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Method for preparing polyhedral tungsten trioxide by using template

A tungsten trioxide and polyhedron technology, applied in tungsten oxide/tungsten hydroxide, pressure vessels used in chemical processes, etc., can solve the problems of expensive precursors, easy to destroy sol structure, easy to explode, etc., to reduce the phenomenon of agglomeration , the effect of shortening the reaction time and low cost

Inactive Publication Date: 2022-03-25
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although it is feasible to prepare tungsten trioxide by sol-gel method, the precursors of the reaction are generally expensive and volatile and prone to explosion hazards, and the temperature required to remove crystal water is relatively high, generally at a high temperature of about 400 °C Under high temperature, it is easy to destroy the sol structure

Method used

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  • Method for preparing polyhedral tungsten trioxide by using template
  • Method for preparing polyhedral tungsten trioxide by using template
  • Method for preparing polyhedral tungsten trioxide by using template

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Put the solution containing 10mL of 80% hydrazine hydrate in a 50mL reaction kettle, and then add 20mL of toluene solution containing 0.035mol / L iron acetylacetonate and 1mL of oleic acid to form a two-phase reaction system. Put it into a 130°C oven, take it out after 24h and let it cool down to room temperature naturally. The poured mixed solution was added to ethanol for ultrasonication, and under the action of a magnet, it was repeatedly washed with ethanol until the solution was partially clear, and dried at room temperature. Weigh 3mmol sodium tungstate dihydrate into 30mL deionized water, stir continuously until it is completely dissolved, adjust the pH between 4-5 with 1mol / L HCl, add the prepared ferric oxide, mix and place in 50mL for reaction React in the kettle at 160°C for 6 hours. After cooling, the solid part of the kettle is washed with deionized water and dried. Soak the resulting solid in 2mol / L hydrogen chloride solution for 3 days.

Embodiment 2

[0032] A solution containing 10 mL of 80% hydrazine hydrate was placed in a 50 mL reaction kettle, and a two-phase reaction system formed by adding 20 mL of a toluene solution containing 0.035 mol / L iron acetylacetonate and 1 mL of oleic acid in sequence, without stirring during the whole process , the reactor was placed in an oven at 130 °C, and after 12 h, it was taken out and cooled to room temperature naturally. The poured mixed solution was added to ethanol for ultrasonication, and under the action of a magnet, it was repeatedly washed with ethanol until the solution was partially clear, and dried at room temperature. Weigh 3 mmol of sodium tungstate dihydrate into 30 mL of deionized water, stir continuously until it is completely dissolved, adjust the pH between 4-5 with 1 mol / L HCl, add the prepared ferric oxide, mix and place React in a 50 mL reactor at 160 °C for 12 h. After cooling, the solid part of the kettle was washed with deionized water and dried. Soak the res...

Embodiment 3

[0034] A solution containing 20 mL of 80% hydrazine hydrate was placed in a 100 mL reaction kettle, and a two-phase reaction system formed by adding 40 mL of a toluene solution containing 0.07 mol / L iron acetylacetonate and 2 mL of oleic acid in sequence, without stirring during the whole process , the reactor was placed in an oven at 130 °C, and after 24 h, it was taken out and cooled to room temperature naturally. The poured mixed solution was added to ethanol for ultrasonication, and under the action of a magnet, it was repeatedly washed with ethanol until the solution was partially clear, and dried at room temperature. Weigh 6 mmol of sodium tungstate dihydrate in 60 mL of deionized water, stir continuously until completely dissolved, and add 1 mol / L of H 2 SO 4 Adjust the pH between 4-5, add the prepared ferric oxide, mix and place it in a 100 mL reactor at 160 °C for 10 h. After cooling, the solid part of the kettle is washed with deionized water and dried. Soak the re...

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Abstract

The invention discloses a method for preparing polyhedral tungsten trioxide by using a template, and relates to a method for preparing polyhedral tungsten trioxide, which comprises the following steps of: putting hydrazine hydrate, ferric acetylacetonate, oleic acid and sodium tungstate dihydrate serving as main raw materials into a reaction kettle at 130 DEG C for 24 hours, repeatedly cleaning a ferroferric oxide crude product by using ethanol, and grinding the treated solid in an agate mortar to obtain the polyhedral tungsten trioxide. Then adding Fe3O4 into a sodium tungstate solution of which the pH value is pre-adjusted to be 4-5 by using an acid solution, putting into a reaction kettle at the temperature of 160 DEG C, taking out the solution after 6 hours, and repeatedly cleaning and drying the obtained WO3 / Fe2O3 composite material by using deionized water. Soaking the obtained composite material template with 2 mol / L hydrochloric acid for 3 days to obtain the product tungsten trioxide. The prepared tungsten trioxide has the characteristics of nano size, high yield, stable product, simple production process, small particle size, good dispersity, surface effect, no pollution to the environment and the like. Especially, the material has a semiconductor effect, so that the material can be widely used as a gas sensitive material in the aspects of photohydrolysis hydrogen production, photocatalysis and electrochromism.

Description

technical field [0001] The invention relates to a method for preparing tungsten trioxide, in particular to a method for preparing polyhedral tungsten trioxide with a template. Background technique [0002] Tungsten trioxide is an oxide with a wide bandgap and also an n-type semiconductor with excellent physical and chemical properties. It is widely used as catalysts, sensors, electrochromic devices, ceramics, solar cells and pigments. industrial field. [0003] At present, the most traditional method of synthesizing tungsten trioxide is the sol-gel method. The general process of the sol-gel method is to use W(OEt) 6 or WOCl 4 As a tungsten source, they are dissolved in an alcoholic solvent and stirred into a uniform solution. The solvent and solute undergo hydrolysis and condensation reactions to form a stable sol. After aging, they are further polymerized to form a network-like spatial structure. The final product generally needs to be heated at 400°C to remove the wate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/02B01J3/04
CPCC01G41/02B01J3/04C01P2002/72C01P2004/03
Inventor 徐曼王凯刘利鑫曹旋
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY