CN107502744A - 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 PDFInfo
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- CN107502744A CN107502744A CN201710662685.XA CN201710662685A CN107502744A CN 107502744 A CN107502744 A CN 107502744A CN 201710662685 A CN201710662685 A CN 201710662685A CN 107502744 A CN107502744 A CN 107502744A
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- Prior art keywords
- lead
- barium
- slag
- separating residues
- processing method
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Links
- -1 barium silver Chemical compound 0.000 title claims abstract description 28
- 238000003672 processing method Methods 0.000 title claims abstract description 18
- 229910052788 barium Inorganic materials 0.000 claims abstract description 92
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium(0) Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims abstract description 78
- 239000002893 slag Substances 0.000 claims abstract description 60
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 41
- BQCADISMDOOEFD-UHFFFAOYSA-N silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052709 silver Inorganic materials 0.000 claims abstract description 26
- 239000004332 silver Substances 0.000 claims abstract description 26
- 239000007787 solid Substances 0.000 claims abstract description 25
- 239000002253 acid Substances 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 16
- PIJPYDMVFNTHIP-UHFFFAOYSA-L Lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 claims abstract description 12
- 238000003916 acid precipitation Methods 0.000 claims abstract description 11
- 150000005323 carbonate salts Chemical class 0.000 claims abstract description 8
- 230000001360 synchronised Effects 0.000 claims abstract description 6
- 229910052718 tin Inorganic materials 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 15
- ATJFFYVFTNAWJD-UHFFFAOYSA-N tin hydride Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 13
- 238000005272 metallurgy Methods 0.000 claims description 11
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 7
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate dianion Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M NaHCO3 Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- TYJJADVDDVDEDZ-UHFFFAOYSA-M Potassium bicarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 2
- 238000006396 nitration reaction Methods 0.000 claims description 2
- 239000011736 potassium bicarbonate Substances 0.000 claims description 2
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 125000005588 carbonic acid salt group Chemical group 0.000 claims 1
- 239000002699 waste material Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 16
- 238000000605 extraction Methods 0.000 abstract description 5
- 239000011133 lead Substances 0.000 description 99
- 238000002386 leaching Methods 0.000 description 24
- 201000002574 conversion disease Diseases 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 7
- 239000010949 copper Substances 0.000 description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 5
- 229910052737 gold Inorganic materials 0.000 description 5
- 239000010931 gold Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- TZCXTZWJZNENPQ-UHFFFAOYSA-L Barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 206010054949 Metaplasia Diseases 0.000 description 1
- 208000008425 Protein Deficiency Diseases 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 230000000903 blocking Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000005591 charge neutralization Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000003818 cinder Substances 0.000 description 1
- 238000009867 copper metallurgy Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000005712 crystallization Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003978 infusion fluid Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 238000011068 load Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000001264 neutralization Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000001184 potassium carbonate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001698 pyrogenic Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000001340 slower Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000001187 sodium carbonate Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001180 sulfating Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- 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
- C22B11/044—Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
-
- 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
-
- 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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
-
- 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
-
- 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
Abstract
The invention discloses a kind of processing method of high lead barium silver separating residues, it is characterised in that comprises the following steps：1) silver separating residues are converted using soluble carbonate salt, separation of solid and liquid obtains converting slag after conversion；2) using the lead in acidleach dissolving conversion slag, barium, realize that lead barium synchronous high-efficiency removes, separation of solid and liquid obtains de- lead barium slag and lead barium leachate；3) lead barium leachate described in sulfuric acid precipitation is used, obtains lead sulfate barium slag, and regenerated acid.The processing method costs of high lead barium silver separating residues of the present invention is low, flow is short, resource is able to high-efficiency comprehensive utilization；Synchronous high-efficiency extraction barium, lead are realized compared to traditional barium, the independent extractive technique of lead, this method.
Description
Technical field
The invention belongs to non-ferrous metal metallurgy technical field, more particularly to a kind of processing method of high lead barium silver separating residues.
Background technology
Silver separating residues are that copper anode mud divides copper, chlorination parting and sub- sodium to divide the step process such as silver by sulfating roasting, water logging
Principal by product afterwards.China is the production and consumption big country of copper, and tens thousand of tons of earth of positive pole silver separating residues are produced per annual meeting.With
The fast development of economic society, country will further increase to the demand of copper, will also produce more silver separating residues.
The silver separating residues recycling difficulty of high lead barium content is big, and huge difficulty is brought to metal comprehensive reutilization.
Due to the main system processing of unsuitable handling process, for a long time high lead barium silver separating residues return Copper making, 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 is worth, and causes the significant wastage of resource；In addition, the impurity such as Sn, Pb, Sb not only deteriorates the working of a furnace but also can influence to lead
The quality of metallic copper, and add copper metallurgy industry processing load and energy resource 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.
At present, gold, silver in silver separating residues, lead, tin, barium synthetical recovery research it is relatively fewer.CN201410221705.6、
CN201410221892.8 puies forward 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, and equipment corrosion is serious, and production operation is difficult, it is difficult to realizes commercial application.
CN106967884A uses high villaumite method（Hydrochloric acid and villaumite）Lead, the gold, silver leached in silver separating residues are core, are turned with reference to carbonate
Change de- barium technique, realize the synthetical recovery of gold, silver, lead, barium, tin, but the technique also has problems and do not solved, and can not make
For preferable silver separating residues synthetical recovery scheme.This method is primarily present some following problem：（1）It is well known that high villaumite method is
Very efficient method of removing lead, principle are the Cl in hot conditions high concentration-With Pb2+Reaction, generate the PbCl of solubilityn 2-n
(Pb2+ + nCl- = PbCln 2-n(n=1,2,3 ...)) realize the removing of lead.But lead leaches during the production of actual industrial metaplasia
Rate is not high, because lead chloride easily crystallizes precipitation and returns to slag phase；And material has substantial amounts of chlorine in filtering, transmitting procedure
The crystal of salt and lead chloride separates out, and causes the blocking of equipment and pipeline, makes production can not normal operation；In addition, high villaumite
Acid system is serious to equipment corrosion, and equipment replacement is frequent, and equipment investment cost is big；In addition, this kind of high villaumite gold, silver, lead
Infusion solution is very difficult, follow-up gold, silver, lead separation circuit length, and equally exists the problem of villaumite crystallizes, last neutralization
Slag is the solid waste containing heavy metal lead, environmental issue be present.（2）In CO3 2-Concentration 50g/L~450g/L, SO4 2-, concentration 0g/L~
200g/L, liquid-solid ratio 1:1~10:1st, under conditions of 20 DEG C~100 DEG C of extraction temperature, extraction time 1h~8h, it is difficult to realize
The efficient Leaching Removal barium sulfate of one-level, the multistage de- barium technique of carbonate conversion is used in this way, this also further results in work
Skill flow and production cycle are long, equipment investment is big, production cost is high.
The content of the invention
To solve the shortcomings that prior art and deficiency, it is an object of the invention to provide a kind of low cost, short route, resource
The processing method of the high lead barium silver separating residues of high-efficiency comprehensive utilization, realize the synchronous extraction recovery of barium, lead, compared to it is traditional
The leaching rate of barium, lead isolation technics, barium and lead, which has, to be greatly enhanced.
To achieve the above object, the technical solution adopted in the present invention is：A kind of processing method of high lead barium silver separating residues, bag
Include following steps：
1) silver separating residues are converted using soluble carbonate salt, separation of solid and liquid obtains converting slag after conversion；
2) using the lead in acidleach dissolving conversion slag, barium, realize that lead barium synchronous high-efficiency removes, separation of solid and liquid obtains de- lead barium slag
With lead barium leachate；
3) lead barium leachate described in sulfuric acid precipitation is used, obtains lead sulfate barium slag, and regenerated acid.
Further, the carbonate conversion reaction conditions are：Solvable carbonate concentration is 0.2 ~ 3mol/L, pressure limit
For normal pressure ~ 1.8MPa, reaction temperature 50 answers temperature P normal pressures, 0.5 ~ 5.0h of reaction time, liquid-solid ratio 4:1~20:1, stirring speed
Spend for 50 ~ 400 revs/min.
Preferably, the soluble carbonate salt is Na2CO3、NaHCO3、K2CO3、KHCO3、(NH4)2CO3In one kind
Or several mixtures.
Further, in the step 2), acid is HNO used by the lead, barium in acid soak dissolving conversion slag3, acetic acid
One or more of nitration mixture, liquid-solid ratio 2:1~10:1, temperature is normal temperature ~ 60 DEG C, PH≤3 of reaction end solution.
Further, in the step 3), the sulfuric acid solution in sulfuric acid precipitation is used to be given up for technical pure sulfuric acid or sulfuric acid
Liquid.
Further, in the step 3), using the lead sulfate barium slag obtained in sulfuric acid precipitation as lead raw materials for metallurgy.
Further, the regenerated acid return to step 2 in the step 3)) in recycled with acid as acidleach dissolving, 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 cost of high lead barium silver separating residues of the present invention is low, flow is short, resource is able to high-efficiency comprehensive utilization, phase
Than traditional barium, the independent extractive technique of lead (such as patent CN106967884A), shorten technological process, reduce production cost,
The problems such as avoiding high concentration chloride crystallization, equipment corrosion, Selective Separation effect difference, realize barium lead synchronous high-efficiency selectivity
Extraction.
2. present invention optimizes technological parameter so that the recovering effect of barium and lead reaches optimal；Reaction acid recycles,
Cost has been saved, has improved production efficiency.
3. experiment is found, when soluble carbonate salt converts to silver separating residues, suitably increase reaction pressure, Neng Gouxian
The leaching for improving follow-up barium, lead is write, and the content influence on taking off tin in lead barium slag is very big.The present invention is optimized by lot of experiments,
Production cost and operation possibility problem are taken into account, moulding pressure is limited to normal pressure under 1.8MPa, maximum barium, lead can be obtained
In the case of leaching rate, the resources of production are not wasted.
Brief description of the drawings
Fig. 1 is the flow chart of the present invention；
Fig. 2 is to take off Sn contents in lead barium slag, the graph of a relation of lead, barium leaching rate and conversion reaction pressure.
Embodiment
As shown in figure 1, a kind of processing method of high lead barium silver separating residues, comprises the following steps：
1) silver separating residues are converted using soluble carbonate salt, separation of solid and liquid obtains converting slag after conversion；
2) de- lead barium slag and lead barium leachate are obtained using the lead in acid soak dissolving conversion slag, barium, separation of solid and liquid；
3) lead barium leachate described in sulfuric acid precipitation is used, obtains lead sulfate barium slag, and regenerated acid.
More detailed description is made to the method for the invention 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, the high lead barium silver separating residues 1.0kg of composition such as table 1 is taken, sodium carbonate liquor is added and silver separating residues is turned
Change, wherein conversion reaction conditions are：It is 10 to control liquid-solid ratio:1、Na2CO3Solution that concentration is 2mol/L, pressure 1.6MPa,
Reaction temperature is 150 temperature, mixing speed is 300 revs/min, reaction time 3.0h.Separation of solid and liquid obtains after the completion of conversion reaction
Slag must be converted, conversion slag is then soaked into dissolving in acid, the condition of conversion slag acidleach is：It is 10 to control liquid-solid ratio:1st, react
Temperature is answered for 50, and lead, barium in slag, reaction end PH=3 are converted from acetate dissolution.Separation of solid and liquid after the completion of reaction, obtain de- lead
Barium slag and lead barium leachate, table 2 are the main chemical compositions and the leaching rate of barium and lead of de- lead barium slag, take off tin in lead barium slag
Content is 45.20%, can be used as tin raw materials for metallurgy.Using lead barium leachate as raw material, technical pure sulfuric acid precipitation lead, barium, reaction are added
Terminal is that supernatant instills sulfuric acid without white precipitate generation.Reaction is separated by filtration to obtain lead sulfate barium slag and regenerated acid after terminating
Liquid, 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, the high lead barium silver separating residues 1.0kg of composition such as table 1 is taken, solution of potassium carbonate is added and silver separating residues is turned
Change, wherein conversion reaction conditions are：It is 12 to control liquid-solid ratio:1、K2CO3Solution that concentration is 1.8mol/L, pressure 1.2MPa,
Reaction temperature is 120 DEG C, mixing speed is 300 revs/min, reaction time 4.0h.Separation of solid and liquid obtains after the completion of conversion reaction
Slag must be converted, conversion slag is then soaked into dissolving in acid, the condition of conversion slag acidleach is：It is 10 to control liquid-solid ratio:1st, react
Temperature is normal temperature, dissolves lead, barium in conversion slag, reaction end PH≤H from nitric acid.Separation of solid and liquid after the completion of reaction, is taken off
Lead barium slag and lead barium leachate, table 3 are the main chemical compositions and the leaching rate of barium and lead of de- lead barium slag, take off tin in lead barium slag
Content be 44.19%, tin raw materials for metallurgy can be used as.Using lead barium leachate as raw material, technical pure sulfuric acid precipitation lead, barium are added, instead
Answer terminal to instill sulfuric acid for supernatant to generate without white precipitate, reaction is separated by filtration to obtain lead sulfate barium slag and regenerated acid after terminating
Liquid, 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, the high lead barium silver separating residues 1.0kg of composition such as table 1 is taken, sal volatile is added and silver separating residues is turned
Change, wherein conversion reaction conditions are：It is 20 to control liquid-solid ratio:1、(NH4)2CO3Solution that concentration is 2.5mol/L, pressure are normal
Pressure, reaction temperature is 95 DEG C, mixing speed is 400 revs/min, reaction time 5.0h.Separation of solid and liquid after the completion of conversion reaction
Conversion slag is obtained, conversion slag is then soaked into dissolving in acid, the condition of conversion slag acidleach is：It is 10 to control liquid-solid ratio:1st, it is anti-
It is normal temperature to answer temperature, is dissolved from nitric acid and converts lead, barium in slag, reaction end PH lead,.Separation of solid and liquid after the completion of reaction, obtain
De- lead barium slag and lead barium leachate, table 4 are the main chemical compositions and the leaching rate of barium and lead of de- lead barium slag, are taken off in lead barium slag
The content of tin is 41.70%, can be used as tin raw materials for metallurgy.Using lead barium leachate as raw material, technical pure sulfuric acid precipitation lead, barium are added,
Reaction end is that supernatant instills sulfuric acid without white precipitate generation, reacts and is separated by filtration to obtain lead sulfate barium slag and regeneration after terminating
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
Experiment is found, when soluble carbonate salt converts to silver separating residues, suitably increases reaction pressure, after can significantly improving
The leaching of continuous barium, lead, and the content influence on taking off tin in lead barium slag is very big.Under showing comparison of design for example：
Comparative example 1~7
As described in Example 1, it differs only in soluble carbonate salt to dividing to the process parameter value and test method of each comparative example
Silver-colored slag carries out pressure difference during conversion reaction, its parameter such as table 5 below.
In order to more intuitively state, by above-mentioned data drafting pattern 2.As shown in Fig. 2 in other conditions identical situation
Under, increase conversion reaction pressure, take off trend of the lead barium slag amount containing Sn in increase, 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 embodiment 1 of table 5 and the de- lead barium slag main chemical compositions (/ %) of comparative example 1~7 and the contrast of lead barium leaching rate
In addition, comparative example 1~3 and patent CN106967884A, the method for the invention is compared to patent
The leaching rate of CN106967884A barium has declined, but fall is little；The leaching rate of lead, which but greatly improves, (to be contrasted special
Pb in profit 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 simultaneouslies can significantly improve Pb leaching in the case where Ba leaching rates decline seldom, and resultant effect ten is clearly demarcated
It is aobvious.
Final statement：The scope of the present invention is not limited thereto, technique according to the invention scheme and its inventive concept
It is subject to equivalent substitution or change, should be all included within the scope of the present invention.
Claims (8)
1. a kind of processing method of high lead barium silver separating residues, it is characterised in that comprise the following steps：
1) silver separating residues are converted using soluble carbonate salt, separation of solid and liquid obtains converting slag after conversion；
2) using the lead in acidleach dissolving conversion slag, barium, realize that lead barium synchronous high-efficiency removes, separation of solid and liquid obtains de- lead barium slag
With lead barium leachate；
3) lead barium leachate described in sulfuric acid precipitation is used, obtains lead sulfate barium slag, and regenerated acid.
A kind of 2. processing method of high lead barium silver separating residues according to claim 1, it is characterised in that the carbonate conversion
Reaction condition is：Solvable carbonate concentration is 0.2 ~ 3mol/L, and pressure limit is normal pressure ~ 1.8MPa, and reaction temperature 50 answers temperature P
Normal pressure, 0.5 ~ 5.0h of reaction time, liquid-solid ratio 4:1~20:1, mixing speed is 50 ~ 400 revs/min.
A kind of 3. processing method of high lead barium silver separating residues according to claim 2, it is characterised in that the soluble carbonic acid
Salt is Na2CO3、NaHCO3、K2CO3、KHCO3、(NH4)2CO3In one or more of mixtures.
A kind of 4. processing method of high lead barium silver separating residues according to claim 1, it is characterised in that in the step 2),
Acid is HNO used by lead, barium in acidleach dissolving conversion slag3, acetic acid one or more of nitration mixture, liquid-solid ratio 2:1~10:
1, temperature is normal temperature ~ 60 DEG C, pH≤3 of reaction end solution.
A kind of 5. processing method of high lead barium silver separating residues according to claim 1, it is characterised in that in the step 3),
The sulfuric acid solution in sulfuric acid precipitation is used as technical pure sulfuric acid or sulfuric acid waste.
A kind of 6. processing method of high lead barium silver separating residues according to claim 1, it is characterised 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.
7. the processing method of a kind of high lead barium silver separating residues according to any one of claim 1~6, it is characterised in that described
Regenerated acid return to step 2 in step 3)) in recycled with acid as acidleach dissolving, the de- lead barium slag in step 2) is as tin
Raw materials for metallurgy.
8. the processing method of a kind of high lead barium silver separating residues according to any one of Claims 1 to 5, it is characterised in that described
Contain lead 10% ~ 30%, baric 30% ~ 50%, stanniferous 5% ~ 15% in high lead barium silver separating residues.
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| CN108467054A (en) * | 2018-06-08 | 2018-08-31 | 广州科城环保科技有限公司 | A kind of method and its application of waste printed circuit board remanufacture feed grade basic copper chloride |
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| 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 |
| CN111304452A (en) * | 2020-04-15 | 2020-06-19 | 烟台国润铜业有限公司 | Method for recovering lead, gold and silver 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 |
| CN113528850A (en) * | 2021-07-26 | 2021-10-22 | 中南大学 | Method for purifying gold by controlling potential |
| CN113528850B (en) * | 2021-07-26 | 2022-06-07 | 中南大学 | Method for purifying gold by controlling potential |
| CN113604672A (en) * | 2021-08-09 | 2021-11-05 | 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 |
| 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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