Method for selectively extracting gallium and germanium from peracid lixivium containing gallium and germanium

A high acid leaching and selectivity technology, applied in the field of hydrometallurgy, can solve the problems of high environmental damage, consumption of reducing agent and high cost, and achieve the effects of reducing production cost, simplifying process and easy operation.

Active Publication Date: 2013-09-25
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

The disadvantages of these processes are: (1) germanium sinking from tannin and germanium extraction from chlorination distillation are harmful to the environment, the equipment requirements are harsh, and the price of tannin is high
(2) When P204 is extracted, the acid adjustment process needs to be carried out first. Since the leaching process needs to be controlled under high acid and high pressure to ensure a high leaching rate of gallium and germanium, the resulting leachate contains a large amount of free acid, which can generally reach 1-2mol / L, or even higher, so the acid adjustment process not only consumes a large amount of neutralizer, but also makes the acid in the leachate unable to be reused
(3) Before the extraction of tertiary carbon carboxylic acid, etc., the reduction process of iron is carried out, which consumes a large amount of reducing agent, and the conditions are not easy to control
In summary, the existing processes for extracting and recovering gallium and germanium from high-acid leaching solutions containing gallium and germanium generally have disadvantages such as harsh equipment, high cost, and difficult operation.

Method used

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  • Method for selectively extracting gallium and germanium from peracid lixivium containing gallium and germanium
  • Method for selectively extracting gallium and germanium from peracid lixivium containing gallium and germanium
  • Method for selectively extracting gallium and germanium from peracid lixivium containing gallium and germanium

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] according to figure 1 The process flow is operated;

[0059] The feed liquid is a simulated industrial feed liquid, containing gallium 0.2042g / L, germanium 0.2468g / L, free acid concentration 2.3mol / L, sulfuric acid system;

[0060] The organic phase is 20% oxime chelating extractant + 80% sulfonated kerosene;

[0061] A separatory funnel was used for single-stage extraction, the extraction ratio was O / A=1:1, the extraction time was 20 min, the temperature was 25°C, and the phase separation time was 1 min. The results are shown in Table 1.

[0062] Table 1 Extraction Process Separation Results

[0063] Element

[0064] The results in Table 1 show that the single-stage extraction rate of germanium in the extraction process can reach 79.1666%, only a small amount of Cu is extracted, and Ga, Fe, Cu, Zn, Al, As, Cd, etc. are almost not extracted.

Embodiment 2

[0066] according to figure 1 The process flow is operated;

[0067] The feed liquid is a simulated industrial feed liquid, containing gallium 0.2042g / L, germanium 0.2468g / L, free acid concentration 2.3mol / L, sulfuric acid system;

[0068] The organic phase is different proportions of oxime chelating extractant + sulfonated kerosene (volume fraction)

[0069] A separatory funnel was used for single-stage extraction, the extraction ratio was O / A=1:1, the extraction time was 20 minutes, the temperature was 25°C, and the phase separation time was 1 minute. The results are shown in Table 2.

[0070] The impact of different extractant concentrations in table 2 on the extraction

[0071] Extractant concentration (%)

[0072] The results in Table 2 show that the organic phase is 30% oxime chelating extractant+70% sulfonated kerosene, and the extraction rate of germanium above 93% can be obtained.

Embodiment 3

[0074] according to figure 1 The process flow is operated;

[0075] The feed liquid is a simulated industrial feed liquid, containing gallium 0.2042g / L, germanium 0.3247g / L, hydrochloric acid system;

[0076] The organic phase is 30% oxime chelating extractant + 70% sulfonated kerosene (volume fraction)

[0077] A separatory funnel was used for single-stage extraction, the extraction ratio was O / A=1:1, the extraction time was 15 minutes, the temperature was 25°C, and the phase separation time was 1 minute. The results are shown in Table 3.

[0078] Table 3 Effects of different feed liquid free acid concentrations on extraction

[0079] Free acid concentration (mol / L)

[0080] The results in Table 3 show that when the free acidity is 1.0-4.5mol / L, the extraction rate of Ge reaches more than 80%, and as the acidity increases, the extraction rate tends to increase; at the same time, other impurities are hardly extracted, and only a small amount of co-extraction The e...

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Abstract

The invention discloses a method for selectively extracting gallium and germanium from peracid lixivium containing gallium and germanium. The method comprises the following steps of: performing liquid-liquid extraction I on the peracid lixivium containing gallium and germanium by an oxime chelate extracting agent, and performing reverse extraction on a loading organic phase obtained from liquid-liquid extraction I by a sodium hydroxide solution to obtain a sodium germanate solution; adding an adjustor to raffinate obtained from liquid-liquid extraction I for adjusting, and performing liquid-liquid extraction II on the adjusted raffinate by phosphate or a phosphate extracting agent; and performing reverse extraction II on a loading organic phase obtained from liquid-liquid extraction II by a sulfuric acid solution to obtain a gallium sulfate solution, or washing the loading organic phase obtained from liquid-liquid extraction II by hydrochloric acid, and then, performing reverse extraction II on the washed organic phase by a sulfuric acid solution to obtain a gallium sulfate solution. The method selectively and efficiently extracts and separates gallium and germanium from the peracid lixivium containing gallium and germanium by the oxime chelate extracting agent and the phosphate or phosphate extracting agent. The extraction recovery rate of germanium is up to 98% and that of gallium is up to 99%. The method disclosed by the invention is simple in process and low in cost, and industrialization is easy to realize.

Description

technical field [0001] The invention relates to a method for selectively extracting gallium and germanium from a high-acid leach solution containing gallium and germanium, which belongs to the field of hydrometallurgy. Background technique [0002] Gallium and germanium are important scattered metals, which play an important role in the fields of national defense, aerospace, energy and communication, and mainly exist in the form of associated deposits, among which bauxite, lead-zinc ore, coal and iron ore are common Associated resources of germanium. [0003] The recovery and extraction methods for gallium and germanium mainly include: chlorination distillation, electrolysis, ion exchange, resin adsorption, tannin, and extraction. Among them, the chlorination distillation method and the tannin method have high requirements on equipment and harsh environment; the efficiency of the electrolysis method is low, and the ion exchange method and resin adsorption method need to con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/30C22B3/38C22B41/00C22B58/00
CPCY02P10/20
Inventor 曹佐英张魁芳曾理肖连生张贵清李青刚王超
Owner CENT SOUTH UNIV
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