CN111705216B - Treatment process of tin soldering electrolytic anode mud - Google Patents
Treatment process of tin soldering electrolytic anode mud Download PDFInfo
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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
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- C—CHEMISTRY; METALLURGY
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
- C22B11/021—Recovery of noble metals from waste materials
- C22B11/023—Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/044—Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
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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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
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- C—CHEMISTRY; METALLURGY
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/02—Obtaining antimony
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/06—Obtaining bismuth
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- C—CHEMISTRY; METALLURGY
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- 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
- C22B7/02—Working-up flue dust
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/14—Electrolytic production, recovery or refining of metals by electrolysis of solutions of tin
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/18—Electrolytic production, recovery or refining of metals by electrolysis of solutions of lead
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Abstract
A treatment process of soldering tin electrolysis anode mud comprises the steps of mixing the soldering tin electrolysis anode mud with silicofluoric acid according to a liquid-solid ratio of 3-7: 1, and carrying out three-stage countercurrent leaching at 75-85 ℃; electrodepositing to produce the soldering tin after the first-stage leaching solution is purified; performing redox smelting on the third-stage leaching slag to produce smoke dust, slag and crude silver, and conveying the smoke dust to a comprehensive recovery process of valuable metals such as antimony and the like; the slag is sent back to the rotary kiln for antimony removal to produce antimony-removed slag; the antimony-removed slag is sent to a fuming furnace for tin recovery; leaching the crude silver by using nitric acid after water quenching to obtain leaching slag and leaching liquid; and (3) delivering the leaching residue to a crude smelting system of tin to recycle tin, precipitating silver in the leaching solution by using sodium chloride to obtain silver chloride, and reducing the silver chloride to obtain silver powder and casting the silver powder to obtain a silver product. The method can efficiently recover valuable metals such as tin, silver, antimony, copper, bismuth and the like in the tin soldering electrolytic anode mud with low consumption, realizes comprehensive recovery of resources, and has remarkable economic benefit.
Description
Technical Field
The invention belongs to the technical field of comprehensive recovery of tin smelting, and particularly relates to a treatment process of tin soldering electrolytic anode mud.
Background
The soldering tin electrolysis anode mud contains high-value metals such as tin, silver and the like and valuable metals such as antimony, bismuth, copper and the like, and has better practical significance for comprehensively recovering the valuable metals.
In recent years, the following processes are mainly used for treating the soldering tin electrolytic anode mud: (1) the sulfuration volatilization antimony removal process has the problems that when the sulfuration volatilization antimony removal process is carried out, partial tin liquid is sulfuration volatilized to enter smoke dust, the direct yield of tin is low, the smoke dust is difficult to treat and the like; (2) the vacuum carbothermic reduction treatment process has good technical indexes, little pollution and simple flow, but has high control temperature, low vacuum degree, higher requirement on equipment and higher industrial application difficulty; (3) the oxidation/chlorination/alkaline roasting-wet combined process has serious metal dispersion and larger wastewater treatment pressure; (4) the tin tetrachloride leaching-inductive coupling electrodeposition process has the advantages of simple process flow and high metal recovery rate, but chlorine is easily generated by improperly controlling the anode, and safety accidents are easily caused; (5) the molten salt electrolysis process is used for reference of the aluminum molten salt electrolysis process, and the prior art is not mature. In addition, the treatment process comprises oxygen pressure/chlorination leaching and the like. These solder electrolytic anode slime treatment processes are well adapted in some respects, but are more or less deficient.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a treatment process which is simple and reliable in process and remarkable in economic benefit and can comprehensively recover valuable metals in the tin soldering electrolytic anode mud.
The purpose of the invention is realized by the following technical means:
a treatment process of soldering tin electrolysis anode mud comprises the following process steps:
(1) mixing silicofluoric acid and soldering tin electrolysis anode mud according to a liquid-solid ratio L/S of 3-7: 1, and carrying out three-stage countercurrent leaching on the soldering tin electrolysis anode mud at the temperature of 75-85 ℃;
the process of the three-stage countercurrent leaching is as follows: filtering the anode mud subjected to the silicofluoric acid and soldering tin electrolysis, wherein the filtrate is a first-stage leaching solution, the filter residue is first-stage leaching residue, and the first-stage leaching residue is subjected to second-stage leaching; filtering after the second-stage leaching, wherein the filtrate is a second-stage leaching solution, the filter residue is second-stage leaching residue, the second-stage leaching solution returns to the first-stage leaching, and the second-stage leaching residue is subjected to third-stage leaching; filtering after the third-stage leaching, wherein the filtrate is a third-stage leaching solution, the filter residue is third-stage leaching residue, and the third-stage leaching solution returns to the second-stage leaching;
(2) purifying the first-stage leachate obtained in the step (1), returning the purified first-stage leachate to a soldering tin electrolysis system, and recovering tin and lead;
(3) carrying out redox smelting on the third-stage leaching slag obtained in the step (1) to produce smoke dust, slag and crude silver;
(4) sending the smoke dust produced in the step (3) to a comprehensive valuable metal recovery process to recover antimony; the slag is sent to a rotary kiln to be roasted to remove arsenic and antimony to produce arsenic and antimony removed slag; leaching the crude silver by using nitric acid after water quenching to obtain leaching slag and leaching liquid;
(5) sending the arsenic-removed antimony slag obtained in the step (4) to a fuming furnace for recovering tin; sending the leached slag to a crude tin refining system for tin recovery; precipitating silver from the leachate by using sodium chloride to obtain silver chloride;
(6) reducing the silver chloride obtained in the step (5) by using ammonia hydrazine to obtain silver powder;
(7) and (4) casting the silver powder obtained in the step (6) to obtain a silver product.
The invention adopts the hydrofluoric acid to carry out three-stage countercurrent leaching on the soldering tin electrolysis anode slime, and can leach more than 96 percent of tin and lead in the anode slime into the leaching solution and return the leaching solution to a soldering tin electrolysis system for recycling. Valuable metals such as silver, antimony, copper, bismuth and the like enter leaching residues, the leaching residues with the reduction are treated by an oxidation-reduction smelting method, antimony and the like are recovered from oxidation-reduction smelting smoke dust, the oxidation-reduction smelting residues are returned to a rotary kiln for treatment, after crude silver is leached by nitric acid, the nitric acid leaching residues are sent to a crude smelting system of tin for recovering tin, the leaching solution is used for precipitating silver by sodium chloride, and then the silver ingot product is cast after reduction by ammonia hydrazine.
The process disclosed by the invention is combined with the tin smelting main system, the process of the tin smelting main system is fully utilized, the valuable metals of the tin soldering electrolytic anode mud are comprehensively recovered, the process is simple and reliable, and the economic benefit is obvious.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
As shown in fig. 1, a treatment process of solder electrolytic anode mud comprises the following specific process steps:
(1) mixing silicofluoric acid and soldering tin electrolysis anode mud according to the liquid-solid ratio L/S of 3-7: 1, carrying out three-stage countercurrent leaching at the temperature of 75-85 ℃, and leaching more than 96% of tin and lead in the anode mud into a leaching solution. The specific process of the three-stage countercurrent leaching is as follows: filtering the anode mud subjected to the silicofluoric acid and soldering tin electrolysis, wherein the filtrate is a first-stage leaching solution, the filter residue is first-stage leaching residue, and the first-stage leaching residue is subjected to second-stage leaching; filtering after the second-stage leaching, wherein the filtrate is a second-stage leaching solution, the filter residue is second-stage leaching residue, the second-stage leaching solution returns to the first-stage leaching, and the second-stage leaching residue is subjected to third-stage leaching; and filtering after the third-stage leaching, wherein the filtrate is third-stage leaching liquid, the filter residue is third-stage leaching residue, and the third-stage leaching liquid returns to the second-stage leaching.
(2) The first-stage leachate obtained in the step (1) is treatedThe purified tin and lead are returned to a soldering tin electrolysis system to recover tin and lead, and alloy of tin and lead, namely soldering tin, is produced by electrolysis; the process for recovering tin and lead by a soldering tin electrolysis system is a process in the prior art, and comprises the following specific process steps: the anode plate is cast from the coarse soldering tin, the cathode plate is made from the soldering tin, the cathode plate and the anode plate are put into the silicofluoric acid solution of lead and tin for electrifying electrolysis after being arranged, because the electrode potentials of lead and tin are close, the lead and tin in the coarse soldering tin are dissolved into electrolyte in the electrolysis process, the lead and tin in the electrolyte are separated out at the cathode, and the main chemical reaction is the anode: pb-2e ═ Pb2+,Sn-2e=Sn2+(ii) a Cathode: pb2++2e=Pb,Sn2++2e=Sn。
(3) Feeding the third-stage leaching slag obtained in the step (1) into a smelting furnace for oxidation-reduction smelting to produce smoke dust, slag and crude silver; the redox reaction process of the smelting process is as follows: adding scrap iron, reducing coal, soda, quartz and the like into the third-stage leaching slag, uniformly mixing, putting into a smelting furnace for redox smelting, and oxidizing and volatilizing metals such as arsenic, antimony, lead and the like in the leaching slag into smoke dust along with the rise of temperature; as the furnace temperature continues to rise, the furnace burden is melted, and partial arsenic, antimony and lead oxides enter the slag, wherein the chemical reaction formula of the oxides is Na2CO3=Na2O+CO2↑,Na2O+As2O5=Na2O·As2O5,Na2O+Sb2O5=Na2O·Sb2O5,Na2O+SiO2=Na2O·SiO2,PbO+SiO2=PbO·SiO2,GaO+SiO2=GaO·SiO2(ii) a Part of the lead, bismuth, tin and other metals in the leaching slag capture the noble metals such as silver and the like to form coarse silver.
(4) Sending the smoke dust produced in the step (3) to a comprehensive valuable metal recovery process to recover antimony and the like; the antimony recovery process is a prior art process, and comprises the following specific steps: and (3) performing dearsenification operation after the smoke dust is prepared, performing antimony volatilization operation on the dearsenified smoke dust, and recovering antimony in the form of antimony white powder.
Conveying the slag produced in the step (3) to a rotary kiln to roast arsenic and antimony to produce arsenic and antimony removed slag; roasting to remove arsenic and antimonyThe formula is as follows: 2C + O2=2CO,As2O5+CO=As2O3+CO2↑,Sb2O5+CO=Sb2O3+CO2↑。
Quenching the crude silver produced in the step (3) with water, and leaching with nitric acid to obtain leaching slag and leaching liquid; the reaction formula is as follows: ag + HNO3→AgNO3+NOx↑+H2O。
(5) Sending the arsenic-removed antimony slag obtained in the step (4) to a fuming furnace, and recovering tin by adopting a method in the prior art, wherein the specific recovery method comprises the following steps: and (3) sulfurizing and volatilizing the arsenic-antimony-removing slag in a pyrite in a fuming furnace to recover tin, and volatilizing the tin into smoke dust in the form of stannous sulfide.
And (4) sending the leaching slag obtained in the step (4) to a tin rough smelting system, and recovering tin by adopting a method in the prior art, wherein the specific recovery method comprises the following steps: and (4) matching the leached slag with the tin concentrate, and then sending the mixture into a top-blown furnace for smelting.
Precipitating silver from the leachate obtained in the step (4) by using sodium chloride to obtain silver chloride, wherein the reaction formula is as follows: AgNO3+NaCl =AgCl↓+NaNO3。
(6) And (3) reducing the silver chloride obtained in the step (5) by using hydrazine ammonia to obtain silver powder, wherein the reaction formula is as follows: 4AgCl +8NH3·H2O +N2H4·H2O=4Ag+8NH3↑+N2↑+9H2O+4HCl。
(7) And (4) casting the silver powder obtained in the step (6) to obtain a silver product.
The method is combined with a tin smelting main system, fully utilizes the technological processes of the tin smelting main system, such as a soldering tin electrolysis process, an oxidation reduction smelting process, a tin and other valuable metal recovery process and the like, has simple and reliable technological processes, can recover tin, silver, antimony, copper, bismuth and other valuable metals in soldering tin electrolysis anode mud with low consumption and high efficiency, realizes the comprehensive recycling of resources to the maximum degree, and has remarkable economic benefit.
Claims (1)
1. The treatment process of the soldering tin electrolysis anode mud is characterized by comprising the following process steps:
(1) mixing silicofluoric acid and soldering tin electrolysis anode mud according to a liquid-solid ratio L/S of 3-7: 1, and carrying out three-stage countercurrent leaching on the soldering tin electrolysis anode mud at the temperature of 75-85 ℃;
the process of the three-stage countercurrent leaching is as follows: filtering the anode mud subjected to the silicofluoric acid and soldering tin electrolysis, wherein the filtrate is a first-stage leaching solution, the filter residue is first-stage leaching residue, and the first-stage leaching residue is subjected to second-stage leaching; filtering after the second-stage leaching, wherein the filtrate is a second-stage leaching solution, the filter residue is second-stage leaching residue, the second-stage leaching solution returns to the first-stage leaching, and the second-stage leaching residue is subjected to third-stage leaching; filtering after the third-stage leaching, wherein the filtrate is a third-stage leaching solution, the filter residue is third-stage leaching residue, and the third-stage leaching solution returns to the second-stage leaching;
(2) purifying the first-stage leachate obtained in the step (1), returning the purified first-stage leachate to a soldering tin electrolysis system, and recovering tin and lead;
(3) carrying out redox smelting on the third-stage leaching slag obtained in the step (1) to produce smoke dust, slag and crude silver;
(4) sending the smoke dust produced in the step (3) to a comprehensive valuable metal recovery process to recover antimony; the slag is sent to a rotary kiln to be roasted to remove arsenic and antimony to produce arsenic and antimony removed slag; leaching the crude silver by using nitric acid after water quenching to obtain leaching slag and leaching liquid;
(5) sending the arsenic-removed antimony slag obtained in the step (4) to a fuming furnace for recovering tin; sending the leached slag to a crude tin refining system for tin recovery; precipitating silver from the leachate by using sodium chloride to obtain silver chloride;
(6) reducing the silver chloride obtained in the step (5) by using ammonia hydrazine to obtain silver powder;
(7) and (4) casting the silver powder obtained in the step (6) to obtain a silver product.
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