CN108070712A - The recovery method of valuable metal in a kind of silver electrolysis mother liquor purification slag - Google Patents
The recovery method of valuable metal in a kind of silver electrolysis mother liquor purification slag Download PDFInfo
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- CN108070712A CN108070712A CN201711348569.7A CN201711348569A CN108070712A CN 108070712 A CN108070712 A CN 108070712A CN 201711348569 A CN201711348569 A CN 201711348569A CN 108070712 A CN108070712 A CN 108070712A
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting 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
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
- C22B11/021—Recovery of noble metals from waste materials
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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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
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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
- C22B13/00—Obtaining lead
- C22B13/02—Obtaining lead by dry processes
- C22B13/025—Recovery from waste materials
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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
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
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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
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
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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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/06—Obtaining bismuth
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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
- C22B7/001—Dry 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
- 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
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
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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
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Abstract
The invention discloses it is a kind of silver electrolysis mother liquor purification slag in valuable metal recovery method, including：The purification slag is calcined into 1 3h except nitre at 450 550 DEG C of temperature；Sulfuric acid solution is added in except the purification slag after nitre, is stirred, leachate and leached mud is obtained by filtration in heating；Leachate and leached mud are handled, recycling obtains valuable metal.The rate of recovery of each valuable metal is all higher, the rate of recovery of copper is more than 97%, silver, bismuth, the rate of recovery of lead are respectively 99%, 97%, more than 96%, the method environmental pollution of the present invention is small, is discharged without " three wastes ", and flow is simple, it is easy to operate, operating cost is low, and synthetical recovery degree is high, has stronger practicability.
Description
Technical field
The invention belongs to smelting field of nonferrous metal, and in particular to valuable metal returns in a kind of silver electrolysis mother liquor purification slag
Receiving method.
Background technology
The electrorefining processes of silver, are to make anode with thick silver, titanium plate makees cathode, silver nitrate AgNO3Aqueous solution makees electrolyte,
In DC voltage 2-3V, electric current 250-300A/m2Under conditions of refine available 99.99% silver, while the pH value of electrolyte
It is to be adjusted by adding acid.Thick silver before electrolysis, generally all containing the various metals such as a small amount of lead Pb, copper Cu, bismuth Bi, antimony Sb into
Divide impurity.In electrolytic process, these impurity enter electrolyte, and with the extension of electrolysis activity duration, impurity is constantly assembled
Electrolyte is polluted in the electrolytic solution.Therefore people are directed to controlling the pollution of electrolyte and changing its component always, but come from
The complex chemical composition of thick silver and cannot completely effectively avoid, during use, pollution level can be increasingly for entire electrolyte
Greatly, when impurity in the electrolytic solution be more than certain content after, electrolyte cannot then reuse and it is to be replaced fall.Using dirty
The shortcomings that electrolyte of dye, also resides in, and the impurity in electrolyte can be mixed by absorption to be precipitated in the lattice of silver-colored crystal, so as to reduce
The quality of electrolytic silver requires contaminated electrolyte carrying out purified treatment therefore.
Traditional silver electrolysis mother liquor purification method is that alkali or silver oxide tune pH are added in into mother liquor, makes lead, bismuth, copper, palladium etc.
Most impurity hydrolytic precipitations, also hydrolytic precipitation, such slag charge are electrolysed mother liquor purification slag to part silver we term it silver-colored therewith,
Above-mentioned metal mainly exists in the form of hydroxide and oxide in this purification slag.Valuable metal in purification slag is returned
It receives to recycle and not only reduces production cost, also economize on resources, it is environmentally friendly.
Country's Processing Ag electrolysis mother liquor purification slag usually directly returns to big converter and lead anode slurry mixed smelting at present, should
For technique on the one hand there are the production cycle is long, valuable metal synthetical recovery degree is low, on the other hand, does not open a way, causes to copper
Copper is constantly accumulated in system, seriously affects the electrorefining processes of silver, serious threat quality of cathode silver power.Therefore develop a kind of
Effective Processing Ag electrolysis mother liquor purification slag, makes the technique that copper is opened a way have important practical significance.
Grant number CN104962749A patents of invention disclose a kind of processing method of the heavy copper ashes of silver electrolysis mother liquor alkalescence, should
The technology path of technique is that hydrochloric acid is added in into heavy copper ashes, and copper, bismuth are with the leachate that enters of chlorate, and silver, lead are with silver chlorate, chlorine
The form for changing lead enters in silver-colored slag, then into leachate plus piece alkali neutralization sinks copper and obtains copper ashes, copper metallurgy industry is sent to recycle copper.Silver
Slag after converting dechlorination by entering silver converter recycling silver.The chloride bisulfate waste liquor generated in the process, which is evaporated, to be crystallized industrial
Salt.The technique is long there are technological process, trivial operations, and production cost is high, and metal recovery rate is low etc., and only silver and copper are carried out
Recycling, other metals are not recycled, enter the features such as system is high to equipment anticorrosion requirement additionally, due to chlorion.
The content of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide valuable metal in a kind of silver electrolysis mother liquor purification slag
Recovery method.
The present invention provides a kind of recovery method of valuable metal in silver electrolysis mother liquor purification slag, comprises the following steps：
A) by the purification slag, calcining except nitre, is obtained except nitre slag at 450-550 DEG C of temperature；
B) sulfuric acid solution is added in except nitre slag, stirred, leachate and leached mud is obtained by filtration, and the sulfuric acid is molten in heating
Liquid concentration is 120-180g/L, and sulfuric acid solution is 4-6mL with the volume mass ratio except nitre slag:1g, heating temperature are 40-85 DEG C；
C) leachate directly send eddy flow electrodeposition process to carry out electrodeposition and sinks copper, obtain cathode copper products, leached mud is sent to silver
Valuable metal of the smelting system synthetical recovery including Pb, Ag, Bi.
Preferably, purification slag described in step a) includes the substance of following weight percent content：Cu15-40%, Ag8-
45%, Bi0.2-8.0%, Pb0.1-2%.
Preferably, calcination time described in step a) is 1-3h.
Preferably, mixing speed described in step b) is 500-700r/min.
Preferably, the reaction time described in step b) is 1-1.5h.
The beneficial effects of the invention are as follows：
1. using sulfuric acid solution the hydrochloric acid solution in patent CN104962749A is replaced to be leached in the present invention, it is omitted
Subsequent dechlorination reaction, realizes the separation of metallic copper and the valuable metal including bismuth, and the metal ion in leachate is only
There is copper, it is simple to the post processing of leachate.
2. the method for the present invention recycles valuable metal, the recycling of each valuable metal suitable for being electrolysed from silver mother liquor purification slag
Rate is all higher, and the rate of recovery of copper is more than 97%, and silver, bismuth, the rate of recovery of lead are respectively 99%, 97%, more than 96%.
3. the method environmental pollution of the present invention is small, to be discharged without " three wastes ", flow is simple, easy to operate, and operating cost is low,
Synthetical recovery degree is high, has stronger practicability.
The present invention reaction principle be：Using silver electrolysis mother liquor purification slag as raw material, calcining is carried out except nitre, passes through control technology
Condition makes the silver nitrate contained in purification slag, copper nitrate remove nitrate ion therein by pyrolytic.After calcining
Purification slag is leached with sulfuric acid, and copper oxide enters with sulfuric acid reaction generation copper sulphate in leachate, and silver, bismuth, lead are respectively with sulphur
Sour silver, bismuth sulfate, the form of lead sulfate are stayed in leached mud.
Description of the drawings
Fig. 1 is the process flow chart of the present invention.
Specific embodiment
Understand to make the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, and reference
Technical scheme is clearly and completely described in attached drawing.
Embodiment 1
Process flow chart is as shown in Figure 1, be as follows：
By 200g silver electrolysis mother liquor purification slags (Cu32.05%；Ag12.33%；Bi1.51%；Pb0.83%) it is packed into oxidation
It in aluminium crucible, is then placed in Muffle furnace and is calcined, adjust 480 DEG C of temperature, take out and obtained except nitre slag, Ran Houjia after calcining 1.5h
Enter the sulfuric acid solution that concentration is 120g/L to be leached, sulfuric acid solution is 6 with the volume mass ratio (mL/g) except nitre slag:1, i.e. 1g
Except 6mL sulfuric acid solutions are added in nitre slag, under temperature 45 C, leaching is obtained by filtration after reacting 1.25h in mixing speed 600r/min
Liquid and leached mud.
Copper in purification slag enters leachate in the form of copper sulphate, and silver, bismuth, lead are respectively with silver sulfate, bismuth sulfate, sulfuric acid
The form of lead is stayed in leached mud, and obtaining copper leaching rate through assay is up to 98.75%, and cupric leachate directly send eddy flow electrodeposition
Process, which carries out electrodeposition, sinks copper and obtains cathode copper products, and purity 99.972% meets the requirement of national standard 1# tough cathodes product quality, electric
Product waste liquid returns to leaching tanks and is recycled as leaching solvent.Leached mud returns silver-colored smelting system recycling Ag, Bi, Pd valuable element.
Embodiment 2
By 200g silver electrolysis mother liquor purification slags (Cu35.09%；Ag11.79%；Bi1.05%；Pb0.67%) it is packed into oxidation
It in aluminium crucible, is then placed in Muffle furnace and is calcined, adjust 550 DEG C of temperature, taken out after calcining 1h and obtain, except nitre slag, then adding in
Concentration is that the sulfuric acid solution of 180g/L is leached, and sulfuric acid solution is 4 with the volume mass ratio (mL/g) except nitre slag:1, i.e. 1g is removed
In nitre slag add in 4mL sulfuric acid solutions, at 85 DEG C of temperature, mixing speed 700r/min, react 1h after be obtained by filtration leachate and
Leached mud.
Copper in purification slag enters leachate in the form of copper sulphate, and silver, bismuth, lead are respectively with silver sulfate, bismuth sulfate, sulfuric acid
The form of lead is stayed in leached mud, and obtaining copper leaching rate through assay is up to 98.93%, and cupric leachate directly send eddy flow electrodeposition
Process, which carries out electrodeposition, sinks copper and obtains cathode copper products, and purity 99.967% meets the requirement of national standard 1# tough cathodes product quality, electric
Product waste liquid returns to leaching tanks and is recycled as leaching solvent.Leached mud returns silver-colored smelting system recycling Ag, Bi, Pd valuable element.
Embodiment 3
By 200g silver electrolysis mother liquor purification slags (Cu28.63%；Ag33.26%；Bi6.44%；Pb1.64%) it is packed into oxidation
It in aluminium crucible, is then placed in Muffle furnace and is calcined, adjust 450 DEG C of temperature, taken out after calcining 3h and obtain, except nitre slag, then adding in
Concentration is that the sulfuric acid solution of 150g/L is leached, and sulfuric acid solution is 5 with the volume mass ratio (mL/g) except nitre slag:1, i.e. 1g is removed
5mL sulfuric acid solutions are added in nitre slag, at 40 DEG C of temperature, leachate is obtained by filtration after reacting 1.5h in mixing speed 500r/min
And leached mud.
Copper in purification slag enters leachate in the form of copper sulphate, and silver, bismuth, lead are respectively with silver sulfate, bismuth sulfate, sulfuric acid
The form of lead is stayed in leached mud, and obtaining copper leaching rate through assay is up to 97.96%, and cupric leachate directly send eddy flow electrodeposition
Process, which carries out electrodeposition, sinks copper and obtains cathode copper products, and purity 99.979% meets the requirement of national standard 1# tough cathodes product quality, electric
Product waste liquid returns to leaching tanks and is recycled as leaching solvent.Leached mud returns silver-colored smelting system recycling Ag, Bi, Pd valuable element.
Comparative example 1
To 200g silver electrolysis mother liquor purification slags (Cu20.56%；Ag37.34%；Bi1.59%；Pb0.74% added in) dense
It spends and is leached for the hydrochloric acid solution of 20g/L, the volume mass ratio (mL/g) of hydrochloric acid solution and purification slag slag is 10:1, i.e. 1g is net
10mL hydrochloric acid solutions are added in slugging, at 40 DEG C of temperature, leachate is obtained by filtration after reacting 0.5h in mixing speed 700r/min
And leached mud.
Kocide SD in purification slag is obtained by the reaction copper chloride with hydrochloric acid and stays in leachate, and silver oxide is reacted with hydrochloric acid
It obtains silver nitride precipitation to stay in leached mud, adds in sodium hydroxide into leachate, keep pH of leaching solution in 6-7, it is to be precipitated
Filtering after completely, is Kocide SD by gained filter residue, send to copper metallurgy industry and recycles copper, and gained filtrate evaporative crystallization obtains industry
Salt；Add in sodium carbonate liquor into leached mud, wherein the quality of sodium carbonate be theoretically with chlorination silver reaction needed for quality,
Liquid consolidates mass ratio as 2:1, reaction temperature is 30 DEG C, is filtered after reacting 1h, obtains dechlorination silver slag silver carbonate, gained filtrate evaporation knot
Crystalline substance obtains Nacl；What obtained dechlorination silver slag was added in the precious metals containing lead that blows divides silver stove to blow, and obtains meeting electrorefining
Thick silver.
Method using the present invention is electrolysed in mother liquor purification slag from silver and recycles the rate of recovery of each metal with being used in comparative example 1
Process ration such as the following table 1.
The comparison of each recovery rate of valuable metals in 1 silver medal of table electrolysis mother liquor purification slag
Data can be seen that each metal in method recycling silver electrolysis mother liquor purification slag using the present invention from upper table, respectively
The rate of recovery of metal has all reached more than 96%, and compared with comparative example 1, the rate of recovery of copper and silver increases, and further
The lead and bismuth in purification slag are recycled.
Claims (5)
1. the recovery method of valuable metal in a kind of silver electrolysis mother liquor purification slag, which is characterized in that comprise the following steps：
A) by the purification slag, calcining except nitre, is obtained except nitre slag at 450-550 DEG C of temperature；
B) sulfuric acid solution is added in except nitre slag, stirred, leachate and leached mud is obtained by filtration, and the sulfuric acid solution is dense in heating
It spends for 120-180g/L, sulfuric acid solution and except the volume mass ratio of nitre slag is 4-6mL:1g, heating temperature are 40-85 DEG C；
C) leachate directly send eddy flow electrodeposition process to carry out electrodeposition and sinks copper, obtain cathode copper products, leached mud is sent to silver and is smelted
Valuable metal of the system synthetical recovery including Pb, Ag, Bi.
2. the recovery method of valuable metal in silver electrolysis mother liquor purification slag as described in claim 1, which is characterized in that step a)
Described in purification slag include the substance of following weight percent content：Cu15-40%, Ag8-45%, Bi0.2-8.0%,
Pb0.1-2%.
3. the recovery method of valuable metal in silver electrolysis mother liquor purification slag as described in claim 1, which is characterized in that step a)
Described in calcination time be 1-3h.
4. the recovery method of valuable metal in silver electrolysis mother liquor purification slag as described in claim 1, which is characterized in that step b)
Described in mixing speed be 500-700r/min.
5. such as the recovery method of valuable metal in claim 1-4 any one of them silver electrolysis mother liquor purification slag, feature exists
In the reaction time described in step b) is 1-1.5h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711348569.7A CN108070712B (en) | 2017-12-15 | 2017-12-15 | A kind of silver is electrolysed the recovery method of valuable metal in mother liquor purification slag |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711348569.7A CN108070712B (en) | 2017-12-15 | 2017-12-15 | A kind of silver is electrolysed the recovery method of valuable metal in mother liquor purification slag |
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| CN108070712A true CN108070712A (en) | 2018-05-25 |
| CN108070712B CN108070712B (en) | 2019-12-03 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1237162A1 (en) * | 2001-03-02 | 2002-09-04 | Hitachi, Ltd. | Method of reprocessing spent nuclear fuel |
| CN101440434A (en) * | 2008-12-17 | 2009-05-27 | 昆明金湖冶金有限公司 | Technique for extracting copper from high-calcium high-magnesium cupric sulfide by wet method |
| CN102690947A (en) * | 2012-05-24 | 2012-09-26 | 赤峰中色锌业有限公司 | Smelting process of silver concentrate |
| CN103352116A (en) * | 2013-04-07 | 2013-10-16 | 昆明理工大学 | Method for recovering zinc from high iron and high lead leaching residue through microwave-ultrasonic wave combination |
| CN104451172A (en) * | 2014-08-26 | 2015-03-25 | 云南罗平锌电股份有限公司 | Method for comprehensively recovering valuable metals from zinc hydrometallurgy high-temperature purification slags |
| CN105543479A (en) * | 2015-12-16 | 2016-05-04 | 株洲冶炼集团股份有限公司 | Comprehensive recovery method of bismuth matte |
| CN106756069A (en) * | 2017-02-08 | 2017-05-31 | 陕西理工学院 | A kind of method that valuable metal is reclaimed in the waste residue from zinc abstraction |
-
2017
- 2017-12-15 CN CN201711348569.7A patent/CN108070712B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1237162A1 (en) * | 2001-03-02 | 2002-09-04 | Hitachi, Ltd. | Method of reprocessing spent nuclear fuel |
| CN101440434A (en) * | 2008-12-17 | 2009-05-27 | 昆明金湖冶金有限公司 | Technique for extracting copper from high-calcium high-magnesium cupric sulfide by wet method |
| CN102690947A (en) * | 2012-05-24 | 2012-09-26 | 赤峰中色锌业有限公司 | Smelting process of silver concentrate |
| CN103352116A (en) * | 2013-04-07 | 2013-10-16 | 昆明理工大学 | Method for recovering zinc from high iron and high lead leaching residue through microwave-ultrasonic wave combination |
| CN104451172A (en) * | 2014-08-26 | 2015-03-25 | 云南罗平锌电股份有限公司 | Method for comprehensively recovering valuable metals from zinc hydrometallurgy high-temperature purification slags |
| CN105543479A (en) * | 2015-12-16 | 2016-05-04 | 株洲冶炼集团股份有限公司 | Comprehensive recovery method of bismuth matte |
| CN106756069A (en) * | 2017-02-08 | 2017-05-31 | 陕西理工学院 | A kind of method that valuable metal is reclaimed in the waste residue from zinc abstraction |
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