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Preparation method of catalyst for synthesis of benzophenone by dehydrogenation of benzhydrol

A technology of diphenylmethanol and benzophenone, which is applied in the field of heterogeneous catalytic reactions, can solve problems such as complex processes, inability to meet the requirements of green environmental protection development, and expensive raw materials, and achieve high reaction efficiency, long life, and high selectivity. Effect

Active Publication Date: 2020-04-10
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method and application of a catalyst for synthesizing benzophenone by dehydrogenation of diphenylmethanol in order to overcome the defects of expensive raw materials, complex process or inability to meet the development requirements of green environmental protection in the above-mentioned prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] This embodiment is a preparation method for the synthesis of benzophenone catalyst through the dehydrogenation of diphenylmethanol, and the steps are as follows:

[0036] (1) Preparation of mesoporous silica material Cu-Fe-HMS

[0037] 33mL concentration is 0.068mol L -1 Cu(NO 3 ) 2 Aqueous solution, 0.068mol·L -1 Fe(NO 3 ) 3 Aqueous solution, 1.0mL (1mol L -1) hydrochloric acid and 15.0 g of absolute ethanol were successively added into a 50 ml beaker, stirred magnetically for 30 min, and then the mixed solution was added into a three-necked flask containing 3.26 g of hexadecylamine, and stirred for 30 min in a water bath at 45°C. Then, a mixed solution of 3.0 g of isopropanol and 10.4 g of tetraethyl orthosilicate was slowly added dropwise, and stirring was continued for 18 hours in a water bath at 45°C. The obtained product was centrifuged and washed several times, and the obtained solid powder was dried in an oven at 100 °C for 10 h, then transferred to a muf...

Embodiment 2

[0043] The Pd-L-Cu-Fe-HMS catalyst obtained in Example 1 is used for the synthesis of benzophenone by the dehydrogenation of diphenylmethanol, and the specific steps are to add 20 mg of Pd-L-Cu-Fe- HMS catalyst, 0.25g benzhydryl alcohol and 35ml ethanol, react under normal pressure, stirring and heating under reflux conditions for 18h, after the reaction is completed, filter out the catalyst, distill and remove the solvent to obtain benzophenone with a yield of 99.7%.

Embodiment 3

[0045] The catalyst recovered in Example 2 is used for the synthesis of benzophenone by the dehydrogenation of diphenylmethanol, and the specific steps are: in a 100mL round-bottomed flask, add the catalyst 15mg Pd-L-Cu-Fe- HMS catalyst, 0.2g benzphenyl alcohol and 35ml ethanol, react under normal pressure, stirring and heating under reflux conditions for 18h, after the reaction is completed, filter out the catalyst, distill off the solvent to obtain benzophenone, the yield is greater than 99.4%.

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PUM

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Abstract

The invention relates to a preparation method of a catalyst for synthesis of benzophenone by dehydrogenation of benzhydrol. The preparation method comprises the following steps: preparing a Cu-Fe-HMSmesoporous silica material doped with Cu and Fe; carrying out surface modification on the Cu-Fe-HMS by adopting a surface modifier to obtain aminated Cu-Fe-HMS; carrying out surface modification on the aminated Cu-Fe-HMS by adopting a surface modifier so as to introduce a pyridine ring to obtain L-Cu-Fe-HMS of which the surface contains an L-Cu-Fe-HMS capable of being coordinated with metal to form a stable chelate structure; and loading Pd in L-Cu-Fe-HMS through a coordination reaction so as to obtin the target product Pd-L-Cu-Fe-HMS catalyst. Compared with the methods in the prior art, the method has the advantages of high catalytic efficiency, high selectivity of the target product benzophenone, easiness in separation and cyclic utilization after reaction and the like.

Description

technical field [0001] The invention relates to the technical field of heterogeneous catalytic reactions, in particular to a preparation method and application of a catalyst for synthesizing benzophenone through dehydrogenation of benzyl alcohol. Background technique [0002] Benzophenone and its derivatives are ultraviolet absorbers and initiators, used in organic pigments, UV-curable coatings, inks, fragrances and cosmetics, and also used as fine organic chemical intermediates such as medicines and insecticides. In the pharmaceutical industry, benzophenone is used in the production of bicycline, benzotropine hydrobromide and diphenhydramine salt, etc. Benzophenone is also a styrene polymerization inhibitor and a fragrance fixative, which can give fragrances a sweet smell and is used in many perfumes and soap essences. [0003] The synthetic method of benzophenone mainly contains phosgene method, which is to utilize phosgene and benzene in anhydrous A1C1 3 In the presence...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/035C07C45/00C07C49/786
CPCB01J29/0356C07C45/002B01J2229/18B01J35/647C07C49/786Y02P20/584
Inventor 李俊陶韶薄戚蓥梦吴丽陈睿付晓静
Owner SHANGHAI INST OF TECH