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Preparing method of ammonium tungsten bronze

A technology of tungsten bronze and ammonium metatungstate, applied in chemical instruments and methods, tungsten compounds, inorganic chemistry, etc., can solve the problem of high preparation cost, and achieve the effect of strong activity, good reproducibility and large specific surface area

Inactive Publication Date: 2019-10-11
HENAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, both the solvothermal method and the hydrothermal method involve many kinds of raw materials and the reaction temperature is not lower than 100°C when preparing ammonium tungsten bronze, so the preparation cost is relatively high

Method used

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  • Preparing method of ammonium tungsten bronze
  • Preparing method of ammonium tungsten bronze
  • Preparing method of ammonium tungsten bronze

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preparation example Construction

[0023] The preparation method of ammonium tungsten bronze provided by the present invention comprises the following steps: preparing ammonium metatungstate into a precursor solution with pH<1; Separation, that is.

[0024] In the specific embodiment of the preparation method of the ammonium tungsten bronze of the present invention, the ammonium metatungstate is prepared into a precursor solution of pH3 template, the pH of the precursor solution should be strictly guaranteed to be less than 1. In addition, the pH of the precursor affects the time of the hydrothermal reaction, and the time of the hydrothermal reaction can be changed by adjusting the pH of the precursor.

[0025] In a specific embodiment of the method for preparing ammonium tungsten bronze of the present invention, the solid-liquid separation is suction filtration.

[0026] The airtight container adopted in the specific embodiment of the preparation method of the ammonium tungsten bronze of the present invention...

Embodiment 1

[0032] The preparation method of the ammonium tungsten bronze of the present embodiment may further comprise the steps:

[0033] 1) Weigh 300g of ammonium metatungstate powder [(NH 4 ) 6 h 2 W 12 o 40 ];

[0034] 2) Measure 150ml of commercially available nitric acid (mass concentration is 63%, density is 1.4g / m 1 ), diluted to 450ml with distilled water and placed in a clean beaker;

[0035] 3) Add the ammonium metatungstate in step 1) into the above-mentioned beaker containing the nitric acid solution, stir for 10 minutes to mix evenly, and obtain a precursor solution with pH<1;

[0036] 4) Transfer the precursor solution obtained in step 3) to a hydrothermal reactor with a polytetrafluoroethylene liner (the filling degree is 90%), seal it and place it in a vacuum drying oven, react at 60°C for 38h, and then Take out, cool to room temperature naturally, obtain hydrothermal product;

[0037] 5) The hydrothermal reaction product obtained in step 4) is subjected to vacuu...

Embodiment 2

[0039] The preparation method of the ammonium tungsten bronze of the present embodiment may further comprise the steps:

[0040] 1) Weigh 300g of ammonium metatungstate powder [(NH 4 ) 6 h 2 W 12 o 40 ];

[0041] 2) Measure 350ml of commercially available nitric acid (mass concentration is 63%, density is 1.4g / m 1 ), diluted to 450ml with distilled water and placed in a clean beaker;

[0042] 3) Add the ammonium metatungstate in step 1) into the above-mentioned beaker containing the nitric acid solution, stir for 15 minutes to mix evenly, and obtain a precursor solution with pH<1;

[0043] 4) Transfer the precursor solution obtained in step 3) to a polytetrafluoroethylene-lined hydrothermal reactor (filling degree is 85%), seal it and place it in a vacuum drying oven, react at 65°C for 35h, and then take it out , cooled naturally to room temperature to obtain a hydrothermal product;

[0044] 5) The hydrothermal reaction product obtained in step 4) is subjected to vacuum...

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Abstract

The invention relates to a preparing method of ammonium tungsten bronze, and belongs to the technical field of preparation of tungsten bronze materials. The preparing method of the ammonium tungsten bronze includes the following steps of preparing precursor liquid with the pH smaller than 1 from ammonium metatungstate, putting the precursor liquid in a sealed container for hydrothermal reaction at60-80 DEG C, and then conducting solid-liquid separating to obtain the ammonium tungsten bronze. According to the preparing method of the ammonium tungsten bronze, the ammonium metatungstate serves as the raw material, the pH of the solution is controlled to be smaller than 1 for hydrothermal reaction, and the ammonium tungsten bronze is prepared at a low temperature; the method is simple in process, convenient to operate and low in cost. The prepared ammonium tungsten bronze is a hexagonal phase, has the granularity of 3.5-6.2 micron, and is large in specific surface area, high in activity,repeatability and quality stability and suitable for being used and popularized industrially.

Description

technical field [0001] The invention relates to a preparation method of ammonium tungsten bronze, belonging to the technical field of preparation of tungsten bronze materials. Background technique [0002] WO 3 It is a typical semiconductor material with a band gap of 2.5-3.0eV, rich non-stoichiometric compounds, unique defect structure, and can be derived from a variety of functional materials. For example, when in WO 3 When oxygen vacancies or interstitial cation donors are introduced into the lattice, low-valence tungsten oxides (WO 3-x ) or tungsten bronze material (M x WO 3 , M = Li, Na, K, Rb, Cs, NH 4 or In,0<x<1), for transparent thermal insulation coatings, filtering or cancer photothermal fields. In particular, hexagonal ammonium tungsten bronze has great application prospects in the fields of photoelectrochemistry, catalytic degradation, gas sensors, and color-changing devices. [0003] The synthesis methods of tungsten bronze nanocrystals that have b...

Claims

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Application Information

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IPC IPC(8): C01G41/00
CPCC01G41/00C01P2002/72C01P2004/03
Inventor 魏世忠肖方闹徐流杰周玉成潘昆明李继文李秀青王喜然毛丰王晓东陈冲张程熊美靳东亮张国赏
Owner HENAN UNIV OF SCI & TECH