Preparation method of one-dimensional Euphorbia-milii-shaped WO3 microcrystal

A technology of thorn plum and microcrystal, which is applied in the field of preparing one-dimensional thorn plum-like WO3 microcrystal, can solve the process conditions and structure design of powder easy to agglomerate, difficult to obtain oriented growth one-dimensional nanomaterials, microwave-assisted solvothermal The problem of fast reaction rate, etc., achieves the effect of being conducive to rapid diffusion and mass transfer, single oriented growth morphology, and controllable morphology.

Active Publication Date: 2015-09-16
安徽翰邦科技咨询有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Microemulsion method, spray drying method and acidification precipitation method all need to synthesize WO under high temperature calcination conditions. 3 , the powder is easy to agglomerate and the process conditions and structure design are difficult to control, which is very important for the preparation of WO 3 The utilization rate of the required raw materials is very small, and it is difficult to obtain one-dimensional nanomaterials grown in orientation; and the template replication technology and the sol-gel method also require post-heat treatment and crystallization process, which will also cause the agglomeration of nanocrystals, and the grains are abnormally long Large, the microstructure of the material is difficult to control
At the same time, the chemical vapor deposition method requires high equipment and the ratio of reactants is difficult to control. The prepared WO 3 Impurities are easily introduced into nanomaterials
In addition, the hydrothermal method can only react in an aqueous medium, and cannot control the polarity of the reaction solvent to control the crystallization and morphology of the product; the microwave-assisted solvothermal reaction rate is fast, the nucleation-growth rate is fast, and it is difficult to control the product oriented growth

Method used

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  • Preparation method of one-dimensional Euphorbia-milii-shaped WO3 microcrystal
  • Preparation method of one-dimensional Euphorbia-milii-shaped WO3 microcrystal

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Step 1: Add analytically pure WCl 6 Add in the mixed solvent of isopropanol and distilled water, the volume ratio of control solvent isopropanol and distilled water is V 异丙醇 :V 水 =1:1, and keep stirring until WCl 6 dissolved to produce W 6+ A solution with a concentration of 0.06mol / L;

[0023] Step 2: Add analytically pure polyoxyethylene polyoxypropylene block copolymer (F127) to the above solution, control the addition of polyoxyethylene polyoxypropylene block copolymer to 20g / L, and heat at 45°C stirring to fully dissolve the polyoxyethylene polyoxypropylene block copolymer to obtain a precursor solution;

[0024] Step 3: Pour the precursor solution into the hydrothermal kettle, control the filling degree at 60%, then seal the hydrothermal kettle, put the sealed hydrothermal kettle into the homogeneous reactor, and control the solvent heating temperature to 160 ℃, the rotation speed is 40r / min (the hydrothermal kettle rotates around a fixed axis during the heat...

Embodiment 2

[0028] Step 1: Add analytically pure WCl 6 Add in the mixed solvent of isopropanol and distilled water, the volume ratio of control solvent isopropanol and distilled water is V 异丙醇 :V 水 =3:2, keep stirring until WCl 6 dissolved to produce W 6+ A solution with a concentration of 0.01mol / L;

[0029] Step 2: Add analytically pure polyoxyethylene polyoxypropylene block copolymer (F127) to the above solution, control the addition of polyoxyethylene polyoxypropylene block copolymer to 15g / L, and heat at 40°C stirring to fully dissolve the polyoxyethylene polyoxypropylene block copolymer to obtain a precursor solution;

[0030] Step 3: Pour the precursor solution into the hydrothermal kettle, control the filling degree at 65%, then seal the hydrothermal kettle, put the sealed hydrothermal kettle into the homogeneous reactor, and control the solvent heating temperature to 140 ℃, the rotation speed is 30r / min (the hydrothermal kettle rotates around a fixed axis during the heat pre...

Embodiment 3

[0034] Step 1: Add analytically pure WCl 6 Add in the mixed solvent of isopropanol and distilled water, the volume ratio of control solvent isopropanol and distilled water is V 异丙醇 :V 水 =4:1, keep stirring until WCl 6 dissolved to produce W 6+ A solution with a concentration of 0.005mol / L;

[0035] Step 2: Add analytically pure polyoxyethylene polyoxypropylene block copolymer (F127) to the above solution, control the addition amount of polyoxyethylene polyoxypropylene block copolymer to 5g / L, and heat at 35°C stirring to fully dissolve the polyoxyethylene polyoxypropylene block copolymer to obtain a precursor solution;

[0036] Step 3: Pour the precursor solution into the hydrothermal kettle, control the filling degree at 70%, then seal the hydrothermal kettle, put the sealed hydrothermal kettle into the homogeneous reactor, and control the solvent heat temperature to 120 ℃, the rotation speed is 20r / min (the hydrothermal kettle rotates around a fixed axis during the heat...

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Abstract

The invention provides a preparation method of a one-dimensional Euphorbia-milii-shaped WO3 microcrystal, which comprises the following steps: adding WCl6 into an isopropanol-distilled water mixed solvent, adding a polyoxyethylene-polyoxypropylene block copolymer into the solution to obtain a precursor solution, pouring the precursor solution into a hydrothermal kettle, and reacting while controlling the temperature at 80-240 DEG C under the pressure of 2-16 MPa for 4-36 hours, wherein the hydrothermal kettle is fixed in an homogeneous reaction instrument, and rotates around a fixed axis at the rate of 20-70 r/min in the insulating process; and taking out the product, washing and drying. The prepared one-dimensional Euphorbia-milii-shaped WO3 microcrystal has the advantages of high purity, favorable crystallinity, favorable dispersity, uniform size, uniform shape and obvious oriented growth.

Description

technical field [0001] The invention relates to a method for preparing one-dimensional tiger thorn plum-shaped WO 3 The microcrystalline method, in particular to a homogeneous nonionic surfactant-assisted solvothermal method for the preparation of one-dimensional thornberry-like WO 3 microcrystalline method. Background technique [0002] Tungsten trioxide (WO 3 ) is usually a yellow powder, insoluble in water, soluble in lye, slightly soluble in acid. It is used to make high melting point alloys and hard alloys, tungsten wires and fireproof materials, etc. When the temperature reaches 850℃, it sublimates significantly, hardly reacts with inorganic acids except hydrofluoric acid, and can be slowly dissolved in ammonia water or concentrated alkali solution. It reacts with chlorine gas to form oxychloride, but it cannot react with bromine and iodine. WO 3 The crystal structure depends on the temperature: it is a tetragonal crystal system above 740°C, an orthorhombic cryst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/02
Inventor 黄剑锋王鑫曹丽云李嘉胤郝巍殷立雄许占位费杰周磊
Owner 安徽翰邦科技咨询有限公司
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