Method for preparing high-purity niobium oxide through niobium-tantalum-iron alloy

A technology of ferroalloy and niobium oxide, which is applied in the field of niobium oxide preparation, can solve problems such as explosion, failure to meet actual needs, and influence on the purity and quality of niobium oxide, and achieve efficient removal effect

Active Publication Date: 2018-10-12
稀美资源(广东)有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

A large amount of hydrogen gas will be produced in the process of hydrometallurgy, which is easy to cause explosion. Therefore, before hydrometallurgy, niobium-tantalum iron alloys are usually not pulverized and the concentration of acid is reduced. Although this method can control the generation rate of hydrogen gas and reduce However, due to the inability to effectively remove impurity elements such as antimony, copper, carbon, sulfur, and phosphorus in the niobium-tantalum iron alloy during the extraction process, the purity and quality of the obtained niobium oxide are greatly affected and cannot meet the actual needs of the market.

Method used

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  • Method for preparing high-purity niobium oxide through niobium-tantalum-iron alloy

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preparation example Construction

[0047] In the present invention, the preparation method of the purification agent preferably includes: melting the raw materials according to the chemical composition of the purification agent to obtain an alloy melt; water quenching, crushing and sieving the alloy melt in sequence to obtain purifier. The present invention has no special requirements on the specific sources of the raw materials, and commercially available products well known to those skilled in the art can be used. In the present invention, there is no special requirement on the smelting method of the raw materials, and a method well known to those skilled in the art can be used. The present invention has no special requirements on the specific implementation methods of the water quenching, crushing and sieving, and methods well known to those skilled in the art can be used.

[0048] In the present invention, the volume ratio of the mass of the purifying agent to the diluent is preferably 110 to 125 kg / m 3 ,...

Embodiment 1

[0067] The niobium-tantalum-iron alloy powder with the composition shown in Table 1 was used.

[0068] Table 1 Chemical composition of niobium-tantalum-iron alloy

[0069] element

Ta

Nb

W

Si

Al

Cu

Fe

Sb

S

P

C

Mass content

3.51

39.62

0.06

18.3

1.7

1.5

28.4

0.12

2.17

2.2

1.09

[0070] The niobium-tantalum-iron alloy was crushed and ground to 300 mesh, and roasted at 850°C for 3 hours to obtain a solid oxide; the main impurities in the solid oxide were detected and analyzed: copper: 1.35%, antimony: 0.1%, sulfur: 0.52%, phosphorus: 0.31%, Carbon: 0.06%;

[0071] Carry out acid leaching with hydrofluoric acid and sulfuric acid by the ratio of mass ratio 1:1.4:0.9 of solid oxide, react for 16 hours, wherein, hydrofluoric acid mass concentration is 55%, sulfuric acid mass concentration is 98%, obtains acid leaching solution, Its chemical composition is as follows: Nb 2 o 5 :185.6g / L,Ta ...

Embodiment 2

[0077] The tantalum-niobium-iron alloy is processed according to the method of Example 1, the difference is that the chemical composition of the purifying agent (shown in Table 2), the particle size of the tantalum-niobium-iron alloy powder is 280 mesh, and the oxidation roasting temperature is 870 ° C. 6.5% NaNO 2 , the extractant used is MIBK, calcined at 850°C for 5h, other details are shown in Table 2-3. The results obtained in this example are tested, and the purity of high-purity niobium oxide meets the non-ferrous metal industry standard FNb 2 o 5 -04 grade requirements.

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Abstract

The invention relates to a method for preparing high-purity niobium oxide through niobium-tantalum-iron alloy. The method comprises the steps that the niobium-tantalum-iron alloy is roasted,carbon,sulphur and phosphorus impurity elements in the niobium-tantalum-iron alloy are removed,metal elementary substances in the niobium-tantalum-iron alloy are converted into metallic oxide at the same time,and the situation is avoided that the metal elementary substances and acid react to generate hydrogen; then,through following acid leaching and purification treatment,a purification agent is used for removing difficultly-separated impurity elements such as antimony and copper in an acid leaching solution in the following extraction process,in cooperation with extraction,acid leaching,niobium returning,tantalum extraction and other processes,separation purification is conducted,and a niobium-containing solution is obtained; finally,niobium ions are precipitated through ammonium hydroxide,and high-purity niobium oxide is obtained after roasting. According to the method,the impurity elements in the niobium-tantalum-iron alloy can be efficiently removed,the content of the antimony element is lowered to the value smaller than 10 ppm,the content of the copper element is lowered to the value below 3.0 ppm,and accordingly a high-purity niobium oxide product with the purity larger than or equalto 99.95% is obtained.

Description

technical field [0001] The invention belongs to the technical field of niobium oxide preparation, and in particular relates to a method for preparing high-purity niobium oxide from a niobium-tantalum iron alloy. Background technique [0002] Compared with ferro-niobium alloy, niobium-tantalum alloy has a much lower content of niobium. The niobium content is 25-45%, the tantalum content is about 4%, and the rest are impurities such as iron, silicon, aluminum, carbon, sulfur, phosphorus, etc., which cannot be directly Used as an additive to ferrous alloys, impurity removal treatment is required. The conventional impurity removal method is to use wet smelting, acid leaching the niobium tantalum iron alloy to remove impurities that can react with acid, and then obtain niobium oxide. A large amount of hydrogen gas will be produced in the process of hydrometallurgy, which is easy to cause explosion. Therefore, before hydrometallurgy, niobium-tantalum iron alloys are usually not p...

Claims

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Application Information

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IPC IPC(8): C01G33/00
CPCC01G33/00C01G33/003C01P2006/80
Inventor 石波胡松吴宇锦
Owner 稀美资源(广东)有限公司
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