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A method for preparing PD nanoparticles

A nanoparticle and aniline technology, applied in the field of preparing Pd nanoparticles, can solve the problems of unfavorable recovery and reuse, difference in substrate adaptability, easy pollution of the environment, etc., and achieve the effect of low catalyst consumption, simple operation and high reactivity

Inactive Publication Date: 2020-10-30
HENAN ACADEMY OF SCI CHEM RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although Pd is one of the more commonly used transition metal catalysts, the catalytic process of different Pd catalysts is not the same, and the adaptability to substrates is also quite different.
Moreover, traditional homogeneous catalysts are not conducive to recycling and reuse, not only waste resources, but also easily pollute the environment. Therefore, it is necessary to study reusable Pd catalysts.

Method used

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  • A method for preparing PD nanoparticles
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  • A method for preparing PD nanoparticles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Preparation method of Pd nanoparticles

[0017] (1) First add 2ml of ethanol solvent to the 10ml reaction bottle, then add 5mmol of aniline, 12.5mmol of tetrafluoroboric acid and mix evenly, add 12.5mmol of tert-butyl nitrite dropwise to the mixed solution under ice bath conditions, return to room temperature, and react After 0.5h, a small amount of diethyl ether was added to the reaction solution, and a white precipitate was formed, filtered and dried to obtain 0.92g (4.8mmol) of phenyldiazonium tetrafluoroborate, with a yield of 96%;

[0018] (2) Add 4mmol phenyldiazonium tetrafluoroborate (dissolved in 50ml tetrahydrofuran) into a 250ml reaction flask, then add 1mmol acetic acid Pd (dissolved in 50ml methanol), stir at room temperature for 10min~15min, the reaction solution turns orange , add dropwise 5mmol sodium borohydride (dissolved in 50ml methanol) solution under ice-bath conditions, and react at room temperature for 1h until the reaction is complete; the react...

Embodiment 2

[0020] Catalytic hydrogenation of p-nitrobenzene with Pd nanoparticles

[0021] In the 25ml reaction bottle, add 2mmol nitrobenzene, 10ml water is made solvent, 2.4mg Pd nanoparticles prepared by the present invention, feed H under normal temperature and pressure. 2 , after reacting for 12h, TLC detects that the reaction is complete, the reaction solution is extracted with dichloromethane, and the organic phase is extracted with anhydrous Na 2 SO 4 After drying, the solvent was evaporated under reduced pressure, and purified by column chromatography to obtain 0.18 g (1.94 mmol) of the corresponding target compound aniline, with a yield of 97%. analyze data: 1 H NMR (400MHz, CDCl 3 )δ=7.11(t, J=8.0Hz, 2H), 6.72(t, J=8.0Hz, 21H), 6.59(d, J=8.0Hz, 2H), 3.53(s, br, 2H); GC- MS,m / z,93[M + ].

Embodiment 3

[0023] Catalytic hydrogenation of p-chloronitrobenzene with Pd nanoparticles

[0024] In the 25ml reaction flask, add 2mmol p-chloronitrobenzene, 10ml water as solvent, 3mg of Pd nanoparticles prepared by the present invention, feed H under normal temperature and pressure. 2 , after reacting for 12h, TLC detects that the reaction is complete, the reaction solution is extracted with dichloromethane, and the organic phase is extracted with anhydrous Na 2 SO 4 After drying, the solvent was evaporated under reduced pressure, and purified by column chromatography to obtain 0.25 g (1.96 mmol) of the corresponding target compound p-chloroaniline, with a yield of 98%. The analysis data is: 1 H NMR (400MHz, CDCl 3 )δ=7.07(d, J=8.0Hz, 2H), 6.54(d, J=8.0Hz, 2H), 3.62(s, 2H); GC-MS, m / z, 127[M + ].

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Abstract

The invention provides a method for preparing Pd nanoparticles and belongs to the technical field of organic synthesis. The method comprises the following steps: preparing an ethanol solution of aniline and tetrafluoroboric acid by taking cheap aniline as a starting raw material, and adding tert-butyl nitrite into the solution dropwise under the condition of ice bath to obtain phenyl diazonium tetrafluoroborate; and mixing the phenyl diazonium tetrafluoroborate and acetic acid Pd into a uniform solution, performing stirring reaction at room temperature, adding a methanol solution of sodium borohydride dropwise under the condition of ice bath, and performing reaction to obtain the Pd nanoparticles. The method takes the aniline as a starting substrate, is simple, convenient and safe to operate and is low in cost; furthermore, the obtained Pd nanoparticles have the characteristics of high reaction activity and insusceptibility to deactivation.

Description

technical field [0001] The invention relates to a method for preparing Pd nanoparticles and an application thereof, belonging to the technical field of organic synthesis. Background technique [0002] The transition metal Pd (palladium) has excellent catalytic performance, and as a catalyst, it is widely used in catalytic oxidation, reduction and coupling reactions. Although Pd is one of the more commonly used transition metal catalysts, the catalytic process of different Pd catalysts is not the same, and the adaptability to substrates is also quite different. Moreover, traditional homogeneous catalysts are not conducive to recovery and reuse, which not only wastes resources, but also easily pollutes the environment. Therefore, the research on reusable Pd catalysts is very necessary. The traditional way to improve the catalytic efficiency of Pd is to change the combination state of the ligand and Pd. However, recent studies have shown that making Pd nanoparticles is also a ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/44B01J37/16C07C211/46C07C211/52C07C209/36
CPCB01J23/44B01J35/0013B01J37/16C07C209/36C07C209/365C07C211/46C07C211/52
Inventor 代本才刘长春赵永德霍萃萌陈瑨魏爱勤陈杰英周洋
Owner HENAN ACADEMY OF SCI CHEM RES INST CO LTD
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