CN109536714A - A kind of synthetical recovery zinc method of iron content cobalt zinc waste residue - Google Patents
A kind of synthetical recovery zinc method of iron content cobalt zinc waste residue Download PDFInfo
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- CN109536714A CN109536714A CN201811460326.7A CN201811460326A CN109536714A CN 109536714 A CN109536714 A CN 109536714A CN 201811460326 A CN201811460326 A CN 201811460326A CN 109536714 A CN109536714 A CN 109536714A
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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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
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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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
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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
- 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
- C25C1/16—Electrolytic production, recovery or refining of metals by electrolysis of solutions of zinc, cadmium or mercury
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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
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/02—Electrodes; Connections thereof
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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
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/06—Operating or servicing
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Abstract
The present invention relates to technical field of wet metallurgy, especially a kind of synthetical recovery zinc method of iron content cobalt zinc waste residue, after iron content cobalt zinc waste residue is prepared into slurries using oxidizing acid, filtering, filtrate is electrolysed under magnetic field condition, it realizes iron, cobalt while removing, shorten process flow, and by rationally controlling magnetic field strength, reduce iron cobalt content in electrolytic process cathode mud, Zn content in electrolytic liquid is reduced, so that a large amount of zinc enters cathode mud, improves the separation rate of zinc and iron, cobalt ions.
Description
Technical field
The present invention relates to technical field of wet metallurgy, especially a kind of synthetical recovery zinc method of iron content cobalt zinc waste residue.
Background technique
In zinc hydrometallurgy, often using lead franklinite as raw material, sulfuric acid leaching preparation, and in lead franklinite, contain
A large amount of ferro element and a small amount of cobalt element.In the prior art, it needs to use a large amount of zinc dust precipitation wherein iron, be removed using organic
Cobalt agent carries out saponifiable extraction cobalt ions；In this course, it not only needs to consume a large amount of zinc powder, but also removes cobalt agent soap organic
During changing extraction cobalt ions, zinc ion will be also extracted, or even preferential extraction, cause cobalt ions extraction undesirable,
The rate of recovery of zinc is undesirable, and higher to the cost recovery of zinc.Especially iron, cobalt need substep to remove, and cause zinc recovering work
Skill process is longer, and energy consumption is larger, higher cost.In addition to this, also have pickle liquor, alkali immersion liquid neutralizing hydrolysis precipitating or conventional leaching
Out, after aoxidizing, neutralizing hydrolysis；The treatment process, although the mixed precipitation of the impurity such as iron, cobalt as goethite is enabled to go out
Come, but its zinc ion for still suffering from 8-10% or so is adsorbed precipitating, cause precipitation slag still face to zinc recovering separate iron,
The problem of cobalt, it is lower otherwise to still remain zinc recovery, needs to carry out secondary treatment to precipitation slag, causes process flow longer,
And higher cost；And for acidleach after, using oxalic acid precipitation cobalt oxalate, zinc can also be precipitated with zinc oxalate, cause need
Secondary separation cobalt, zinc precipitation slag are carried out, causes process flow longer, higher cost.
In conclusion this researcher combines the research to lead franklinite zinc hydrometallurgy treatment process for a long time, to lead franklinite
Middle lead, zinc, iron plasma magnetic case analyzed, using electrolytic recovery of zinc is carried out under magnetic field environment, realize that a step is de-
Except iron and cobalt, avoid that process flow caused by substep removing iron and cobalt is long, and the defect of higher cost is iron content cobalt zinc waste residue
Middle zinc recovering provides a kind of new approaches.
Summary of the invention
In order to solve the above technical problems existing in the prior art, the present invention provides a kind of synthesis of iron content cobalt zinc waste residue
Recycle zinc method.
It is achieved particular by following technical scheme:
The synthetical recovery zinc method of iron content cobalt zinc waste residue, comprising the following steps:
(1) it uses concentration for the nitric acid solution of 150-180g/L in iron content cobalt zinc waste residue, is 1:3-5 according to solid-liquid mass ratio
Slurries are hybridly prepared into, filters, obtains filtrate and filter residue；Filter residue is handled for secondary slurrying；
(2) permanent magnet is installed in electrolytic cell two sides, is formed across the magnetic field of electrolytic cell, so that electrolytic cell is generally in magnetic field
In；Electrolytic cell is divided into anode region and cathodic region using diaphragm, and anode electrolytic cell is installed in anode region, and electrolytic cell yin is installed in cathodic region
Pole；Electrolytic condition uses voltage 3-3.5V, current density 500-1000A/m2, electrolysis temperature control is at 40-50 DEG C, electrolysing period
28-30h；Filtrate is injected, be powered electrolysis；Collect the earth of positive pole and cathode mud, electrolytic liquid；The earth of positive pole is used to prepare metallic cobalt, gold
Belong to the raw material of iron；Cathode mud is used to prepare metallic zinc and makees raw material；The same pole span of anode and cathode is 80-95mm；Magnetic field strength is
7-9A/m。
It is preferred that the same pole span of the anode and cathode is 87mm；Magnetic field strength is 8A/m.
It is preferred that the nitric acid solution concentration is 170g/L.
It is preferred that the nitric acid solution is replaced using liquor natrii hypochloritis.
It is preferred that the electrolytic liquid, which is returned, carries out slurrying processing to iron content cobalt zinc waste residue.
It is preferred that the slurry temperature is 80-90 DEG C.
It is preferred that the anode is made using magnetic material, cathode is made using stainless steel.
It is preferred that the magnetic material is the permanent magnet of alkali corrosion resistance and electrochemical corrosion resistant.
In the course of the research, due to zinc ion (Zn2+) electronic configuration outermost electron be 3d10, do not have lone electron,
So that zinc ion has stronger diamagnetism, the influence of magnetic force not will receive in magnetic field；And cobalt ions (Co2+) electronic configuration
Outermost electron is 3d7, iron ion (Fe3+) electronic configuration outermost electron be 3d5, there is lone electron pair, so that cobalt ions,
Iron ion has compared with over paramagnetism, in magnetic field, it will influenced by magnetic force, so that magnetic occurs in filtrate electrolytic process in it
Deflection, it is difficult to normally power on and parse in cathodic region, cathode according to electrolysis direction (power line direction)；Realize that cobalt, iron take off simultaneously
It removes, shortens in recycling zinc technology and remove iron, Technology for removing cobalt process.But in the course of the research, hence it is evident that discovery: for magnetic field strength
It is excessively high, it will the influence of high degree is distributed in electrolytic process intermediate ion, causes the oxygen occurred in anode region, cation etc.
Quantity influenced by high degree, and then cobalt ions (Co will be will affect2+), iron ion (Fe3+) anode region oxidation analyse
Extracting rate causes from electrolytic liquid except influence of the cobalt rate by high degree, and weaker for magnetic field strength, it will influence cobalt from
Son (Co2+), iron ion (Fe3+) arranging enters the ability of anode region, cause iron ion, cobalt ions eduction rate, influences electrolytic liquid
In iron ion, cobalt ions extrusion rate.
Specific embodiment
It is limited below with reference to specific embodiment technical solution of the present invention is further, but claimed
Range is not only limited to made description.
In the examples below, anode is made using magnetic material (such as electromagnet, permanent magnet), what cathode used
It is that stainless steel is made；In particular by the magnetic material of alkali corrosion resistance and electrochemical corrosion resistant.
Embodiment 1
The synthetical recovery zinc method of iron content cobalt zinc waste residue, comprising the following steps:
(1) it uses concentration for the nitric acid solution of 150g/L in iron content cobalt zinc waste residue, is that 1:3 mixing is matched according to solid-liquid mass ratio
80 DEG C of slurries of temperature are made, filters, obtains filtrate and filter residue；Filter residue is handled for secondary slurrying；Detect and adjust iron in filtrate,
The content of cobalt, zinc, respectively zinc 43.6g/L, cobalt 1.7g/L, iron 3.5g/L；
(2) permanent magnet is installed in electrolytic cell two sides, is formed across the magnetic field of electrolytic cell, so that electrolytic cell is generally in magnetic field
In；Electrolytic cell is divided into anode region and cathodic region using diaphragm, and anode electrolytic cell is installed in anode region, and electrolytic cell yin is installed in cathodic region
Pole；Electrolytic condition uses voltage 3-3.5V, current density 500-1000A/m2, electrolysis temperature control is at 40-50 DEG C, electrolysing period
28-30h；Filtrate is injected, be powered electrolysis；Collect the earth of positive pole and cathode mud, electrolytic liquid；The earth of positive pole is used to prepare metallic cobalt, gold
Belong to the raw material of iron；Cathode mud is used to prepare metallic zinc and makees raw material；The same pole span of anode and cathode is 80mm；Magnetic field strength is 7A/
m。
Detect Zn content in anode electrolytic cell area electrolytic liquid, iron content, cobalt content in the electrolytic liquid of cathodic region；Cathode mud
Middle cobalt content, iron content.
Embodiment 2
The synthetical recovery zinc method of iron content cobalt zinc waste residue, comprising the following steps:
(1) it uses concentration for the nitric acid solution of 180g/L in iron content cobalt zinc waste residue, is that 1:5 mixing is matched according to solid-liquid mass ratio
90 DEG C of slurries of temperature are made, filters, obtains filtrate and filter residue；Filter residue is handled for secondary slurrying；Detect and adjust iron in filtrate,
The content of cobalt, zinc, respectively zinc 42.8g/L, cobalt 1.6g/L, iron 2.9g/L；
(2) permanent magnet is installed in electrolytic cell two sides, is formed across the magnetic field of electrolytic cell, so that electrolytic cell is generally in magnetic field
In；Electrolytic cell is divided into anode region and cathodic region using diaphragm, and anode electrolytic cell is installed in anode region, and electrolytic cell yin is installed in cathodic region
Pole；Electrolytic condition uses voltage 3-3.5V, current density 500-1000A/m2, electrolysis temperature control is at 40-50 DEG C, electrolysing period
28-30h；Filtrate is injected, be powered electrolysis；Collect the earth of positive pole and cathode mud, electrolytic liquid；The earth of positive pole is used to prepare metallic cobalt, gold
Belong to the raw material of iron；Cathode mud is used to prepare metallic zinc and makees raw material；The same pole span of anode and cathode is 95mm；Magnetic field strength is 9A/
m。
Detect Zn content in anode electrolytic cell area electrolytic liquid, iron content, cobalt content in the electrolytic liquid of cathodic region；Cathode mud
Middle cobalt content, iron content.
Embodiment 3
The synthetical recovery zinc method of iron content cobalt zinc waste residue, comprising the following steps:
(1) it uses concentration for the nitric acid solution of 170g/L in iron content cobalt zinc waste residue, is that 1:4 mixing is matched according to solid-liquid mass ratio
85 DEG C of slurries of temperature are made, filters, obtains filtrate and filter residue；Filter residue is handled for secondary slurrying；Detect and adjust iron in filtrate,
The content of cobalt, zinc, respectively zinc 43.3g/L, cobalt 1.8g/L, iron 3.3g/L；
(2) permanent magnet is installed in electrolytic cell two sides, is formed across the magnetic field of electrolytic cell, so that electrolytic cell is generally in magnetic field
In；Electrolytic cell is divided into anode region and cathodic region using diaphragm, and anode electrolytic cell is installed in anode region, and electrolytic cell yin is installed in cathodic region
Pole；Electrolytic condition uses voltage 3-3.5V, current density 500-1000A/m2, electrolysis temperature control is at 40-50 DEG C, electrolysing period
28-30h；Filtrate is injected, be powered electrolysis；Collect the earth of positive pole and cathode mud, electrolytic liquid；The earth of positive pole is used to prepare metallic cobalt, gold
Belong to the raw material of iron；Cathode mud is used to prepare metallic zinc and makees raw material；The same pole span of anode and cathode is 87mm；Magnetic field strength is 8A/
m。
Detect Zn content in anode electrolytic cell area electrolytic liquid, iron content, cobalt content in the electrolytic liquid of cathodic region；Cathode mud
Middle cobalt content, iron content.
Embodiment 4
The synthetical recovery zinc method of iron content cobalt zinc waste residue, comprising the following steps:
(1) it uses concentration for the nitric acid solution of 160g/L in iron content cobalt zinc waste residue, is that 1:3 mixing is matched according to solid-liquid mass ratio
88 DEG C of slurries of temperature are made, filters, obtains filtrate and filter residue；Filter residue is handled for secondary slurrying；Detect and adjust iron in filtrate,
The content of cobalt, zinc, respectively zinc 42.9g/L, cobalt 1.5g/L, iron 3.4g/L；
(2) permanent magnet is installed in electrolytic cell two sides, is formed across the magnetic field of electrolytic cell, so that electrolytic cell is generally in magnetic field
In；Electrolytic cell is divided into anode region and cathodic region using diaphragm, and anode electrolytic cell is installed in anode region, and electrolytic cell yin is installed in cathodic region
Pole；Electrolytic condition uses voltage 3-3.5V, current density 500-1000A/m2, electrolysis temperature control is at 40-50 DEG C, electrolysing period
28-30h；Filtrate is injected, be powered electrolysis；Collect the earth of positive pole and cathode mud, electrolytic liquid；The earth of positive pole is used to prepare metallic cobalt, gold
Belong to the raw material of iron；Cathode mud is used to prepare metallic zinc and makees raw material；The same pole span of anode and cathode is 95mm；Magnetic field strength is 7A/
m。
Detect Zn content in anode electrolytic cell area electrolytic liquid, iron content, cobalt content in the electrolytic liquid of cathodic region；Cathode mud
Middle cobalt content, iron content.
Embodiment 5
On the basis of embodiment 1, nitric acid solution is substituted using the liquor natrii hypochloritis of equal concentrations.It detects and adjusts filter
The content of iron, cobalt, zinc in liquid, respectively zinc 43.1g/L, cobalt 1.6g/L, iron 3.1g/L；And by filtrate according to the place of embodiment 1
Reason mode carries out electrolysis processing: Zn content in detection anode electrolytic cell area electrolytic liquid, iron content, cobalt in the electrolytic liquid of cathodic region
Content；Cobalt content, iron content in cathode mud.
Testing result statistics after above-described embodiment 1-5 processing is as shown in table 1 below.
And in above-mentioned treatment process, according to the processing of embodiment 1, by magnetic field strength using 6A/m processing as control 1；
By magnetic field strength using 10A/m processing as control 2, and the detection of same procedure is carried out, statistical result is as shown in table 1.
Table 1
The leachate as it can be seen that for leaching in electrolysis iron content cobalt zinc waste residue oxidizing acid is shown by the data of table 1, by magnetic
Under the environment of field, high degree improves electrolysis except cobalt, the efficiency except iron, and realizes and analyse iron and cobalt in anode electrolysis together
Out, promote that zinc electrolysis in leachate is precipitated, while shortening process flow, control reasonable magnetic field strength, so that iron, cobalt are de-
Except rate is more excellent, reduce cobalt, the iron content in electrolytic liquid, avoid cobalt, iron enters in cathode mud, realize zinc and cobalt and
The removing of iron improves zinc recovering ability.
The electrolytic liquid obtained is handled by above-described embodiment, can be used for return step (1), prepare slurries.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of synthetical recovery zinc method of iron content cobalt zinc waste residue, which comprises the following steps:
(1) it uses concentration for the nitric acid solution of 150-180g/L in iron content cobalt zinc waste residue, is 1:3-5 mixing according to solid-liquid mass ratio
Slurries are configured to, filters, obtains filtrate and filter residue；Filter residue is handled for secondary slurrying；
(2) permanent magnet is installed in electrolytic cell two sides, is formed across the magnetic field of electrolytic cell, so that electrolytic cell is in magnetic field；
Electrolytic cell is divided into anode region and cathodic region using diaphragm, and anode electrolytic cell is installed in anode region, and electric tank cathode is installed in cathodic region；Electricity
Solution condition uses voltage 3-3.5V, current density 500-1000A/m2, electrolysis temperature control is at 40-50 DEG C, electrolysing period 28-
30h；Filtrate is injected, be powered electrolysis；Collect the earth of positive pole and cathode mud, electrolytic liquid；The earth of positive pole is used to prepare metallic cobalt, metallic iron
Raw material；Cathode mud is used to prepare metallic zinc and makees raw material；The same pole span of anode and cathode is 80-95mm；Magnetic field strength is 7-9A/
m。
2. the synthetical recovery zinc method of iron content cobalt zinc waste residue as described in claim 1, which is characterized in that the anode and yin
The same pole span of pole is 87mm；Magnetic field strength is 8A/m.
3. the synthetical recovery zinc method of iron content cobalt zinc waste residue as described in claim 1, which is characterized in that the nitric acid solution
Concentration is 170g/L.
4. the synthetical recovery zinc method of iron content cobalt zinc waste residue as claimed in claim 1 or 3, which is characterized in that the nitric acid
Solution is replaced using liquor natrii hypochloritis.
5. the synthetical recovery zinc method of iron content cobalt zinc waste residue as described in claim 1, which is characterized in that the electrolytic liquid
It returns and slurrying processing is carried out to iron content cobalt zinc waste residue.
6. the synthetical recovery zinc method of iron content cobalt zinc waste residue as described in claim 1, which is characterized in that the slurry temperature
It is 80-90 DEG C.
7. the synthetical recovery zinc method of iron content cobalt zinc waste residue as described in claim 1, which is characterized in that the anode uses
Magnetic material is made, and cathode is made using stainless steel.
8. the synthetical recovery zinc method of iron content cobalt zinc waste residue as claimed in claim 7, which is characterized in that the magnetic material
It is the permanent magnet of alkali corrosion resistance and electrochemical corrosion resistant.
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| CN106834692A (en) * | 2016-12-30 | 2017-06-13 | 贵州宏达环保科技有限公司 | The comprehensive recovering process of valuable metal in a kind of zinc dust precipitation slag |
| CN107746969A (en) * | 2017-10-30 | 2018-03-02 | 六盘水中联工贸实业有限公司 | It is a kind of containing zinc, nickel, cobalt purification slag comprehensive recovering process |
| CN108085498A (en) * | 2017-12-11 | 2018-05-29 | 贵州省兴安环保科技有限公司 | A kind of comprehensive recovering process of Containing Zinc Chloride solution |
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2018
- 2018-12-01 CN CN201811460326.7A patent/CN109536714A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101713031A (en) * | 2009-10-26 | 2010-05-26 | 德阳市南邡有色金属有限公司 | Method for removing impurities by oxidation in process of zinc hydrometallurgy |
| CN105018738A (en) * | 2015-07-14 | 2015-11-04 | 六盘水中联工贸实业有限公司 | Method for recovering Cu, Cd, Ni, Co and Zn from copper-cadmium slag |
| CN106834692A (en) * | 2016-12-30 | 2017-06-13 | 贵州宏达环保科技有限公司 | The comprehensive recovering process of valuable metal in a kind of zinc dust precipitation slag |
| CN107746969A (en) * | 2017-10-30 | 2018-03-02 | 六盘水中联工贸实业有限公司 | It is a kind of containing zinc, nickel, cobalt purification slag comprehensive recovering process |
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