CN114525403A - Method for removing thallium from indium-containing scum - Google Patents
Method for removing thallium from indium-containing scum Download PDFInfo
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- CN114525403A CN114525403A CN202210107661.9A CN202210107661A CN114525403A CN 114525403 A CN114525403 A CN 114525403A CN 202210107661 A CN202210107661 A CN 202210107661A CN 114525403 A CN114525403 A CN 114525403A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B58/00—Obtaining gallium or indium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for removing thallium from indium-containing scum, which comprises the following steps: (1) mixing indium-containing scum with a hydrochloric acid solution, and then carrying out solid-liquid separation to obtain leached slag and a thallium-containing solution; (2) adding a sulfide solution into a thallium-containing solution for reaction; (3) and (3) carrying out solid-liquid separation on the product obtained in the step (2) so as to obtain a liquid after thallium removal. Therefore, the method can realize the open circuit of thallium, has good thallium removal effect, can realize the separation of indium and thallium, and has low cost and convenient operation.
Description
Technical Field
The invention belongs to the technical field of wet metallurgy, and particularly relates to a method for removing thallium from indium-containing scum.
Background
In the impurity removal and purification process of indium, thallium removal is mainly adoptedThe method comprises the following steps: firstly, removing thallium from ammonium chloride and glycerol; ② thallium is removed by crude indium vacuum distillation; extraction method for removing thallium. Wherein the main reaction formula of removing thallium by ammonium chloride and glycerol is as follows: 2Tl +2NH4Cl＝2TlCl+2NH3↑+H2×) @. Based on the fact that thallium has certain solubility in an ammonium chloride melt, glycerol is continuously added for skimming after stirring reaction is completed at 300 ℃, chloride is skimmed from an indium melt, and thallium and indium are separated. Although the chlorination thallium removal is simple and convenient to operate and low in cost, a large amount of glycerin volatilizes in a high-temperature molten body, so that pungent gas is generated, in addition, in the chlorination thallium removal process, part of indium is inevitably chlorinated to generate indium chloride, the indium chloride enters scum along with the scum skimming process, metal indium is attached to the scum, the indium and the thallium in the scum are difficult to separate, and the recovery rate of the indium is reduced.
The principle of crude indium vacuum distillation thallium removal: in vacuum distillation, thallium has a lower boiling point than indium and a greater difference, and it evaporates before being enriched in the gas phase and easily removed.
In the process of thallium removal by crude indium vacuum distillation, facilities such as a vacuum furnace and the like need to be invested, the investment cost is high, in the process of thallium removal at high temperature, partial volatilization of indium cannot be avoided, and in the process of gas phase cooling crystallization, partial indium and thallium are difficult to separate. In addition, when thallium is removed by adopting a vacuum distillation process, a strict air draft system is required because the thallium content is high, and environmental protection and potential safety hazards exist.
The thallium extraction and removal method is to extract thallium from an indium chloride solution by adopting N235 (trioctylamine, also called trioctylalkyltertiary amine) and TBP and kerosene, and has good thallium extraction and removal effects from related data.
Therefore, the existing thallium removal method is in need of improvement.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. To this end, it is an object of the present invention to provide a method for removing thallium from indium-containing dross. The method can realize the open circuit of thallium, has good thallium removal effect, can realize the separation of indium and thallium, and has low cost and convenient operation.
In one aspect of the invention, the invention provides a method for removing thallium from indium-containing dross, the method comprising, in accordance with an embodiment of the invention:
(1) mixing indium-containing scum with a hydrochloric acid solution, and then carrying out solid-liquid separation to obtain leached slag and a thallium-containing thallium chloride solution;
(2) adding a sulfide solution into the thallium-containing solution to react;
(3) and (3) carrying out solid-liquid separation on the product obtained in the step (2) so as to obtain the sulfide slag and the liquid after thallium removal.
According to the method for removing thallium from indium-containing dross, disclosed by the embodiment of the invention, the indium-containing dross is mixed with a hydrochloric acid solution, so that elements such as indium, thallium, zinc, iron and the like in the indium-containing dross are dissolved in the hydrochloric acid solution, then solid-liquid separation is carried out to obtain leaching residues and a thallium-containing solution containing indium ions, zinc ions, ferrous ions and thallium ions, then a sulfide salt solution is added into the thallium-containing solution, and the Tl in the thallium-containing solution can be added into the thallium-containing solution through the sulfide salt solution3+Reduction to Tl+Cl in hydrochloric acid solution-And Tl+The TlCl precipitate formed. Meanwhile, the sulfide salt solution can react with indium ions in the thallium-containing solution to generate indium sulfide, Tl3+With indium sulfide and chloride ions will be at 3Tl3++In2S3+3Cl-→3TlCl↓+3S↓+2In3+The solution of the sulfide salt can also react with zinc ions in the thallium-containing solution to form zinc sulfide, and then Tl3+With indium sulfide and chloride ions will be Tl3++ZnS+Cl-→TlCl↓+S↓+Zn2+The solution of the sulfide salt can also react with ferrous ions in the thallium-containing solution to generate ferrous sulfide, and then Tl3+With ferrous sulfide and chloride ions will be Tl3++FeS+Cl-→TlCl↓+S↓+Fe2+The chemical reaction formula is used for reaction, and finally, the sulfide slag containing TlCl and S and the thallium-removed liquid containing indium, thallium, zinc, iron and the like can be obtained by separation through solid-liquid separation. Thus, the method can realize thalliumThe method has the advantages of good thallium removal effect, low cost and convenient operation, and can realize the separation of indium and thallium.
In addition, the method for removing thallium from the indium-containing dross according to the above embodiment of the present invention may have the following additional technical features:
in some embodiments of the invention, in step (1), the indium-containing dross is derived from dross skimmed from a refined indium casting and impurity removal process.
In some embodiments of the present invention, In the step (1), the indium-containing dross contains 50 to 80% of In, 0.05 to 0.3% of Zn, 0.5 to 1% of Fe, 0.05 to 0.3% of Tl, and 0.001 to 0.008% of Sn.
In some embodiments of the invention, in step (1), the final pH of the indium-containing dross mixed with the hydrochloric acid solution is 3.0-4.0. Therefore, the open circuit of thallium can be realized, the thallium removing effect is good, and the indium and thallium separating effect is good.
In some embodiments of the present invention, in the step (2), the concentration of the sulfide salt solution is 60-100 g/L. Therefore, the open circuit of thallium can be realized, the thallium removing effect is good, and the indium and thallium separating effect is good.
In some embodiments of the invention, in the step (2), a sulfide salt in the sulfide salt solution is mixed with the thallium-containing solution according to a solid-to-liquid ratio of (0.2-0.5): 1. Therefore, the open circuit of thallium can be realized, the thallium removing effect is good, and the indium and thallium separating effect is good.
In some embodiments of the present invention, in the step (2), the reaction time is 1-2 h.
In some embodiments of the invention, in the step (2), the sulfide salt solution is added to the thallium-containing solution at a dropping rate of 20 to 40 drops/min. Therefore, the open circuit of thallium can be realized, the thallium removing effect is good, and the indium and thallium separating effect is good.
In some embodiments of the invention, in step (3), the solid-liquid separation is performed by vacuum filtration.
In some embodiments of the invention, further comprising: and (3) cleaning the sulfide slag, and returning the cleaning liquid to the step (1) to be mixed with the indium-containing dross and the hydrochloric acid solution.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic flow chart of a method for removing thallium from indium-containing dross according to an embodiment of the invention;
FIG. 2 is a schematic flow chart of a method for removing thallium from indium-containing dross according to another embodiment of the invention;
fig. 3 is a schematic diagram of a process flow for removing thallium from indium-containing dross in accordance with an embodiment of the invention.
Detailed Description
The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In one aspect of the invention, the invention provides a method for removing thallium from indium-containing dross, the method comprising, in accordance with an embodiment of the invention and with reference to fig. 1:
s100: mixing indium-containing dross with hydrochloric acid solution, and performing solid-liquid separation
In the step, indium-containing scum is mixed with a hydrochloric acid solution, elements such as metal indium, thallium, zinc, iron and the like in the indium-containing scum are dissolved in the hydrochloric acid solution, and then solid-liquid separation is carried out to obtain leaching residues and a thallium-containing solution containing indium ions, zinc ions, ferrous ions and thallium ions. The solid-liquid separation method can be selected by those skilled in the art according to actual needs, for example, the solid-liquid separation method is performed by filtration. Specifically, the indium-containing dross is derived from dross skimmed from the refined indium casting and impurity removing process, and the indium-containing dross contains 50-80% of In, 0.05-0.3% of Zn, 0.5-1% of Fe, 0.05-0.3% of Tl and 0.001-0.008% of Sn.
Further, the final pH value of the indium-containing scum after being mixed with the hydrochloric acid solution is 3.0-4.0. The inventors found that if the end point pH is too small, the efficiency of thallium removal decreases, and there is a portion of H2S is generated, the working environment has larger potential safety hazard, if the end point pH is too large, part of indium can be hydrolyzed and settled, and is mixed with thallium-removing slag, so that the loss of indium is caused.
S200: adding a sulfide solution into a thallium-containing solution to react
In the step, a sulfide salt solution is added into the thallium-containing solution, and the sulfide salt solution can lead Tl in the thallium-containing solution3+Reduction to Tl+Cl in hydrochloric acid solution-And Tl+The TlCl precipitate formed. Simultaneously, the sulfide salt solution can react with indium ions in the thallium-containing solution to generate indium sulfide, and then Tl3+With indium sulfide and chloride ions will be at 3Tl3++In2S3+3Cl-→3TlCl↓+3S↓+2In3+The solution of the sulfide salt can also react with zinc ions in the thallium-containing solution to form zinc sulfide, and then Tl3+With zinc sulphide and chloride ions will be expressed as Tl3++ZnS+Cl-→TlCl↓+S↓+Zn2+The solution of the sulfide salt can also react with ferrous ions in the thallium-containing solution to generate ferrous sulfide, and then Tl3+With ferrous sulfide and chloride ions will be Tl3++FeS+Cl-→TlCl↓+S↓+Fe2+The chemical reaction formula (2) is used for carrying out the reaction. Therefore, the open circuit of thallium can be realized, the thallium removing effect is good, and the separation of indium and thallium can be realized.
Further, the concentration of the sulfide salt solution is 60-100 g/L. The inventor finds that if the concentration of the sulfide salt solution is too high, a local overbasing phenomenon is generated, so that indium is precipitated, and if the concentration of the sulfide salt solution is too low, the addition amount of water is increased, so that the production cost is increased, and the thallium content in the thallium-containing solution is diluted, so that the thallium removal effect is reduced. Therefore, the open circuit of thallium can be realized, the thallium removing effect is good, and the indium and thallium separating effect is good.
Furthermore, the sulfide salt and the thallium-containing solution in the sulfide salt solution are mixed according to the solid-to-liquid ratio of (0.2-0.5): 1. The inventor finds that if the solid-liquid ratio of sulfide to the thallium-containing solution in the sulfide solution is too high, the input cost is increased, the sulfide solution is alkaline, the excessive sulfide allows the indium to reach the settled pH value, the indium enters the thallium removal slag after settling, the loss of the indium is caused, and if the solid-liquid ratio of sulfide to the thallium-containing solution in the sulfide solution is too low, the thallium removal effect cannot be achieved.
Further, the reaction time is 1-2 h. The inventors found that if the reaction time is too long, hydrogen sulfide gas is continuously generated in the intermediate reaction process, and thallium removal efficiency is lowered, and if the reaction time is too short, the thallium removal effect cannot be achieved.
Further, the sulfide salt solution is added into the thallium-containing solution at a dropping rate of 20-40 drops/min. The inventor finds that the solution needs to be added uniformly and slowly in the process of adding the sulfide solution, and if the adding speed is too high, indium sulfide is formed, the thallium removal effect is reduced, and the indium loss is large. Meanwhile, the reaction is carried out at normal temperature, and if the temperature is too high, part of sulfur can form hydrogen sulfide to be volatilized, so that the thallium removal effect is reduced. Therefore, the thallium removing effect is good, and meanwhile, the indium and thallium can be ensured to obtain a better separation effect.
S300: carrying out solid-liquid separation on the product obtained in the step S200
In the step, the product obtained In the step S200 is subjected to solid-liquid separation to obtain a sulfide slag and a thallium-removed liquid, wherein the sulfide slag mainly contains TlCl and S and a small amount of FeS, ZnS and In2S3The liquid after thallium removal is mainly indium ions, and the rest are zinc ions, ferrous ions, tin ions and the like. The solid-liquid separation method can be selected by those skilled in the art according to actual needs, for example, the solid-liquid separation method is performed by vacuum filtration.
Further, referring to fig. 2 and fig. 3, the method for removing thallium from the indium-containing dross further includes: and cleaning the sulfide slag, and returning the cleaning liquid to the step S100 to mix with the indium-containing scum and the hydrochloric acid solution.
According to the bookThe method for removing thallium from indium-containing scum of the embodiment of the invention comprises the steps of mixing the indium-containing scum with a hydrochloric acid solution, dissolving elements such as indium, thallium, zinc, iron and the like in the indium-containing scum into the hydrochloric acid solution, then carrying out solid-liquid separation to obtain leaching residues and a thallium-containing solution containing indium ions, zinc ions, ferrous ions and thallium ions, then adding a sulfide salt solution into the thallium-containing solution, wherein the Tl in the thallium-containing solution can be removed by the sulfide salt solution3+Reduction to Tl+Cl in hydrochloric acid solution-And Tl+The TlCl precipitate formed. Meanwhile, the sulfide solution can react with indium ions in the thallium-containing solution to generate indium sulfide, Tl3+With indium sulfide and chloride ions will react at 3Tl3++In2S3+3Cl-→3TlCl↓+3S↓+2In3+The solution of the sulfide salt can also react with zinc ions in the thallium-containing solution to form zinc sulfide, and then Tl3+With indium sulfide and chloride ions will be Tl3++ZnS+Cl-→TlCl↓+S↓+Zn2+The solution of the sulfide salt can also react with ferrous ions in the thallium-containing solution to generate ferrous sulfide, and then Tl3+With ferrous sulfide and chloride ions will be Tl3++FeS+Cl-→TlCl↓+S↓+Fe2+The chemical reaction formula is used for reaction, and finally, the sulfide slag containing TlCl and S and the thallium-removed liquid containing indium, thallium, zinc, iron and the like can be obtained by separation through solid-liquid separation. Therefore, the method can realize the open circuit of thallium, has good thallium removal effect, can realize the separation of indium and thallium, and has low cost and convenient operation.
The following embodiments of the present invention are described in detail, and it should be noted that the following embodiments are exemplary only, and are not to be construed as limiting the present invention. In addition, all reagents used in the following examples are commercially available or can be synthesized according to methods herein or known, and are readily available to those skilled in the art for reaction conditions not listed, if not explicitly stated.
Example 1
(1) And (3) dissolving scum produced by impurity removal of refined indium in an indium recovery system of a certain smelting plant by using a hydrochloric acid solution, wherein the concentration of the hydrochloric acid solution is 8mol/L, and the end point pH is controlled to be 3-4. Filtering, taking 1L of filtrate to obtain a thallium-containing solution, and measuring the main components and the concentration of the thallium-containing solution as follows: 395.16g/L of In, 0.87g/L of Zn, 2.5g/L of Fe, 350mg/L of Tl and 0.48mg/L of Sn;
(2) weighing 30g of sodium sulfide solid particles, and dissolving the particles by 300mL of water to prepare a sodium sulfide solution with the volume of 300mL and the concentration of 100 g/mL;
(3) stirring the sodium sulfide solution at normal temperature, adding the sodium sulfide solution prepared in the step (2) into the thallium-containing solution by a pipette at 30 drops/min with stirring after stirring and dissolving, wherein the stirring and adding time of the sodium sulfide solution is 1 h;
(4) after the reaction of the sodium sulfide solution and the thallium-containing solution is finished, carrying out suction filtration by using a vacuum pump, wherein the volume of a filtrate is 1279mL, and then taking the filtrate for assay, wherein the main components and the concentration are as follows: 376.24g/L of In, 0.67g/L of Zn, 2.1g/L of Fe, 6mg/L of Tl and 0.36mg/L of Sn, the thallium removal rate reaches 97.8 percent, and the loss amount of indium is small.
Example 2
(1) And (3) dissolving scum produced by impurity removal of refined indium in an indium recovery system of a certain smelting plant by using a hydrochloric acid solution, wherein the concentration of the hydrochloric acid solution is 6mol/L, and the end point pH is controlled to be 3-4. Filtering, taking 1L of filtrate to obtain a thallium-containing solution, and measuring the main components and the concentration of the thallium-containing solution as follows: 369.4g/L of In, 1.2g/L of Zn, 2.8g/L of Fe, 390mg/L of Tl and 0.69mg/L of Sn;
(2) weighing 30g of sodium sulfide solid particles, and dissolving the particles by 300mL of water to prepare a sodium sulfide solution with the volume of 300mL and the concentration of 100 g/mL;
(3) stirring the sodium sulfide solution at normal temperature, adding the sodium sulfide solution prepared in the step (2) into the thallium-containing solution at a speed of 30 drops/min by using a pipette with stirring and dissolving, wherein the stirring and adding time of the sodium sulfide solution is 1 h;
(4) after the reaction of the sodium sulfide solution and the thallium-containing solution is finished, carrying out suction filtration by using a vacuum pump, wherein the volume of a filtrate is 1269mL, and then taking the filtrate for assay, wherein the main components and the concentration of the filtrate are as follows: in 346.6g/L, Zn 0.82g/L, Fe 2.3g/L, Tl 8mg/L and Sn 0.41mg/L, the thallium removal rate reaches 97.4 percent, and the loss amount of indium is small.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are exemplary and not to be construed as limiting the present invention, and that changes, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A method for removing thallium from indium-containing dross, comprising:
(1) mixing indium-containing scum with a hydrochloric acid solution, and then carrying out solid-liquid separation to obtain leached slag and a thallium-containing solution;
(2) adding a sulfide solution into the thallium-containing solution to react;
(3) and (3) carrying out solid-liquid separation on the product obtained in the step (2) so as to obtain the sulfide slag and the liquid after thallium removal.
2. The method of claim 1, wherein in step (1), the indium-containing dross is derived from dross skimmed from a refined indium casting and impurity removal process.
3. The method according to claim 1 or 2, wherein In the step (1), the indium-containing dross contains 50 to 80% of In, 0.05 to 0.3% of Zn, 0.5 to 1% of Fe, 0.05 to 0.3% of Tl, and 0.001 to 0.008% of Sn.
4. The method of claim 3, wherein the final pH of the indium-containing dross and the hydrochloric acid solution mixed in step (1) is 3.0-4.0.
5. The method according to claim 1, wherein in the step (2), the concentration of the sulfide salt solution is 60-100 g/L.
6. The method according to claim 1 or 5, wherein in the step (2), a sulfide salt in the sulfide salt solution is mixed with the thallium-containing solution at a solid-to-liquid ratio of (0.2-0.5): 1.
7. The method of claim 1, wherein in the step (2), the reaction time is 1-2 h.
8. The method according to claim 1 or 7, wherein in the step (2), the sulfide salt solution is added to the thallium-containing solution at a dropping rate of 20 to 40 drops/min.
9. The method according to claim 1, wherein in step (3), the solid-liquid separation is performed by vacuum filtration.
10. The method of claim 1, further comprising: and (3) cleaning the sulfide slag, and returning the cleaning liquid to the step (1) to be mixed with the indium-containing dross and the hydrochloric acid solution.
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| CN116239142A (en) * | 2023-03-14 | 2023-06-09 | 广西埃索凯循环科技有限公司 | Method for preparing thallium iodide by taking industrial thallium-containing solid waste residues as raw materials |
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