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Method for recovering germanium in lignite smoke

A soot and lignite technology, which is applied in the field of resource utilization and industrial waste treatment, can solve the problems of long reaction time, waste acid generation, complicated process, etc., and achieve the effect of long reaction time, low recovery rate and clean treatment process

Inactive Publication Date: 2015-09-16
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It adopts complete hydrometallurgical technology, the reaction time is long, the process is complicated, waste acid is produced, and waste water is more

Method used

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  • Method for recovering germanium in lignite smoke
  • Method for recovering germanium in lignite smoke
  • Method for recovering germanium in lignite smoke

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] First place lignite dust and 5wt% coke in a vacuum furnace, then maintain the vacuum in the furnace below 0.1Pa, and keep the temperature at 1000°C, heat for 40 minutes to make it fully react, and the tail gas generated during the vacuum reduction process Pass through the gas discharge channel, and discharge after purification treatment; vacuum reduction reaction obtains germanium metal and its oxide with a recovery rate of 95.30%. Then through the chlorination distillation process, the chloride GeCl of germanium is obtained 4 , followed by hydrolysis and H 2 After reduction treatment, metallic germanium with a purity of more than 90% is obtained.

Embodiment 2

[0048] First place lignite dust and 15wt% coke in a vacuum furnace, then maintain the vacuum in the furnace below 10Pa, and keep the temperature at 1200°C for 40 minutes to fully react, and the tail gas generated during the vacuum reduction process passes through The gas is discharged from the channel and discharged after purification treatment; the vacuum reduction reaction obtains germanium metal and its oxide with a recovery rate of 96.48%. Then through the chlorination distillation process, the chloride GeCl of germanium is obtained 4 , followed by hydrolysis and H 2 After reduction treatment, metallic germanium with a purity of more than 90% is obtained.

Embodiment 3

[0050] First place lignite dust and 25wt% coke in a vacuum furnace, then maintain the vacuum in the furnace below 0.01Pa, and keep the temperature at 900°C, heat for 60 minutes to make it fully react, and the tail gas generated during the vacuum reduction process Pass through the gas discharge channel and discharge after purification treatment; the vacuum reduction reaction obtains germanium metal and its oxide with a recovery rate of 90.12%. Then through the chlorination distillation process, the chloride GeCl of germanium is obtained 4 , followed by hydrolysis and H 2 After reduction treatment, metallic germanium with a purity of more than 90% is obtained.

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Abstract

The invention discloses a method for recovering germanium in lignite smoke by virtue of a vacuum reduction-chlorination distillation technology. The method comprises the following steps: firstly, placing the lignite smoke and 5-25wt% of coke in a vacuum heating furnace, and carrying out a vacuum reduction reaction at 800-1000 DEG C to obtain a product containing metal Ge, GeO and some impurities, for example, the condensation product of As2O3; secondly, carrying out chlorination distillation on the condensation product to obtain pure GeCl4 with a purity of more than 90%; thirdly, carrying out a hydrolysis reaction on GeCl4 to obtain pure GeO2; finally, carrying out the reaction of reducing the pure GeO2 by H2 to obtain metal Ge with a purity of more than 90%. The method achieves the recovery rates of 90% or above respectively, has the characteristics of being efficient, environment-friendly and high in recycling degree, and is suitable for large-scale industrialized applications.

Description

technical field [0001] The invention relates to a method for recovering germanium in lignite dust by using vacuum reduction-chlorination distillation technology, which is an environmentally friendly and efficient method for recovering germanium in lignite dust. The invention belongs to the field of industrial waste treatment and recycling in the technical field of environmental protection. Background technique [0002] Germanium, as a rare metal, has been widely used in semiconductor, electronic and optical devices. Many countries also regard germanium as a strategic reserve metal. According to the distribution of germanium application fields, the global use of germanium is mainly in optical fiber, infrared equipment and chemical catalysts, accounting for 30%, 22% and 34% respectively. However, as the use of germanium continues to increase, germanium resources are very scarce worldwide. The global germanium reserves are only 8,600 tons, which is only 1 / 10 of the gold rese...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/02C22B41/00
CPCY02P10/20
Inventor 许振明张灵恩
Owner SHANGHAI JIAO TONG UNIV
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