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Nitrogen-doped ultra-thin carbon nanosheet loaded monoatomic catalyst and preparation method and application thereof

A technology of carbon nanosheets and nitrogen doping, which is applied in the direction of catalyst activation/preparation, amino compound preparation, chemical instruments and methods, etc., can solve the problem of low catalyst activity, and achieve simple and easy preparation methods, good reproducibility, The effect of adjustable metal loading

Active Publication Date: 2019-06-28
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The catalyst can solve the problem of low activity of existing catalysts

Method used

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  • Nitrogen-doped ultra-thin carbon nanosheet loaded monoatomic catalyst and preparation method and application thereof
  • Nitrogen-doped ultra-thin carbon nanosheet loaded monoatomic catalyst and preparation method and application thereof
  • Nitrogen-doped ultra-thin carbon nanosheet loaded monoatomic catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Example 1 Preparation of nitrogen-doped ultrathin carbon nanosheet-supported cobalt single-atom catalyst

[0055] 1) Weigh 12.7mg of cobalt acetate tetrahydrate and 18.4mg of 1,10-phenanthroline into a 100mL single-necked bottle, add 25mL of ethanol, and obtain Co(phen) after ultrasonication for 15 minutes 2 solution.

[0056] 2) Weigh 500mg g-C 3 N 4 Add to the aforementioned solution, sonicate for 15 minutes to make g-C 3 N 4 Disperse evenly. The one-necked bottle was placed in an 80°C oil bath to reflux for 4 hours, and then rotary evaporated at 40°C and 60 rpm for 30 minutes.

[0057] 3) The obtained solid Co(phen) 2 / g -C 3 N 4 Disperse in 150mL of methanol and sonicate at 50W for 5 minutes. Weigh 1.814g of pH buffer solution Tris (Tris) and dissolve it in 140mL of methanol, weigh 1.360g of polymerized monomer dopamine hydrochloride (DA) and dissolve it in 60mL of methanol, and dissolve the methanol of Tris and DA under stirring. The solution was added dr...

Embodiment 2

[0061] Example 2 Preparation of nitrogen-doped ultrathin carbon nanosheet-supported nickel single-atom catalyst

[0062] 1) Weigh 8.29mg of nickel acetate tetrahydrate and 18.4mg of 1,10-phenanthroline into a 100mL single-necked bottle, add 50mL of ethanol, and obtain Ni(phen) after ultrasonication for 15 minutes 3 solution.

[0063] 2) Weigh 1g g-C 3 N 4 Add to the aforementioned solution, sonicate for 30 minutes to make g-C 3 N 4 Disperse evenly. The one-necked bottle was refluxed in an oil bath at 60°C for 15 hours, and then rotary evaporated at 40°C and 60 rpm for 30 minutes.

[0064] 3) The obtained solid Ni(phen) 3 / g -C 3 N 4 Disperse in 150mL methanol and ultrasonicate for 5 minutes. Weigh 1.814g Tris and dissolve in 140mL of methanol, weigh 1.360g of dopamine hydrochloride and dissolve in 60mL of methanol, add the methanol solution of Tris and DA dropwise to the above dispersion liquid successively under stirring, and stir for 30h Afterwards, the solid was c...

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Abstract

The invention discloses a nitrogen-doped ultra-thin carbon nanosheet loaded monoatomic catalyst and a preparation method and application thereof. The monoatomic catalyst uses the nitrogen-doped ultrathin carbon nanosheet as a carrier, the metal loading is adjustable, the preparation method is simple and feasible and the reproducibility is good, and the preparation method is suitable for various metals (such as Co, Fe, Ni, Cu, Mn and the like). According to the technical scheme, the method comprises the following steps of: (1) adsorbing a complex formed by a metal salt and a ligand on g-C3N4;(2) spreading a layer of dopamine polymer outside the obtained complex; (3) carrying out high-temperature treatment on the coated material in an inert atmosphere to obtain the metal monoatomic catalystloaded on the nitrogen-doped ultrathin carbon nanosheet. The cobalt monatomic catalyst shows excellent activity and selectivity in nitrobenzene hydrogen transfer reaction, and the TOF value of the catalyst under similar reaction conditions is 20 times of the best result reported by the literature, so that the cobalt monatomic catalyst has great application prospect.

Description

technical field [0001] The invention belongs to the field of catalysts, and relates to a single-atom catalyst supported by nitrogen-doped ultra-thin carbon nanosheets, a preparation method and application thereof. Background technique [0002] Aromatic amines are very important intermediates in the preparation of polymers, pharmaceuticals and fine chemicals, and can be prepared by hydrogenation of aromatic nitro compounds. In recent years, a series of heterogeneous catalysts based on non-precious metals such as Fe and Co have been developed to catalyze this reaction. However, the reaction conditions required by this method are relatively harsh, the requirements for equipment are high, and dangerous hydrogen will be used. Therefore, as Complementary to this method, the reaction conditions for the hydrogen transfer reaction of aromatic nitro compounds are milder and the hydrogen donors are safer and easier to obtain. The non-noble metal heterogeneous catalysts reported in the...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J37/08C07C211/46C07C209/32
Inventor 宋卫国李会宁曹昌燕
Owner INST OF CHEM CHINESE ACAD OF SCI
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