Method for separating, enriching and recycling indium from low-concentration indium sulphate solution

A technology of separation and enrichment and indium sulfate, applied in the direction of improving process efficiency, etc., can solve the problems of unresolved chlorine-containing waste acid discharge, unsuitable for separation and recovery, etc., to reduce adverse effects, eliminate dispersion losses, and reduce production cost effect

Active Publication Date: 2015-11-04

KUNMING UNIV OF SCI & TECH

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[0003] The paper "Industrial Practice of Recovering Indium from Chlorinated Distillation Raffinate of Germanium Extraction" published in "Nonferrous Metallurgy of China" in 2011 disclosed a method of using TBP-P204 combined extraction process for recovering indium, but this process technology is only suitable for separating and recovering indium from hydrochloric acid solution, not suitable for separating and reco...

Abstract

The invention relates to a method for separating, enriching and recycling indium from a low-concentration indium sulphate solution, and belongs to the technical field of hydrometallurgy. The method comprises the following steps: firstly performing P204 extraction on the low-concentration indium sulphate solution, and then performing hydrochloric acid back extraction so as to obtain an indium chloride strip solution; performing TBP extraction on the obtained indium chloride strip solution; performing dilute sulphuric acid back extraction so as to obtain a high-concentration indium sulphate solution; and finally performing metal replacement on the high-concentration indium sulphate solution so as to obtain sponge indium. According to the method disclosed by the invention, the indium is obtained through back extraction of sulphuric acid in the end, the high-concentration indium sulphate solution is produced, the hydrochloric acid used in a middle process can be circularly used, so that the consumption of the hydrochloric acid is reduced, large-scale emission of chloride waste water can be avoided, and negative influences of chlorine ions on zinc hydrometallurgy electrodeposition operational procedures are reduced.

Application Domain

Process efficiency improvement

Technology Topic

IonHigh concentration +11

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Experimental program(5)

Example Embodiment

[0028] Example 1

[0029] like figure 1As shown, the method for separating, enriching and recovering indium from a low-concentration indium sulfate solution includes the following steps: firstly extracting the low-concentration indium sulfate solution with P204, and then using hydrochloric acid for back extraction to obtain an indium chloride back-extraction solution; The obtained indium chloride back-extraction solution is then extracted with TBP, and back-extracted with dilute sulfuric acid to obtain a high-concentration indium sulfate solution, and finally the high-concentration indium sulfate solution is replaced by metal to obtain sponge indium.

[0030] The specific steps are:

[0031] (1) P204 extraction: First, mix P204 and sulfonated kerosene with a volume ratio of 20:80 to obtain an organic phase, and then mix the low-concentration indium sulfate solution and the organic phase with a volume ratio of 2:1 into the box-type mixing and clarifying tank. Three-stage countercurrent extraction is carried out in the 50 °C temperature for 5 min, and the clarification time is 15 min after the extraction is completed to prepare the P204 indium-loaded organic phase and raffinate; the low-concentration indium sulfate solution includes the following components by mass percentage: indium The ion concentration is 120mg/L, the sulfuric acid concentration is 25g/L, the zinc ion concentration is 85g/L, the arsenic ion concentration is 0.2g/L, the divalent iron ion concentration is 30g/L, and the ferric ion concentration is 0.1g/L; The discharged raffinate contained 8.0 mg/L indium, and the indium extraction rate was 93.3%;

[0032] (2) Hydrochloric acid back extraction: The P204 indium-carrying organic phase prepared in step (1) and the 6mol/L hydrochloric acid solution were mixed uniformly in a mixing and clarification tank according to the volume ratio of 10:1 to carry out three-stage countercurrent back extraction, and then at temperature Back-extraction at 50°C for 10 minutes, and clarification time for 20 minutes after the back-extraction is completed, the indium chloride back-extraction solution and the P204-lean organic phase are prepared; the indium chloride back-extraction solution contains 2230 mg/L of indium, and the indium back-extraction rate is greater than 99%. %;

[0033] (3) TBP extraction: Mix TBP and sulfonated kerosene uniformly in a volume ratio of 40:60 to obtain an organic phase, and then mix the indium chloride back-extraction solution obtained in step (2) with the organic phase in a volume ratio of 4:1. Mix in the mixing and clarifying tank for two-stage countercurrent extraction, and then extract at a temperature of 35 °C for 8 minutes. After the extraction is completed, the clarification time is 20 minutes to prepare TBP indium-loaded organic phase and hydrochloric acid solution. The hydrochloric acid solution is returned to step (2) for use; hydrochloric acid The solution contains 275 mg/L of indium and 4.5 mol/L of hydrochloric acid;

[0034] (4) Dilute sulfuric acid stripping: The TBP indium-loaded organic phase prepared in step (3) was mixed with the 60g/L dilute sulfuric acid solution in a volume ratio of 8:1 in a mixing and clarifying tank for three-stage countercurrent stripping. The temperature was 32 °C for back extraction for 8 minutes, and the clarification time was 20 minutes after the back extraction was completed to prepare a high-concentration indium sulfate solution and a TBP-lean organic phase; The concentration ratio of indium in high-concentration indium sulfate solution and low-concentration indium sulfate solution) is 520.

[0035] (5) The high-concentration indium sulfate solution obtained in step (4) is replaced with a metal according to the solid-liquid ratio of 0.2:1 g/ml for 24 hours to obtain sponge indium, wherein the metal is zinc flakes, the replacement temperature is 60 ° C, and the pH value of the replacement end solution is is 2.0, and the mass percentage of indium in the obtained sponge indium is 82.2%.

Example Embodiment

[0036] Example 2

[0037] like figure 1 As shown, the method for separating, enriching and recovering indium from a low-concentration indium sulfate solution includes the following steps: firstly extracting the low-concentration indium sulfate solution with P204, and then using hydrochloric acid for back extraction to obtain an indium chloride back-extraction solution; The obtained indium chloride back-extraction solution is then extracted with TBP, and back-extracted with dilute sulfuric acid to obtain a high-concentration indium sulfate solution, and finally the high-concentration indium sulfate solution is replaced by metal to obtain sponge indium.

[0038] The specific steps are:

[0039] (1) P204 extraction: First, mix P204 and sulfonated kerosene with a volume ratio of 30:70 to obtain an organic phase, and then mix the low-concentration indium sulfate solution and the organic phase with a volume ratio of 2:1 into the box-type mixing and clarifying tank. Four-stage countercurrent extraction was carried out in the middle, extraction was performed at a temperature of 45 °C for 5 min, and the clarification time was 15 min after the extraction was completed to prepare the P204 indium-loaded organic phase and raffinate; the low-concentration indium sulfate solution included the following components by mass percentage: indium The ion concentration is 280mg/L, the sulfuric acid concentration is 15g/L, the zinc ion concentration is 95g/L, the arsenic ion concentration is 0.8g/L, the divalent iron ion concentration is 30g/L, and the ferric ion concentration is 0.1g/L; The discharged raffinate contains 15 mg/L of indium, and the indium extraction rate is 94.6%;

[0040] (2) Hydrochloric acid back extraction: The P204 indium-loaded organic phase prepared in step (1) and the 5mol/L hydrochloric acid solution were mixed uniformly in the mixing and clarifying tank according to the volume ratio of 8:1 to carry out three-stage countercurrent back extraction, and then at the temperature Back-extraction at 20 °C for 8 minutes, and clarification time for 20 minutes after the back-extraction is completed, the indium chloride back-extraction solution and the P204-lean organic phase are prepared; the indium chloride back-extraction solution contains 4200 mg/L of indium, and the indium back-extraction rate is greater than 99% %;

[0041] (3) TBP extraction: Mix TBP and sulfonated kerosene uniformly in a volume ratio of 30:70 to obtain an organic phase, and then mix the indium chloride back-extraction solution obtained in step (2) with the organic phase in a volume ratio of 3:1. Mix in the mixing and clarifying tank for two-stage countercurrent extraction, and then extract at a temperature of 35 ° C for 10 minutes. After the extraction is completed, the clarifying time is 20 minutes to prepare the TBP indium-loaded organic phase and hydrochloric acid solution. The hydrochloric acid solution is returned to step (2) for use; hydrochloric acid The solution contains 405 mg/L of indium and 3.8 mol/L of hydrochloric acid;

[0042] (4) Dilute sulfuric acid stripping: The TBP indium-loaded organic phase prepared in step (3) was mixed in a mixing and clarifying tank according to the volume ratio of 100g/L dilute sulfuric acid solution of 6:1 to carry out three-stage countercurrent stripping. The temperature was 32 °C for back extraction for 10 minutes, and the clarification time was 20 minutes after the back extraction was completed to prepare a high-concentration indium sulfate solution and a TBP-lean organic phase; The concentration ratio of indium in high-concentration indium sulfate solution and low-concentration indium sulfate solution) is 239.

[0043] (5) The high-concentration indium sulfate solution obtained in step (4) is replaced with metal according to the solid-liquid ratio of 0.3:1 g/ml for 24 hours to obtain sponge indium, wherein the metal is zinc flakes, the replacement temperature is 65 ° C, and the pH value of the replacement end point solution is is 2.5, and the mass percentage of indium in the obtained sponge indium is 79.8%.

Example Embodiment

[0044] Example 3

[0045] like figure 1 As shown, the method for separating, enriching and recovering indium from a low-concentration indium sulfate solution includes the following steps: firstly extracting the low-concentration indium sulfate solution with P204, and then using hydrochloric acid for back extraction to obtain an indium chloride back-extraction solution; The obtained indium chloride back-extraction solution is then extracted with TBP, and back-extracted with dilute sulfuric acid to obtain a high-concentration indium sulfate solution, and finally the high-concentration indium sulfate solution is replaced by metal to obtain sponge indium.

[0046] The specific steps are:

[0047] (1) P204 extraction: First, mix P204 and sulfonated kerosene with a volume ratio of 25:75 to obtain an organic phase, and then mix the low-concentration indium sulfate solution and the organic phase with a volume ratio of 2:1 into the box-type mixing and clarifying tank. Three-stage countercurrent extraction is carried out in the middle, extraction is performed at a temperature of 40 ° C for 5 minutes, and the clarification time is 15 minutes after the extraction is completed, and the P204 indium-loaded organic phase and raffinate are prepared; the low-concentration indium sulfate solution includes the following components by mass percentage: indium The ion concentration is 160mg/L, the sulfuric acid concentration is 20g/L, the zinc ion concentration is 72g/L, the arsenic ion concentration is 1.3g/L, the divalent iron ion concentration is 39g/L, and the ferric ion concentration is 0.1g/L; The discharged raffinate contains 9 mg/L of indium, and the indium extraction rate is 94.4%;

[0048] (2) Hydrochloric acid back extraction: The P204 indium-loaded organic phase prepared in step (1) and the 4mol/L hydrochloric acid solution were mixed uniformly in the mixing and clarifying tank according to the volume ratio of 10:1 to carry out three-stage countercurrent back extraction, and then at the temperature Back-extraction at 20°C for 8 minutes, and clarification time for 20 minutes after the back-extraction is completed, the indium chloride back-extraction solution and the P204-poor organic phase are prepared; the indium chloride back-extraction solution contains 3000 mg/L of indium, and the indium back-extraction rate is greater than 99% %;

[0049] (3) TBP extraction: Mix TBP and sulfonated kerosene uniformly in a volume ratio of 35:65 to obtain an organic phase, and then mix the indium chloride back-extraction solution obtained in step (2) with the organic phase in a volume ratio of 4:1. Mix in the mixing and clarifying tank for two-stage countercurrent extraction, and then extract at a temperature of 35 ° C for 10 minutes. After the extraction is completed, the clarifying time is 20 minutes to prepare the TBP indium-loaded organic phase and hydrochloric acid solution. The hydrochloric acid solution is returned to step (2) for use; hydrochloric acid The solution contains 350 mg/L of indium and 3.1 mol/L of hydrochloric acid;

[0050] (4) Dilute sulfuric acid stripping: The TBP indium-loaded organic phase prepared in step (3) was mixed in a mixing and clarifying tank in a volume ratio of 6:1 to a 40g/L dilute sulfuric acid solution for three-stage countercurrent stripping. The temperature was 30 °C for back extraction for 10 minutes, and the clarification time was 20 minutes after the back extraction was completed to prepare a high-concentration indium sulfate solution and a TBP-lean organic phase; The concentration ratio of indium in high-concentration indium sulfate solution and low-concentration indium sulfate solution) is 292.

[0051] (5) The high-concentration indium sulfate solution obtained in step (4) is replaced with metal according to the solid-liquid ratio of 0.1:1 g/ml for 24 hours to obtain sponge indium, wherein the metal is zinc flakes, the replacement temperature is 60 ° C, and the pH value of the replacement end point solution is is 2.5, and the mass percentage of indium in the obtained sponge indium is 78.5%.

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reduce consumption

Method for separating, enriching and recycling indium from low-concentration indium sulphate solution

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