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Process method for improving chlorination distillation recovery rate of coarse germanium dioxide

A germanium dioxide and chlorinated distillation technology, applied in germanium halide and other directions, can solve the problems of excessive arsenic content and unqualified high-purity germanium dioxide.

Active Publication Date: 2011-02-09
YUNNAN LINCANG XINYUAN GERMANIUM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, in the process of producing high-purity germanium dioxide from crude germanium dioxide, the method of directly adopting hydrochloric acid chlorination distillation to recover germanium is usually due to the presence of 5-10% hydrochloric acid in the crude germanium dioxide produced from some raw materials Insoluble germanium, i.e. tetragonal germanium dioxide, so when using traditional direct hydrochloric acid distillation to produce high-purity germanium dioxide from crude germanium dioxide, due to the influence of tetragonal germanium dioxide, the distillation recovery rate Generally around 90%, in addition, because the arsenic content in the raw material of producing this kind of crude germanium dioxide is too high, the arsenic content of the germanium tetrachloride produced by conventional hydrochloric acid distillation method will seriously exceed the standard, thereby making the output High-purity germanium dioxide is unqualified, so it is necessary to study a purification method to improve the recovery rate of germanium and suppress the distillation and escape of arsenic in crude germanium dioxide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: in the dissolving reactor of 500L, add the water of 120L, then add the sodium hydroxide of 18kg, start stirring and make sodium hydroxide dissolve completely, be made into the sodium hydroxide solution of mass percentage concentration about 13.0%. Then add 12kg of germanium dioxide, the mass percentage of germanium in the crude germanium dioxide is 68.74%, the amount of germanium metal is 8.249kg, and the mass percentage of arsenic is 0.10%. It is fully dissolved and reacted for 1.5-2h until the germanium dioxide is completely dissolved. After the temperature was raised to the boiling point of the solution, 65L of water in the solution was evaporated, and the volume of the solution was 55L. Use a pump to extract the evaporated concentrated liquid and transfer it to a 500L enamel distillation reaction axe. After the liquid is cooled, add 10mol / L industrial hydrochloric acid to neutralize the solution until the pH value of the solution is 0.48. Measure with ...

Embodiment 2

[0032]Embodiment 2: in the dissolving reactor of 500L, add the water of 100L, then add the sodium hydroxide of 20kg, start stirring and make sodium hydroxide dissolve completely, be made into the sodium hydroxide solution of mass percentage concentration about 16.7%. Then add 12kg of germanium dioxide, the mass percentage of germanium in the crude germanium dioxide is 68.46%, the amount of germanium metal is 8.215kg, and the mass percentage of arsenic is 0.03%, heat to 80-85 ° C, start stirring to make It is fully dissolved and reacted for 1.5-2h until the germanium dioxide is completely dissolved. After the temperature is raised to the boiling point of the solution, 50L of water in the solution is evaporated, and the volume of the solution is 50L. Use a pump to extract the evaporated concentrated liquid and transfer it to a 500L enamel distillation reaction axe. After the liquid is cooled, add 10mol / L industrial hydrochloric acid to neutralize the solution until the pH value ...

Embodiment 3

[0033] Embodiment 3: in the dissolving reactor of 500L, add the water of 150L, ​​then add the sodium hydroxide of 24kg, start stirring and make sodium hydroxide dissolve completely, be made into the sodium hydroxide solution of mass percentage concentration about 13.8%. Then add 12kg of germanium dioxide, the mass percentage of germanium in the crude germanium dioxide is 68.12%, the amount of germanium metal is 8.174kg, the mass percentage of arsenic is 0.56%, heat to 80-85 ° C, start stirring to make It is fully dissolved and reacted for 1.5-2.0 hours until the germanium dioxide is completely dissolved. After the temperature is raised to the boiling point of the solution, 100L of water in the solution is evaporated, and the volume of the solution is 50L. Use a pump to extract the evaporated concentrated liquid and transfer it to a 500L enamel distillation reaction axe. After the liquid is cooled, add 10mol / L industrial hydrochloric acid to neutralize the solution until the pH...

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Abstract

The invention relates to the technical field of hydrometallurgy, in particular to a method for recovering germanium from coarse germanium dioxide by sodium chlorate oxidization arsenic removal and hydrochloric acid chlorination distillation. The process method for improving the chlorination distillation recovery rate of the coarse germanium dioxide recovers the germanium by a hydrochloric acid distillation method. The method is characterized in that: the process steps of sodium hydroxide dissolving and the sodium chlorate arsenic removal are added before the hydrochloric acid distillation; and by the process of the method, the recovery rate of the germanium can reach over 99.0 percent, the content of arsenic in produced germanium tetrachloride is below 10.0 ppm, the recovery rate of the germanium is 9.0 percent higher than that of the conventional hydrochloric acid direct distillation method, the content of the arsenic in the produced germanium tetrachloride is 10 to 15 percent lower than that of the conventional hydrochloric acid direct distillation method, and the distillate efficiency of the arsenic is below 1.0 percent. Processes such as rectification, hydrolyzation, precipitation, drying and the like are performed on the distilled germanium tetrachloride to produce high-purity germanium dioxide. The quality of the high-purity germanium dioxide produced by the process method meets the requirements of over 5N in national standard GB / in T11069.

Description

technical field [0001] The invention relates to the technical field of hydrometallurgy, in particular to a method for recovering germanium by chlorinating and distilling crude germanium dioxide with hydrochloric acid. Background technique [0002] Germanium dioxide has three crystal structures: hexagonal, amorphous and tetragonal. Hexagonal and amorphous germanium dioxide are easily soluble in hydrochloric acid, while tetragonal germanium dioxide is insoluble in hydrochloric acid. At present, in the process of producing high-purity germanium dioxide from crude germanium dioxide, the method of directly adopting hydrochloric acid chlorination distillation to recover germanium is usually due to the presence of 5-10% hydrochloric acid in the crude germanium dioxide produced from some raw materials Insoluble germanium, i.e. tetragonal germanium dioxide, so when using traditional direct hydrochloric acid distillation to produce high-purity germanium dioxide from crude germanium di...

Claims

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Application Information

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IPC IPC(8): C01G17/04
Inventor 普世坤何贵段鑫敏李振芬朱知国张云
Owner YUNNAN LINCANG XINYUAN GERMANIUM IND
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