Niobic acid-based sulfide composite material and preparation method thereof

A composite material and sulfide technology, applied in chemical instruments and methods, chemical/physical processes, special compound water treatment, etc. The effect of reducing the difficulty of synthesis

Inactive Publication Date: 2019-12-20
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in recent studies, the metal phases in composite materials are mostly concentrated in noble metals, and there are few studies on non-noble metal composites based on niobium-based solid acids.

Method used

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  • Niobic acid-based sulfide composite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] MoS 2 -H 4 Nb 2 o 7 preparation of

[0027] 1) Weigh 0.1g of tin niobate and add it to the PTFE lining, add 1.84g of ammonium molybdate and 2.4g of thiourea, add 30mL of 0.12mol / L hydrochloric acid solution to adjust the pH to 0.9, and put it into the kettle , reacted at 160°C for 12h to obtain a black precipitate;

[0028] 2) The black precipitate obtained after the reaction in 1) was filtered and washed, and dried in a vacuum oven at 60°C for 6 hours to obtain MoS 2 -H 4 Nb 2 o 7 composite material.

Embodiment 2

[0030] CoS 2 -H 4 Nb 2 o 7 preparation of

[0031] 1) Weigh 0.2g of tin niobate and add it to the PTFE lining, add 2.9g of cobalt nitrate hexahydrate and 2.4g of thiourea, add 60mL of 0.12mol / L hydrochloric acid solution to adjust the pH to 0.9, and put it into the kettle In the reaction at 200°C for 2 hours, a black precipitate was obtained;

[0032] 2) The black precipitate obtained after the reaction in 1) was filtered and washed, and dried in a vacuum oven at 60°C for 6 hours to obtain CoS 2 -H 4 Nb 2 o 7 composite material.

Embodiment 3

[0034] FeS 2 -H 4 Nb 2 o 7 preparation of

[0035] 1) Weigh 0.15g tin niobate and add it to the polytetrafluoroethylene lining, add 2.8g ferrous sulfate and 1.2 thiourea, add 0.12mol / L hydrochloric acid solution 45mL to adjust the pH to 0.9, put it into the kettle, React at 200°C for 12 hours to obtain a black precipitate;

[0036] 2) The black precipitate obtained after the reaction in 1) was filtered and washed, and dried in a vacuum oven at 60°C for 6 hours to obtain FeS 2 -H 4 Nb 2 o 7 composite material.

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Abstract

The invention relates to a niobic acid-based sulfide composite material and a preparation method thereof. The structural formula of the niobic acid-based sulfide composite material is AxBySz-H4Nb2O7,in the formula, A and B are one or two of different metal elements of Co, Mo, Ni, Cu, Zn and Fe; x is greater than 0 and smaller than 10; y is greater than or equal to 0 and less than 10; z is greaterthan 0 and smaller than 10; and specific values are determined according to specific valence states of compounds. The preparation method comprises the following steps: weighing tin niobate, adding the tin niobate into a polytetrafluoroethylene lining, adding one or two of soluble metal salts and thiourea, dissolving the components with water, and performing a hydrothermal reaction so as to obtainblack precipitate; performing suction filtration washing on the black precipitate, putting the black precipitate into a vacuum drying tank, and performing drying, so as to obtain an AxBySz-H4Nb2O7 composite material. The composite material is low in preparation condition and simple in operation, sulfides are uniformly grown on the surface of niobic acid, rich reaction activity sites can be provided for reactions, and the reaction activity of metal sulfides in catalysis reactions can be sufficiently improved.

Description

technical field [0001] The invention belongs to the technical field of synthesis of new catalytic materials, and is specifically expressed as the preparation of a novel microspherical metal sulfide-niobic acid composite material. Background technique [0002] Sulfide materials have been widely studied because of their catalytic ability in photolysis of water to produce hydrogen, photocatalytic degradation of dyes, photocatalytic reduction of carbon dioxide, electrocatalysis and biomass conversion. Sulfides are cheap and are considered cheap materials that can replace precious metals in industrial production. Among them, the material represented by molybdenum disulfide is a typical transition metal dihalogenated alkane. Adjacent nanosheets are connected together through weak van der Waals interactions to form a sandwich structure, and each unit nanosheet is formed by a covalent bond. composed of combined three-atom (S-Mo-S) layers. [0003] Transition metal sulfide catalyti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/04B01J27/043B01J27/051C01B3/04C02F1/30C02F101/30C02F101/38
CPCB01J27/051B01J27/043B01J27/04B01J27/0515B01J35/004C01B3/042C02F1/30C01B2203/0277C01B2203/1052C01B2203/1058C02F2101/38C02F2101/308C02F2305/10Y02E60/36
Inventor 宋春风王振娇刁新勇李婷婷刘庆岭纪娜
Owner TIANJIN UNIV
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