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Process for reducing consumption of hydrochloric acid during chlorination distillation of germanium-containing raw material

A technology of chlorination distillation and process method, which is applied in the field of germanium recovery of germanium-containing raw materials, can solve the problems of increased consumption of quicklime, consumption of hydrochloric acid, and increased consumption of quicklime, and achieve the effect of reducing emissions and reducing consumption

Active Publication Date: 2011-07-13
YUNNAN LINCANG XINYUAN GERMANIUM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Our company's processing method for regenerated germanium raw materials is generally to use germanium peroxide hydroxide metal as germanium (Ⅳ) ions in lye, then evaporate and concentrate the liquid volume, and then use hydrochloric acid to distill and separate germanium. See our company Applied patent "Recovering germanium from germanium waste by wet method, patent number ZL 200610048818.6"; In addition to using germanium peroxide hydroxide metal as germanium (IV) ions in the lye, during the distillation process Also use manganese dioxide to carry out 2-3 times of chromium-germanium oxide method, see the patent applied by our company "recovering germanium from chromium-germanium alloy waste by wet method, patent number ZL 200610048817.1", these two types of processes are in During processing, due to the high content of germanium and the addition of alkali, the amount of hydrochloric acid required has reached more than 32 times the amount of germanium material, and a large amount of waste acid produced thereby has also increased the consumption of quick lime, which greatly increases the consumption of quick lime; for The soot and germanium concentrate extracted from coal also consume a lot of hydrochloric acid, and the consumption ratio of industrial hydrochloric acid to germanium concentrate reaches 8-12 times

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: in the pretreatment reactor of 500L, first add the water of 60L, then add 22.5kg sodium hydroxide, stir after sodium hydroxide is dissolved completely, drop into through being crushed to 15kg of germanium waste material more than 200 orders, The content of germanium is 92.51%, and the amount of germanium metal is 13.877kg. After stirring evenly, 90L of hydrogen peroxide with a mass fraction of 30% is introduced within 8 hours. After the oxidation reaction is 8 hours, the volume of the liquid is evaporated and concentrated to 50L; Transfer the final germanium raw material solution into a 500L distillation reactor, add 150kg of magnesium chloride, 250kg of industrial hydrochloric acid, open the steam and heat up to boiling, then carry out distillation. The distillation speed is 0.4-0.5L per minute, and the distillation time is 1.5h to obtain germanium tetrachloride. Metal 13.805kg, the yield from germanium waste to germanium tetrachloride is 99.49%. After th...

Embodiment 2

[0031]Embodiment 2: in the pretreatment reactor of 500L, first add the water of 120L, then add the sodium hydroxide of 24kg, after stirring makes sodium hydroxide dissolve completely, drop into 60kg of germanium concentrates through being pulverized to 200-400 purpose, The content of germanium is 8.48%, and the amount of germanium metal is 5.088kg. Stir evenly, heat to 80°C, and react for 1.5 hours. After heating to boiling and evaporating 60 liters of water, cool, and then transfer the solution into a 500L distillation reactor. Add 175kg of magnesium chloride, 250kg of industrial hydrochloric acid, turn on the steam and heat up to boiling, then carry out distillation. The distillation speed is controlled at 0.3-0.4 L / min, and the distillation time is 2.0h to obtain 4.987kg of germanium tetrachloride metal. From germanium waste to germanium tetrachloride The yield is 98.01%. After the distillation is over, after the reactor is cooled and warm, open the bottom valve of the reac...

Embodiment 3

[0032] Embodiment 3: in the pretreatment reactor of 500L, first add the water of 40L, then add the concentrated sulfuric acid that the mass percent concentration of 120kg is 98%, stir after making evenly dissolving completely, drop into germanium soot 120kg, germanium content is 3.16 %, the amount of germanium metal is 3.792kg, stir evenly, heat to 90-95°C, let it mature for 1.5h, after cooling, then transfer the solution into a 500L distillation reactor, add 200kg of magnesium chloride, 250kg of industrial hydrochloric acid, Turn on the steam and heat up to boiling, then carry out distillation, the distillation speed is 0.3-0.4L per minute, the distillation time is 2.0h, and 4.987kg of germanium tetrachloride metal is obtained, and the yield from germanium waste to germanium tetrachloride is 98.01%. After the distillation is over, after the reactor is cooled and warm, open the bottom valve of the reactor to release two-thirds of the distillation raffinate, leaving one-third of...

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Abstract

The invention relates to the technical field of hydrometallurgy, in particular to a method for recycling germanium from a germanium-containing raw material through the magnesium chloride-hydrochloric acid distillation method. The invention discloses a process for reducing the consumption of hydrochloric acid during the chlorination distillation of the germanium-containing raw material. The process is characterized in that after the germanium-containing raw material is pretreated, magnesium chloride is used to replace a part of industrial hydrochloric acid to react with the germanium-containing raw material, and a part of distillation residual liquid is recycled to distill. By adopting the two measures, the consumption of hydrochloric acid during the chlorination distillation of each germanium raw material can be greatly reduced and the consumption of quick lime for neutralizing the waste liquid can be greatly reduced. Therefore, the aim of reducing the production cost can be achieved.

Description

technical field [0001] The invention relates to the technical field of hydrometallurgy, in particular to a method for recovering germanium in germanium-containing raw materials by adopting a magnesium chloride-hydrochloric acid distillation method. Background technique [0002] The germanium-containing raw materials include two types of regenerated germanium raw materials and germanium concentrates. Among them, the regenerated germanium raw materials are recyclable germanium-containing raw materials generated from the production, processing and use of germanium, and the germanium concentrates are made from lead containing germanium. The by-products obtained when other metals are extracted from raw materials such as zinc ore, iron ore, and copper ore, or the germanium enrichment directly extracted from coal, these two types of germanium-containing raw materials are used as raw materials for the production of germanium tetrachloride. Our company's processing method for regener...

Claims

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Application Information

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IPC IPC(8): C22B3/04C22B3/20C22B41/00
CPCY02P10/20
Inventor 普世坤尹国文施昱鲁梅
Owner YUNNAN LINCANG XINYUAN GERMANIUM IND
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