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Preparation method of sulfur vacancy Cu-MoS2 catalyst

A cu-mos2 and catalyst technology, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problem of low catalytic activity and achieve high catalytic activity and mild reaction conditions.

Active Publication Date: 2021-03-12
HANGZHOU NORMAL UNIVERSITY
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Problems solved by technology

[0006] The present invention aims to overcome the problem of low catalytic activity of existing electrocatalytic nitrogen fixation catalysts, and provides a sulfur vacancy Cu-MoS 2 The preparation method of the catalyst, the present invention realizes the preparation of a sulfide sulfur vacancy catalyst, the prepared MoS 2 The catalyst presents a nanoflower structure. The doping of Cu forms a heteronuclear diatom center, and at the same time introduces sulfur vacancies, which perfectly realizes the structural design of defect catalysts and heteronuclear diatoms. The present invention prepares Cu-MoS 2 The catalyst exhibits excellent electrocatalytic nitrogen reduction activity, and the synthesis method has mild reaction conditions and high yield, which is suitable for large-scale production of the catalyst

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  • Preparation method of sulfur vacancy Cu-MoS2 catalyst
  • Preparation method of sulfur vacancy Cu-MoS2 catalyst

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preparation example Construction

[0035] A sulfur-vacancy Cu-MoS 2 The preparation method of catalyst comprises the following steps:

[0036] (1) Dissolve sodium molybdate with a concentration of 0.1-1mol / L in water, then add nitric acid dropwise and stir, react in the reactor at 150-250°C for 16-20h, and then centrifugally wash to obtain MoO 3 Nanobelt; the volume ratio of sodium molybdate, water and nitric acid is 0.5-0.8:5-10:1

[0037] (2) MoO 3 Dissolve the nanobelts in water and stir until dissolved, add thiourea and divalent copper compounds and stir until dissolved, react in the reactor at 100-200°C for 10-14h, and then centrifugally wash to obtain Cu-doped MoS 2 Catalyst; MoO 3 The compound molar ratio of nanobelt, thiourea and divalent copper is 0.08:1-1.1:0.005-0.01; the compound of divalent copper is one of copper chloride, copper sulfate, copper nitrate and copper acetate;

[0038] (3) MoS doped with Cu 2 The catalyst is calcined at 350-500°C for 180-320min under protective gas (argon, nitrog...

Embodiment 1

[0040] A sulfur-vacancy Cu-MoS2 The preparation method of catalyst comprises the following steps:

[0041] (1) Dissolve sodium molybdate with a concentration of 0.5 mol / L in water, then add nitric acid dropwise and stir, react in the reactor at 200°C for 18 hours, and then centrifugally wash to obtain MoO 3 Nanobelt; the volume ratio of sodium molybdate, water and nitric acid is 0.65:8:1

[0042] (2) MoO 3 Dissolve the nanobelts in water and stir until dissolved, add thiourea and divalent copper compounds and stir until dissolved, react in the reactor at 150°C for 12 hours, then centrifuge and wash to obtain Cu-doped MoS 2 Catalyst; MoO 3 The compound molar ratio of nanobelt, thiourea and divalent copper is 0.08:1.05:0.008; the compound of divalent copper is copper chloride;

[0043] (3) MoS doped with Cu 2 The catalyst was calcined at 430°C for 250min under protective gas nitrogen;

[0044] (4) Calcined Cu-doped MoS 2 Treat with plasma for 60 minutes to obtain the produ...

Embodiment 2

[0046] A sulfur-vacancy Cu-MoS 2 The preparation method of catalyst comprises the following steps:

[0047] (1) Dissolve sodium molybdate with a concentration of 0.1mol / L in water, then add nitric acid dropwise and stir, react in the reactor at 250°C for 16-20h, and then centrifugally wash to obtain MoO 3 Nanobelt; the volume ratio of sodium molybdate, water and nitric acid is 0.5:10:1

[0048] (2) MoO 3 Dissolve the nanobelts in water and stir until dissolved, add thiourea and divalent copper compounds and stir until dissolved, react in the reactor at 100°C for 14 hours, then centrifuge and wash to obtain Cu-doped MoS 2 Catalyst; MoO 3 The compound molar ratio of nanobelt, thiourea and divalent copper is 0.08:1:0.01; the compound of divalent copper is copper chloride;

[0049] (3) MoS doped with Cu 2 The catalyst was calcined at 350°C for 320min under the protective gas of argon;

[0050] (4) Calcined Cu-doped MoS 2 Treat with plasma for 50 minutes to obtain the produc...

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Abstract

The invention relates to the field of catalytic materials, and discloses a preparation method of a sulfur vacancy Cu-MoS2 catalyst in allusion to the problem of low catalytic activity of the existingelectro-catalytic nitrogen fixation catalyst. The preparation method comprises the steps of preparing a MoO3 nanobelt; dissolving the MoO3 nanobelt in a first solvent, stirring until the MoO3 nanobeltis dissolved, adding thiourea and a bivalent copper compound, stirring until the thiourea and the bivalent copper compound are dissolved, reacting in a reaction kettle, and centrifugally washing to obtain a Cu-doped MoS2 catalyst; calcining the Cu-doped MoS2 catalyst under a protective gas; and carrying out plasma treatment on the calcined Cu-doped MoS2. According to the prepared MoS2 catalyst, Cu is doped to form a heteronuclear diatom center, meanwhile, sulfur vacancies are introduced, the structural design of a defective catalyst and heteronuclear diatoms is achieved, the prepared CuMoS2 catalyst shows excellent electrocatalytic nitrogen reduction activity, and the synthesis method is mild in reaction condition, high in yield and suitable for large-scale production of the catalyst.

Description

technical field [0001] The invention relates to the field of catalytic materials, in particular to a sulfur vacancy Cu-MoS 2 Catalyst preparation method. Background technique [0002] NH 3 It is an important chemical substance for the production of fertilizers, dyes, explosives and resins. Its most important application is the production of fertilizers, with an annual output of up to 200 million tons. Therefore, artificial nitrogen fixation is particularly important. Although N 2 is the most abundant molecule in the atmosphere, but its thermodynamic stability and non-polarity make it chemically inert, and N 2 reduced to NH 3 is a very difficult challenge. The industrial nitrogen fixation method adopts the Haber-Bosch method, that is, the process in which nitrogen and hydrogen react to form ammonia at 400 degrees Celsius and 200 atmospheric pressure. The process reaction requires high temperature and high pressure conditions, the reaction conditions are relatively hars...

Claims

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Application Information

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IPC IPC(8): B01J27/051B01J35/00B01J35/02B01J37/08B01J37/10B01J37/34C25B1/27C25B11/091
CPCB01J37/349B01J37/08B01J37/10B01J27/051C25B1/00B01J35/50B01J35/33Y02P20/52
Inventor 叶伟陶婷
Owner HANGZHOU NORMAL UNIVERSITY
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