zinc powder or aluminum powder and lye are mixed and used. This method requires the use of a large amount of zinc powder or aluminum powder. After the reaction, a large amount of waste liquid containing heavy metals is produced. The product purity is...

Claims

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Application Information

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IPC IPC(8): C07C29/145C07C33/24B01J23/72B01J23/89B01J23/78B01J23/83B01J29/46B01J23/755B01J23/75B01J23/889B01J23/80
CPCC07C29/145B01J23/72B01J23/8926B01J23/78B01J23/83B01J29/46B01J23/755B01J23/75B01J23/8892B01J23/80C07C33/24Y02P20/52
Inventor 陈兴坤丁云杰翁高翔王赛赛
Owner ZHEJIANG NORMAL UNIVERSITY
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