CN107267761A - A kind of lead copper matte oxygen presses the handling process of acid leaching residue - Google Patents
A kind of lead copper matte oxygen presses the handling process of acid leaching residue Download PDFInfo
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- CN107267761A CN107267761A CN201710516340.3A CN201710516340A CN107267761A CN 107267761 A CN107267761 A CN 107267761A CN 201710516340 A CN201710516340 A CN 201710516340A CN 107267761 A CN107267761 A CN 107267761A
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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
- C22B13/00—Obtaining lead
- C22B13/02—Obtaining lead by dry processes
- C22B13/025—Recovery from waste materials
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/12—Electrolytic production, recovery or refining of metals by electrolysis of solutions of copper
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses the handling process that a kind of lead copper matte oxygen presses acid leaching residue, belong to non-ferrous metal metallurgy comprehensive reutilization field.The technique comprises the following steps：First stage:(1) lead copper matte is presoaked using prepreg solution, then oxygen pressure acidleach, acid leaching residue and leachate are obtained, then leachate eddy flow electrodeposition obtains electrodeposition lean solution and metallic copper；(2) acid leaching residue that the electrodeposition lean solution washing step (1) obtained using step (1) is obtained, obtains filtrate and filter residue；(3) add auxiliary material in the filter residue obtained to step (2) and carry out dispensing, then reduction melting obtains flue gas, lead bullion and slag；Second stage：Using the filtrate produced in first stage step (2) as the prepreg solution in second stage step (1), remaining operates the same first stage；Follow-up phase circulates second stage.The technological process is short, simple to operate, the prepreg solution preimpregnation lead copper matte that the filtrate obtained after acid leaching residue is used as next stage is washed using electrodeposition lean solution on last stage, without the discharge of many waste liquids.
Description
Technical field
The present invention relates to non-ferrous metal metallurgy comprehensive reutilization field, a kind of lead copper matte oxygen pressure acid leaching residue is particularly related to
Handling process.
Background technology
Lead copper matte is PbS, Cu2The eutectic of S, FeS sulfides, while also having dissolved your gold such as part Ag, Au, Pt
Category, is mainly generated in pyrometallurgical smelting of lead process, most of enterprise produces lead copper matte and sells to metallurgy of copper generally as copper raw material
Enterprise, lead metal is without charge, and the valuation coefficient of the metal such as gold, silver, copper is not also high, causes the damage of lead smelting enterprise economically
Lose.
Using oxygen pressure acid leaching process processing lead copper matte material, appropriate temperature, acidity, liquid-solid ratio and extraction time is controlled,
Be passed through pure oxygen under the conditions of HTHP peracid, most iron in the form of bloodstone and yellow calcium siderotil with lead, silver, Jin Dengyou
Valency metal enters in slag together, and copper enters in solution, therefore effectively realizes the Selective Separation of copper, and the copper sulphate after press filtration is molten
Liquid directly carries out cyclone electrolytic cell after acid adjustment and obtains qualified negative electrode copper products, and leached mud then needs to handle synthetical recovery wherein in addition
Valuable element.
It is a kind of raw material for reclaiming valuable metal containing valuable elements such as lead, silver, gold in lead copper matte oxygen pressure acid leaching residue, by
In the slag charge water capacity higher (30~40%) and cupric about 5~8%, the copper for having 70% in slag charge through analyzing is soluble sulfuric acid
Copper is unrecovered, has had a strong impact on the direct yield of copper.Slag charge is also brought to reclaiming valuable metal therein containing wet and cupric is too high
Problems, such as influence yield, increase energy consumption, cost etc., economic loss of enterprise etc. is caused, presses and soaks currently for lead copper matte oxygen
The integrated treatment scheme of this new slag charge of slagging tap has not been reported.
The content of the invention
In view of this, it is an object of the invention to propose that a kind of lead copper matte oxygen presses the handling process of acid leaching residue, the technique is adopted
With wet scrubbing press filtration-united method of fire reduction melting, the acid leaching residue obtained after the pressure acidleach of lead copper matte oxygen is solved containing wet
The problem that amount is big, copper content is high, direct yield is low, the integrated treatment for pressing the acid leaching residue obtained after acidleach for lead copper matte oxygen is provided newly
Thinking, with preferable directive significance.
The handling process of acid leaching residue is pressed based on a kind of lead copper matte oxygen that the above-mentioned purpose present invention is provided, is comprised the following steps：
First stage:(1) lead copper matte is presoaked using prepreg solution, then oxygen pressure acidleach, acid leaching residue and leachate are obtained, is then soaked
Go out liquid eddy flow electrodeposition and obtain electrodeposition lean solution and metallic copper；
(2) acid leaching residue that the electrodeposition lean solution washing step (1) obtained using step (1) is obtained, obtains filtrate and filter residue；
(3) auxiliary material is added in the filter residue obtained to step (2) and carries out dispensing, then reduction melting obtains flue gas, lead bullion and melted
Slag；
Second stage：Using the filtrate produced in first stage step (2) as the prepreg solution in second stage step (1),
Remaining operates the same first stage；
Follow-up phase circulates second stage.
Preferably, the prepreg solution in the first stage step (1) is sulfuric acid, and the solid mass ratio of the liquid of sulfuric acid and lead copper matte is
(4~5):1；The preimpregnation time is 1~1.5h..
It is highly preferred that the concentration of the sulfuric acid is 100~120g/L.
Preferably, in addition to the first stage, the prepreg solution in step (1) is the middle filtrate produced of step (2) on last stage, and
The solid mass ratio of the liquid of the filtrate and lead copper matte is (4~5):1, the preimpregnation time is 1~1.5h.
Preferably, in each stage etch (1) by lead copper matte carry out oxygen pressure acidleach processing when, reaction temperature be 140~
160 DEG C, pressure is 0.6~0.8MPa, and the reaction time is 2~3h；1~2h of heat-insulation pressure keeping after reaction completely.
Preferably, the solid mass ratio of the liquid of electrodeposition lean solution and acid leaching residue is (5~6) in each stage etch (2):1, it is described
The quality of acid leaching residue is the quality that acid leaching residue is converted to acid leaching residue dry sample according to moisture percentage；Wash time is 30~60min.
Preferably, the auxiliary material added in each stage etch (3) is cigarette ash, iron ore, calcium oxide and coke；Cigarette ash
Addition is 1~2.5 times of filter residue quality, and the addition of iron ore is the 8~12% of filter residue quality, and the addition of calcium oxide is
The 8~12% of filter residue quality, the addition of coke is the 15~25% of filter residue quality；The quality of the filter residue be by filter residue according to
Moisture percentage is converted to the quality of filter residue dry sample.
Preferably, when carrying out reduction melting to filter residue and auxiliary material in each stage etch (3), reaction temperature is 1150~
1200 DEG C, the reaction time is 2~3h.
According to moisture percentage by the quality that acid leaching residue is converted to acid leaching residue dry sample be according to formula (1) carry out：
Acid leaching residue dry sample quality=acid leaching residue quality * (1- moisture percentages) (1)
According to moisture percentage by the quality that filter residue is converted to filter residue dry sample be according to formula (2) carry out：
Filter residue dry sample quality=filter residue quality * (1- moisture percentages) (2)
The acid leaching residue moisture content that lead copper matte obtained after oxygen pressure acidleach processing is 30~40%, by acid leaching residue sample preparation point
Analysis detection, and acid leaching residue is converted to after dry sample to calculate Cu contents be that 5~8%, Pb contents are 12~18% according to moisture percentage,
Also contain a small amount of Fe and other precious metals.It is poor with the electrodeposition obtained after eddy flow electrodeposition due to containing a small amount of Fe in acid leaching residue
When liquid washs acid leaching residue, the Fe in acid leaching residue can be partly dissolved, and the amount containing Fe in the filtrate obtained by secondary press filtration that carries out increases, it is impossible to
Return to cyclone electrolytic cell and carry copper, otherwise can largely influence eddy flow electrodeposition to put forward the efficiency of copper.
Presoak what is produced in lead copper matte, first stage step (2) as prepreg solution using sulfuric acid in first stage step (1)
Filtrate as in second stage step (1) prepreg solution presoak lead copper matte, second stage remaining operation with first stage phase
Together；Prepreg solution in follow-up phase step (1) is that using the filtrate produced in step (2) on last stage, i.e. follow-up phase is followed
Ring second stage.
In each stage etch (1), Cu concentration is 2~6g/L in the electrodeposition lean solution obtained after leachate eddy flow electrodeposition.
In each stage etch (2), the solid quality ratio scope control of liquid of electrodeposition lean solution and acid leaching residue is (5~6):1, electrodeposition is poor
The solid mass ratio of the liquid of liquid and acid leaching residue is too low, can not reach good copper clean result；The liquid stereoplasm of electrodeposition lean solution and acid leaching residue
Amount then increases the press filtration operating time than too high, reduces operating efficiency, and add the loss of valuable metal.
The auxiliary material added in each stage etch (3) is cigarette ash, iron ore, calcium oxide and coke, and auxiliary material is added into corresponding step
Suddenly dispensing is carried out in the filter residue that (2) are obtained to be well mixed, and is then charged into after silica crucible and is sent fire reduction melting.Wherein cigarette ash is
Powder is dried, its main component is lead oxide, and the content of lead oxide is the 50% of cigarette ash total amount, and adding cigarette ash can effectively reduce
The moisture percentage of the acid leaching residue obtained after the pressure acidleach of lead copper matte oxygen reclaims valuable metal therein suitably to carry out reduction melting；Iron ore
Stone and calcium oxide are common slag formers, and the slag suitable for construction material can effectively be prepared by adding iron ore and calcium oxide；It is burnt
Charcoal is a kind of conventional reducing agent, is reduced into simple substance to form alloy, i.e. lead bullion by oxidation state metal under the high temperature conditions, makes
Valuable metal is reclaimed to greatest extent, improves economic value.The filter residue that auxiliary material and step (2) are obtained in reduction melting,
Lime stone, iron ore and silica combine to form slag, and slag is used for construction material；Lead oxide etc. obtains metal after being reduced and is sunken to
Bottom, is stood after cooling and substantially layering occurs, and bottom valuable metal is carried out to reclaim power transmission solution；The flue gas that reduction melting is produced enters
Capable processing of gathering dust.
From the above it can be seen that the advantages of the present invention are：
(1) the lead copper matte oxygen that the present invention is provided presses the handling process of acid leaching residue, lead copper matte is carried out first at oxygen pressure acidleach
Leachate and acid leaching residue are managed to obtain, acid leaching residue is washed using the electrodeposition lean solution obtained after leachate eddy flow electrodeposition, not only by acid leaching residue
Middle soluble copper sulphate is washed out, and due to containing in electrodeposition lean solution in acid hydrogen ion, hydrogen ion can with acid leaching residue
Insoluble cupric oxide carries out the soluble mantoquita of reaction generation, that is, acid leaching residue is carried out secondary response, it is overall to improve
The direct yield of metallic copper.
(2) the lead copper matte oxygen that the present invention is provided presses the handling process of acid leaching residue, after acid leaching residue is washed using electrodeposition lean solution
Carry out reduction melting after press filtration, obtained filter residue plus auxiliary material dispensing, i.e., it is united using wet scrubbing press filtration-fire reduction melting
Technique, solves the problem of acid leaching residue copper content is high, water capacity is big, valuable metal therein, economic valency has been reclaimed to greatest extent
Value is notable.
(3) the lead copper matte oxygen that the present invention is provided presses the handling process of acid leaching residue, in order to be obtained after reducing the pressure acidleach of lead copper matte oxygen
To the moisture percentage of acid leaching residue suitably to carry out reduction melting reclaim valuable metal therein, by adding existing dry cigarette ash
Deng coordinating obtained filter residue dispensing after acid leaching residue washing, and add necessary slag former and reducing agent carries out fire reduction melting,
Valuable metal is all recycled processing, the slag of gained can be used for construction material, be that lead copper matte oxygen presses the acid obtained after acidleach
The integrated treatment of phase analysis provides new thinking, with preferable directive significance.
(4) the lead copper matte oxygen that the present invention is provided presses the handling process of acid leaching residue, and technological process is short, simple to operate, using upper
The filtrate obtained after one stage electrodeposition lean solution washing acid leaching residue is used as the prepreg solution preimpregnation lead copper matte of next stage, without unnecessary useless
Liquid is discharged, environmental protection and economy, with stronger applicability.
Brief description of the drawings
Fig. 1 is the process flow diagram of the embodiment of the present invention.
Embodiment
Embodiment 1
A kind of lead copper matte oxygen presses the handling process of acid leaching residue, comprises the following steps：
(1) lead copper matte is crushed and is milled to 100 mesh, added concentration and presoaked for 100g/L sulfuric acid, sulfuric acid and lead copper matte
The solid mass ratio of liquid be 5:1, presoak 1h；Then slurries are pumped into autoclave and carry out oxygen pressure acidleach, reaction temperature is 140 DEG C, pressure
Power is 0.8MPa, and the reaction time is 2h, and heat-insulation pressure keeping 1h after reaction completely, then press filtration obtains acid leaching residue and leachate；Leachate
Carry out eddy flow electrodeposition and obtain the concentration of Cu in electrodeposition lean solution and metallic copper, electrodeposition lean solution for 3.63g/L, acid leaching residue quality is
800.0g, acid leaching residue moisture percentage is 37.5%, acid leaching residue is converted into dry sample for 500g according to moisture percentage, sample preparation analysis is detected
Cu contents are that 7.64%, Pb contents are 16.85%.
(2) the electrodeposition lean solution for obtaining 2.70L steps (1) is added in the acid leaching residue that step (1) is obtained, now electrodeposition lean solution
It is 6 to be converted to the solid mass ratio of the liquid after dry sample according to moisture percentage with acid leaching residue:1, under normal temperature after agitator treating 30min, secondary pressure
Filter, obtains filtrate and filter residue；The volume of filtrate is 2.80L, and wherein Cu concentration is 10.57g/L；Filter residue quality is 610.0g, filter
Slag moisture percentage is 34.9%, and filter residue is converted into dry sample for 397.0g according to moisture percentage, and obtaining Cu contents after sample preparation analysis detection is
4.15%, Pb content are 17.12%；The wash-off rate for calculating copper in acid leaching residue according to copper content in acid leaching residue and filter residue is
56.9%.
(3) 800g cigarette ashes, 40g iron ores, 40g calcium oxide and 80g coke is added in the filter residue obtained to step (2) to carry out
Dispensing, turns in silica crucible after being well mixed, then silica crucible is placed in Muffle furnace and carries out reduction melting, reaction temperature
For 1200 DEG C, the reaction time is 2h, has reacted and metal 447.6g is obtained after rear stratification, cooling；After reduction melting, metal
The rate of recovery is 92.4%.
Process chart is as shown in Figure 1.
The filtrate produced in above-mentioned steps (2) is used as in the prepreg solution of next stage preimpregnation lead copper matte, and later stage, on
The filtrate produced in one stage etch (2) both functions as the prepreg solution preimpregnation lead copper matte in next stage step (1), in next stage
Remaining operation be same as a stage.
Embodiment 2
A kind of lead copper matte oxygen presses the handling process of acid leaching residue, comprises the following steps：
(1) lead copper matte is crushed and is milled to 100 mesh, added concentration and presoaked for 120g/L sulfuric acid, sulfuric acid and lead copper matte
The solid mass ratio of liquid be 4:1, presoak 1.5h；Then slurries are pumped into autoclave and carry out oxygen pressure acidleach, reaction temperature is 160 DEG C,
Pressure is 0.6MPa, and the reaction time is 2h, and heat-insulation pressure keeping 1.5h after reaction completely, then press filtration obtains acid leaching residue and leachate；Leaching
Go out liquid progress eddy flow electrodeposition and obtain the concentration of Cu in electrodeposition lean solution and metallic copper, electrodeposition lean solution for 4.58g/L, acid leaching residue quality is
800.0g, acid leaching residue moisture percentage is 35.7%, and acid leaching residue is converted into dry sample for 514.4g according to moisture percentage, sample preparation analysis detection
It is that 6.32%, Pb contents are 15.64% to obtain Cu contents.
(2) the electrodeposition lean solution for obtaining 2.29L steps (1) is added in the acid leaching residue that step (1) is obtained, now electrodeposition lean solution
It is 5 to be converted to the solid mass ratio of the liquid after dry sample according to moisture percentage with acid leaching residue:1, under normal temperature after agitator treating 30min, secondary pressure
Filter, obtains filtrate and filter residue；The volume of filtrate is 2.40L, and wherein Cu concentration is 10.84g/L；Filter residue quality is 620.0g, filter
Slag moisture percentage is 35.8%, and filter residue is converted into dry sample for 398.1g according to moisture percentage, sample preparation analysis detect Cu contents are
4.03%, Pb content are 17.20%；The wash-off rate for calculating copper in acid leaching residue according to copper content in acid leaching residue and filter residue is
49.4%.
(3) 800g cigarette ashes, 40g iron ores, 40g calcium oxide and 80g coke is added in the filter residue obtained to step (2) to carry out
Dispensing, turns in silica crucible after being well mixed, then silica crucible is placed in Muffle furnace and carries out reduction melting, reaction temperature
For 1200 DEG C, the reaction time is 2h, has reacted and metal 441.4g is obtained after rear stratification, cooling；After reduction melting, metal
The rate of recovery is 91.1%.
Process chart is as shown in Figure 1.
The filtrate produced in above-mentioned steps (2) is used as in the prepreg solution of next stage preimpregnation lead copper matte, and later stage, on
The filtrate produced in one stage etch (2) both functions as the prepreg solution preimpregnation lead copper matte in next stage step (1), in next stage
Remaining operation be same as a stage.
Embodiment 3
A kind of lead copper matte oxygen presses the handling process of acid leaching residue, comprises the following steps：
(1) lead copper matte is crushed and is milled to 100 mesh, added concentration and presoaked for 110g/L sulfuric acid, sulfuric acid and lead copper matte
The solid mass ratio of liquid be 4.5:1, presoak 1.2h；Then slurries are pumped into autoclave and carry out oxygen pressure acidleach, reaction temperature is 150
DEG C, pressure is 0.7MPa, and the reaction time is 2.5h, and heat-insulation pressure keeping 2h after reaction completely, then press filtration obtains acid leaching residue and leachate；
Leachate carries out eddy flow electrodeposition and obtains the concentration of Cu in electrodeposition lean solution and metallic copper, electrodeposition lean solution for 2.0g/L, and acid leaching residue quality is
800.0g, acid leaching residue moisture percentage is 40.0%, and acid leaching residue is converted into dry sample for 480.0g according to moisture percentage, sample preparation analysis detection
It is that 5.0%, Pb contents are 12.0% to obtain Cu contents.
(2) the electrodeposition lean solution for obtaining 2.32L steps (1) is added in the acid leaching residue that step (1) is obtained, now electrodeposition lean solution
It is 5.5 to be converted to the solid mass ratio of the liquid after dry sample according to moisture percentage with acid leaching residue:1, it is secondary under normal temperature after agitator treating 40min
Press filtration, obtains filtrate and filter residue；The volume of filtrate is 2.38L, and wherein Cu concentration is 6.7g/L；Filter residue quality is 616.0g, filter
Slag moisture percentage is 36.5%, and filter residue is converted into dry sample for 391.2g according to moisture percentage, sample preparation analysis detect Cu contents are
3.2%, Pb content are 12.5%；The wash-off rate for calculating copper in acid leaching residue according to copper content in acid leaching residue and filter residue is
47.8%.
(3) 950g cigarette ashes, 32g iron ores, 45g calcium oxide and 60g coke is added in the filter residue obtained to step (2) to carry out
Dispensing, turns in silica crucible after being well mixed, then silica crucible is placed in Muffle furnace and carries out reduction melting, reaction temperature
For 1150 DEG C, the reaction time is 3h, has reacted and metal 457.8g is obtained after rear stratification, cooling；After reduction melting, metal
The rate of recovery is 85.3%.
Process chart is as shown in Figure 1.
The filtrate produced in above-mentioned steps (2) is used as in the prepreg solution of next stage preimpregnation lead copper matte, and later stage, on
The filtrate produced in one stage etch (2) both functions as the prepreg solution preimpregnation lead copper matte in next stage step (1), in next stage
Remaining operation be same as a stage.
Embodiment 4
A kind of lead copper matte oxygen presses the handling process of acid leaching residue, comprises the following steps：
(1) lead copper matte is crushed and is milled to 100 mesh, added concentration and presoaked for 105g/L sulfuric acid, sulfuric acid and lead copper matte
The solid mass ratio of liquid be 5:1, presoak 1.5h；Then slurries are pumped into autoclave and carry out oxygen pressure acidleach, reaction temperature is 155 DEG C,
Pressure is 0.7MPa, and the reaction time is 2h, and heat-insulation pressure keeping 1.5h after reaction completely, then press filtration obtains acid leaching residue and leachate；Leaching
Go out liquid progress eddy flow electrodeposition and obtain the concentration of Cu in electrodeposition lean solution and metallic copper, electrodeposition lean solution for 6.0g/L, acid leaching residue quality is
800.0g, acid leaching residue moisture percentage is 30.0%, and acid leaching residue is converted into dry sample for 560.0g according to moisture percentage, sample preparation analysis detection
It is that 8.0%, Pb contents are 18.0% to obtain Cu contents.
(2) the electrodeposition lean solution for obtaining 2.56L steps (1) is added in the acid leaching residue that step (1) is obtained, now electrodeposition lean solution
It is 5 to be converted to the solid mass ratio of the liquid after dry sample according to moisture percentage with acid leaching residue:1, under normal temperature after agitator treating 60min, secondary pressure
Filter, obtains filtrate and filter residue；The volume of filtrate is 2.60L, and wherein Cu concentration is 14.8g/L；Filter residue quality is 634g, and filter residue contains
Wet rate is 37.3%, and filter residue is converted into dry sample for 397.5g according to moisture percentage, sample preparation analysis detect Cu contents are 5.2%,
Pb contents are 18.7%；The wash-off rate for calculating copper in acid leaching residue according to copper content in acid leaching residue and filter residue is 53.8%.
(3) 600g cigarette ashes, 47g iron ores, 32g calcium oxide and 99g coke is added in the filter residue obtained to step (2) to carry out
Dispensing, turns in silica crucible after being well mixed, then silica crucible is placed in Muffle furnace and carries out reduction melting, reaction temperature
For 1180 DEG C, the reaction time is 2.5h, has reacted and metal 368.1g is obtained after rear stratification, cooling；After reduction melting, gold
It is 93.2% to belong to the rate of recovery.
Process chart is as shown in Figure 1.
The filtrate produced in above-mentioned steps (2) is used as in the prepreg solution of next stage preimpregnation lead copper matte, and later stage, on
The filtrate produced in one stage etch (2) both functions as the prepreg solution preimpregnation lead copper matte in next stage step (1), in next stage
Remaining operation be same as a stage.
Embodiment 5
A kind of lead copper matte oxygen presses the handling process of acid leaching residue, comprises the following steps：
(1) lead copper matte is crushed and is milled to 100 mesh, added concentration and presoaked for 115g/L sulfuric acid, sulfuric acid and lead copper matte
The solid mass ratio of liquid be 4.2:1, presoak 1.4h；Then slurries are pumped into autoclave and carry out oxygen pressure acidleach, reaction temperature is 145
DEG C, pressure is 0.8MPa, and the reaction time is 2.7h, and heat-insulation pressure keeping 1h after reaction completely, then press filtration obtains acid leaching residue and leachate；
Leachate carries out eddy flow electrodeposition and obtains the concentration of Cu in electrodeposition lean solution and metallic copper, electrodeposition lean solution for 2.58g/L, and acid leaching residue quality is
800g, acid leaching residue moisture percentage is 32.6%, and acid leaching residue is converted into dry sample for 539.2g according to moisture percentage, sample preparation analysis detection
It is that 5.54%, Pb contents are 13.54% to obtain Cu contents.
(2) the electrodeposition lean solution for obtaining 2.54L steps (1) is added in the acid leaching residue that step (1) is obtained, now electrodeposition lean solution
It is 5.2 to be converted to the solid mass ratio of the liquid after dry sample according to moisture percentage with acid leaching residue:1, it is secondary under normal temperature after agitator treating 50min
Press filtration, obtains filtrate and filter residue；The volume of filtrate is 2.58L, and wherein Cu concentration is 9.0g/L；Filter residue quality is 612.0g, filter
Slag moisture percentage is 34.7%, and filter residue is converted into dry sample for 399.6g according to moisture percentage, sample preparation analysis detect Cu contents are
3.3%, Pb content are 14.1%；The wash-off rate for calculating copper in acid leaching residue according to copper content in acid leaching residue and filter residue is
55.9%.
(3) 800g cigarette ashes, 36g iron ores, 44g calcium oxide and 68g coke is added in the filter residue obtained to step (2) to carry out
Dispensing, turns in silica crucible after being well mixed, then silica crucible is placed in Muffle furnace and carries out reduction melting, reaction temperature
For 1160 DEG C, the reaction time is 2.7h, has reacted and metal 421.6g is obtained after rear stratification, cooling；After reduction melting, gold
It is 89.8% to belong to the rate of recovery.
Process chart is as shown in Figure 1.
The filtrate produced in above-mentioned steps (2) is used as in the prepreg solution of next stage preimpregnation lead copper matte, and later stage, on
The filtrate produced in one stage etch (2) both functions as the prepreg solution preimpregnation lead copper matte in next stage step (1), in next stage
Remaining operation be same as a stage.
Embodiment 6
A kind of lead copper matte oxygen presses the handling process of acid leaching residue, comprises the following steps：
(1) lead copper matte is crushed and is milled to 100 mesh, added concentration and presoaked for 120g/L sulfuric acid, sulfuric acid and lead copper matte
The solid mass ratio of liquid be 4.7:1, presoak 1h；Then slurries are pumped into autoclave and carry out oxygen pressure acidleach, reaction temperature is 150 DEG C,
Pressure is 0.7MPa, and the reaction time is 3h, and heat-insulation pressure keeping 2h after reaction completely, then press filtration obtains acid leaching residue and leachate；Leach
Liquid carries out eddy flow electrodeposition and obtains the concentration of Cu in electrodeposition lean solution and metallic copper, electrodeposition lean solution for 5.41g/L, and acid leaching residue moisture percentage is
38.2%, acid leaching residue quality is 800.0g, acid leaching residue is converted into dry sample for 494.4g according to moisture percentage, sample preparation analysis is detected
Cu contents are that 6.98%, Pb contents are 12.77%.
(2) the electrodeposition lean solution for obtaining 2.66L steps (1) is added in the acid leaching residue that step (1) is obtained, now electrodeposition lean solution
It is 6 to be converted to the solid mass ratio of the liquid after dry sample according to moisture percentage with acid leaching residue:1, under normal temperature after agitator treating 40min, secondary pressure
Filter, obtains filtrate and filter residue；The volume of filtrate is 2.70L, and wherein Cu concentration is 12.8g/L；Filter residue quality is 615.0g, filter residue
Moisture percentage is 31.7%, and filter residue is converted into dry sample for 420.0g according to moisture percentage, sample preparation analysis detect Cu contents are
4.5%, Pb content are 13.0%；The wash-off rate for calculating copper in acid leaching residue according to copper content in acid leaching residue and filter residue is
52.2%.
(3) 420g cigarette ashes, 46g iron ores, 37g calcium oxide and 92g coke is added in the filter residue obtained to step (2) to carry out
Dispensing, turns in silica crucible after being well mixed, then silica crucible is placed in Muffle furnace and carries out reduction melting, reaction temperature
For 1170 DEG C, the reaction time is 3h, has reacted and metal 257.7g is obtained after rear stratification, cooling；After reduction melting, metal
The rate of recovery is 90.9%.
Process chart is as shown in Figure 1.
The filtrate produced in above-mentioned steps (2) is used as in the prepreg solution of next stage preimpregnation lead copper matte, and later stage, on
The filtrate produced in one stage etch (2) both functions as the prepreg solution preimpregnation lead copper matte in next stage step (1), in next stage
Remaining operation be same as a stage.
The lead copper matte oxygen that the present invention is provided it can be seen from embodiment 1~6 presses the handling process of acid leaching residue, first to lead
Matte carries out oxygen pressure acidleach and handles to obtain leachate and acid leaching residue, using the electrodeposition lean solution washing acid obtained after leachate eddy flow electrodeposition
Phase analysis, not only washes out soluble copper sulphate in acid leaching residue, and due to containing in electrodeposition lean solution in acid hydrogen ion, hydrogen from
Son can carry out the soluble mantoquita of reaction generation with insoluble cupric oxide in acid leaching residue, that is, making acid leaching residue carry out two
Secondary response, is integrally improved the direct yield of metallic copper；The handling process using press filtration after the washing of electrodeposition lean solution, obtains acid leaching residue
Filter residue add reduction melting carried out after auxiliary material dispensing, i.e., using wet scrubbing press filtration-united technique of fire reduction melting, solve
The problem of acid leaching residue copper content is high, water capacity is big, has reclaimed valuable metal therein, economic value is notable to greatest extent；For
The moisture percentage of the acid leaching residue obtained after the oxygen pressure acidleach of reduction lead copper matte reclaims valuable gold therein suitably to carry out reduction melting
Category, coordinates the filter residue dispensing obtained after acid leaching residue washing, and add necessary slag former by adding existing dry cigarette ash etc.
Fire reduction melting is carried out with reducing agent, valuable metal is all recycled processing, the slag of gained can be used for construction material, be
The integrated treatment of the acid leaching residue obtained after the pressure acidleach of lead copper matte oxygen provides new thinking, with preferable directive significance.
Those of ordinary skills in the art should understand that：The discussion of any of the above embodiment is exemplary only, not
It is intended to imply that the scope of the present disclosure (including claim) is limited to these examples；Under the thinking of the present invention, above example
Or can also not be combined between the technical characteristic in be the same as Example, and there is the different aspect of the present invention as described above
Many other changes, in order to it is concise they provided not in details.Therefore, within the spirit and principles of the invention,
Any omission, modification, equivalent substitution, improvement for being made etc., should be included in the scope of the protection.
Claims (8)
1. a kind of lead copper matte oxygen presses the handling process of acid leaching residue, it is characterised in that comprise the following steps：
First stage:(1) lead copper matte is presoaked using prepreg solution, then oxygen pressure acidleach, acid leaching residue and leachate are obtained, then leachate
Eddy flow electrodeposition obtains electrodeposition lean solution and metallic copper；
(2) acid leaching residue that the electrodeposition lean solution washing step (1) obtained using step (1) is obtained, obtains filtrate and filter residue；
(3) add auxiliary material in the filter residue obtained to step (2) and carry out dispensing, then reduction melting obtains flue gas, lead bullion and slag；
Second stage：Using the filtrate produced in first stage step (2) as the prepreg solution in second stage step (1), remaining
Operate the same first stage；
Follow-up phase circulates second stage.
2. lead copper matte oxygen according to claim 1 presses the handling process of acid leaching residue, it is characterised in that the first stage step
Suddenly the prepreg solution in (1) is sulfuric acid, and the solid mass ratio of the liquid of sulfuric acid and lead copper matte is (4~5):1；The preimpregnation time is 1~1.5h.
3. lead copper matte oxygen according to claim 2 presses the handling process of acid leaching residue, it is characterised in that the concentration of the sulfuric acid
For 100~120g/L.
4. lead copper matte oxygen according to claim 1 presses the handling process of acid leaching residue, it is characterised in that in addition to the first stage,
Prepreg solution in step (1) is the middle filtrate produced of step (2), and the solid mass ratio of liquid of the filtrate and lead copper matte on last stage
For (4~5):1, the preimpregnation time is 1~1.5h.
5. lead copper matte oxygen according to claim 1 presses the handling process of acid leaching residue, it is characterised in that each stage etch
(1) when lead copper matte being carried out into oxygen pressure acidleach processing in, reaction temperature is 140~160 DEG C, and pressure is 0.6~0.8MPa, during reaction
Between be 2~3h；1~2h of heat-insulation pressure keeping after reaction completely.
6. lead copper matte oxygen according to claim 1 presses the handling process of acid leaching residue, it is characterised in that each stage etch
(2) the solid mass ratio of the liquid of electrodeposition lean solution and acid leaching residue is (5~6) in:1, the quality of the acid leaching residue be by acid leaching residue according to containing
Wet rate is converted to the quality of acid leaching residue dry sample；Wash time is 30~60min.
7. lead copper matte oxygen according to claim 1 presses the handling process of acid leaching residue, it is characterised in that each stage etch
(3) auxiliary material added in is cigarette ash, iron ore, calcium oxide and coke；The addition of cigarette ash is 1~2.5 times of filter residue quality, iron
The addition of ore is the 8~12% of filter residue quality, and the addition of calcium oxide is the 8~12% of filter residue quality, the addition of coke
Measure as the 15~25% of filter residue quality；The quality of the filter residue is the quality that filter residue is converted to filter residue dry sample according to moisture percentage.
8. lead copper matte oxygen according to claim 1 presses the handling process of acid leaching residue, it is characterised in that each stage etch
(3) when carrying out reduction melting to filter residue and auxiliary material in, reaction temperature is 1150~1200 DEG C, and the reaction time is 2~3h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108285982A (en) * | 2018-03-06 | 2018-07-17 | 中国恩菲工程技术有限公司 | A method of recycling copper, cobalt from Cu-S ore |
| CN112626340A (en) * | 2020-12-07 | 2021-04-09 | 阳谷祥光铜业有限公司 | Treatment method of copper anode plate washing slag |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS568899B2 (en) * | 1975-02-26 | 1981-02-26 | ||
| CN102051478A (en) * | 2010-11-28 | 2011-05-11 | 郴州市金贵银业股份有限公司 | Wet process for treating lead copper matte |
| CN103320614A (en) * | 2013-07-10 | 2013-09-25 | 郴州市金贵银业股份有限公司 | Lead matte pyrogenic process treatment technology |
| CN104233372A (en) * | 2014-09-30 | 2014-12-24 | 济源市欣欣实业有限公司 | Method for recovering copper from lead matte |
| CN104789783A (en) * | 2015-05-18 | 2015-07-22 | 郴州市金贵银业股份有限公司 | Process for selective efficient copper extraction and comprehensive recovery from lead copper matte |
| CN104831078A (en) * | 2015-04-21 | 2015-08-12 | 云南驰宏锌锗股份有限公司 | Method for processing zinc wet smelting slag by use of warm slag side blowing reducing furnace |
-
2017
- 2017-06-29 CN CN201710516340.3A patent/CN107267761B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS568899B2 (en) * | 1975-02-26 | 1981-02-26 | ||
| CN102051478A (en) * | 2010-11-28 | 2011-05-11 | 郴州市金贵银业股份有限公司 | Wet process for treating lead copper matte |
| CN103320614A (en) * | 2013-07-10 | 2013-09-25 | 郴州市金贵银业股份有限公司 | Lead matte pyrogenic process treatment technology |
| CN104233372A (en) * | 2014-09-30 | 2014-12-24 | 济源市欣欣实业有限公司 | Method for recovering copper from lead matte |
| CN104831078A (en) * | 2015-04-21 | 2015-08-12 | 云南驰宏锌锗股份有限公司 | Method for processing zinc wet smelting slag by use of warm slag side blowing reducing furnace |
| CN104789783A (en) * | 2015-05-18 | 2015-07-22 | 郴州市金贵银业股份有限公司 | Process for selective efficient copper extraction and comprehensive recovery from lead copper matte |
Non-Patent Citations (2)
| Title |
|---|
| 杨国才: "《闪速炼铜工艺与控制》", 31 December 2010 * |
| 王毓等: "《铜矿选矿技术》", 31 January 2012 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108285982A (en) * | 2018-03-06 | 2018-07-17 | 中国恩菲工程技术有限公司 | A method of recycling copper, cobalt from Cu-S ore |
| CN112626340A (en) * | 2020-12-07 | 2021-04-09 | 阳谷祥光铜业有限公司 | Treatment method of copper anode plate washing slag |
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Inventor after: Tan Lin Inventor after: Yuan Ninghui Inventor after: Jiang Zhaohui Inventor after: Xie Zhaofeng Inventor after: Huang Qianjun Inventor before: Yuan Ninghui Inventor before: Jiang Zhaohui Inventor before: Xie Zhaofeng Inventor before: Huang Qianjun Inventor before: Tan Lin |