Method for recovering indium-containing alloy from indium-containing silicon material and indium-containing alloy

By adding bone glue and high carbon alcohol during the enrichment and extraction process of indium, the influence of silica on indium extraction rate is solved, and the effect of improving indium extraction rate and recovery efficiency is achieved.

CN119614907APending Publication Date: 2025-03-14XIANDAO THIN FILM MATERIALS GUANGDONG CO LTD
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Patent Information

Application Number
CN202411843459.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-14
Publication Date
2025-03-14

AI Technical Summary

Technical Problem

During the enrichment and extraction process of indium, the presence of silica leads to colloids that are not easy to filter, affecting the extraction rate and recovery quality of indium.

Method used

Add bone glue to the indium-containing ion filtrate and add it with high carbon alcohol and P204 during the extraction process to stabilize the extraction system, adsorb silica and reduce its impact on the extraction effect.

Benefits of technology

It effectively improves the extraction rate of indium, reduces the content of silicon ions in the indium chloride solution, reduces the recovery amount of silicon, and improves the recovery efficiency of indium.

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Abstract

The invention belongs to the field of scattered metal recovery, and discloses a method for recovering an indium-containing alloy from an indium-containing silicon material, which comprises the following steps of: crushing an indium-containing adhesive tape, putting the crushed indium-containing adhesive tape into a vacuum tube furnace, heating, decomposing, cooling, grinding and sieving to obtain indium-containing powder; adding indium-containing powder into a sulfuric acid solution, stirring, adding an additive, standing, and filtering to obtain indium ion-containing filtrate; then adding into an organic extraction agent for extraction to obtain an indium-containing organic phase; and finally, adding a hydrochloric acid solution, stirring, standing to obtain an indium chloride solution, adding excessive alkali into the indium chloride solution to enable the pH value of the solution to be greater than 3, filtering, carrying out primary calcination on the solid, introducing hydrogen, and carrying out secondary calcination to obtain the indium-containing alloy. The extraction rate of indium can be effectively increased by extracting the indium ion-containing filtrate after bone glue treatment by using an extraction agent consisting of P204, TBP and sulfonated kerosene; in addition, the invention further provides the indium-containing alloy which is prepared through the method for recycling the indium-containing alloy from the indium-silicon-containing material.
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Description

Technical Field

[0001] The invention relates to the field of rare metal recovery, and in particular to a method for recovering an indium-containing alloy from an indium-containing silicon material and an indium-containing alloy. Background Art

[0002] Indium is a typical rare metal, which is mainly obtained by enrichment and extraction from mineral raw materials, smelting byproducts or industrial waste. In the process of enriching and extracting indium-containing alloys, due to the addition of mineral associations, smelting auxiliary materials or slag produced by smelting, silica will be contained in the extraction process. Especially when extraction is used, silica is easy to form a colloid that is difficult to filter in an acidic solution. This colloidal silica is not only difficult to remove by conventional filtration and other methods, but also dispersed in the solution, affecting the subsequent process operation and the recovery quality of indium, and reducing the extraction rate of indium.

[0003] Chinese patent application 201310029344.0 discloses a pretreatment method for indium-containing zinc oxide acid supernatant. By adding bone glue to the solution, silica in the solution can be adsorbed. However, the silica cannot be completely removed by adsorption using only bone glue. Some silica still exists in the pre-extraction solution, which will affect the extraction rate of indium.

[0004] Through experiments, it was found that the use of bone glue before extraction can absorb silica in the pre-extraction liquid, and combined with high-carbon alcohols during the extraction process to further stabilize the extraction system, which can increase the extraction rate of indium.

[0005] The problem that this solution needs to solve is: how to provide a method for recovering indium with a low silicon content. Summary of the invention

[0006] The purpose of the present invention is to propose a method for recovering indium-containing alloys from indium-containing silicon materials. By adding bone glue to the indium ion filtrate and adding high-carbon alcohols together with P204 during the extraction process, the extraction system can be stabilized and the extraction efficiency of indium in the indium-containing solution can be effectively improved.

[0007] To achieve the above object, the present application discloses a method for recovering indium-containing alloy from indium-containing silicon material, comprising the following steps:

[0008] Step 1: adding an indium-containing silicon material into an acidic solution to dissolve and filter to obtain an indium-containing filtrate;

[0009] Step 2: adding an organic extractant to the indium ion-containing filtrate for extraction to obtain an indium-containing organic phase and a raffinate;

[0010] Step 3: adding a hydrochloric acid solution to the indium-containing organic phase for stripping to obtain an indium chloride solution, then adding an alkaline solution to the indium chloride solution to make the pH value of the solution greater than 3, filtering to obtain an indium hydroxide precipitate;

[0011] Step 4: calcining the indium hydroxide precipitate once to obtain indium oxide, and then calcining the indium oxide twice in a reducing gas atmosphere to obtain an indium-containing alloy;

[0012] The acidic solution in step 1 further comprises bone glue;

[0013] The organic extractant in step 2 is composed of P204, high carbon alcohol and sulfonated kerosene.

[0014] In the process of dissolving the indium-containing silicon material, according to the initial pH of indium ion precipitation known to those skilled in the art, the pH value of the acidic solution should be less than or equal to 3.2 to ensure that the indium in the indium-containing silicon material is completely dissolved in the solution in the form of ions;

[0015] During the extraction process, the presence of silica will lead to the generation of a third phase between the oil phase and the water phase, affecting the extraction rate of indium. The pre-extraction solution is treated with bone glue, which can adsorb silica and reduce the content of silica in the pre-extraction solution. Then, by adding high-carbon alcohols and performing extraction simultaneously with the extractant, the extraction system can be stabilized, further avoiding the influence of silica on the extraction effect, reducing the content of silicon ions in the indium chloride solution, and improving the extraction rate of indium.

[0016] In the technical solution of the present invention, the indium-containing silicon material can directly use the indium-containing silicon waste obtained in the indium extraction process or the indium-containing silicon waste purchased from outside.

[0017] Preferably, the indium-silicon-containing material is obtained by crushing, thermal decomposition and grinding in sequence;

[0018] More preferably, the specific operation of the thermal decomposition is: placing the crushed indium silicon-containing material into a vacuum tube furnace, and performing thermal decomposition for 6 hours at 300-600°C and a nitrogen filling flow rate of 5L / min; during the process, the vacuum tube furnace is connected to a VOC burner.

[0019] More preferably, the pH of the indium ion-containing filtrate is less than or equal to 2.

[0020] Preferably, the acidic solution is selected from at least one of an aqueous solution of sulfuric acid, an aqueous solution of hydrochloric acid, and an aqueous solution of nitric acid.

[0021] Further preferably, the acidic solution is an aqueous solution of sulfuric acid, and step 1 specifically comprises: adding the indium silicon-containing material to an aqueous solution of sulfuric acid containing gelatin, stirring, standing, and filtering to obtain an indium ion-containing filtrate having a pH less than or equal to 2;

[0022] The mass ratio of the indium silicon-containing material to the sulfuric acid aqueous solution is 1:4-6;

[0023] The concentration of sulfuric acid in the aqueous solution of sulfuric acid is 160 g / L, and the concentration of bone glue is 0.1-0.2 g / L.

[0024] Preferably, the volume ratio of P204, higher alcohol, and sulfonated kerosene in the organic extractant is 5-20:5-10:70-90;

[0025] High carbon alcohol is C 18 ~C 20 One of the alcohols.

[0026] Preferably, in step 2, the O / A volume ratio of the organic extractant to the indium ion-containing filtrate is 5 to 10:1.

[0027] Preferably, in step 3, the O / A volume ratio of the indium-containing organic phase to the hydrochloric acid solution is 10 to 15:1;

[0028] The concentration of hydrochloric acid in the hydrochloric acid solution is 2 to 4 mol / L;

[0029] The alkaline solution is an aqueous solution with a sodium hydroxide concentration of 40 to 50 g / L.

[0030] In addition, an indium-containing alloy is also disclosed. The alloy is prepared by the method for recovering the indium-containing alloy from the indium-containing silicon material described above, and the silicon content in the indium-containing alloy is not higher than 0.01%.

[0031] The beneficial effects of the present invention are:

[0032] The invention provides a method for recovering an indium-containing alloy from an indium-containing silicon material. The method comprises the following steps: adding bone glue to an acidic solution, adsorbing silicon dioxide while the indium-containing silicon material is dissolved, and adding a high-carbon alcohol and an extractant during the extraction process to perform extraction simultaneously. The extraction system can be stabilized, the influence of silicon dioxide on the extraction effect can be further avoided, the content of silicon ions in an indium chloride solution can be reduced, and the extraction rate of indium can be improved. DETAILED DESCRIPTION

[0033] In the description of the present invention, it should be noted that, if the specific conditions are not specified in the examples, the experiments were carried out according to conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments used, if the manufacturer is not specified, are all conventional products that can be purchased commercially.

[0034] Example 1

[0035] Step 1: 10 kg of indium-silicon-containing material (after testing, the mass of indium element is 10093 ppm of the total mass of indium-silicon-containing material, and the mass of silicon element is 5742 ppm of the total mass of indium-silicon-containing material) and a sulfuric acid aqueous solution containing 0.15 g / L bone glue are mixed and stirred at a mass ratio of 1:5 for 3 hours, allowed to stand for 1 hour, and filtered to obtain an indium ion filtrate with a pH of 2.5±0.2;

[0036] The concentration of sulfuric acid in the sulfuric acid aqueous solution is 160 g / L, and concentrated sulfuric acid needs to be added during the stirring and standing process to keep the pH of the sulfuric acid aqueous solution at 2.5±0.2;

[0037] Step 2: adding an organic extractant to the indium ion-containing filtrate for extraction, and the O / A volume ratio of the organic extractant to the indium ion-containing filtrate is 7.5:1, to obtain an indium-containing organic phase and a raffinate;

[0038] Step 3: adding a hydrochloric acid solution with a hydrochloric acid concentration of 3 mol / L to the indium-containing organic phase for back extraction, and the O / A volume ratio of the indium-containing organic phase to the hydrochloric acid solution is 13:1, to obtain an indium chloride solution, and then adding an aqueous solution with a sodium hydroxide concentration of 45 g / L to the indium chloride solution to make the solution pH = 3.5±0.2, filtering to obtain an indium hydroxide precipitate;

[0039] Step 4: The indium hydroxide precipitate is heated to 500° C. in an air atmosphere and calcined for 5 h to obtain indium oxide, and then the indium oxide is placed in a hydrogen atmosphere and heated to 700° C. and calcined for 7 h to obtain 200 g of indium-containing alloy (after testing, the mass of indium element is 488602 ppm of the mass of the indium-containing alloy, and the mass of silicon element is 30 ppm of the mass of the indium-containing alloy);

[0040] The organic extractant is composed of P204, octadecyl alcohol and sulfonated kerosene, and the volume ratio of P204, octadecyl alcohol and sulfonated kerosene is 12:8:80.

[0041] Example 2

[0042] Step 1: 10 kg of indium-silicon-containing material (after testing, the mass of indium element is 9820 ppm of the total mass of indium-silicon-containing material, and the mass of silicon element is 5800 ppm of the total mass of indium-silicon-containing material) and a sulfuric acid aqueous solution containing 0.15 g / L bone glue are mixed and stirred at a mass ratio of 1:6 for 2 h, allowed to stand for 1.5 h, filtered, and filtered to obtain an indium ion filtrate with a pH of 2.5±0.2;

[0043] The concentration of sulfuric acid in the sulfuric acid aqueous solution is 160 g / L, and concentrated sulfuric acid needs to be added during the stirring and standing process to keep the pH of the sulfuric acid aqueous solution at 2.5±0.2;

[0044] Step 2: adding an organic extractant to the indium ion-containing filtrate for extraction, and the O / A volume ratio of the organic extractant to the indium ion-containing filtrate is 5:1, to obtain an indium-containing organic phase and a raffinate;

[0045] Step 3: adding a hydrochloric acid solution with a hydrochloric acid concentration of 2 mol / L to the indium-containing organic phase for back extraction, and the O / A volume ratio of the indium-containing organic phase to the hydrochloric acid solution is 10:1, to obtain an indium chloride solution, and then adding an aqueous solution with a sodium hydroxide concentration of 45 g / L to the indium chloride solution to make the solution pH = 3.5±0.2, filtering to obtain an indium hydroxide precipitate;

[0046] Step 4: The indium hydroxide precipitate is heated to 400° C. in an air atmosphere and calcined for 6 h to obtain indium oxide, and then the indium oxide is placed in a hydrogen atmosphere and heated to 600° C. and calcined for 8 h to obtain 183 g of indium-containing alloy (after testing, the mass of indium element is 507259 ppm of the mass of the indium-containing alloy, and the mass of silicon element is 50 ppm of the mass of the indium-containing alloy);

[0047] The organic extractant is composed of P204, octadecyl alcohol and sulfonated kerosene, and the volume ratio of P204, octadecyl alcohol and sulfonated kerosene is 12:8:80.

[0048] Example 3

[0049] Step 1: 10 kg of indium-silicon-containing material (after testing, the mass of indium element is 10302 ppm of the total mass of indium-silicon-containing material, and the mass of silicon element is 5866 ppm of the total mass of indium-silicon-containing material) and a sulfuric acid aqueous solution containing 0.15 g / L bone glue are mixed in a mass ratio of 1:4, stirred for 4 hours, allowed to stand for 0.5 hours, and filtered to obtain an indium ion filtrate with a pH of 2.5±0.2;

[0050] The concentration of sulfuric acid in the sulfuric acid aqueous solution is 160 g / L, and concentrated sulfuric acid needs to be added during the stirring and standing process to keep the pH of the sulfuric acid aqueous solution at 2.5±0.2;

[0051] Step 2: adding an organic extractant to the indium ion-containing filtrate for extraction, and the O / A volume ratio of the organic extractant to the indium ion-containing filtrate is 10:1, to obtain an indium-containing organic phase and a raffinate;

[0052] Step 3: adding a hydrochloric acid solution with a hydrochloric acid concentration of 4 mol / L to the indium-containing organic phase for back extraction, and the O / A volume ratio of the indium-containing organic phase to the hydrochloric acid solution is 15:1, to obtain an indium chloride solution, and then adding an aqueous solution with a sodium hydroxide concentration of 45 g / L to the indium chloride solution to make the solution pH = 3.5 ± 0.2, filtering to obtain an indium hydroxide precipitate;

[0053] Step 4: The indium hydroxide precipitate is heated to 600° C. in an air atmosphere and calcined for 4 h to obtain indium oxide, and then the indium oxide is placed in a hydrogen atmosphere and heated to 800° C. and calcined for 6 h to obtain 213 g of indium-containing alloy (after testing, the mass of indium element is 456045 ppm of the mass of the indium-containing alloy, and the mass of silicon element is 50 ppm of the mass of the indium-containing alloy);

[0054] The organic extractant is composed of P204, octadecyl alcohol and sulfonated kerosene, and the volume ratio of P204, octadecyl alcohol and sulfonated kerosene is 12:8:80.

[0055] Example 4

[0056] The method is substantially the same as Example 1, except that the concentration of bone glue in the sulfuric acid solution is 0.1 g / L;

[0057] In the indium silicon-containing material, the mass of the indium element is detected to be 10223ppm of the total mass of the indium silicon-containing material, and the mass of the silicon element is 5730ppm of the total mass of the indium silicon-containing material;

[0058] In step 4, 197 g of indium-containing alloy is obtained. After testing, the mass of indium element is 483231 ppm of the mass of the indium-containing alloy, and the mass of silicon element is 60 ppm of the mass of the indium-containing alloy.

[0059] Example 5

[0060] The method is substantially the same as Example 1, except that the concentration of bone glue in the sulfuric acid solution is 0.2 g / L;

[0061] In the indium silicon-containing material, the mass of the indium element is detected to be 10075ppm of the total mass of the indium silicon-containing material, and the mass of the silicon element is detected to be 5729ppm of the total mass of the indium silicon-containing material;

[0062] In step 4, 198 g of indium-containing alloy is obtained. After testing, the mass of indium element is 477647 ppm of the mass of the indium-containing alloy, and the mass of silicon element is 62 ppm of the mass of the indium-containing alloy.

[0063] Example 6

[0064] The method is basically the same as Example 1, except that the organic extractant is composed of P204, octadecanol, and sulfonated kerosene, and the volume ratio of P204, octadecanol, and sulfonated kerosene is 5:10:70;

[0065] In the indium silicon-containing material, the mass of the indium element is detected to be 9783ppm of the total mass of the indium silicon-containing material, and the mass of the silicon element is 5750ppm of the total mass of the indium silicon-containing material;

[0066] In step 4, 198 g of indium-containing alloy is obtained. After testing, the mass of indium element is 461135 ppm of the mass of the indium-containing alloy, and the mass of silicon element is 62 ppm of the mass of the indium-containing alloy.

[0067] Example 7

[0068] The method is basically the same as Example 1, except that the organic extractant is composed of P204, octadecanol, and sulfonated kerosene, and the volume ratio of P204, octadecanol, and sulfonated kerosene is 20:5:90;

[0069] In the indium silicon-containing material, the mass of the indium element is detected to be 9835ppm of the total mass of the indium silicon-containing material, and the mass of the silicon element is detected to be 5834ppm of the total mass of the indium silicon-containing material;

[0070] In step 4, 199 g of indium-containing alloy is obtained. After testing, the mass of indium element is 464815 ppm of the mass of the indium-containing alloy, and the mass of silicon element is 54 ppm of the mass of the indium-containing alloy.

[0071] Example 8

[0072] The method is basically the same as Example 1, except that, in step 1, concentrated sulfuric acid is added during the stirring and standing process to make the pH of the indium ion-containing filtrate be 1.5±0.2;

[0073] In the indium silicon-containing material, the mass of the indium element is detected to be 10764ppm of the total mass of the indium silicon-containing material, and the mass of the silicon element is detected to be 5716ppm of the total mass of the indium silicon-containing material;

[0074] In step 4, 210 g of indium-containing alloy is obtained. After testing, the mass of indium element is 499398 ppm of the mass of the indium-containing alloy, and the mass of silicon element is 10 ppm of the mass of the indium-containing alloy.

[0075] Comparative Example 1

[0076] The method is substantially the same as Example 1, except that the aqueous sulfuric acid solution does not contain gelatin, and the organic extractant does not contain high-carbon alcohols;

[0077] In the indium silicon-containing material, the mass of the indium element is detected to be 10852ppm of the total mass of the indium silicon-containing material, and the mass of the silicon element is detected to be 5831ppm of the total mass of the indium silicon-containing material;

[0078] In step 4, 126 g of indium-containing alloy is obtained. After testing, the mass of indium element is 352776 ppm of the mass of the indium-containing alloy, and the mass of silicon element is 4300 ppm of the mass of the indium-containing alloy.

[0079] Comparative Example 2

[0080] The method is substantially the same as Example 1, except that the acidic solution does not contain bone glue;

[0081] In the indium silicon-containing material, the mass of the indium element is detected to be 9935ppm of the total mass of the indium silicon-containing material, and the mass of the silicon element is detected to be 5857ppm of the total mass of the indium silicon-containing material;

[0082] In step 4, 154 g of indium-containing alloy is obtained. After testing, the mass of indium element is 392562 ppm of the mass of the indium-containing alloy, and the mass of silicon element is 3500 ppm of the mass of the indium-containing alloy.

[0083] Comparative Example 3

[0084] The method is substantially the same as Example 1, except that the organic extractant is composed of P204 and sulfonated kerosene, and the volume ratio of P204 to sulfonated kerosene is 12:80;

[0085] In the indium silicon-containing material, the mass of the indium element is detected to be 10369ppm of the total mass of the indium silicon-containing material, and the mass of the silicon element is 5716ppm of the total mass of the indium silicon-containing material;

[0086] In step 4, 174 g of indium-containing alloy is obtained. After testing, the mass of indium element is 436213 ppm of the mass of the indium-containing alloy, and the mass of silicon element is 930 ppm of the mass of the indium-containing alloy.

[0087] Comparative Example 4

[0088] The method is basically the same as Example 1, except that an equal volume of n-butanol is used to replace octadecyl alcohol in the organic extractant for extraction;

[0089] In the indium silicon-containing material, the mass of the indium element is detected to be 10109ppm of the total mass of the indium silicon-containing material, and the mass of the silicon element is detected to be 5760ppm of the total mass of the indium silicon-containing material;

[0090] In step 4, 175 g of indium-containing alloy is obtained. After testing, the mass of indium element is 437344 ppm of the mass of the indium-containing alloy, and the mass of silicon element is 1020 ppm of the mass of the indium-containing alloy.

[0091] Performance Testing:

[0092] Indium recovery rate: The content of indium in the indium-containing silicon material and the content of indium in the indium-containing alloy are measured by ICP-OES spectrometer. The mass of the indium-containing alloy is obtained by weighing:

[0093] Indium recovery rate = (mass of indium element in indium-containing alloy / mass of indium element in indium-containing silicon material) × 100%.

[0094] Silicon content test: ICP-OES is used to measure the silicon content in indium-silicon-containing materials and the silicon content in indium-containing alloys.

[0095] The performance test results are shown in Table 1:

[0096] Table 1

[0097]

[0098]

[0099] Result analysis:

[0100] 1. It can be seen from Examples 1-3 that when the process parameters such as the ratio of the indium ion filtrate to the organic extractant or the standing time of the added gelatin are changed during the extraction process, the indium recovery rate and the silicon content in the indium-containing alloy will also change. As can be seen from Table 1, the extraction process parameters in Example 1 are the best.

[0101] 2. It can be seen from Examples 1 and 4-5 that when the amount of bone glue added is changed, if the amount of bone glue added is reduced, the silica content in the indium ion filtrate will increase, reducing the indium extraction rate, thereby affecting the indium recovery efficiency; and when the amount of bone glue added is increased, the viscosity of the indium-containing solution before filtration will increase, increasing the difficulty of filtration, affecting the indium extraction rate, and further affecting the indium recovery efficiency.

[0102] 3. It can be seen from Example 1 and Examples 6-7 that when the ratio of P204, higher alcohols and sulfonated kerosene in the organic extractant is changed, the extraction rate of indium will also be affected, thereby affecting the recovery efficiency of indium. It can be seen that the ratio of P204, higher alcohols and sulfonated kerosene in the organic extractant in Example 1 is the optimal ratio.

[0103] 4. It can be seen from Example 1 and Example 8 that when the pH of the indium ion-containing filtrate is lowered, it can further ensure that the indium in the indium-containing silicon material is completely dissolved in the solution in the form of ions, thereby further improving the indium extraction rate and further improving the indium recovery efficiency.

[0104] 5. It can be seen from Example 1 and Comparative Examples 1-3 that when the acidic solution does not contain gelatin and no high-carbon alcohol is added to the organic extractant, the silicon dioxide content in the indium ion-containing filtrate is too high, and a third phase will appear during the extraction process, affecting the extraction effect of indium, thereby reducing the recovery rate of indium;

[0105] Further observation of Comparative Examples 2-3 shows that when only bone glue is used to remove silica from the indium ion-containing filtrate or only high-carbon alcohol is used to stabilize the extraction system, the recovery rate of indium is still low. This shows that the addition of bone glue and high-carbon alcohol are both indispensable.

[0106] 6. It can be seen from Example 1 and Comparative Example 4 that when low-carbon alcohols are used to replace high-carbon alcohols, low-carbon alcohols have fewer chemical chains composed of carbon atoms. Compared with high-carbon alcohols, they are more hydrophilic and less hydrophobic, and cannot act as an emulsifier, and thus cannot reduce the surface tension between different phases to form a colloid structure to reduce or reduce the formation of the third phase of extraction, thereby resulting in a lower indium extraction rate and a low indium recovery rate.

[0107] The above embodiments are preferred implementation modes of the present invention, but the implementation modes of the present invention are not limited to the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications made without departing from the spirit and principles of the present invention shall be equivalent replacement methods and shall be included in the protection scope of the present invention.

Claims

1. A method for recovering indium-containing alloy from indium-containing silicon material, characterized in that: The following steps are involved: Step 1: adding an indium-containing silicon material into an acidic solution to dissolve and filter to obtain an indium-containing filtrate; Step 2: adding an organic extractant to the indium ion-containing filtrate for extraction to obtain an indium-containing organic phase and a raffinate; Step 3: adding a hydrochloric acid solution to the indium-containing organic phase for stripping to obtain an indium chloride solution, then adding an alkaline solution to the indium chloride solution to make the pH value of the solution greater than 3, filtering to obtain an indium hydroxide precipitate; Step 4: calcining the indium hydroxide precipitate once to obtain indium oxide, and then calcining the indium oxide twice in a reducing gas atmosphere to obtain an indium-containing alloy; The acidic solution in step 1 further comprises bone glue; The organic extractant in step 2 is composed of P204, high carbon alcohol and sulfonated kerosene.

2. The method for recovering indium-containing alloy from indium-containing silicon material according to claim 1, characterized in that: The pH of the indium ion-containing filtrate is less than or equal to 2.

3. The method for recovering indium-containing alloy from indium-containing silicon material according to claim 1, characterized in that: The acidic solution is selected from at least one of an aqueous solution of sulfuric acid, an aqueous solution of hydrochloric acid, and an aqueous solution of nitric acid.

4. The method for recovering indium-containing alloy from indium-containing silicon material according to claim 1, characterized in that: The acidic solution is an aqueous solution of sulfuric acid, and the step 1 specifically comprises: adding the indium silicon-containing material to the aqueous solution of sulfuric acid containing gelatin, stirring for 2 to 4 hours, standing for 0.5 to 1.5 hours, and filtering to obtain an indium ion-containing filtrate having a pH value less than or equal to 2; The mass ratio of the indium silicon-containing material to the sulfuric acid aqueous solution is 1:4-6 The concentration of sulfuric acid in the aqueous solution of sulfuric acid is 160 g / L, and the concentration of bone glue is 0.1-0.2 g / L.

5. The method for recovering indium-containing alloy from indium-containing silicon material according to claim 1, characterized in that: The volume ratio of P204, high carbon alcohol and sulfonated kerosene in the organic extractant is 5-20:5-10:70-90; The high carbon alcohol is C 18 ~C 20 One of the alcohols.

6. The method for recovering indium-containing alloy from indium-containing silicon material according to claim 1, characterized in that: In the step 2, the O / A volume ratio of the organic extractant to the indium ion-containing filtrate is 5 to 10:

1.

7. The method for recovering indium-containing alloy from indium-containing silicon material according to claim 1, characterized in that: In step 3, the O / A volume ratio of the indium-containing organic phase to the hydrochloric acid solution is 10 to 15:1; The concentration of hydrochloric acid in the hydrochloric acid solution is 2 to 4 mol / L; The alkaline solution is an aqueous solution with a sodium hydroxide concentration of 40 to 50 g / L.

8. The method for recovering indium-containing alloy from indium-containing silicon material according to claim 1, characterized in that: In step 4, the primary calcination temperature is 400-600° C. and the time is 4-6 hours; The secondary calcination temperature is 600-800°C and the time is 6-8h; The reducing gas is hydrogen, and the hydrogen flow rate is 5 to 10 L / min.

9. An indium-containing alloy, characterized in that: The indium-containing alloy is obtained by the method for recovering an indium-containing alloy from an indium-containing silicon material as described in any one of claims 1 to 8, wherein the silicon content in the indium-containing alloy is not higher than 0.01%.

Citation Information

Patent Citations

  • Method for pretreating indium-containing zinc oxide acid supernatant

    CN103045863A