Thermal treatment of hydrothermal precursors to obtain ws 2 /wo 3 hollow microsphere method

A hollow microsphere and precursor technology, which is applied in the fields of water pollutants, microsphere preparation, water/sewage treatment, etc., can solve the problems of danger in the sulfidation reduction process, influence on product quality, danger of high temperature sulfidation, etc., and achieve uniform size, The effect of eliminating influencing factors and having few influencing factors

Active Publication Date: 2017-11-10
CHANGCHUN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation of the carbon microsphere template used in this method, the control of the size of the carbon microsphere, the control of the amount added, and the efficiency of the template all increase the difficulty of preparation and directly affect the quality of the product.
In addition, there is danger in the vulcanization reduction process, and high-temperature vulcanization is even more dangerous; the amount of sulfur becomes another factor affecting product quality, and excessive sulfur will pollute the environment
It can be seen that there are many factors affecting the product morphology in this method, and the process is complicated and difficult to control.

Method used

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  • Thermal treatment of hydrothermal precursors to obtain ws <sub>2</sub> /wo <sub>3</sub> hollow microsphere method
  • Thermal treatment of hydrothermal precursors to obtain ws <sub>2</sub> /wo <sub>3</sub> hollow microsphere method
  • Thermal treatment of hydrothermal precursors to obtain ws <sub>2</sub> /wo <sub>3</sub> hollow microsphere method

Examples

Experimental program
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Effect test

example 1

[0022] The first step is to prepare the reaction solution: Weigh 1.19055g of tungsten hexachloride and 1.125g of thioacetamide respectively with an electronic balance, add them to 80mL of deionized water, and stir magnetically for 30min, during which O 2 10min.

[0023] The second step, hydrothermal preparation of WS 2 / WO 3 Precursor: Add the reaction liquid into the inner tank of the reaction kettle in an amount of 2 / 3 of the volume of the inner tank of the reactor. In the high-pressure reactor, at 235°C, hydrothermally treat the reaction solution for 24 hours to obtain a hollow Microspherical WS 2 / WO 3 Precursor.

[0024] The third step, heat treatment of the WS 2 / WO 3 Precursor: at 500°C, in N 2 Heat treatment of the WS in a protective atmosphere 2 / WO 3 Precursor 1h, the product WS 2 / WO 3 hollow microspheres.

example 2

[0026] The first step is to prepare the reaction solution: Weigh 1.19055g of tungsten hexachloride and 1.125g of thioacetamide respectively with an electronic balance, add them to 80mL of deionized water, and stir magnetically for 25min, during which O 2 15min.

[0027] The second step, hydrothermal preparation of WS 2 / WO 3 Precursor: Add the reaction liquid into the inner tank of the reaction kettle in an amount of 2 / 3 of the volume of the inner tank of the reactor. In the high-pressure reactor, the reaction solution is hydrothermally treated for 30 hours at a temperature of 230°C to obtain a hollow Microspherical WS 2 / WO 3 Precursor.

[0028] The third step, heat treatment of the WS 2 / WO 3 Precursor: at 470°C, in N 2 Heat treatment of the WS in a protective atmosphere 2 / WO 3 Precursor 1.5h, get the product WS 2 / WO 3 hollow microspheres.

example 3

[0030] The first step is to prepare the reaction solution: Weigh 1.19055g of tungsten hexachloride and 1.125g of thioacetamide respectively with an electronic balance, add them to 80mL of deionized water, and stir magnetically for 35min, during which O 2 5min.

[0031] The second step, hydrothermal preparation of WS 2 / WO 3 Precursor: add the reaction solution into the inner tank of the reaction kettle, the addition amount is 2 / 3 of the volume of the inner tank of the reaction kettle, and in the high-pressure reactor, at 240 ° C, hydrothermally treat the reaction solution for 20 hours to obtain a hollow Microspherical WS 2 / WO 3 Precursor.

[0032] The third step, heat treatment of the WS 2 / WO 3 Precursor: at a temperature of 520°C, in N 2 Heat treatment of the WS in a protective atmosphere 2 / WO 3 Precursor 0.5h, the product WS 2 / WO 3 hollow microspheres.

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Abstract

Belonging to the technical field of composite nanomaterials, the invention provides a method for acquiring WS2 / WO3 hollow microspheres by heat treatment of a hydrothermal precursor. The existing technology has the disadvantages of complex process, dangerous procedure, and multiple influence factors. The method is characterized by: first of all, preparation of a reaction solution, i.e. adding tungsten chloride and thioacetamide into deionized water, performing stirring, and introducing O2 at the same time; then, hydrothermal method preparation of a WS2 / WO3 precursor: in a high-pressure reaction kettle, conducting hydrothermal treatment on the reaction solution at 230-240DEG C for 20-30h to obtain a hollow microspherical WS2 / WO3 precursor; and finally, heat treatment of the WS2 / WO3 precursor: performing heat treatment on the WS2 / WO3 precursor at 470-520DEG C for 0.5-1.5h to obtain the product WS2 / WO3 hollow microspheres. The prepared product can quickly and thoroughly adsorb dye rhodamine B, methyl orange and methylene blue and other dyes, and can be used for treatment of printing and dyeing wastewater.

Description

technical field [0001] The invention relates to a kind of heat treatment hydrothermal precursor to obtain WS 2 / WO 3 The hollow microsphere method, as a composite material, the prepared product can quickly and thoroughly absorb rhodamine B, methyl orange, methylene blue and other dyes, can be used for printing and dyeing wastewater treatment, and belongs to the technical field of composite nanomaterials. Background technique [0002] Organic dyes have complex structures, are difficult to degrade, and are potentially toxic. Printing and dyeing wastewater has high organic content, high chroma, and complex components. In order to avoid environmental pollution from printing and dyeing wastewater, it must be purified. Nanomaterials are an effective adsorption material because of their high specific surface area, active surface activity and high surface energy. WS 2 / WO 3 Composite nanomaterial is a kind of material with rapid adsorption to rhodamine B, methyl orange, methylen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/06B01J20/30B01J20/28B01J13/02C02F1/28C02F1/58
CPCB01J13/02B01J20/0218B01J20/0285B01J20/06B01J20/28021B01J2220/42B01J2220/4806B01J2220/4812C02F1/283C02F2101/308
Inventor 楚学影周敬博都秉龙李金华徐铭泽金芳军王晓华
Owner CHANGCHUN UNIV OF SCI & TECH
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