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A kind of molybdenum disulfide supported IR single-atom catalyst and its preparation method and application

A molybdenum disulfide catalyst technology, applied in the field of molybdenum disulfide-supported Ir single-atom catalysts and its preparation, can solve the problems of poor transition metal H activation ability, limited wide application, harsh reaction conditions, etc., to reduce the content of precious metals, The effect of large specific surface area and high loading concentration

Active Publication Date: 2022-02-22
SHAANXI SCI TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

A yield of 51% was also obtained when the reaction used fructose as starting material, however the transition metal H 2 Poor activation ability and easy inactivation limit their wide application
[0005] According to the research results of the literature, the selective hydrodeoxygenation of 5-hydroxymethylfurfural currently reported requires relatively harsh reaction conditions, and usually requires the addition of additional acid or alkali, causing serious pollution to the environment.

Method used

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  • A kind of molybdenum disulfide supported IR single-atom catalyst and its preparation method and application
  • A kind of molybdenum disulfide supported IR single-atom catalyst and its preparation method and application
  • A kind of molybdenum disulfide supported IR single-atom catalyst and its preparation method and application

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Experimental program
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Effect test

Embodiment 1

[0027] Dissolve 0.12g of sulfur powder in 50mL of oleylamine and stir magnetically for 20min to obtain a sulfur source precursor; dissolve 0.32g of ammonium molybdate tetrahydrate and 0.0023g of chloroiridic acid in 3mL of water and mix to obtain solution 1; 1 part of the solution was added dropwise to 50 parts by volume of the sulfur source precursor, and stirred rapidly at 20-30°C for 1 hour; then transferred to a 100mL stainless steel reaction kettle, and the temperature was raised to 220°C at 5°C / min for 48h. Subsequently, it was centrifuged and filtered, and washed several times with ethanol and cyclohexane until the ligand oleylamine on the surface of the catalyst was washed off to obtain a black solid, and the collected black solid was vacuum-dried for 10 hours. Reduction at 300°C for 1 hour in a hydrogen atmosphere to obtain 0.2% Ir 1 / MoS 2 catalyst.

Embodiment 2

[0029] Add 0.12g of sulfur powder to 50mL of oleylamine and stir at room temperature for 20min to obtain a sulfur source precursor; dissolve 0.32g of ammonium molybdate tetrahydrate and 0.008g of chloroiridic acid in 3mL of water and mix to obtain solution 1; The solution 1 was added dropwise to 50 parts by volume of the sulfur source precursor, and stirred rapidly at 20-30°C for 1 hour; then transferred to a 100mL stainless steel reaction kettle, and heated at 5°C / min to 220°C for 48 hours. Subsequently, it was centrifuged and filtered, and washed several times with ethanol and cyclohexane until the ligand oleylamine on the surface of the catalyst was washed off to obtain a black solid, and the collected black solid was vacuum-dried for 10 hours. Reduction at 300°C for 1 hour in a hydrogen atmosphere to obtain 0.7% Ir 1 / MoS 2 catalyst.

[0030] The catalyst was photographed with a high-power transmission electron microscope, such as figure 1 shown, from figure 1 It can b...

Embodiment 3

[0032]Add 0.12 g of sulfur powder to 50 mL of oleylamine and stir at room temperature for 20 minutes to obtain a sulfur source precursor; dissolve 0.32 g of ammonium molybdate tetrahydrate and 0.024 g of chloroiridic acid in 3 mL of water and mix to obtain solution 1; The solution 1 was added dropwise to 50 parts by volume of the sulfur source precursor, and stirred rapidly at 20-30°C for 1 hour; then transferred to a 100mL stainless steel reaction kettle, and heated at 5°C / min to 220°C for 48 hours. Subsequently, it was centrifuged and filtered, and washed several times with ethanol and cyclohexane until the ligand oleylamine on the surface of the catalyst was washed off to obtain a black solid, and the collected black solid was vacuum-dried for 10 hours. 2.1% Ir / MoS was obtained by reduction at 300°C for 1 h in a hydrogen atmosphere 2 catalyst.

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Abstract

The invention discloses a molybdenum disulfide supported Ir single-atom catalyst, a preparation method and application thereof. The present invention dissolves the sulfur source in oleylamine and stirs it magnetically for 10-20 minutes to obtain a sulfur source precursor with a sulfur source concentration of 1.0-1.2 mM; dissolves the molybdenum source and the Ir precursor in water and mixes them evenly to obtain metal Ir ions A solution 1 with a concentration of 0.1-6.0 mM; adding 3 parts by volume of the solution 1 dropwise to 50 parts by volume of the sulfur source precursor, and stirring rapidly at 20-30°C for 1-2 hours to obtain a clear solution 2; Heat solution 2 at 200-240°C for 24-48 hours to obtain a suspension; centrifuge the suspension, wash, and dry to obtain a solid; put the solid into a tube furnace, and heat it at 200-400 After heat treatment at ℃ for 0.5-3 hours, then naturally cool to room temperature to obtain the catalyst. The catalyst is used to catalyze the selective hydrodeoxygenation of 5-hydroxymethylfurfural, which is beneficial to improving the activity and selectivity of the catalyst, and at the same time can improve the utilization rate of catalyst atoms, reduce the content of noble metals, and thus reduce the cost of the catalyst.

Description

technical field [0001] The invention belongs to the technical field of biomass energy development, and in particular relates to a molybdenum disulfide-supported Ir single-atom catalyst and a preparation method and application thereof. Background technique [0002] Facing the severe challenges of rapid growth in energy demand, deteriorating environmental pollution, and depletion of fossil resources, actively exploring and developing new energy sources has become a key issue that urgently needs to be solved in my country's sustainable development. The conversion and utilization of lignocellulose resources is one of the important ways to solve energy and environmental problems, and has attracted great attention from all over the world. Efforts are currently underway to develop strategies for the efficient conversion of biomass. For example, lignocellulose is hydrolyzed or hydrogenolyzed to obtain valuable chemicals (such as phenols, alcohols, acids and furfurals). It is worth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/051B01J35/10C07D307/36
Inventor 季建伟任传清杜全超宋娟
Owner SHAANXI SCI TECH UNIV
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