Apparatus and method for preparing ultrafine WO3

A liquid storage tank and microchannel technology, which is applied in the field of powder metallurgy, can solve the problems of long preparation cycle, high equipment requirements, and easy powder agglomeration, and achieve good industrialization prospects, high control precision, and narrow particle size distribution.

Inactive Publication Date: 2017-12-22
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the process of preparing ultrafine tungsten powder by solid phase decomposition method is simple, some toxic gases are easy to be generated during the decomposition process, causing environmental pollution, and the generated powder is easy to agglomerate
The liquid phase method can precisely control the size of the product components and particles, mainly including: precipitation method, hydrothermal method, microemulsion method, sol-gel method, etc. The precipitation method is obtained by adding an appropriate precipitant to the metal salt solution. The precursor precipitate is dehydrated and calcined to form a nano-powder, but this method has larger particles, unstable particles, and easy agglomeration, which needs to be pulverized again, resulting in an increase in cost
Although the oxide powder particles prepared by the sol-gel method are small, the preparation process is complicated, the preparation cycle is long, and some toxic organic solvents are often added.
The product prepared by the hydrothermal method has high purity, good dispersibility, good and controllable crystal form, but its high equipment requirements, high cost, and high energy consumption limit its practical application.

Method used

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  • Apparatus and method for preparing ultrafine WO3
  • Apparatus and method for preparing ultrafine WO3
  • Apparatus and method for preparing ultrafine WO3

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Weigh 3.29g of Na 2 WO 4 Dissolve 5 mL of acetic acid in deionized water, and prepare 100 mL of 0.1 mol / L sodium tungstate solution as reaction solution A. Measure 12.5 mL of concentrated hydrochloric acid, dilute it to 100 mL with deionized water, prepare 1.5 mol / L hydrochloric acid as reaction solution B, and transfer it into two storage tanks respectively.

[0033] (2) Turn on the power supply, respectively set the flow rate of the two pumps to 100mL / min, and the pipe diameter of the T-shaped tee to be 0.6mm. as attached figure 1 As shown, the two pumps are started at the same time, and a yellow suspension after the reaction is obtained after impacting the sediment.

[0034] (3) Continue to age the obtained suspension at room temperature for 6 hours, wash with dediluted hydrochloric acid and ionized water for 3-4 times, and dry the precursor at 120° C. for 2 hours.

[0035] (4) Grind the dried sample for 10-20min, and calcinate at 600°C for 3h to obtain 30-80...

Embodiment 2

[0038] (1) Weigh 2g of ammonium tungstate and 5mL of acetic acid and dissolve them in deionized water at 60°C, and cool to a constant volume in a 100mL volumetric flask as the reaction solution A. Measure 12.5 mL of concentrated hydrochloric acid, dilute to 100 mL, and prepare 1.5 mol / L hydrochloric acid as reaction solution B.

[0039] (2) Turn on the power supply, set the flow rate of the pumps connecting the two solutions of A and B to 100mL / min, and the pipe diameter of the T-shaped tee to be 0.6mm. as attached figure 1 As shown, the two pumps are started at the same time, and a yellow suspension after the reaction is obtained after impacting the sediment.

[0040] (3) The obtained suspension was aged at room temperature for 6 hours, washed with dilute hydrochloric acid and deionized water for 3-4 times, and the washed precursor was dried at 120° C. for 2 hours.

[0041](4) Grind the dried sample for 10-20min, and calcinate at 600°C for 3h to obtain 30-80nm ultrafine tun...

Embodiment 3

[0044] (1) Weigh 3.29g of Na 2 WO 4 Dissolve 5 mL of acetic acid in deionized water, and prepare 100 mL of 0.1 mol / L sodium tungstate solution as reaction solution A. Measure 12.5 mL of concentrated hydrochloric acid, dilute it to 100 mL with deionized water, prepare 1.5 mol / L hydrochloric acid as reaction solution B, and transfer it into two storage tanks respectively.

[0045] (2) Turn on the power supply, respectively set the flow rate of the two pumps to 100mL / min, and the pipe diameter of the T-shaped tee to be 0.6mm. as attached figure 1 As shown, the two pumps are started at the same time, and a yellow suspension after the reaction is obtained after impacting the sediment.

[0046] (3) Continue to age the obtained suspension at room temperature for 6 hours, wash with dilute hydrochloric acid and deionized water for 3-4 times, and dry the precursor at 120° C. for 2 hours.

[0047] (4) Grind the dried sample for 10-20min, and calcinate at 600°C for 4h to obtain 30-80n...

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Abstract

The invention discloses an apparatus and a method for preparing ultrafine WO3, and belongs to the technical field of powder metallurgy, and the apparatus and the method can be applied to the preparation of the ultrafine WO3 powder. The apparatus comprises two liquid reservoirs for storage of reaction liquids and constant-flux pumps which are respectively connected with the liquid reservoirs, the constant-flux pumps are connected with a T-type tee by capillary tubes, the vertical end of the T-type tee is a reaction liquid outlet, and the apparatus belongs to a micro impinging stream reactor. The reaction method is as follows: a hydrochloric acid solution and a tungstate solution are impacted and mixed through the T-type tee connector to synthesize precursor tungstic acid, and the precursor tungstic acid is calcined to obtain the ultrafine WO3 powder. The preparation method and the apparatus can be used to strengthen the mixing reaction process of components to obtain the WO3 with a regular morphology, small particle size and narrow particle size range. The method has the advantages of simple process, high control precision, continuous production and many other advantages, and has a good industrialization prospect.

Description

technical field [0001] The invention belongs to the technical field of powder metallurgy, in particular to the preparation of superfine WO 3 devices and methods. Background technique [0002] Tungsten has high density, high melting point, high hardness, high wear resistance, low thermal expansion coefficient, excellent electrical and thermal conductivity, and good corrosion resistance, so it has been widely used in high-density alloys and hard alloys. With the expansion of micron and ultra-fine grain cemented carbide market, the demand for ultra-fine tungsten powder is increasing day by day. In summary, it can be mainly used in: making heat-resistant and wear-resistant alloys, aero-engines, turbine blades and other parts that are subject to strong wear, making electric light sources and heating elements, making contact alloys and high-density alloys, etc. Agglomerated tungsten powder is the key to improve tungsten-based high-density alloy and WC-Co cemented carbide. The p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/02B82Y40/00
CPCC01G41/02C01P2002/72C01P2004/03C01P2004/32C01P2004/64
Inventor 文利雄刘春晓陈建峰
Owner BEIJING UNIV OF CHEM TECH
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