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Preparation technology for hafnium carbonate

A technology of carbonic acid and hafnium sulfate, which is applied in the field of hydrometallurgy, can solve the problems that the preparation of hafnium carbonate has not been reported, and achieve the effect of high metal recovery and good solubility

Active Publication Date: 2011-09-07
有研资源环境技术研究院(北京)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there have been many studies on the preparation methods of some compounds of zirconium, such as Luo Fangcheng, Lu Wenguang and others in September 2002 in "Jiangxi Nonferrous Metals" Volume 16, No. 3, and Xiong Bingkun, Yang Xinmin, Luo Fangcheng, Zhang Wei and others reported that zirconium carbonate is easily soluble in inorganic strong acids and has certain solubility in some organic acids in "Application of Zirconium, Hafnium and Its Compounds" in 2002. Active zirconium carbonate is soluble in potassium carbonate solution, but the preparation of hafnium carbonate has not been reported

Method used

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  • Preparation technology for hafnium carbonate
  • Preparation technology for hafnium carbonate
  • Preparation technology for hafnium carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Concentration [HfO 2 ]=292.15g / L, [H + ]=1.64mol / L hafnium oxychloride solution. Take 0.55L of this hafnium oxychloride solution, add 1.05L of water, and make the concentration [HfO 2 ]=100.4g / L feed liquid 1.6L. According to the molar ratio Hf 4+ : SO 4 2- = 1: 0.67 add H 2 SO 4 33 mL of analytically pure sulfuric acid with a content of 95% to 98%, add NH 3 60mL of analytically pure ammonia water with a content of 25% to 28%, the concentration of [HCl] neutralized into the solution is 1 to 1.5g / L, and stirred evenly. Divide into 4 beakers. Put it into a water bath for hydrolysis, and keep it warm at 95°C for 8 hours. After the reaction is finished, filter and wash the filter cake 4 to 5 times, and keep the filtered cake after washing.

[0023] Prepare 1.46L of 10% sodium carbonate solution. Put the filtered and dried filter cake into the sodium carbonate solution and stir evenly. Then put it into 4 beakers, put it into a water bath for transformation, and ...

Embodiment 2

[0033] Concentration [HfO 2 ]=349.83g / L, [H + ]=2.14mol / L hafnium oxychloride solution. Take this hafnium oxychloride solution 0.114L, add 0.286L water, make the concentration [HfO 2 ]=100.5g / L feed liquid 0.4L. According to the molar ratio Hf +4 : SO 4 2- = 1: 0.88 added H 2 SO 4 9.1 mL of analytically pure sulfuric acid with a content of 95% to 98%, add NH 3 15mL of analytically pure ammonia water with a content of 25% to 28%, the concentration of [HCl] neutralized into the solution is 1 to 1.5g / L, and stirred evenly. Put it into a water bath for hydrolysis, and keep it warm at 95°C for 8 hours. After the reaction is finished, filter and wash the filter cake 4 to 5 times, and keep the filtered cake after washing.

[0034] Prepare 0.36L of 10% sodium carbonate solution. Put the filter cake into the sodium carbonate solution and stir well. Put it into a water bath for transformation, and keep it warm at 85°C for 2 hours. After the reaction is finished, filter and ...

Embodiment 3

[0038] Concentration [HfO 2 ]=349.83g / L, [H + ]=2.14mol / L hafnium oxychloride solution. Take 0.46L of this hafnium oxychloride solution, add 1.14L of water, and make the concentration [HfO 2 ]=100.5g / L feed liquid 1.6L. According to the molar ratio Hf 4+ : SO 4 2- = 1: 0.88 added H 2 SO 4 36.4 mL of analytically pure sulfuric acid with a content of 95% to 98%, add NH 3 64mL of analytically pure ammonia water with a content of 25% to 28%, the concentration of [HCl] neutralized into the solution is 1 to 1.5g / L, and stirred evenly. Pour into 4 beakers. Put it into a water bath for hydrolysis, and keep it warm at 95°C for 8 hours. After the reaction is finished, filter and wash the filter cake 4 to 5 times, and keep the filtered cake after washing.

[0039] Prepare 1.16L of 10% ammonium bicarbonate solution. Put the filter cake into the ammonium bicarbonate solution and stir well. Put them into 4 beakers respectively, put them into a water bath for transformation, and...

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Abstract

The invention discloses a method for preparing hafnium carbonate in the field of hydrometallurgy. Hafnium carbonate powder is prepared through a two-step method of: (1) preparing basic hafnium sulfate by hydrolysis: dissolving hafnium oxydichloride in deionized water to obtain the solution of the hafnium oxydichloride, adding a certain amount of sulfuric acid and ammonia water into the solution for thermal insulation hydrolysis for 8 hours in water bath; and (2) transforming the basic hafnium sulfate into the hafnium carbonate: dissolving a certain amount of carbonate in the deionized water to obtain solution of the carbonate, mixing the basic hafnium sulfate prepared in the last step and the solution of the carbonate uniformly for a thermal insulation reaction for 2 hours in water bath. By adjusting the molar ratio of transforming agents, namely SO42- and Hf4+, the method can ensure that the hydrolytic precipitation in the first step is more complete, the concentration of the Hf4+ inhydrolysis mother liquor is quite low, and the recovery rate of metal is high; and by using different carbonate transforming agents, the method can prepare the hafnium carbonates with different carbon contents, and the hafnium carbonates have different solubilities in citric acid, but all have good dissolubility in acetic acid.

Description

technical field [0001] The invention belongs to the field of hydrometallurgy, in particular to a preparation method of hafnium carbonate. Background technique [0002] Zirconium and hafnium are two elements with very similar chemical properties. So far, there have been many studies on the preparation methods of some compounds of zirconium, such as Luo Fangcheng, Lu Wenguang and others in September 2002 in "Jiangxi Nonferrous Metals" Volume 16 No. 3, and Xiong Bingkun, Yang Xinmin, Luo Fangcheng, Zhang Wei and others reported that zirconium carbonate is easily soluble in inorganic strong acids and has certain solubility in some organic acids in "Application of Zirconium, Hafnium and Its Compounds" in 2002. Active zirconium carbonate is soluble in potassium carbonate solution, but the preparation of hafnium carbonate has not been reported yet. [0003] The composition of hafnium carbonate is relatively complex, and the composition of hafnium carbonate produced under differen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G27/00
Inventor 何芬张明贤张少辉张碧田王星明段华英潘德明龚述荣孙静
Owner 有研资源环境技术研究院(北京)有限公司
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