CN107502744B - A kind of processing method of high lead barium silver separating residues - Google Patents

A kind of processing method of high lead barium silver separating residues Download PDF

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CN107502744B
CN107502744B CN201710662685.XA CN201710662685A CN107502744B CN 107502744 B CN107502744 B CN 107502744B CN 201710662685 A CN201710662685 A CN 201710662685A CN 107502744 B CN107502744 B CN 107502744B
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lead
barium
slag
separating residues
conversion
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CN107502744A (en
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汪秋雨
吴语
王日
欧阳辉
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Jiangxi Copper Corp
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Jiangxi Copper Corp
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • C22B7/007Wet processes by acid leaching
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B11/00Obtaining noble metals
    • C22B11/04Obtaining noble metals by wet processes
    • C22B11/042Recovery of noble metals from waste materials
    • C22B11/044Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B13/00Obtaining lead
    • C22B13/04Obtaining lead by wet processes
    • C22B13/045Recovery from waste materials
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/20Obtaining alkaline earth metals or magnesium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention discloses a kind of processing methods of high lead barium silver separating residues, which comprises the following steps: 1) is converted using soluble carbonate salt to silver separating residues, be separated by solid-liquid separation after conversion and obtain conversion slag;2) using lead, the barium in acidleach dissolution conversion slag, the removing of lead barium synchronous high-efficiency is realized, separation of solid and liquid obtains de- lead barium slag and lead barium leachate;3) using lead barium leachate described in sulfuric acid precipitation, lead sulfate barium slag, and regenerated acid are obtained.The processing method of high lead barium silver separating residues of the present invention is at low cost, process is short, resource is able to high-efficiency comprehensive utilization;Compared to traditional barium, the independent extractive technique of lead, this method realize synchronous high-efficiency extract barium, lead.

Description

A kind of processing method of high lead barium silver separating residues
Technical field
The invention belongs to non-ferrous metal smelting technology, in particular to a kind of processing method of high lead barium silver separating residues.
Background technique
Silver separating residues be copper anode mud by sulfating roasting, water logging divide copper, chlorination parting and sub- sodium point silver and etc. processing Principal by product afterwards.China is the production and consumption big country of copper, and every annual meeting produces tens of thousands of tons of earth of positive pole silver separating residues.With The fast development of economic society, country will further increase the demand of copper, will also generate more silver separating residues.
The silver separating residues recovery processing difficulty of high lead barium content is big, brings huge difficulty to metal comprehensive reutilization. Due to unsuitable treatment process, high lead barium silver separating residues return to the main system processing of Copper making for a long time, in the pyrogenic process of copper In smelting process, about 80% tin, 90% lead and other valuable metals will largely enter smelted furnace cinder, no economy in silver separating residues Recycling and reusing value, causes the significant wastage of resource;In addition, the impurity such as Sn, Pb, Sb not only deteriorate the working of a furnace but also will affect master The quality of metallic copper, and increase copper metallurgy industry processing load and energy consumption.Therefore, from energy-saving, resource comprehensive Considered using, maximization of economic benefit angle, it is significant to research and develop high lead barium silver separating residues processing method.
Currently, the research of the synthetical recovery of gold, silver in silver separating residues, lead, tin, barium is relatively fewer.CN201410221705.6, CN201410221892.8 proposes the techniques such as tin using concentrated sulfuric acid leaching silver, barium, concentrated nitric acid leaching silver, alkali fusion roasting, realize silver, barium, tin, The synthetical recovery of lead, but process conditions are harsh, equipment seriously corroded, and production operation is difficult, it is difficult to realize industrial application. CN106967884A uses high chloride salt method (hydrochloric acid and villaumite) to leach the lead in silver separating residues, gold, silver as core, turns in conjunction with carbonate Change de- barium technique, realizes the synthetical recovery of gold, silver, lead, barium, tin, but there is also problems not to solve for the technique, can not make For ideal silver separating residues synthetical recovery scheme.This method is primarily present following problem: (1) it is well known that high chloride salt method is Very efficient method of removing lead, principle are the Cl in hot conditions high concentration-With Pb2+Reaction generates soluble PbCln 2-n (Pb2+ + nCl- = PbCln 2-n(n=1,2,3 ...)) realize lead removing.However lead leaches when the production of actual industrial metaplasia Rate is not high, because lead chloride is easy crystallization and return slag phase is precipitated;And material has a large amount of chlorine in filtering, transmission process The crystal of salt and lead chloride is precipitated, and causes the blocking of equipment and pipeline, is unable to operate normally production;In addition, high villaumite Acid system severe corrosion to equipment, equipment replacement is frequent, and equipment input cost is big;In addition, this kind of high villaumite gold, silver, lead Infusion solution is very difficult, and subsequent gold, silver, lead separation process are long, and equally exists the problem of villaumite crystallizes, last neutralization Slag is the solid waste containing heavy metal lead, and there are environmental issues.(2) in CO3 2-Concentration 50g/L~450g/L, SO4 2-, concentration 0g/L~ 200g/L, liquid-solid ratio are 1:1~10:1, under conditions of 20 DEG C~100 DEG C of extraction temperature, extraction time 1h~8h, it is difficult to be realized The efficient Leaching Removal barium sulfate of level-one uses multistage carbonate to convert de- barium technique in this way, this also further results in work Skill process and production cycle are long, equipment investment is big, high production cost.
Summary of the invention
To solve the disadvantage that the prior art and deficiency, the purpose of the present invention is to provide a kind of low costs, short route, resource The processing method of the high lead barium silver separating residues of high-efficiency comprehensive utilization, realizes barium, the synchronous of lead extracts recycling, compared to it is traditional The leaching rate of barium, lead isolation technics, barium and lead, which has, to be greatlyd improve.
To achieve the above object, the technical scheme adopted by the invention is that: a kind of processing method of high lead barium silver separating residues, packet Include following steps:
1) silver separating residues are converted using soluble carbonate salt, is separated by solid-liquid separation after conversion and obtains conversion slag;
2) using lead, the barium in acidleach dissolution conversion slag, the removing of lead barium synchronous high-efficiency is realized, separation of solid and liquid obtains de- lead Barium slag and lead barium leachate;
3) using lead barium leachate described in sulfuric acid precipitation, lead sulfate barium slag, and regenerated acid are obtained.
Further, the carbonate conversion reaction conditions are as follows: solvable carbonate concentration is 0.2 ~ 3mol/L, pressure limit For normal pressure ~ 1.8MPa, reaction temperature 50 answers temperature P normal pressure, 0.5 ~ 5.0h of reaction time, and liquid-solid ratio is 4:1 ~ 20:1, stirring speed Degree is 50 ~ 400 revs/min.
Preferably, the soluble carbonate salt is Na2CO3、NaHCO3、K2CO3、KHCO3、(NH4)2CO3One of Or several mixtures.
Further, in the step 2), acid used by the lead, barium in acid soak dissolution conversion slag is HNO3, acetic acid One or more of nitration mixture, liquid-solid ratio be 2:1 ~ 10:1, temperature be room temperature ~ 60 DEG C, PH≤3 of reaction end solution.
Further, in the step 3), use the sulfuric acid solution in sulfuric acid precipitation useless for technical pure sulfuric acid or sulfuric acid Liquid.
Further, in the step 3), using lead sulfate barium slag obtained in sulfuric acid precipitation as lead raw materials for metallurgy.
Further, the regenerated acid return step 2 in the step 3)) in recycled with acid as acidleach dissolution, walk It is rapid 2) in de- lead barium slag as tin raw materials for metallurgy.
Further, lead 10% ~ 30%, baric 30% ~ 50%, stanniferous 5% ~ 15% are contained in the high lead barium silver separating residues.
The beneficial effects of the present invention are:
1. the processing method of high lead barium silver separating residues of the present invention is at low cost, process is short, resource is able to efficiently comprehensive benefit With shortening process flow, reduce production compared to traditional barium, the independent extractive technique of lead (such as patent CN106967884A) Cost avoids the problems such as high concentration chloride crystallizes, equipment burn into Selective Separation effect is poor, realizes barium lead synchronous high-efficiency Selective extraction.
2. present invention optimizes technological parameter, so that the recovering effect of barium and lead reaches best;Reaction acid recycles, Cost has been saved, production efficiency is improved.
3. test discovery suitably increases reaction pressure, Neng Gouxian when soluble carbonate salt converts silver separating residues The leaching for improving subsequent barium, lead is write, and the content of tin in de- lead barium slag is influenced very big.The present invention is optimized by a large number of experiments, Production cost and operation possibility problem are taken into account, moulding pressure is limited under normal pressure to 1.8MPa, maximum barium, lead can be obtained In the case where leaching rate, resources of production are not wasted.
Detailed description of the invention
Fig. 1 is flow chart of the invention;
Fig. 2 is Sn content in de- lead barium slag, the relational graph of lead, barium leaching rate and conversion reaction pressure.
Specific embodiment
As shown in Figure 1, a kind of processing method of high lead barium silver separating residues, comprising the following steps:
1) silver separating residues are converted using soluble carbonate salt, is separated by solid-liquid separation after conversion and obtains conversion slag;
2) using lead, the barium in acid soak dissolution conversion slag, separation of solid and liquid obtains de- lead barium slag and lead barium leachate;
3) using lead barium leachate described in sulfuric acid precipitation, lead sulfate barium slag, and regenerated acid are obtained.
More detailed description is made to the method for the invention below with reference to specific embodiment:
Embodiment 1
Main chemical compositions/% of the high lead barium silver separating residues of table 1
According to above-mentioned steps, take the high lead barium silver separating residues 1.0kg of ingredient such as table 1, be added sodium carbonate liquor to silver separating residues into Row converts, wherein conversion reaction conditions are as follows: control liquid-solid ratio is 10:1, Na2CO3Solution that concentration is 2mol/L, pressure are 1.6MPa, reaction temperature is 150 temperature, mixing speed is 300 revs/min, reaction time 3.0h.Solid-liquid after the completion of conversion reaction Separation obtains conversion slag, then conversion slag is impregnated dissolution in acid, converts the condition of slag acidleach are as follows: control liquid-solid ratio is 10: 1, reaction temperature is answered for 50, selects lead, barium in acetate dissolution conversion slag, reaction end PH=3.It is separated by solid-liquid separation, obtains after the reaction was completed Lead barium slag and lead barium leachate must be taken off, table 2 is the main chemical compositions of de- lead barium slag and the leaching rate of barium and lead, takes off lead barium slag The content of middle tin is 45.20%, can be used as tin raw materials for metallurgy.Using lead barium leachate as raw material, addition technical pure sulfuric acid precipitation lead, Barium, reaction end are that supernatant instills sulfuric acid without white precipitate generation.Be separated by filtration to obtain after reaction lead sulfate barium slag and Acid solution is regenerated, the content of lead is 34.7% in obtained lead sulfate barium slag, can be used as lead raw materials for metallurgy.
Table 2 takes off lead barium slag main chemical compositions (/ %) and lead barium leaching rate
Embodiment 2
According to above-mentioned steps, take the high lead barium silver separating residues 1.0kg of ingredient such as table 1, be added solution of potassium carbonate to silver separating residues into Row converts, wherein conversion reaction conditions are as follows: control liquid-solid ratio is 12:1, K2CO3Solution that concentration is 1.8mol/L, pressure are 1.2MPa, reaction temperature is 120 DEG C, mixing speed is 300 revs/min, reaction time 4.0h.Solid-liquid after the completion of conversion reaction Separation obtains conversion slag, then conversion slag is impregnated dissolution in acid, converts the condition of slag acidleach are as follows: control liquid-solid ratio is 10: 1, reaction temperature is room temperature, selects lead, barium in nitric acid dissolution conversion slag, reaction end PH≤H.It is separated by solid-liquid separation after the reaction was completed, De- lead barium slag and lead barium leachate are obtained, table 3 is the main chemical compositions of de- lead barium slag and the leaching rate of barium and lead, takes off lead barium The content of tin is 44.19% in slag, can be used as tin raw materials for metallurgy.Using lead barium leachate as raw material, technical pure sulfuric acid precipitation is added Lead, barium, reaction end are that supernatant instills sulfuric acid without white precipitate generation, are separated by filtration to obtain lead sulfate barium slag after reaction With regeneration acid solution, the content of lead is 35.2% in obtained lead sulfate barium slag, can be used as lead raw materials for metallurgy.
Table 3 takes off lead barium slag main chemical compositions (/ %) and lead barium leaching rate
Embodiment 3
According to above-mentioned steps, take the high lead barium silver separating residues 1.0kg of ingredient such as table 1, be added sal volatile to silver separating residues into Row converts, wherein conversion reaction conditions are as follows: control liquid-solid ratio is 20:1, (NH4)2CO3Concentration is the solution of 2.5mol/L, pressure For normal pressure, reaction temperature is 95 DEG C, mixing speed is 400 revs/min, reaction time 5.0h.Solid-liquid after the completion of conversion reaction Separation obtains conversion slag, then conversion slag is impregnated dissolution in acid, converts the condition of slag acidleach are as follows: control liquid-solid ratio is 10: 1, reaction temperature is room temperature, selects nitric acid to dissolve and converts lead, barium in slag, reaction end PH lead,.It is separated by solid-liquid separation after the reaction was completed, De- lead barium slag and lead barium leachate are obtained, table 4 is the main chemical compositions of de- lead barium slag and the leaching rate of barium and lead, takes off lead barium The content of tin is 41.70% in slag, can be used as tin raw materials for metallurgy.Using lead barium leachate as raw material, technical pure sulfuric acid precipitation is added Lead, barium, reaction end are that supernatant instills sulfuric acid without white precipitate generation, are separated by filtration to obtain lead sulfate barium slag after reaction With regeneration acid solution, the content of lead is 34.4% in obtained lead sulfate barium slag, can be used as lead raw materials for metallurgy.
Table 4 takes off lead barium slag main chemical compositions (/ %) and lead barium leaching rate
Test discovery suitably increases reaction pressure, can significantly mention when soluble carbonate salt converts silver separating residues The leaching of high subsequent barium, lead, and the content of tin in de- lead barium slag is influenced very big.Under showing comparison of design for example:
Comparative example 1~7
The process parameter value and test method of each comparative example are as described in Example 1, and difference is only that soluble carbonate salt Pressure when silver separating residues are carried out with conversion reaction is different, parameter such as the following table 5.
In order to more intuitively state, by above-mentioned data drafting pattern 2.As shown in Fig. 2, the situation identical in other conditions Under, increase conversion reaction pressure, takes off lead barium slag amount containing Sn in the trend increased, after reaction pressure is more than 1.8MPa, increase speed Degree slows down.Meanwhile as the increase of conversion reaction pressure, barium leaching rate and lead leaching rate all increase substantially, and in 1.8MPa After remain basically stable.
The de- lead barium slag main chemical compositions (/ %) and the comparison of lead barium leaching rate of 5 embodiment 1 of table and comparative example 1~7
In addition, comparative example 1~3 and patent CN106967884A, the method for the invention is compared to patent The leaching rate of CN106967884A barium is declined, but fall is little;The leaching rate of lead, which but greatly improves, (to be compared special Pb in benefit does not provide the definite test data of leaching rate not as main leaching target), illustrate using Pb of the present invention, The process of Ba leaching simultaneously can significantly improve the leaching of Pb in the case where the decline of Ba leaching rate is few, and resultant effect ten is clearly demarcated It is aobvious.
Final statement: the scope of the present invention is not limited thereto, according to the technical scheme of the invention and its inventive conception It is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.

Claims (3)

1. a kind of processing method of high lead barium silver separating residues, which comprises the following steps:
1) silver separating residues are converted using soluble carbonate salt, is separated by solid-liquid separation after conversion and obtains conversion slag;Wherein, the carbon Hydrochlorate conversion reaction conditions are as follows: soluble carbonate salt concentration is 1.8 ~ 3mol/L, and pressure limit is 1.2 MPa ~ 1.8MPa, instead Answer temperature be 150 DEG C, 120 DEG C or 95 DEG C, 3 ~ 5h of reaction time, liquid-solid ratio be 10:1 ~ 20:1, mixing speed be 300 ~ 400 turns/ Minute;
2) using lead, the barium in acidleach dissolution conversion slag, the removing of lead barium synchronous high-efficiency is realized, separation of solid and liquid obtains de- lead barium slag With lead barium leachate;Wherein, the lead in acidleach dissolution conversion slag, acid used by barium are HNO3, the one or more of acetic acid it is mixed Acid, liquid-solid ratio are 2:1 ~ 10:1, and reaction temperature is room temperature ~ 60 DEG C, pH≤3 of reaction end solution;
3) using lead barium leachate described in sulfuric acid precipitation, lead sulfate barium slag, and regenerated acid are obtained;Wherein, using in sulfuric acid precipitation Sulfuric acid solution be technical pure sulfuric acid or sulfuric acid waste;
Wherein, the regenerated acid return step 2 in the step 3)) in recycled with acid as acidleach dissolution, in step 2) Lead barium slag is taken off as tin raw materials for metallurgy;
Wherein, lead 10% ~ 30%, baric 30% ~ 50%, stanniferous 5% ~ 15% are contained in the high lead barium silver separating residues.
2. a kind of processing method of high lead barium silver separating residues according to claim 1, which is characterized in that the solubility carbonic acid Salt is Na2CO3、NaHCO3、K2CO3、KHCO3、(NH4)2CO3One or more of mixture.
3. a kind of processing method of high lead barium silver separating residues according to claim 1, which is characterized in that in the step 3), Using lead barium leachate described in sulfuric acid precipitation, obtained lead sulfate barium slag is as lead raw materials for metallurgy.
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CN108467054B (en) * 2018-06-08 2020-05-05 广州科城环保科技有限公司 Method for recycling feed-grade basic copper chloride from waste circuit boards and application of method
CN109759420A (en) * 2019-01-04 2019-05-17 贵州宏凯化工有限公司 A kind of barium slag harmlessness processing equipment and its workflow
CN109706322B (en) * 2019-03-07 2020-12-01 江西铜业股份有限公司 Method for extracting silver, lead and tin from silver separating slag
CN111304452B (en) * 2020-04-15 2022-01-25 烟台国润铜业有限公司 Method for recovering lead, gold and silver from silver separating slag
CN113528850B (en) * 2021-07-26 2022-06-07 中南大学 Method for purifying gold by controlling potential
CN113604672B (en) * 2021-08-09 2022-10-04 四川省乐山锐丰冶金有限公司 Method for recovering lead chloride and rare earth from lead-barium slag

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CN102660683B (en) * 2012-03-13 2013-10-16 北京科技大学 Method for preparing barium plumbate powder by coprecipitation of copper anode mud silver separating residue of circuit board
CN103966456B (en) * 2014-05-23 2015-12-02 江西理工大学 A kind of method from silver separating residue of copper anode slime comprehensively recovering valuable metal
CN105886782B (en) * 2016-06-29 2018-01-23 江西铜业集团公司 A kind of method of valuable metal in Whote-wet method recovery silver separating residues
CN106967884B (en) * 2017-03-20 2019-05-21 北矿力澜科技咨询(北京)有限公司 A kind of method of silver separating residue of copper anode slime step by step arithmetic

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