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Preparation method of ammonium poly-vanadate

A technology of ammonium polyvanadate and calcium vanadate, applied in chemical instruments and methods, vanadium compounds, inorganic chemistry, etc., can solve the problem that potassium and sodium content cannot be controlled correspondingly, the amount of ammonium carbonate added is large, and the production cost is high. problems, to achieve good economic and social benefits, reduce ammonia concentration, and improve the effect of vanadium grade

Inactive Publication Date: 2009-11-11
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This document introduces the process parameters such as reaction temperature, time, and pH value of precipitated calcium vanadate and carbonation leaching, but the vanadium-containing acid leaching solution used in the test is a solution with a very low vanadium concentration; during carbonation leaching, the amount of ammonium carbonate added It is very large, which eventually leads to high production costs and high ammonia content in the vanadium precipitation wastewater; the total vanadium recovery rate in the whole process is only about 90%, and the potassium and sodium content in the ammonium polyvanadate product has not been controlled accordingly

Method used

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  • Preparation method of ammonium poly-vanadate

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Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment one prepares ammonium polyvanadate with the inventive method

[0025] Take 1400ml of a solution with a vanadium concentration of 33.1g / L, add 188ml of a 500g / L calcium chloride solution; under stirring conditions, add milk of lime to adjust the pH of the solution to 9.46; heat to boiling for 40min. Obtain calcium vanadate 153.1g, calcium vanadate TV is 29.83%; Precipitation calcium vanadate supernatant liquid volume is 1120ml, TV is 0.408g / L; Calcium vanadate washing solution volume is 267ml, TV is 0.128g / L; Vanadium The precipitation rate was 98.94%.

[0026] Take 100 g of this calcium vanadate containing 29.83% vanadium, add it into 1000 ml of a solution containing 5% ammonium bicarbonate, stir and heat to boiling, and react for 30 minutes. After the reaction is completed, filter, wash the precipitated vanadium with water, combine the filtrate and washing water, the volume is 1440mL, the TV content is 20.25g / L, and the vanadium leaching rate is 97.77%. Af...

Embodiment 2

[0027] Embodiment two prepares ammonium polyvanadate with the inventive method

[0028] Take 1000ml of a solution with a vanadium concentration of 51.82g / L, add 210ml of a 500g / L calcium chloride solution; under stirring conditions, add milk of lime to adjust the pH of the solution to 9.26; heat to boiling, and react for 30min. Obtain calcium vanadate 185.2g, calcium vanadate TV is 27.62%; Precipitation calcium vanadate supernatant volume is 990ml, TV is 0.58g / L; Calcium vanadate washing solution volume is 210ml, TV is 0.054g / L; Vanadium The precipitation rate was 98.87%.

[0029] Take 100 g of this calcium vanadate containing 27.62% vanadium, add it to 350 mL of a solution containing 15% ammonium bicarbonate, stir and heat to boiling, and react for 30 minutes. After the reaction is completed, filter, wash the precipitated vanadium with water, combine the solution and washing water, the volume is 825mL, the TV content is 32.82g / L, and the vanadium leaching rate is 98.03%. Af...

Embodiment 3

[0030] Embodiment three uses the inventive method to prepare ammonium polyvanadate

[0031] Take 1000ml of a solution with a vanadium concentration of 35.6g / L, add 200ml of a 500g / L calcium nitrate solution; under stirring conditions, add milk of lime to adjust the pH of the solution to 9.1; heat to boiling, and react for 30min. 107.98 g of calcium vanadate was obtained, and the TV of calcium vanadate was 32.45%. After the precipitated calcium vanadate supernatant was combined with washing water, the volume was 1550 ml, the TV was 0.36 g / L, and the vanadium precipitation rate was 98.43%.

[0032] Take 100g of this calcium vanadate containing 32.45% vanadium, add it into 350mL solution containing 15% ammonium bicarbonate, stir and heat to 85°C, and react for 60min. After the reaction is completed, filter, wash the precipitated vanadium with a small amount of water, combine the solution and washing water, the volume is 886mL, the TV content is 36.2g / L, and the vanadium leaching ...

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Abstract

The invention belongs to the field of chemical industry, and in particular relates to a method for preparing ammonium polyvanadate from a vanadium-containing solution. The method of the present invention uses the vanadium-containing solution produced by the traditional sodium roasting-water immersion process as a raw material, first combines the vanadium with the added calcium compound to form calcium vanadate, and then reacts with ammonium bicarbonate and calcium vanadate to transfer the vanadium into the solution, and calcium generates more insoluble calcium carbonate, and the solution after separation generates ammonium polyvanadate under appropriate pH and heating conditions. After the process of generating calcium vanadate and redissolving, ammonium polyvanadate with ∑(Na2O+K2O)<0.1% can be obtained, which can be used to produce vanadium trioxide and dioxypentoxide with very low potassium and sodium content. vanadium; the ammonia content in the vanadium precipitation wastewater is only 60% to 75% of the vanadium extraction wastewater in the traditional process. It has a good application prospect.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for preparing ammonium polyvanadate from a vanadium-containing solution. Background technique [0002] Vanadium is a rare metal with high melting point. It has many excellent properties and is widely used in metallurgy, chemical industry and other industries. With the rapid development of my country's modernization, the demand for vanadium and its compounds is increasing, the scope of use is becoming wider and wider, and its quality requirements are also higher. In the production process of vanadium nitrogen alloy, it is required that ∑(Na 2 O+K 2 The lower the O) content, the better, and in the vanadium oxide products produced by the traditional sodium roasting-water method vanadium extraction process, ∑(Na 2 O+K 2 O) content is generally 0.5% to 2%, which is much higher than that of vanadium-nitrogen alloy to the raw material Σ(Na 2 O+K 2 O) content r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G31/00
Inventor 彭毅李千文夏清荣王小江彭明福付自碧窦伟
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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