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Method for preparing ultrafine tungsten oxide nanopowder by recovering waste hard alloy with hydrothermal method

A technology of cemented carbide and nano-powder, which is applied in the direction of improving process efficiency, etc., to achieve the effects of low energy consumption, good performance and simple equipment

Active Publication Date: 2012-12-05
大厂回族自治县北方电工合金有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, how to quickly prepare low-cost, high-performance adsorbents has become a bottleneck restricting the development of this method.

Method used

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  • Method for preparing ultrafine tungsten oxide nanopowder by recovering waste hard alloy with hydrothermal method
  • Method for preparing ultrafine tungsten oxide nanopowder by recovering waste hard alloy with hydrothermal method
  • Method for preparing ultrafine tungsten oxide nanopowder by recovering waste hard alloy with hydrothermal method

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Experimental program
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Effect test

Embodiment 1

[0017] Embodiment 1: be that the cemented carbide of 3% with cobalt content (SEM photo sees figure 1 ) 10.0g and 0.5g NaF were added to the reactor, and 16M HNO was added 3 10ml and 9.9M H 2 o 2 Add 10ml into the reaction kettle, then put the reaction kettle into the oven and heat it to 165°C, keep it warm for 20h, after the temperature drops to room temperature, open the reaction kettle, separate the solid and liquid phases with filter paper, and rinse several times with distilled water , the obtained solid phase was dried at 60°C for 6h and then ground in a mortar to obtain ultrafine WO 3 0.33H 2 0 nanometer powder, its specific surface area reached 90m 2 g -1 . Income WO 3 0.33H 2 The XRD analysis result of 0 powder is as follows figure 2 As shown, the TEM photographs are as image 3 shown.

[0018] With the obtained WO 3 0.33H 2 0 nanometer powder was used as an adsorbent to conduct adsorption experiments on different concentrations of methylene blue soluti...

Embodiment 2

[0019] Example 2: Add 10.25 g of cemented carbide with 10% cobalt and 1.0 g NaF to the reactor, add 16M HNO 3 5ml and 9.9M HO 2 o 2 Add 25ml into the reaction kettle, then put the reaction kettle into the oven and heat it to 200°C, keep it warm for 6h, after the temperature drops to room temperature, open the reaction kettle, separate the solid and liquid phases with filter paper, and rinse several times with distilled water , the obtained solid phase was dried at 60°C for 6h and then ground in a mortar to obtain ultrafine WO 3 0.33H 2 0 nanometer powder, its specific surface area is 80m 2 g -1 .

[0020] With the obtained WO 3 0.33H 2 0 nanometer powder as an adsorbent for different concentrations of methylene blue solutions and Pb-containing 2+ The solution was subjected to adsorption experiments, and the WO 3 0.33H 2 0 powder for methylene blue and Pb 2+ The maximum adsorption capacity of 115 mg g -1 , 211 mg g -1 .

Embodiment 3

[0021] Embodiment 3: adding 11.5g of cemented carbide and 2.3g of NaF to the reactor with a cobalt content of 15%, adding the HNO of 16M 3 25ml and 9.9M H 2 o 2 Add 5ml into the reaction kettle, then put the reaction kettle into the oven and heat it to 120°C, keep it warm for 48h, after the temperature drops to room temperature, open the reaction kettle, separate the solid and liquid phases with filter paper, and rinse several times with distilled water , the obtained solid phase was dried at 60°C for 6h and then ground in a mortar to obtain ultrafine WO 3 0.33H 2 0 nanometer powder, its specific surface area is 70m 2 g -1 .

[0022] With the obtained WO 3 0.33H 2 0 nanometer powder was used as an adsorbent, and the methylene blue solution with different concentrations was mixed with Pb 2+ The solution was subjected to adsorption experiments, and the WO 3 0.33H 2 0 powder for methylene blue and Pb 2+ The maximum adsorption capacity was 95.2 mg g -1 、198mg g -1 . ...

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Abstract

The invention relates to a method for preparing ultrafine tungsten oxide nanopowder by recovering waste hard alloy with hydrothermal method, belonging to the field of hard alloy recovery technology. Waste hard alloy is cleaned up, and then is put into a reaction kettle; fluoride capable of providing fluoride can be added; concentrated nitric acid and hydrogen peroxide are added to oxidize all tungsten carbides in hard alloy; the reaction kettle is processed at constant temperature of 120-200 degrees centigrade for 6-48 h; solid phases and liquid phases are separated from each other after the reaction kettle is cooled; solid phases are dried and then crushed with a mortar to obtain ultrafine WO3.0.33H20 nanopowder. According to the invention, hard alloy can be recycled directly without crushing in advance; and tungsten oxide hydrate has larger specific surface area.

Description

technical field [0001] The invention discloses a method for preparing tungsten oxide nanomaterials by recovering cemented carbide by a hydrothermal method, which belongs to the technical field of cemented carbide recovery. Background technique [0002] Cemented carbide is called the "teeth" of modern industry, and is widely used in cutting tools, geological mining tools, metal forming tools and parts requiring wear resistance and corrosion resistance. With the development of the economy, the output of cemented carbide is increasing year by year, and the output of scrap cemented carbide is also increasing. my country is short of cobalt resources and needs to import a large amount every year. Although tungsten resources are relatively abundant, with the sharp increase in output in recent years, the reserves have dropped from 45% in the early years to 35%. Therefore, the recycling and reuse of waste cemented carbide is of great significance for the rational use and protection ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00
CPCY02P10/20
Inventor 王金淑李洪义李志飞吴俊书刘柏雄
Owner 大厂回族自治县北方电工合金有限公司
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