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A method for separating tungsten and molybdenum from ammonium tungstate solution with high molybdenum content

A technology of ammonium tungstate and ammonium paratungstate, which is applied in the field of separating tungsten and molybdenum, can solve the problems of increased cost of molybdenum removal, high price, and low proportion of molybdenum product value, and achieve the effect of reducing cost and burden

Active Publication Date: 2019-09-03
CENT SOUTH UNIV
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Problems solved by technology

[0005] The above molybdenum removal method is mainly suitable for the treatment of ammonium tungstate solution with low molybdenum content (selective precipitation method is suitable for Mo / WO 3 3 4 ) 2 S is expensive, and the consumption of ammonium sulfide reagent increases linearly with the increase of molybdenum content in tungstate solution, while other reagents such as copper salt or NaOH increase simultaneously, so the molybdenum removal cost per unit of tungsten product increases with the increase of ammonium tungstate solution The content of molybdenum in the molybdenum increases significantly; 3 When the molybdenum content is low, the proportion of molybdenum product value is low, and the impact on the overall economic benefit is not significant. When the molybdenum content increases, the value of molybdenum product becomes the key factor affecting the overall economic benefit; 3) the molybdenum removal process produces copper molybdenum slag or MoS 3 Still contains a certain amount of tungsten, of which WO 3 / Mo is more than 10%, lost in copper molybdenum slag or MoS 3 The tungsten in the ammonium tungstate solution increases synchronously with the increase of molybdenum content, when the Mo content increases, the loss of tungsten is significant
Based on the above reasons, for the ammonium tungstate solution with high molybdenum content (such as Mo / WO 3 >5%), using the above method to remove molybdenum from ammonium tungstate solution is difficult to meet the requirements of industrial production in terms of cost, tungsten loss and molybdenum product value. It is of great significance to prepare high-quality tungsten and molybdenum products with high efficiency and low cost

Method used

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  • A method for separating tungsten and molybdenum from ammonium tungstate solution with high molybdenum content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Raw material solution: molybdenum-containing ammonium tungstate solution, in which WO 3 140.5g / L, Mo 16.3g / L, Mo / WO 3 Mass ratio = 11.6%.

[0046] The first step is rough separation of evaporation and crystallization.

[0047] Take 7000mL of raw material solution and put it into a 10000mL glass reactor, stir and heat in an oil bath to evaporate and crystallize. After filtration, 1180.0 g of crude APT and 2400 mL of crystalline mother liquor were obtained. Crude APT contains 10% water, dry basis contains WO 3 87.2%, Mo 0.76%, Mo / WO 3 Mass ratio=0.87%; crystallization mother liquor WO 3 25.2g / L, Mo 43.7g / L, Mo / WO 3 =1.73, according to crystallization mother liquor, WO 3 The crystallization rate was 93.8%, and the Mo crystallization rate was 8.1%.

[0048] The second step is to remove molybdenum deeply.

[0049] Take 500.0 g of the crude APT obtained in the first step, place it in a 2L stainless steel electric heating autoclave, add 1.5L of 3mol / L ammonia water...

Embodiment 2

[0053] Raw material solution: molybdenum-containing ammonium tungstate solution, in which WO 3 80.0g / L, Mo 40.0g / L, Mo / WO 3 = 50.0%.

[0054] The first step is rough separation of evaporation and crystallization.

[0055] Take 7000mL of raw material solution into a 10000mL glass reactor, stir in an oil bath, heat, evaporate and crystallize, control the temperature between 100±5°C, operate under normal pressure, heat and evaporate for 6 hours, stop evaporation, cool and filter, and obtain 650.8g of crude APT and 2600 mL crystallization mother liquor. Crude APT contains 10.5% water and WO on a dry basis 3 83.7%, Mo 3.37%, Mo / WO 3 =4.03%; crystallization mother liquor WO 3 33.1g / L, Mo 118.4g / L, Mo / WO 3 =3.58, according to the crystallization mother liquor WO 3 The crystallization rate was 87.0%, and the Mo crystallization rate was 7.0%.

[0056] The second step is to remove molybdenum deeply.

[0057] Take 500.0g of the crude APT obtained in the first step, put it in ...

Embodiment 3

[0061] Raw material solution: molybdenum-containing ammonium tungstate solution, in which WO 3 300.2g / L, Mo 16.3g / L, Mo / WO 3 = 5.4%.

[0062] The first step is rough separation of evaporation and crystallization.

[0063] Take 7000mL of raw material solution and put it into a 10000mL glass reactor, stir and heat in an oil bath to evaporate and crystallize. After filtration, 2568.0 g of crude APT and 2100 mL of crystalline mother liquor were obtained. Crude APT contains 10.3% water and WO on a dry basis 3 88.1%, Mo 0.60%, Mo / WO 3 Mass ratio=0.68%; WO in crystallization mother liquor 3 34.2g / L, Mo 47.8g / L, Mo / WO 3 Mass ratio=1.39, according to crystallization mother liquor, WO 3 The crystallization rate was 96.5%, and the Mo crystallization rate was 12.0%.

[0064] The second step is to remove molybdenum deeply.

[0065] Take 500.0g of the crude APT obtained in the first step, put it in a 2L stainless steel electric heating high-pressure reactor, add 1.40L of 4.0mol / ...

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Abstract

The invention provides a method for separating tungsten and molybdenum from an ammonium tungstate solution having high molybdenum content. The method comprises the following steps: firstly, processingthe ammonium tungstate solution having the high molybdenum content by adopting evaporative crystallization to obtain tungsten-rich molybdenum-deficiency ammonium paratungstate crystals and molybdenum-rich tungsten-deficiency crystallizing mother liquid so that tungsten and molybdenum are primarily separated; then heating the molybdenum-deficiency ammonium paratungstate with ammonia water and performing airtight dissolution to obtain the ammonium tungstate solution with low molybdenum content; processing the ammonium tungstate solution through thio processing and preferentially adsorbing molybdenum by adopting an ionic exchange method so as to realize deep molybdenum removal of the ammonium tungstate solution to obtain a pure ammonium tungstate solution; preferentially extracting tungstenfrom the molybdenum-rich crystallizing mother liquid by adopting a synergistic extraction method so as to realize deep tungsten removal in an ammonium molybdate solution to obtain a pure ammonium molybdate solution. The method for processing the ammonium tungstate solution with the high molybdenum content provided by the invention has the characteristics of low cost, good separation effect and high added value of molybdenum products.

Description

technical field [0001] The invention relates to the field of extraction and separation of rare metals in hydrometallurgy, in particular to a method for separating tungsten and molybdenum from ammonium tungstate solution with high molybdenum content. Background technique [0002] Tungsten and molybdenum are important strategic rare metals, which are widely used in cemented carbide, alloy steel, electronics, defense aviation, petrochemical and other fields. Molybdenum and tungsten are impurity elements that need to be strictly controlled in tungsten and molybdenum products. For example, the Chinese national standard GB10116-2007 requires the content of molybdenum in zero-grade APT (ammonium paratungstate) (that is, Mo / WO 3 Mass ratio) is not more than 0.002%, and the national standard GB / T3460-2007 stipulates that the tungsten content in zero-grade MSA (ammonium molybdate) products (ie W / MoO 3 mass ratio) is not more than 0.015%. However, tungsten and molybdenum belong to gr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G39/00C01G41/00
Inventor 张贵清肖连生曹佐英关文娟曾理李青刚
Owner CENT SOUTH UNIV
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