Regeneration utilization method of germanium in infrared chalcogenide glass waste material

A technology for chalcogenide glass and waste, which is applied in the field of recycling and comprehensive utilization of waste resources, and achieves the effects of low production cost, short production cycle and easy operation.

Pending Publication Date: 2019-02-26
YUNNAN KIRO CH PHOTONICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no relevant literature report on the technical method of recovering germanium from infrared chalcogenide glass waste with complex components and different grades

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The germanium content is 15.75%, and the infrared chalcogenide glass grinding waste whose main elements are composed of Ge, As, Se, Sb is dried, crushed, and ball-milled until the powder particle size is less than 100 μm, and 50 kg of the ground chalcogenide glass grinding waste is weighed, Add 30.4kg industrial pure sodium hydroxide, stir evenly, obtain mixed raw material. In a 500L distillation reactor, add 150L of industrial pure hydrogen peroxide solution with a mass percentage concentration of 27.5%. Under stirring conditions, add uniformly stirred mixed raw materials into the distillation reactor in 4 batches, and add the first batch of 10kg, add the second batch of 15kg after stirring for 30 minutes, add the third batch of 20kg after stirring for 15 minutes, add the fourth batch of 20kg after stirring for 10 minutes. Continue to stir and heat with steam until there are no more bubbles, open the chlorine gas valve to feed chlorine gas, the flow rate is 5.0L / h, and...

Embodiment 2

[0036]The germanium content is 12.85%, and the infrared chalcogenide glass grinding waste whose main elements are Ge, Sb, Se, As is dried, crushed, and ball-milled until the powder particle size is less than 150 μm, and 70 kg of the ground chalcogenide glass grinding waste is weighed, Add 18.6kg industrial pure sodium hydroxide, stir evenly, obtain mixed raw material. In a 1000L distillation reactor, add 200L of industrial pure hydrogen peroxide solution with a mass percentage concentration of 35%. Under the condition of stirring, add the uniformly stirred mixed raw materials into the distillation reactor in 4 batches, and add the first batch of 15kg, add the second batch of 15kg after stirring for 30 minutes, add the third batch of 20kg after stirring for 15 minutes, add the fourth batch of 20kg after stirring for 10 minutes. Continue to stir and heat with steam until there are no more bubbles, open the chlorine gas valve to feed chlorine gas at a flow rate of 15.0 L / h, and t...

Embodiment 3

[0038] The germanium content is 3.40%, and the infrared chalcogenide glass grinding waste whose main elements are Ge, As, Sb, Se, Si, S, Te is dried, crushed, and ball-milled until the powder particle size is less than 200 μm, and 150 kg of the ground powder is weighed Chalcogenide glass waste, add 9.2kg industrial pure sodium hydroxide, stir evenly, obtain mixed raw material. In a 1000L distillation reactor, add 280L of industrial pure hydrogen peroxide solution with a mass percentage concentration of 27.5%. Under stirring conditions, add the uniformly stirred mixed raw materials into the distillation reactor in 5 batches, and add the first batch of 20kg, add the second batch of 25kg after stirring for 20 minutes, add the third batch of 30kg after stirring for 20 minutes, add the fourth batch of 35kg after stirring for 10 minutes, add the fourth batch of 40kg after stirring for 10 minutes. Continue to stir and heat with steam until no more bubbles are generated, open the chlo...

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Abstract

The invention more specifically relates to a regeneration utilization method of germanium in infrared chalcogenide glass waste material. According to the regeneration utilization method of germanium in infrared chalcogenide glass waste material, germanium is extracted from infrared chalcogenide glass waste material, and the method principles are that: the oxidation performance of H2O2 is adopted to destroy Ge-Se, Ge-As, Ge-Sb bonds in infrared chalcogenide glass waste material, germanium is oxidized into GeO, a single GeO layer is formed on the surface, GeO is oxidized into GeO2, GeO2 is dissolved in water to form germanic acid; when an obtained solution contains an alkali, germanic acid is reacted with the alkali to produce sodium germinate, so that germanium dissolving is accelerated; concentrated sulfuric acid is adopted to neutralize excess sodium hydroxide solution and adjust and control the concentration of hydrogen ions in the solution; FeCl3 is adopted to oxidize As<3+> into As<6+>, and sufficienct chloride ions are provided; concentrated hydrochloric acid is adopted for distillation of germanium tetrachloride from the solution, and AsCl6 is left in a distillation raffinate; the germanium tetrachloride obtained through distillation is subjected to traditional technology including secondary distillation, rectification, hydrolysis, reduction, and zone melting so as to obtain high purity zone-refined germanium ingot.

Description

technical field [0001] The invention belongs to the technical field of comprehensive utilization and recycling of waste resources, and in particular relates to a method for recycling germanium in infrared chalcogenide glass waste. Background technique [0002] Infrared chalcogenide glass has many excellent optical and thermal properties, and is currently one of the best candidate materials to replace germanium in the optical system of thermal imagers. With the development of science and technology and the advancement of infrared technology, the application of infrared chalcogenide glass materials as optical components in civilian night vision devices and thermal imaging systems is increasing day by day. At present, the commonly used germanium-containing infrared chalcogenide glasses mainly include Ge28Sb12Se60, Ge33As12Se55, Ge20Sb15Se65, Ge33As12Se55, etc. These chalcogenide glass materials in the preparation process of the head and tail cuttings, unqualified products, scr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B41/00
CPCC22B41/00Y02P10/20
Inventor 吴绍华王珂木锐李睿茹秋旭张二平姚杨南曲哲郭晨宇李茂忠姜杰
Owner YUNNAN KIRO CH PHOTONICS
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