Low-temperature crystallization method of ammonium polyvanadate

An ammonium polyvanadate and low-temperature crystallization technology is applied in the field of vanadium precipitation, which can solve the problems of increasing the subsequent wastewater treatment pressure, increasing the output of vanadium precipitation wastewater, and demanding process parameters, and reducing the output of vanadium precipitation wastewater. , Reducing energy consumption such as steam, good product quality

Inactive Publication Date: 2015-07-08
HEBEI IRON AND STEEL
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] (1) The vanadium precipitation process is always kept between 80 and 100 °C, which requires a large amount of steam consumption and high energy consumption costs
[0014] (2) The high-temperature vanadium precipitation process usually requires that the concentration of vanadium in the vanadium liquid be ≤30g/L (the ammonium polyvanadate produced due to high vanadium concentration is amorphous, loose in structure, and prone to soluble NH 4 + 、Na + 、K + , Fe 3+ , SO 4 2- , SiO 3 2- and other harmful impurities, which are difficult to remove, and the product qualification rate), which makes a large amount of high-salt and high-ammonia nitrogen wastewater produced by the precipitation of vanadium
[0015] (3) Due to the direct heating of s...

Method used

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  • Low-temperature crystallization method of ammonium polyvanadate

Examples

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Comparison scheme
Effect test

Embodiment 1

[0046] Example 1: Taking the sodiumized roasting water leachate (containing vanadium solution, V=24.5g / l) of vanadium slag in a certain area of ​​Chengde as an example, the specific process of the low-temperature crystallization method of ammonium polyvanadate is as follows.

[0047] (1) Add aluminum sulfate and magnesium chloride to the vanadium-containing solution, stir and react at 50°C for 1 hour, and then filter; the amount of aluminum sulfate added is: aluminum in the aluminum salt: silicon in the vanadium-containing solution = 1.5:1 (mol), and magnesium chloride is added Quantity: Dosed according to magnesium in magnesium salt: phosphorus in vanadium-containing solution = 1.2:1 (mol).

[0048] (2) Add ammonium sulfate, ammonium sulfate: vanadium element in the solution = 1.1:1 (mass).

[0049] (3) Add the seeding agent piperazine, the added mass is 10% of the mass of the ammonium salt, and keep stirring until it is completely dissolved.

[0050] (4) Add sulfuric acid to adjust ...

Embodiment 2

[0053] Example 2: Taking the stone coal acid leaching solution (a solution containing vanadium, V=45.6g / l) in a certain area of ​​Hunan as an example, the specific process of the method for crystallization of ammonium polyvanadate at low temperature is as follows.

[0054] (1) Add aluminum chloride and magnesium nitrate to the vanadium-containing solution, stir and react at 80°C for 0.5h, and then filter; the amount of aluminum chloride added: aluminum in the aluminum salt: silicon in the vanadium-containing solution = 1.5:1 (mol) , The amount of magnesium nitrate added: add magnesium in magnesium salt: phosphorus in vanadium-containing solution = 1.2:1 (mol).

[0055] (2) Add ammonium chloride to the vanadium-containing solution, ammonium chloride: vanadium element in the solution = 0.8:1 (mass).

[0056] (3) Add the seeding agent ethylenediamine, the added mass is 5% of the mass of the vanadium element in the solution, and keep stirring until it is completely dissolved.

[0057] (4)...

Embodiment 3

[0060] Example 3: Taking a vanadium slag calcification roasting acid leaching solution (a solution containing vanadium, V=32.1 g / l) in a certain area of ​​Sichuan as an example, the specific process of the method for crystallization of ammonium polyvanadate at low temperature is as follows.

[0061] (1) Add aluminum nitrate and magnesium chloride to the vanadium-containing solution, stir and react at 60°C for 0.6h, and then filter; the amount of aluminum chloride added: according to aluminum in the aluminum salt: silicon in the vanadium-containing solution = 1.2:1 (mol), add nitric acid The amount of magnesium added: According to the magnesium in the magnesium salt: the phosphorus in the vanadium-containing solution = 1.0:1 (mol).

[0062] (2) Add ammonium nitrate to the vanadium-containing solution, ammonium nitrate: vanadium element in the solution = 0.9:1 (mass).

[0063] (3) Add the seeding agent hexamethylenetetramine, the added mass is 20% of the mass of the vanadium element in...

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Abstract

The invention discloses a low-temperature crystallization method of ammonium polyvanadate. The low-temperature crystallization method includes following steps: (1) adding a crystallization initiator to vanadium liquid and stirring the vanadium liquid to dissolve the crystallization initiator; (2) adding acid to regulate the pH of the vanadium liquid to 1.0-7.0; and (3) continuously stirring the vanadium liquid to precipitate-out ammonium polyvanadate crystal, and performing filtration to obtain the ammonium polyvanadate crystal. The crystallization initiator is a mixture composed of one or more from water-soluble organic amine compounds and derivatives thereof. The method can effectively achieve high-concentration vanadium precipitation, can reduce the production amount of vanadium precipitation waste water by many times, can crystallize the ammonium polyvanadate crystal at room temperature, can effectively reduce energy consumption of steam and the like, can reduce the clean production cost and can increase yield rate. In the invention, the ammonium polyvanadate is precipitated-out in the form of a large-granular crystal being complete in structure. The method can reduce the entrainment of harmful impurities such as NH4<+>, Na<+>, K<+>, Fe<3+>, SO4<2->, SiO3<2-> and the like and can improve product quality.

Description

Technical field [0001] The invention relates to a method for sinking vanadium, in particular to a method for low-temperature crystallization of ammonium polyvanadate. Background technique [0002] Industrially, the process of producing vanadium oxides (including vanadium trioxide, vanadium pentoxide, etc.) using vanadium-containing materials such as vanadium-titanium magnetite, vanadium slag, stone coal, and waste catalysts as raw materials includes the following main steps: [0003] (1) Activation: the vanadium element in the solid-phase raw material is converted into soluble vanadate or vanadic acid through the roasting or acidification process; [0004] (2) Leaching: leaching soluble vanadate to liquid phase from acid, neutral or alkaline aqueous solution; [0005] (3) Precipitation of vanadium (crystallization): the vanadium leaching solution is obtained after purification and impurity removal, and precipitation reagents are added to convert the vanadate into insoluble matter and ...

Claims

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Application Information

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IPC IPC(8): C01G31/00
Inventor 陈东辉祁健
Owner HEBEI IRON AND STEEL
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