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Preparation method of low-antimony niobium oxide and preparation method of low-antimony tantalum oxide

A technology of niobium oxide and niobium hydroxide, which is applied in chemical instruments and methods, inorganic chemistry, tantalum compounds, etc., can solve the problems of difficult industrial production, large ammonium consumption, and difficult industrial application, and achieve easy industrial production and high efficiency. The effect of removal and efficient separation

Active Publication Date: 2018-11-23
稀美资源(广东)有限公司
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Problems solved by technology

Due to the presence of other high-valent metal ions in the leaching solution, a large amount of diammonium will be consumed, which not only increases the amount of diammonium used, but also affects the effect of antimony removal. Therefore, the method has high cost of antimony removal, difficult operation, and difficult industrial application; CN102358918A publishes Add D-296 macroporous anion exchange resin to tantalum liquid to adsorb tantalum, and add D290 macroporous anion exchange resin to niobium liquid to adsorb niobium, so as to achieve the purpose of separating tantalum / niobium and antimony in tantalum liquid and niobium liquid. The adsorption capacity is limited, and this method is also difficult to realize industrial production

Method used

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  • Preparation method of low-antimony niobium oxide and preparation method of low-antimony tantalum oxide
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  • Preparation method of low-antimony niobium oxide and preparation method of low-antimony tantalum oxide

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[0026] The invention provides a method for preparing low-antimony niobium oxide, comprising the following steps:

[0027] (1) mixing the antimony-niobium solution with a reducing agent to carry out a reduction reaction; then mixing the feed solution after the reduction reaction with a complexing agent to carry out a complexation reaction to obtain a niobium liquid containing an antimony complex;

[0028] (2) the niobium liquid of described step (1) is mixed with ammonia gas or liquefied ammonia, carry out neutralization reaction, generate niobium hydroxide precipitation, and antimony exists in the solution with complex form;

[0029] (3) Filtering, washing, drying and calcining the niobium hydroxide in the step (2) in sequence to obtain low-antimony niobium oxide.

[0030] In the following specific embodiments, unless otherwise specified, the reagents used are commercially available products well known to those skilled in the art.

[0031] The invention mixes the solution con...

Embodiment 1

[0054] The chemical composition of the tantalum-niobium ore is shown in Table 1:

[0055] Table 1 Chemical composition of tantalum-niobium ore

[0056] element

Ta

Nb

Sb

Mass content

4.1％

31.2％

0.12％

[0057] Mix tantalum and niobium ore with hydrofluoric acid and sulfuric acid, carry out acid leaching, extraction and stripping, and obtain antimony-niobium solution and antimony-tantalum solution, wherein the content of niobium in the antimony-niobium solution and the tantalum in the antimony-tantalum solution are content is listed in Table 2.

[0058] according to figure 1 The schematic flow chart shown prepares low-antimony niobium oxide: take 3m niobium solution containing antimony 3 In the neutralization tank, add citric acid in an amount of 1kg / L, react at 60°C for 30min, then add triethanolamine in an amount of 1kg / L, react at 80°C for 6h, and obtain a niobium solution containing an antimony complex; Adjust the pH value of the ...

Embodiment 2

[0061] Take 3m niobium solution containing antimony 3 In the neutralization tank, add citric acid in an amount of 0.5kg / L, react at 60°C for 30min, then add triethanolamine in an amount of 0.5kg / L, react at 85°C for 6h, and obtain the niobium containing antimony complex solution; adjust the pH value of the niobium-containing solution to 9 with ammonia water, filter, wash, dry and calcinate after the precipitation is complete, wherein the calcining conditions are: calcining at 850°C for 1.5h to obtain low-antimony niobium oxide.

[0062] Get embodiment 1 gained to contain antimony tantalum liquid 3m 3 In the neutralization tank, add citric acid in an amount of 0.5kg / L, react at 60°C for 30min, then add triethanolamine in an amount of 0.5kg / L, react at 85°C for 6h, and obtain antimony complex-containing tantalum solution; adjust the pH value of the tantalum-containing solution to 9 with ammonia water, filter, wash, dry and calcinate after the precipitation is complete, wherein ...

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Abstract

The invention belongs to the technical field of preparation of rare metals, and specifically relates to a preparation method of low-antimony niobium oxide and the preparation method of low-antimony tantalum oxide. The preparation method comprises the following steps: firstly, converting positive pentavalent antimony in an antimony-containing niobium solution or an antimony-containing tantalum solution into positive trivalent antimony through reduction reaction, and then reacting with a complexing agent, thus generating a stable antimony complex; then, precipitating niobium or tantalum in a solution by utilizing neutralization reaction, and generating niobium hydroxide or tantalum hydroxide, wherein the antimony complex is not damaged and can exist in the solution, thus realizing efficientseparation of a niobium product or a tantalum product from antimony. According to the preparation method disclosed by the invention, antimony impurity in an antimony-containing solution can be efficiently removed, so that the niobium oxide or the tantalum oxide of which the antimony content is smaller than 20ppm can be obtained, the operation is simple, and industrial production is easy.

Description

technical field [0001] The invention belongs to the technical field of rare metal preparation, and in particular relates to a preparation method of low-antimony niobium oxide and a preparation method of low-antimony tantalum oxide. Background technique [0002] Tantalum and niobium products involve many types, including tantalum powder, tantalum wire, tantalum carbide, tantalum and its alloy ingots, tantalum and its alloy processing materials, tantalum targets, tantalum oxide, lithium tantalate single crystal, ferroniobium, niobium nickel, Niobium powder, niobium bars, niobium and its alloy ingots, niobium and its alloy processing materials, niobium oxide, niobium carbide and lithium niobate single crystal, etc. Among them, tantalum and niobium oxide is not only a tantalum and niobium product, but also a source for the production of other tantalum and niobium products Raw materials, therefore, tantalum niobium oxide and its production process have attracted much attention. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G33/00C01G35/00
CPCC01G33/00C01G35/00C01P2006/80
Inventor 马昆鹏钟岳联石波桂训武
Owner 稀美资源(广东)有限公司
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