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Method for preparing hafnium oxide from hafnium-titanium enrichment slag

A hafnium oxide enrichment technology is applied in the field of hafnium oxide preparation and hydrometallurgy preparation, which can solve the problems of waste water, waste gas difficult treatment, increased separation difficulty, poor working environment, etc., so as to save ore dressing and product purity High, production investment cost reduction effect

Active Publication Date: 2017-09-12
XIAN RAREALLOYS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The hafnium production process uses zirconium ore associated with hafnium as raw material. The ratio of zirconium and hafnium is approximately 100:2, and zirconium and hafnium have similar outer electronic structures, and the atomic radius and ionic radius are very close, making their properties similar. Double the difficulty of separation
Traditional MIBK-HSCN system liquid-liquid extraction separation and purification of hafnium is a typical method, but the water solubility of MIBK is as high as 1.7wt%, and the loss is serious, NH 4 SCN and HSCN are easy to decompose, highly toxic, poor working environment, and the waste water and waste gas generated are difficult to treat

Method used

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  • Method for preparing hafnium oxide from hafnium-titanium enrichment slag

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Embodiment 1

[0026] combine figure 1 In this embodiment, a method for preparing hafnium oxide from hafnium-titanium enrichment slag comprises the following steps:

[0027] Step 1. Weigh 1Kg of hafnium-titanium hydrate enriched slag, the liquid-solid ratio is 2:1, and dissolve at room temperature with 65% concentrated nitric acid, stirring and dissolving for 30 minutes, and the slag is completely dissolved to obtain a leaching solution with a hafnium concentration of 14g / L;

[0028] In step 2, the high-concentration hafnium solution gained in step 1, the acidity is adjusted to 6.5mol / L with pure water and nitric acid, and the hafnium ion concentration is 3.5g / L;

[0029] Step 3, choose 100% tributyl phosphate as the organic phase, the solution obtained in step 2 is the water phase, the ratio of O / A is 1:1, the extraction time is 3min, and three-stage countercurrent extraction is carried out, the concentration of hafnium ions in the raffinate is low at 1mg / L;

[0030] Step 4: Prepare the w...

Embodiment 2

[0034] combine figure 1 In this embodiment, a method for preparing hafnium oxide from hafnium-titanium enrichment slag comprises the following steps:

[0035] Step 1. Weigh 1Kg of hafnium-titanium hydrate enriched slag, the liquid-solid ratio is 2.5:1, and dissolve at room temperature with 65% concentrated nitric acid, stirring and dissolving for 40 minutes, and the slag is completely dissolved to obtain a leaching solution with a hafnium concentration of 16g / L;

[0036] In step 2, the high-concentration hafnium solution gained in step 1, the acidity is adjusted to 5.5mol / L with pure water and nitric acid, and the hafnium ion concentration is 5.0g / L;

[0037] Step 3, choose 100% tributyl phosphate as the organic phase, the solution obtained in step 2 is the water phase, the ratio of O / A is 1:1, the extraction time is 3min, carry out five-stage countercurrent extraction, the concentration of hafnium ions in the raffinate is low at 1mg / L;

[0038] Step 4: Prepare the washing s...

Embodiment 3

[0042] combine figure 1 In this embodiment, a method for preparing hafnium oxide from hafnium-titanium enrichment slag comprises the following steps:

[0043] Step 1. Weigh 1.5Kg of hafnium-titanium hydrate enriched slag, with a liquid-solid ratio of 2:1, stir and dissolve at room temperature with 65% concentrated nitric acid for 50 minutes, the slag is completely dissolved, and a leaching solution with a hafnium concentration of 12g / L is obtained;

[0044]In step 2, the high-concentration hafnium solution gained in step 1, the acidity is adjusted to 7.0mol / L with pure water and nitric acid, and the hafnium ion concentration is 6.0g / L;

[0045] Step 3, choose 100% tributyl phosphate as the organic phase, the solution obtained in step 2 is the water phase, the ratio of O / A is 1:1, the extraction time is 3min, and three-stage countercurrent extraction is carried out, the concentration of hafnium ions in the raffinate is low at 1mg / L;

[0046] Step 4: Prepare the washing liquid...

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Abstract

The invention provides a method for preparing hafnium oxide from hafnium-titanium enrichment slag. The method comprises: 1, dissolving hafnium-titanium enrichment slag with 65% concentrated nitric acid; 2, adjusting the hafnium ion concentration and the acidity of the solution obtained in the step 1; 3, carrying out extraction separation on hafnium and other impurity ions in the solution obtained in the step 2 by selecting tributyl phosphate; 4, washing a hafnium-containing loaded organic phase; 5, carrying out reverse extraction on the loaded organic phase obtained in the step 4; and 6, introducing ammonia gas and precipitating hafnium, and calcining hafnium hydroxide to prepare the atomic level hafnium oxide. The method of the present invention has characteristics of short process, low investment cost, low production cost, high product purity, high added value, wide promotion application value, and the like.

Description

technical field [0001] The invention belongs to the technical field of preparing hafnium oxide by hydrometallurgy, and in particular relates to a method for preparing hafnium oxide from hafnium-titanium enrichment slag. Background technique [0002] Hafnium is an important strategic resource. As a control material for nuclear-powered ship reactors, there are almost no other materials that can replace it. At the same time, hafnium is widely used in plasma cutting machines, aerospace materials, camera shutters, radio earphones, tool edges and other fields. Hafnium and zirconium are always associated together in nature, and no single hafnium mineral has been found so far. There are four proven hafnium mines in my country, with a total of 1800 tons, and some mining areas have complex mineral compositions and have not yet been developed. With the rapid development of the nuclear industry and the aerospace field, the demand for hafnium oxide is increasing day by day, and thousan...

Claims

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Application Information

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IPC IPC(8): C01G27/02
Inventor 许万祥张卜升王靖坤
Owner XIAN RAREALLOYS
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