Nanocarbon-loaded atomic-scale dispersion rhodium catalyst, preparation method thereof, and application of catalyst in hydrogenation reaction of nitrile compounds

A rhodium catalyst and hydrogenation reaction technology, applied in the field of organic chemical raw material synthesis, can solve the problems of harsh reaction conditions and poor selectivity, and achieve the effects of low raw material cost, stable performance and simple preparation process

Pending Publication Date: 2021-09-10
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problems of harsh reaction conditions and poor selectivity in the hydrogenation reaction of catalytic nitrile compounds, the invention provides a nanometer carbon-supported atomically dispersed rhodium catalyst and a preparation method thereof for the hydrogenation reaction of nitrile compounds. Nanocarbon-supported rhodium catalysts are rhodium catalysts supported by graphene / nanodiamond composites

Method used

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  • Nanocarbon-loaded atomic-scale dispersion rhodium catalyst, preparation method thereof, and application of catalyst in hydrogenation reaction of nitrile compounds
  • Nanocarbon-loaded atomic-scale dispersion rhodium catalyst, preparation method thereof, and application of catalyst in hydrogenation reaction of nitrile compounds
  • Nanocarbon-loaded atomic-scale dispersion rhodium catalyst, preparation method thereof, and application of catalyst in hydrogenation reaction of nitrile compounds

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Experimental program
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Effect test

Embodiment 1

[0035] The preparation process of the catalyst is as follows:

[0036] (1) Preparation of carbon nanocarriers:

[0037] The nano-diamond raw material is placed in an argon atmosphere at 900-1300° C. and 80-100 mL / min for calcination treatment, and the treatment time is 3-4 hours. After the calcination treatment, a nano-carbon carrier with a core-shell structure is obtained. Such as figure 1 As shown, the prepared carrier has a core-shell structure with nano-diamond as the core and defect-rich graphene as the shell, and a core-shell structure with sp3 carbon core-sp2 carbon shell hybridization.

[0038] (2) The process of deposition precipitation method:

[0039] Add 20-40mL of water into a 100mL round bottom flask, put 200mg of nano-carbon carrier, ultrasonically disperse evenly, and then adjust the pH value to 11-12 with sodium carbonate solution to obtain a nano-carbon carrier dispersion; then prepare 0.01mol / L nitric acid rhodium solution, and calculate the consumption o...

Embodiment 2

[0041] Weigh 30 mg of Rh / ND@G catalyst (rhodium atomic loading is 0.06 wt%) and disperse it in 10 mL of methanol, and add 0.5 mmol of benzonitrile. Filled with 0.6MPa H 2 , heated to 60°C, and stirred for 4h. The conversion rate of benzonitrile was 99.08%, and the selectivity of dibenzylamine was >99%.

Embodiment 3

[0043] Weigh 30 mg of Rh / ND@G catalyst (rhodium atomic loading is 0.06 wt%) and disperse it in 10 mL of methanol, and add 0.5 mmol of benzonitrile. Filled with 0.6MPa H 2 , warmed up to 40°C, and stirred for 4h. The conversion rate of benzonitrile was 81.41%, and the selectivity of dibenzylamine was >99%.

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Abstract

The invention discloses a nanocarbon-loaded atomic-scale dispersion rhodium catalyst, a preparation method thereof, and application of the catalyst in hydrogenation reaction of nitrile compounds, and belongs to the technical field of synthesis of organic chemical raw materials. The catalyst takes nanocarbon as a carrier, precious metal rhodium is uniformly loaded on the surface of the nanocarbon carrier in an atomic-scale dispersion form, and the loading capacity of rhodium is 0.01%-0.38%. The catalyst is used for catalytic hydrogenation reaction of nitrile compounds, and the nitrile compounds are catalyzed under mild reaction conditions to generate secondary amine compounds; the catalytic reaction conditions are as follows: the reaction temperature is 40-80 DEG C, and the pressure is 0.2-0.8 MPa; and the catalyst is low in synthesis raw material cost, simple in preparation process, stable in performance, high in catalytic activity and good in selectivity.

Description

technical field [0001] The invention relates to the technical field of synthesis of organic chemical raw materials, in particular to a nano-carbon-supported atomically dispersed rhodium catalyst, a preparation method thereof, and an application in the hydrogenation reaction of nitrile compounds. Background technique [0002] Secondary amine compounds are an important compound in organic chemistry and widely exist in natural products and bioactive molecules. Although secondary amine compounds are widely used and exist in many different materials, there are still huge challenges in the synthesis of secondary amine compounds, and traditional synthesis methods inevitably produce waste or environmental problems. The study of new synthetic methods is imminent. In recent years, the hydrogenation of nitrile compounds has attracted extensive attention because of its ability to selectively obtain different amine compounds. However, the control of the reaction selectivity largely depe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/46B01J37/03B01J37/08B01J37/18C07C209/48C07C211/27C07C213/02C07C217/58C07C211/29
CPCB01J23/464B01J35/0013B01J35/0093B01J37/035B01J37/08B01J37/18C07C209/48C07C213/02C07C211/27C07C217/58C07C211/29
Inventor 刘洪阳陈家威刁江勇
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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