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Method for preparing nano tungsten oxide from tungstenic waste cemented carbide

A nano-tungsten oxide, cemented carbide technology, applied in tungsten oxide/tungsten hydroxide, nanotechnology, nanotechnology and other directions, can solve the problems of many influencing factors, low tungsten recovery rate, complex process, etc., to avoid agglomeration, experiment The effect of short cycle and simple equipment

Inactive Publication Date: 2018-08-24
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, the recovery process of waste cemented carbide is to obtain high-purity tungstate by leaching and purification, and then process tungstate to obtain tungsten oxide. This process is complicated and there are many influencing factors in the purification process. , so that the recovery rate of tungsten is low and the cost is high
Moreover, waste water will be discharged during the purification process, causing pollution to the environment

Method used

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  • Method for preparing nano tungsten oxide from tungstenic waste cemented carbide
  • Method for preparing nano tungsten oxide from tungstenic waste cemented carbide
  • Method for preparing nano tungsten oxide from tungstenic waste cemented carbide

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Embodiment 1

[0029] The method (such as figure 1 shown), specifically include the following steps:

[0030] (1) Treatment of waste cemented carbide: calcining waste materials (calcination conditions: 30min to 200°C, heat preservation for 50min, 120min to 950°C, heat preservation for 170min), crushing, grinding into powder, powder with absolute ethanol and deionized water Wash and dry.

[0031] (2) Sodium hydroxide solution leaching: The powdery tungsten-containing waste and sodium hydroxide solution are heated and reacted in a stainless steel reactor under vacuum. The concentration of the sodium hydroxide solution is 8%, the reaction time is 3 hours, and the reaction temperature is 120°C to generate tungsten Sodium tungstate solution and precipitation, filtered to obtain sodium tungstate solution.

[0032] (3) Treatment of sodium tungstate solution:

[0033] ① Add sulfuric acid to the sodium tungstate solution obtained in step (2) to adjust the pH, so that the pH of the solution is 3; t...

Embodiment 2

[0039] The method for preparing nano-tungsten oxide with waste cemented carbide described in this embodiment specifically comprises the following steps:

[0040] (1) Treatment of waste cemented carbide: calcining the waste (calcination conditions: 30min to 200°C, heat preservation for 60min, 120min to 850°C, heat preservation for 160min), crushing, grinding into powder, powder with absolute ethanol and deionized water Wash and dry.

[0041] (2) Sodium hydroxide solution leaching: The powdery tungsten-containing waste and sodium hydroxide solution are heated and reacted in a stainless steel reactor under vacuum. The concentration of the sodium hydroxide solution is 9%, the reaction time is 3.5 hours, and the reaction temperature is 130°C. Sodium tungstate solution and precipitation, filtered to obtain sodium tungstate solution.

[0042] (3) Treatment of sodium tungstate solution:

[0043] ① Add sulfuric acid to the sodium tungstate solution obtained in step (2) to adjust the ...

Embodiment 3

[0049] The method for preparing nano-tungsten oxide with waste cemented carbide described in this embodiment specifically comprises the following steps:

[0050] (1) Treatment of waste cemented carbide: calcining the waste (calcination conditions: 30min to 200°C and heat preservation for 50min, 120min to 900°C, heat preservation for 150min), crushing and grinding into powder, powder with absolute ethanol and deionized water Wash and dry.

[0051] (2) Sodium hydroxide solution leaching: The powdery tungsten-containing waste and sodium hydroxide solution are heated and reacted in a stainless steel reactor under vacuum. The concentration of the sodium hydroxide solution is 10%, the reaction time is 3.5 hours, and the reaction temperature is 140°C. Sodium tungstate solution and precipitation, filtered to obtain sodium tungstate solution.

[0052] (3) Treatment of sodium tungstate solution:

[0053] ① Add sulfuric acid to the sodium tungstate solution obtained in step (2) to adju...

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Abstract

The invention discloses a method for preparing nano tungsten oxide from tungstenic waste cemented carbide, and belongs to the technical field of tungstenic waste recovery. The method comprises the following steps: high-temperature and high-pressure leaching is performed on powdery tungstenic waste in a stainless steel reaction kettle with sodium hydroxide, a sulfuric acid liquor is added to a tungstenic alkaline liquor for pH regulation, pH is controlled in the range of 3-5, and the liquor is kept clear all along; a TOA and N235 joint extraction agent and ammonium bicarbonate are added to theliquor for extraction and back extraction, then heating evaporation, crystallization, drying and re-calcination are performed, and nano tungsten oxide is obtained. Nano tungsten oxide prepared with the method has the advantage of small and uniform granularity; heat preservation time is shorter in a roasting process, and advantages of complete grains and high crystallinity are guaranteed.

Description

technical field [0001] The invention relates to a method for preparing nano-tungsten oxide from tungsten-containing waste cemented carbide, and belongs to the technical field of recycling tungsten-containing waste materials. Background technique [0002] Tungsten is an important strategic metal resource, which is widely used in aerospace, military industry, civil and other fields, and is also one of the traditional foreign exchange-earning minerals in my country. In the early days of history, my country's tungsten resources were very rich, but after 60 years of extensive mining and utilization, my country's tungsten reserves have dropped from 65% of the world's reserves at the time of the founding of the People's Republic of China to 37.7%, and its advantages have rapidly weakened; in addition, the country has also issued relevant policies to restrict the mining of resource minerals, and the supply of raw ore has become tighter; the waste of tungsten ore resources is also incr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/02B82Y30/00
CPCB82Y30/00C01G41/02C01P2006/80C01P2006/40C01P2002/72C01P2004/03
Inventor 张正富任艳昆易健宏范苏晓徐嘉辉刘警峰王梓
Owner KUNMING UNIV OF SCI & TECH