CN109055982A - A kind of lead bullion electrolytic smelting method - Google Patents

A kind of lead bullion electrolytic smelting method Download PDF

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CN109055982A
CN109055982A CN201811100152.3A CN201811100152A CN109055982A CN 109055982 A CN109055982 A CN 109055982A CN 201811100152 A CN201811100152 A CN 201811100152A CN 109055982 A CN109055982 A CN 109055982A
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lead
lead bullion
refining
electrolyte
bullion
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尹升
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HUNAN GUIYANG YINXING NONFERROUS SMELTING CO Ltd
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HUNAN GUIYANG YINXING NONFERROUS SMELTING CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25CPROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/18Electrolytic production, recovery or refining of metals by electrolysis of solutions of lead

Abstract

The present invention provides a kind of refining of lead bullion methods, and first by (1- hydroxy ethylene) di 2 ethylhexyl phosphonic acid, acidic ion liquid, 7,7 '-imido bis- (4- hydroxyl -2- naphthalene sulfonic acids) are sequentially added in water, and mixed solution is made in stirring and dissolving at normal temperature;Then lead oxide powder and additive are added in mixed solution to be uniformly mixed, obtain electrolyte, then by after pyro-refining lead bullion and electro-deposition lead bullion cast lead bullion anode and electro-deposition lead electrode respectively in the molten state, then carry out electrorefining.The method of the present invention is simple and easy, can reduce the environmental pollution of electrolytic process and the harm to human body, improves the direct yield, comprehensive recovery and labor productivity of lead, reduces precious metal losses, improves the purity of electrolytic lead.

Description

A kind of lead bullion electrolytic smelting method
Technical field
The invention belongs to the refining techniques fields of lead, are related to a kind of electrolytic method of lead bullion, specifically, being that a kind of will show The method that the lead bullion for having pyrometallurgical smelting process to obtain obtains high-purity electrolytic lead using the method progress electrorefining of electrochemistry.
Background technique
With the development of science and technology, the lead demand of high-purity is increasing.In order to remove the objectionable impurities in lead bullion and return Receive noble metal, it is necessary to refine to it.According to the difference of lead refining techniques, existing refining techniques can be divided into pyro-refining And electrorefining, wherein fire refining process is more mature, but more serious polluting in refining process, is easy to produce leaded useless Slag, lead steam and lead powder dirt cause seriously to pollute to environment, while the direct yield of lead and comprehensive recovery are lower.Therefore, it is electrolysed Refining becomes in practice using relatively wide, the mainstream refining of lead bullion technology given priority to and promoted.
The method that industrial lead bullion electrorefining is widely used at present is Bai Zifa, i.e. lead bullion casts anode plate, uses cathode Lead is processed into starting sheet, is electrolysed in containing fluosilicic lead plumbate and free fluosilicic acid solution.Bai Zifa is widely used at present In the lead smeltery of the states such as China, Canada, Italy, Japan, Peru, Russia, it can steadily obtain purity and be up to 99.99% or more pure lead, at the same it the shortcomings that it is also increasingly of interest by people.Under the system electrolysis primary disadvantage is that: (1) silicofluoric acid is volatile and resolves into toxic HF and SiF4Gas, working site form a large amount of acid mist, and the smell is awful, right Human body and environmental hazard are very big;(2) in 105~200A/m being widely used2Under current density, corresponding tank voltage is up to 0.36 ~0.7V, ton lead direct current consumption are 110~190kwh, and energy consumption is high;(3) current efficiency is low, and only 90% or so.
Therefore, a kind of new lead bullion electrolytic refining process method is developed, the direct yield, comprehensive recovery and labour of lead are improved Productivity, reducing environmental pollution becomes urgent problem to be solved with precious metal losses.
Summary of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of novel thick electrolytic lead refining method, this method Using (1- hydroxy ethylene) diphosphine for containing acidic ion liquid, additive, 7,7 '-imido bis- (4- hydroxyl -2- naphthalene sulfonic acids) Acid solution system is the electrorefining that electrolyte carries out lead bullion, can reduce the environmental pollution of electrolytic process and the harm to human body, Direct yield, comprehensive recovery and the labor productivity of lead are improved, precious metal losses are reduced.
The present invention can be achieved through the following technical solutions:
Refining of lead bullion method according to the present invention, which comprises the following steps:
I configuration electrolyte: by (1- hydroxy ethylene) di 2 ethylhexyl phosphonic acid, acidic ion liquid, the bis- (4- hydroxyl -2- of 7,7 '-imido Naphthalene sulfonic acids) it sequentially adds in water, mixed solution is made in stirring and dissolving at normal temperature;Then lead oxide powder is added in mixed solution End and additive, stirring and dissolving under conditions of temperature is 80-100 DEG C, mixing speed 800-1000r/min, time 5-7h, so After filter, gained filtrate is electrolyte;
The preparation of II electrode: by after pyro-refining lead bullion and electro-deposition lead bullion cast respectively in the molten state lead bullion sun Pole and electro-deposition lead electrode.
III electrolysis: will be added in electrolytic cell by electrolyte made from step I, using by the sun of lead bullion made of step II Pole and electro-deposition lead electrode, are passed through direct current and are electrolysed, when tank voltage rises to 1.0V in electrolytic process, i.e. generation anodic passivity When, take out anode plate and scrub or double teeming anode plate, scrub or double teeming after anode plate return and participate in electrolysis;Joined according to above-mentioned technique It is electrolysed 4-6 days under said conditions, output cathode lead and the earth of positive pole, obtains lead pig after cathode lead melting and casting, the earth of positive pole is washed Noble metal abstraction process is sent to handle after filters pressing.
Preferably, the granularity of the lead oxide powder is 100-150 mesh.
Preferably, (1- hydroxy ethylene) di 2 ethylhexyl phosphonic acid described in step I, acidic ion liquid, 7, bis- (the 4- hydroxyls of 7 '-imido Base -2- naphthalene sulfonic acids), water, lead oxide powder, additive mass ratio be (250-380): (5-10): (5-10): 1400:(90- 140):(1-5)。
Preferably, the additive is selected from one or more of gelatin, lignosulfonates, aloin and betanaphthol.
Preferably, the acidic ion liquid is selected from 1- propionyloxy -3- methylimidazole bromide, 1- fourth sulfonic group -3- methyl One or more of imidazole bisulfate, 1- acetate -3- methylimidazole villaumite, propionyloxy pyridine bromide.
Preferably, the acidic ion liquid is previously prepared, preparation method reference: the synthesis of novel acid ionic liquid And its catalytic performance research, Zhang Xiaolei etc., Speciality Petrochemicals progress, the 10th phase of volume 12,51-54.
Preferably, electrolyte endless form described in step III is bottom in and top out or upper entering and lower leaving.
Further, the specific process parameter of electrolysis described in step III are as follows: 35-55 DEG C of electrolyte temperature, electrolyte follows The ring period is 120-160min, and electrolyte internal circulating load is 20-35L/min. slot, cathode-current density 90-150A/m2, tank voltage 0.3-1V, anodic current density 110-150A/m2, lead bullion anode plate and cathode plate spacing 70-90mm.
A kind of electrolytic lead of high-purity is made of above-mentioned refining of lead bullion method.
Compared with the prior art, the invention has the benefit that
(1) refining of lead bullion method disclosed by the invention avoids various flue dust, the intermediate slag of pyro-refining generation, improves The comprehensive recovery of the direct yield of refining process lead and various valuable metals.
(2) refining of lead bullion method disclosed by the invention, using (1- hydroxy ethylene) diphosphine acid solution electrolysis system to ring The shortcomings that border is friendly, will not generate volatilization flue dust or acid mist, overcome fluosilicic acid system electrolyte contamination environment;Electrolytic efficiency is more It is high.
(3) refining of lead bullion method disclosed by the invention adds acidic ion liquid, additive, 7,7 '-imido in the solution Bis- (4- hydroxyl -2- naphthalene sulfonic acids), are greatly improved the solvability and conductivity of solution, thus to improve low-purity lead bullion Direct Electrolysis refined lead provides precondition;Each ingredient synergistic effect, so that current efficiency and labor productivity are higher, your gold It is less to belong to loss, electrolytic lead purity is higher, and production cost is lower.
Specific embodiment
In order that those skilled in the art will better understand the technical solution of the present invention, below with reference to embodiment to this hair Bright product is described in further detail.
A kind of refining of lead bullion method, which comprises the following steps:
I configuration electrolyte: by (1- hydroxy ethylene) di 2 ethylhexyl phosphonic acid 250g, 1- propionyloxy -3- methylimidazole bromide 5g, 7, Bis- (4- hydroxyl -2- naphthalene sulfonic acids) 5g of 7 '-imido are sequentially added in water 1400g, and mixed solution is made in stirring and dissolving at normal temperature;So Lead oxide powder 90g and gelatin 1g is added in mixed solution afterwards, under conditions of temperature is 80 DEG C, mixing speed 800r/min Stirring and dissolving, time 5h, is then filtered, and gained filtrate is electrolyte;
The preparation of II electrode: by after pyro-refining lead bullion and electro-deposition lead bullion cast respectively in the molten state lead bullion sun Pole and electro-deposition lead electrode.
III electrolysis: will be added in electrolytic cell by electrolyte made from step I, using by the sun of lead bullion made of step II Pole and electro-deposition lead electrode, are passed through direct current and are electrolysed, when tank voltage rises to 1.0V in electrolytic process, i.e. generation anodic passivity When, take out anode plate and scrub or double teeming anode plate, scrub or double teeming after anode plate return and participate in electrolysis;Joined according to above-mentioned technique It is electrolysed 4 days under said conditions, output cathode lead and the earth of positive pole, obtains lead pig, the washed pressure of the earth of positive pole after cathode lead melting and casting Noble metal abstraction process is sent to handle after filter.
The granularity of the lead oxide powder is 100 mesh.
Electrolyte endless form described in step III is bottom in and top out.
The specific process parameter of electrolysis described in step III are as follows: 35 DEG C of electrolyte temperature, electrolyte cycle period is 120min, electrolyte internal circulating load are 20L/min. slot, cathode-current density 90A/m2, tank voltage 0.3V, anodic current density 110A/m2, lead bullion anode plate and cathode plate spacing 70mm.
A kind of electrolytic lead of high-purity is made of above-mentioned refining of lead bullion method.
Meanwhile in order to assess the particular technique effect of lead bullion electrolytic method of the present invention, by ICP quantitative analysis to this Metals content impurity in embodiment lead pig is tested, and specific test data is as shown in table 1:
Table 1
Chemical component (%) Ag Cu Bi Sb Sn Summation
Lead bullion 0.2520 0.1892 0.1589 0.1332 0.0248 0.7581
Lead bullion 0.0005 0.0002 0.0011 0.0004 0.0003 0.0027
As can be seen from Table 1, lead pig GB/T469-2005 national standard is compareed, which has reached national Pb99.994's Standard.It is computed, current efficiency 98.0% in electrolytic process.
Embodiment 2
A kind of refining of lead bullion method, which comprises the following steps:
I configuration electrolyte: by (1- hydroxy ethylene) di 2 ethylhexyl phosphonic acid 280g, 1- fourth sulfonic group -3- methylimidazolium hydrogen sulphate salt 6g, 7, bis- (4- hydroxyl -2- naphthalene sulfonic acids) 7g of 7 '-imido are sequentially added in water 1400g, and it is molten that mixing is made in stirring and dissolving at normal temperature Liquid;Then lead oxide powder 100g and lignosulfonates 2g is added in mixed solution, is 85 DEG C, mixing speed in temperature Stirring and dissolving under conditions of 850r/min, time 5.5h, is then filtered, and gained filtrate is electrolyte;
The preparation of II electrode: by after pyro-refining lead bullion and electro-deposition lead bullion cast respectively in the molten state lead bullion sun Pole and electro-deposition lead electrode.
III electrolysis: will be added in electrolytic cell by electrolyte made from step I, using by the sun of lead bullion made of step II Pole and electro-deposition lead electrode, are passed through direct current and are electrolysed, when tank voltage rises to 1.0V in electrolytic process, i.e. generation anodic passivity When, take out anode plate and scrub or double teeming anode plate, scrub or double teeming after anode plate return and participate in electrolysis;Joined according to above-mentioned technique It is electrolysed 5 days under said conditions, output cathode lead and the earth of positive pole, obtains lead pig, the washed pressure of the earth of positive pole after cathode lead melting and casting Noble metal abstraction process is sent to handle after filter.
The granularity of the lead oxide powder is 110 mesh.
Electrolyte endless form described in step III is upper entering and lower leaving.
The specific process parameter of electrolysis described in step III are as follows: 40 DEG C of electrolyte temperature, electrolyte cycle period is 135min, electrolyte internal circulating load are 25L/min. slot, cathode-current density 110A/m2, tank voltage 0.5V, anodic current density 120A/m2, lead bullion anode plate and cathode plate spacing 75mm.
A kind of electrolytic lead of high-purity is made of above-mentioned refining of lead bullion method.
Meanwhile in order to assess the particular technique effect of lead bullion electrolytic method of the present invention, by ICP quantitative analysis to this Metals content impurity in embodiment lead pig is tested, and specific test data is as shown in table 2:
Table 2
Chemical component (%) Ag Cu Bi Sb Sn Summation
Lead bullion 0.2520 0.1892 0.1589 0.1332 0.0248 0.7581
Lead bullion 0.0004 0.0001 0.0010 0.0005 0.0003 0.0023
As can be seen from Table 2, lead pig GB/T469-2005 national standard is compareed, which has reached national Pb99.994's Standard.It is computed, current efficiency 98.2% in electrolytic process.
Embodiment 3
A kind of refining of lead bullion method, which comprises the following steps:
I configuration electrolyte: by (1- hydroxy ethylene) di 2 ethylhexyl phosphonic acid 320g, 1- acetate -3- methylimidazole villaumite 8g, 7, Bis- (4- hydroxyl -2- naphthalene sulfonic acids) 7g of 7 '-imido are sequentially added in water 1400g, and mixed solution is made in stirring and dissolving at normal temperature;So Lead oxide powder 120g and gelatin 3g is added in mixed solution afterwards, in the condition that temperature is 90 DEG C, mixing speed 900r/min Then lower stirring and dissolving, time 6h are filtered, gained filtrate is electrolyte;
The preparation of II electrode: by after pyro-refining lead bullion and electro-deposition lead bullion cast respectively in the molten state lead bullion sun Pole and electro-deposition lead electrode.
III electrolysis: will be added in electrolytic cell by electrolyte made from step I, using by the sun of lead bullion made of step II Pole and electro-deposition lead electrode, are passed through direct current and are electrolysed, when tank voltage rises to 1.0V in electrolytic process, i.e. generation anodic passivity When, take out anode plate and scrub or double teeming anode plate, scrub or double teeming after anode plate return and participate in electrolysis;Joined according to above-mentioned technique It is electrolysed 4.5 days under said conditions, output cathode lead and the earth of positive pole, obtains lead pig after cathode lead melting and casting, the earth of positive pole is washed Noble metal abstraction process is sent to handle after filters pressing.
The granularity of the lead oxide powder is 120 mesh.
Electrolyte endless form described in step III is bottom in and top out.
The specific process parameter of electrolysis described in step III are as follows: 45 DEG C of electrolyte temperature, electrolyte cycle period is 140min, electrolyte internal circulating load are 30L/min. slot, cathode-current density 135A/m2, tank voltage 0.7V, anodic current density 140A/m2, lead bullion anode plate and cathode plate spacing 80mm.
A kind of electrolytic lead of high-purity is made of above-mentioned refining of lead bullion method.
Meanwhile in order to assess the particular technique effect of lead bullion electrolytic method of the present invention, by ICP quantitative analysis to this Metals content impurity in embodiment lead pig is tested, and specific test data is as shown in table 3.
As can be seen from Table 3, lead pig GB/T469-2005 national standard is compareed, which has reached national Pb99.994's Standard.It is computed, current efficiency 98.5% in electrolytic process.
Table 3
Chemical component (%) Ag Cu Bi Sb Sn Summation
Lead bullion 0.2520 0.1892 0.1589 0.1332 0.0248 0.7581
Lead bullion 0.0004 0.0002 0.0009 0.0005 0.0002 0.0022
Embodiment 4
A kind of refining of lead bullion method, which comprises the following steps:
I configuration electrolyte: by (1- hydroxy ethylene) di 2 ethylhexyl phosphonic acid 365g, acidic ion liquid 9g, the bis- (4- of 7,7 '-imido Hydroxyl -2- naphthalene sulfonic acids) 9g sequentially adds in water 1400g, and mixed solution is made in stirring and dissolving at normal temperature;Then in mixed solution Middle addition lead oxide powder 135g and additive 4.5g is stirred molten under conditions of temperature is 95 DEG C, mixing speed 950r/min Then solution, time 6.5h are filtered, gained filtrate is electrolyte;
The preparation of II electrode: by after pyro-refining lead bullion and electro-deposition lead bullion cast respectively in the molten state lead bullion sun Pole and electro-deposition lead electrode.
III electrolysis: will be added in electrolytic cell by electrolyte made from step I, using by the sun of lead bullion made of step II Pole and electro-deposition lead electrode, are passed through direct current and are electrolysed, when tank voltage rises to 1.0V in electrolytic process, i.e. generation anodic passivity When, take out anode plate and scrub or double teeming anode plate, scrub or double teeming after anode plate return and participate in electrolysis;Joined according to above-mentioned technique It is electrolysed 5.5 days under said conditions, output cathode lead and the earth of positive pole, obtains lead pig after cathode lead melting and casting, the earth of positive pole is washed Noble metal abstraction process is sent to handle after filters pressing.
The granularity of the lead oxide powder is 140 mesh.
The additive is that gelatin, lignosulfonates, aloin and betanaphthol 1:2:2:3 in mass ratio are mixed.
The acidic ion liquid is 1- propionyloxy -3- methylimidazole bromide, 1- fourth sulfonic group -3- methylimidazolium hydrogen sulphate Salt, 1- acetate -3- methylimidazole villaumite, propionyloxy pyridine bromide 2:3:1:2 in mass ratio are mixed.
Electrolyte endless form described in step III is upper entering and lower leaving.
The specific process parameter of electrolysis described in step III are as follows: 53 DEG C of electrolyte temperature, electrolyte cycle period is 150min, electrolyte internal circulating load are 33L/min. slot, cathode-current density 140A/m2, tank voltage 0.8V, anodic current density 140A/m2, lead bullion anode plate and cathode plate spacing 85mm.
A kind of electrolytic lead of high-purity is made of above-mentioned refining of lead bullion method.
Meanwhile in order to assess the particular technique effect of lead bullion electrolytic method of the present invention, by ICP quantitative analysis to this Metals content impurity in embodiment lead pig is tested, and specific test data is as shown in table 4.
As can be seen from Table 4, lead pig GB/T469-2005 national standard is compareed, which has reached national Pb99.994's Standard.It is computed, current efficiency 99.5% in electrolytic process.
Table 4
Chemical component (%) Ag Cu Bi Sb Sn Summation
Lead bullion 0.2520 0.1892 0.1589 0.1332 0.0248 0.7581
Lead bullion 0.0003 0.0002 0.0009 0.0003 0.0002 0.0019
Embodiment 5
A kind of refining of lead bullion method, which comprises the following steps:
I configuration electrolyte: (1- hydroxy ethylene) di 2 ethylhexyl phosphonic acid 380g, propionyloxy pyridine bromide 10g, 7,7 '-imido are double (4- hydroxyl -2- naphthalene sulfonic acids) 10g is sequentially added in water 1400g, and mixed solution is made in stirring and dissolving at normal temperature;Then it is mixing Lead oxide powder 140g and aloin 5g is added in solution, is stirred under conditions of temperature is 100 DEG C, mixing speed 1000r/min Dissolution is mixed, then time 7h is filtered, gained filtrate is electrolyte;
The preparation of II electrode: by after pyro-refining lead bullion and electro-deposition lead bullion cast respectively in the molten state lead bullion sun Pole and electro-deposition lead electrode.
III electrolysis: will be added in electrolytic cell by electrolyte made from step I, using by the sun of lead bullion made of step II Pole and electro-deposition lead electrode, are passed through direct current and are electrolysed, when tank voltage rises to 1.0V in electrolytic process, i.e. generation anodic passivity When, take out anode plate and scrub or double teeming anode plate, scrub or double teeming after anode plate return and participate in electrolysis;Joined according to above-mentioned technique It is electrolysed 6 days under said conditions, output cathode lead and the earth of positive pole, obtains lead pig, the washed pressure of the earth of positive pole after cathode lead melting and casting Noble metal abstraction process is sent to handle after filter.
The granularity of the lead oxide powder is 150 mesh.
Electrolyte endless form described in step III is upper entering and lower leaving.
The specific process parameter of electrolysis described in step III are as follows: 55 DEG C of electrolyte temperature, electrolyte cycle period is 160min, electrolyte internal circulating load are 35L/min. slot, cathode-current density 150A/m2, tank voltage 0.9V, anodic current density 150A/m2, lead bullion anode plate and cathode plate spacing 90mm.
The main component of lead bullion after pyro-refining described in step II, including following mass percent component: Pb >= 95%, Cu≤0.1%, Sb:3%, Sn≤0.05%, Bi:2%, Ag:1%.
A kind of electrolytic lead of high-purity is made of above-mentioned refining of lead bullion method.
Meanwhile in order to assess the particular technique effect of lead bullion electrolytic method of the present invention, by ICP quantitative analysis to this Metals content impurity in embodiment lead pig is tested, and specific test data is as shown in table 5:
Table 5
Chemical component (%) Ag Cu Bi Sb Sn Summation
Lead bullion 0.2520 0.1892 0.1589 0.1332 0.0248 0.7581
Lead bullion 0.0003 0.0001 0.0009 0.0004 0.0002 0.0019
As can be seen from Table 5, lead pig GB/T469-2005 national standard is compareed, which has reached national Pb99.994's Standard.It is computed, current efficiency 100% in electrolytic process.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the present invention in any form;It is all The those of ordinary skill of the industry can implement the present invention by the above and swimmingly;But all technologies for being familiar with this profession Personnel without departing from the scope of the present invention, a little change for being made using disclosed above technology contents, Modification and the equivalent variations developed, are equivalent embodiment of the invention;Meanwhile all substantial technologicals according to the present invention are to above The variation, modification and evolution etc. of any equivalent variations made by embodiment still fall within the protection model of technical solution of the present invention Within enclosing.

Claims (8)

1. a kind of refining of lead bullion method, which comprises the following steps:
I configuration electrolyte: by the bis- (4- hydroxyl -2- naphthalene sulphurs of (1- hydroxy ethylene) di 2 ethylhexyl phosphonic acid, acidic ion liquid, 7,7 '-imido Acid) it sequentially adds in water, mixed solution is made in stirring and dissolving at normal temperature;Then in mixed solution be added lead oxide powder and Additive, stirring and dissolving under conditions of temperature is 80-100 DEG C, mixing speed 800-1000r/min, time 5-7h, then mistake Filter, gained filtrate is electrolyte;
The preparation of II electrode: by after pyro-refining lead bullion and electro-deposition lead bullion cast respectively in the molten state lead bullion anode and Electro-deposition lead electrode.
III electrolysis: will be added in electrolytic cell by electrolyte made from step I, using by lead bullion anode made of step II and Electro-deposition lead electrode is passed through direct current and is electrolysed, in electrolytic process when tank voltage rises to 1.0V, that is, anodic passivity occurs, Anode plate is taken out to scrub or double teeming anode plate, scrub or double teeming after anode plate return and participate in electrolysis;According to above-mentioned technological parameter Under the conditions of be electrolysed 4-6 days, output cathode lead and the earth of positive pole, cathode lead melting and casting after obtain lead pig, the washed pressure of the earth of positive pole Noble metal abstraction process is sent to handle after filter.
2. refining of lead bullion method as described in claim 1, it is characterised in that: the granularity of the lead oxide powder is 100- 150 mesh.
3. refining of lead bullion method as described in claim 1, it is characterised in that: (1- hydroxy ethylene) diphosphine described in step I Acid, acidic ion liquid, 7,7 '-imido bis- (4- hydroxyl -2- naphthalene sulfonic acids), water, lead oxide powder, additive mass ratio be (250-380):(5-10):(5-10):1400:(90-140):(1-5)。
4. refining of lead bullion method as described in claim 1, it is characterised in that: the additive is selected from gelatin, lignin sulfonic acid One or more of salt, aloin and betanaphthol.
5. refining of lead bullion method as described in claim 1, it is characterised in that: the acidic ion liquid is selected from 1- propionyloxy- 3- methylimidazole bromide, 1- fourth sulfonic group -3- methylimidazolium hydrogen sulphate salt, 1- acetate -3- methylimidazole villaumite, propionyloxy pyrrole One or more of pyridine bromide.
6. refining of lead bullion method as described in claim 1, it is characterised in that: the circulation side of the circulation of electrolyte described in step III Formula is bottom in and top out or upper entering and lower leaving.
7. refining of lead bullion method as described in claim 1, it is characterised in that: the specific process parameter of electrolysis described in step III Are as follows: 35-55 DEG C of electrolyte temperature, electrolyte cycle period is 120-160min, and electrolyte internal circulating load is 20-35L/min. slot, Cathode-current density 90-150A/m2, tank voltage 0.3-1V, anodic current density 110-150A/m2, lead bullion anode plate and cathode plate Spacing 70-90mm.
8. a kind of electrolytic lead of high-purity is made of any one of the claim 1-7 refining of lead bullion method.
CN201811100152.3A 2018-09-20 2018-09-20 A kind of lead bullion electrolytic smelting method Pending CN109055982A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110629253A (en) * 2019-09-29 2019-12-31 昆明理工大学 Method for electrorefining lead bullion by using ionic liquid and method for recovering metal bismuth and silver
CN111996549A (en) * 2020-09-02 2020-11-27 太和县大华能源科技有限公司 Crude lead refining process for recycling lead-acid batteries

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102534660A (en) * 2012-01-13 2012-07-04 河南科技大学 Method for electrolytically refining crude lead

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102534660A (en) * 2012-01-13 2012-07-04 河南科技大学 Method for electrolytically refining crude lead
CN102534660B (en) * 2012-01-13 2014-06-18 河南科技大学 Method for electrolytically refining crude lead

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
沈黎: "在BMIMBF4离子液体中电沉积金属铅的研究", 《功能材料》 *
邱竹贤: "《有色金属冶金学》", 31 May 1988, 冶金工业出版社 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110629253A (en) * 2019-09-29 2019-12-31 昆明理工大学 Method for electrorefining lead bullion by using ionic liquid and method for recovering metal bismuth and silver
CN110629253B (en) * 2019-09-29 2021-07-02 昆明理工大学 Method for electrorefining lead bullion by using ionic liquid and method for recovering metal bismuth and silver
CN111996549A (en) * 2020-09-02 2020-11-27 太和县大华能源科技有限公司 Crude lead refining process for recycling lead-acid batteries

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Application publication date: 20181221