Method for extracting germanium from chlorinated distillation slag

A technology of chlorinated distillation and alkali residue is applied in the field of germanium extraction, which can solve problems such as environmental pollution and waste of resources, and achieve the effects of reducing production cost, reducing the accumulation of waste residue and facilitating extraction.

Active Publication Date: 2009-04-29
YUNNAN LINCANG XINYUAN GERMANIUM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

During the storage of acid slag, it will cause environmental pollution and waste of resources

Method used

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  • Method for extracting germanium from chlorinated distillation slag
  • Method for extracting germanium from chlorinated distillation slag
  • Method for extracting germanium from chlorinated distillation slag

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Extract germanium from acid slag, carry out according to the following steps:

[0035] 1) Alkali leaching: add 25kg sodium hydroxide (alkali) to 100kg acid slag, add water (or the filtrate after sinking germanium), so that the solid-liquid ratio = 1:6, the concentration of sodium hydroxide is 5%, stir and heat, the temperature > 90°C, stir and leaching for 1 hour after reaching the temperature, carry out solid-liquid separation, desilicate the filtrate, and enter the alkali slag into the second alkali leaching;

[0036] 2) Secondary alkali leaching: 2000kg of alkali slag, 100kg of sodium hydroxide, and water to make the solid-liquid ratio = 1:6, the concentration of sodium hydroxide is 1.5%, stirring and heating, the temperature is > 90 ℃, stirring and leaching for 1 hour after the temperature reaches ; Carry out solid-liquid separation, filtrate and primary alkali immersion solution are combined to remove silicon, and the secondary alkali slag enters the production sys...

Embodiment 2

[0043] Extract germanium from acid slag, carry out according to the following steps:

[0044] 1) One-time alkaline leaching: add 30kg sodium hydroxide to 100kg acid slag, the concentration of sodium hydroxide is 8%, add water (or the filtrate after sinking germanium), make the solid-liquid ratio = 1:7, stir and heat, the temperature is > 90 ℃, After reaching the temperature, stir and leach for 1.5 hours, carry out solid-liquid separation, remove silicon from the filtrate, and enter the alkali slag into the second alkali leaching;

[0045] 2) Secondary alkali leaching: add 120kg of sodium hydroxide to 2000kg of alkali slag once, the concentration of sodium hydroxide is 2%, add water to make the solid-liquid ratio = 1:7, and the temperature is >90°C. liquid separation, the filtrate and the primary alkali immersion solution are combined to remove silicon, and the secondary alkali slag enters the germanium recovery production system by fire method;

[0046] 3) Removal of silicon:...

Embodiment 3

[0052] Extract germanium from calcium slag, carry out according to the following steps:

[0053] 1) Acid leaching: use hydrochloric acid (or waste hydrochloric acid after chlorination distillation), acid concentration = 4.5mol / L, add 150kg hydrochloric acid to 100kg calcium slag, add acid and heat to 80°C for 40 minutes, measure pH, keep pH2, acid should be added), add a solution containing 2000g of bone glue to remove silicon for 30 minutes, add water until solid: liquid = 1:6, carry out solid-liquid separation, and mix the liquid with the alkali immersion solution after silicon removal to precipitate germanium , the acid leaching residue enters an alkali leaching;

[0054] 2) Alkali leaching: once alkali leaching, 3000kg of acid leaching residue plus 250-280kg of sodium hydroxide, the alkali concentration is 8.3%, adding water (or the filtrate after sinking germanium) to make the solid-liquid ratio = 1:6, stirring and heating, the temperature >90°C, stir and leaching for 1 h...

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Abstract

The invention relates to a method for extracting germanium from chlorination distillation slag. The method comprises the following processes: primary alkaline leaching, secondary alkaline leaching, desiliconization, the alkaline leaching of silica residue, germanium precipitation, drying and ignition, chlorination and distillation, and the like. The germanium leaching efficiency is above 85 percent, the desiliconization rate is above 95 percent, the germanium precipitation rate is above 95 percent, and the recovery rate of germanium is above 70 percent. The method for extracting the germanium can annually process more than 2,000 tons of chlorination slag, recover more than 1 ton of germanium (by Ge in GeCl4), and obtain 4.5 million RMB of profit payment and tax turnover. The method solves the problems of the silicon germanium separation in alkaline liquid, germanium precipitation technology, and the like. The method opens up a reasonable path to extract the germanium from the chlorination distillation slag, reduces the piling amount of the waste slag, reasonably utilizes the resources, reduces the working time, and indirectly reduces the production cost. The cost of germanium precipitation is reduced from 695 RMB/kg Ge which is the cost of germanium precipitation through the prior tannin extract (high price) to 370 RMB/kg Ge.

Description

technical field [0001] The invention relates to the technical field of germanium extraction, in particular to a method for extracting germanium from chlorination distillation slag. Background technique [0002] The chlorination distillation residue is the waste residue produced in the chlorination production process of germanium, containing 0.1-0.8% of Ge. Although the acid slag contains high germanium grade, it also contains a large amount of chloride and silicon dioxide. At present, most smelters use blast furnaces, coal-fired earthen furnaces, and rotary kilns for fire recycling. Due to the low recovery rate of germanium, serious corrosion of equipment, and high processing costs, the recycling work has stopped and the acid slag has been piled up. With the expansion of production scale, the stockpiling of acid slag also increases. During the storage of acid slag, it will cause environmental pollution and waste of resources. Contents of the invention [0003] The purpo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B41/00
CPCY02P10/20
Inventor 张爱华包文东胡德才
Owner YUNNAN LINCANG XINYUAN GERMANIUM IND
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