CN107190143A - The technique that a kind of Whote-wet method reclaims valuable element in complicated low-grade sulphide ore - Google Patents
The technique that a kind of Whote-wet method reclaims valuable element in complicated low-grade sulphide ore Download PDFInfo
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
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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
- C22B13/04—Obtaining lead by wet processes
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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
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- 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
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
- C22B15/0091—Treating solutions by chemical methods by cementation
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/24—Obtaining zinc otherwise than by distilling with leaching with alkaline solutions, e.g. ammonia
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/26—Refining solutions containing zinc values, e.g. obtained by leaching zinc ores
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
- C22B3/46—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes by substitution, e.g. by cementation
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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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/02—Obtaining antimony
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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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/06—Obtaining bismuth
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- Y02P10/20—Recycling
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Abstract
A kind of Whote-wet method reclaims the technique of valuable element in complicated low-grade sulphide ore, and technique is:It will be sieved after raw material crushing grinding, carry out pressure oxidation leaching after being sized mixing with sodium hydroxide solution, obtain alkali immersion liquid and alkali phase analysis；Alkali immersion liquid is acidified to obtain lead sulfate product and heavy lead liquid, and heavy lead liquid substep controlling potential reduces to obtain liquid after impure selenium powder, coarse tellurium powder and reduction；Alkali phase analysis soaks copper with sulfuric acid solution, must soak copper ashes and copper leaching liquid；The copper ashes acid immersion antimony bismuth of chloride ion-containing is soaked, antimony liquid and leaching antimony slag must be soaked, leaching antimony slag send noble metal to reclaim, and leaching antimony liquid adjusted stepwise pH obtains antimony slag and bismuth slag；Copper leaching liquid regulation pH obtains scum and except iron liquid, and scum is wastewater treatment additive, except iron liquid with zinc dust precipitation obtains copper powder and displaced liquid；Liquid and displaced liquid merge after reduction, and condensing crystallizing obtains white vitriol.Present invention process synthetical recovery effect is good, strong to adaptability to raw material, process cleans environmental protection, and low for equipment requirements, implement scale size is adjustable, with stronger practicality.
Description
Technical field
The invention belongs to non-ferrous metal hydrometallurgy field, and in particular to reclaim complicated low-grade sulphide ore to a kind of Whote-wet method
The technique of middle valuable element.
Background technology
By the exploitation and utilization in nearly century more than two, worldwide high-quality nonferrous metal resources significantly subtract
It is few, but modern society is growing to the demand of nonferrous metal product, therefore, how to utilize the low-grade mineral products inferior of complexity
The problem that smelting field of nonferrous metal need to be paid close attention to and study is turned into.
Non-ferrous minerals belong to sulphide ore mostly, and for the processing of complicated low-grade sulphide ore, large enterprise generally adopts
It is thermal process, such as when handling lead copper matte, production is bessemerized by broken-milling-shaft smelting-by certain enterprise
Go out blister copper, then refined copper is produced by electrorefining, thermal process has metal and separates incomplete, environment to some extent
The problems such as seriously polluted, technological process length, production cost are high, energy consumption is big, and the load of enterprise's acid making system is required, and
Medium-sized and small enterprises are general to be sold to large enterprise using its complicated low-grade sulphide ore as raw material, due to this mineral be unsatisfactory for it is any
One class concentrate standard, therefore the valuation coefficient of its contained metal is all often very low, or even some metals are completely without charge, from
And cause the huge economic losses of medium-sized and small enterprises.
In recent years, with pressure leaching technology and equipment development with it is ripe, using pressure leaching as the sulphide ore of core at
Science and engineering skill obtains growing interest, and copper pressure oxidation in bismuth matte is leached, obtained by such as patent CN105543479.A in sulfuric acid medium
To the leachate and the leached mud such as leaded, silver-colored, bismuth of sulfur acid copper, copper is reclaimed by electro-deposition method in leachate, and leached mud is returned
Return silver converter and reclaim the silver-colored bismuth of lead；Patent CN1060482518.A crushes setting form after fine grinding together with sulfuric acid in autoclave, so
After add or be passed through oxide isolation, by copper and arsenic Oxidation Leaching, leachate again with iron compound carry out pressurized high-temperature sink arsenic, obtain
Dearsenification liquid and solid arsenic slag, dearsenification liquid cyclone electrolytic cell obtain tough cathode；Patent CN102586600.B is under strong basicity system by lead ice
Copper pressure oxidation is leached, and the sulphur in raw material is converted into sulfate and removed, leached mud is leached carry out again at ambient pressure with diluted acid
Cu-Pb separation, electrodeposition obtains tough cathode after the obtained purified removal of impurities of cupric leachate, and leaded leached mud returns to lead smelting system；
Patent CN102230083.B uses NH3-(NH4)2SO4Alkalescent compound system carries out oxygen pressure at 110 ~ 200 DEG C to lead copper matte
Leach, copper in raw material is entered solution with ammonia coordination, other metal sulfides are then converted into oxide/hydroxide and sulphur,
Stayed with gold, silver etc. in leached mud, leachate carries out electrodeposition after extracting and purifying and obtains qualified tough cathode, leached mud returns to refining
Lead system.The present invention also provides a kind of Whote-wet method using pressure leaching as core and reclaims valuable element in complicated low-grade sulphide ore
Technique, but from unlike other techniques：Present invention process synthetical recovery effect is good, can the complicated raw material of processes composition, and
And process cleans environmental protection, low is required to equipment investment, implement scale is changeable, is particularly suitable for no pyrogenic process system or acid making system
Small business use.
The content of the invention
The present invention provides the technique that a kind of Whote-wet method reclaims valuable element in complicated low-grade sulphide ore, with other technique phases
Than, the element synthetical recovery effect of present invention process is good, can treatment group into extremely complex raw material, and process cleans environmental protection,
Low is required to equipment investment, implement scale is changeable, and the small business for being particularly suitable for no pyrogenic process system or acid making system uses.
The technical scheme is that：A kind of Whote-wet method reclaims the technique of valuable element in complicated low-grade sulphide ore, bag
Include the step of next coming in order are carried out：
Step 1：50 mesh sieves will be crossed after complicated low-grade sulphide ore drying grinding；
Step 2：Mineral after sieving pour into progress pressure oxidation leaching in reactor after being sized mixing with sodium hydroxide solution, obtain alkali leaching
Liquid and alkali phase analysis；
Step 3：Sulfuric acid is added into alkali immersion liquid to pH value of solution≤7, lead sulfate precipitation and heavy lead liquid is obtained, lead sulfate precipitation is with dilute
Dry, sold as lead sulfate product after sulfuric acid scrubbing.The reducing agent without heavy metal element is added in heavy lead liquid, and controls electricity
Position carries out step-by-step reduction, obtains liquid after impure selenium powder, coarse tellurium powder and reduction；
Step 4：Alkali phase analysis soaks copper with sulfuric acid solution, obtains copper leaching liquid and leaching copper ashes；
Step 5：The acid immersion antimony bismuth of copper ashes chloride ion-containing is soaked, leaching antimony liquid is obtained and soaks antimony slag, soak antimony liquid sodium hydroxide
Solution adjusted stepwise pH obtains liquid after antimony slag, bismuth slag and bismuth are hydrolyzed, and antimony slag and bismuth slag send antimony bismuth to extract, and liquid returns to antimony after bismuth hydrolysis
Bismuth is leached, and leaching antimony slag send noble metal to reclaim；
Step 6：Copper leaching liquid adjusts pH to 3 ~ 4 with alkaline matter, obtains scum and except iron liquid, scum is sent as wastewater treatment additive
Go out, copper sponge and displaced liquid are obtained except iron liquid adds zinc dust precipitation；
Step 7：Displaced liquid in liquid and step 6 after reduction in step 3 is merged, condensing crystallizing obtains white vitriol production
Product, crystalline mother solution send wastewater treatment.
Further, complicated low-grade sulphide ore refers to that some sources are polynary, constitute various but be unsatisfactory for any one in step 1
The sulfide mineral of class concentrate standard, such as copper and zinc bulk concentrate, lead copper matte, bismuth matte, setting form, antimony matte, matte iron；
Further, concentration of sodium hydroxide solution is 70 ~ 140g/L in step 2, and it is 4.0 ~ 20.0 that liquid-solid ratio is leached in pressure oxidation:1,
Reaction temperature is 100 ~ 160 DEG C, and 2.0 ~ 8.0h of reaction time, 0.15 ~ 0.95MPa of partial pressure of oxygen, 1.05 ~ 1.35MPa of stagnation pressure are stirred
200 ~ 700r/min of mix rotating speed.
Further, reduction temperature described in step 3 is 50 ~ 90 DEG C, and step reduction controlling potential is 450 ~ 650mV, is obtained
Impure selenium powder, two steps reduction controlling potential is 160 ~ 350mV, obtains coarse tellurium powder, and the reducing agent without heavy metal element is sulfurous acid
One or more of combinations in sodium, sodium hydrogensulfite, sodium pyrosulfite, pyrosulfurous acid hydrogen sodium, sulfur dioxide and oxalic acid.
Further, sulfuric acid solution concentration is 100 ~ 300g/L, liquid-solid ratio 3.0 ~ 12.0 in step 4:1,40 ~ 90 DEG C of temperature,
0.5 ~ 4.0h of time.
Further, liquid-solid ratio 5.0 ~ 15.0 in step 5:1,40 ~ 90 DEG C of temperature, 0.5 ~ 4.0h of the time, a step section pH is
0.5 ~ 2.5, antimony slag is obtained, two step section pH are 3.0 ~ 5.0, obtain bismuth slag, the Acidic Liquid of the chloride ion-containing is 30 ~ 220g/L hydrochloric acid
The solution of solution and/or 50 ~ 350g/L sodium chloride and 50 ~ 300g/L sulfuric acid.
Further, step 6 neutral and alkali material be sodium hydrate solid, sodium hydroxide solution, sodium carbonate, sodium carbonate liquor,
One or more of combinations in milk of lime, zinc dust precipitation temperature is 30 ~ 90 DEG C.
Compared with other techniques, the beneficial effect of present invention process and have the prominent advantages that：
1）Element synthetical recovery effect is good, and Cu, Pb, Zn, Se, Te, Sb, Bi, Fe are produced with copper sponge, lead sulfate respectively in raw material
Product, white vitriol product, impure selenium powder, coarse tellurium powder, antimony slag, the form of bismuth slag and wastewater treatment additive are reclaimed, and direct yield is equal
More than 90%, the concentration of precious metal such as Au, Ag can further handle recovery noble metal into high-grade noble metal concentrate.
2）Strong to adaptability to raw material, present invention process all has very to element and the complicated low-grade sulphide ore of thing phase composition
Good treatment effect；
3）Substantially produced without waste gas and waste residue, process cleans environmental protection；
4）Simple to operate, implement scale size is adjustable.
Brief description of the drawings
Fig. 1 is the flow chart that a kind of Whote-wet method of the invention reclaims the technique of valuable element in complicated low-grade sulphide ore.
Embodiment
The present invention is described in further detail by the following examples, but the scope of the present invention is not limited to these implementations
Example.
Embodiment 1
Take 300g crushing grindings to cross the lead copper matte of 50 mesh sieves, be to pour into add after 90g/L sodium hydroxide solutions are sized mixing with 3.0L concentration
Press in reactor, kettle opens stirring after installing, rotating speed 300r/min, be filled with oxygen and be depressed into after 0.65MPa and be warming up to 120 DEG C, always
Press as 1.15MPa, kettle discharging is unloaded after reaction 3.0h, alkali immersion liquid and alkali phase analysis is filtered to obtain.Alkali immersion liquid adds sulfuric acid to adjust to pH=6, mistake
Filter, obtains lead sulfate precipitation and heavy lead liquid, lead sulfate precipitation dries to obtain lead sulfate product, lead recovery after being washed with dilute sulfuric acid
99.6%, heavy lead liquid is heated to 60 DEG C, monitors reaction solution current potential when adding oxalic acid solid, stops when reaction solution current potential is 600mV
Only add oxalic acid, filter impure selenium powder and selenium reduction after liquid, selenium reduction after liquid be heated to after 60 DEG C continuously adding oxalic acid solid, directly
To reaction solution current potential be 300mV when stop, filter, obtain coarse tellurium powder and reduction after liquid.Alkali phase analysis presses liquid-solid ratio 5.0:1 and 150g/L
Sulfuric acid solution mixing, be warming up to 70 DEG C, separation of solid and liquid after stirring 1h obtains copper leaching liquid and leaching copper ashes.Soak copper ashes and press liquid-solid ratio
8.0:1 mixes with 110g/L hydrochloric acid solution, is warming up to separation of solid and liquid after 60 DEG C, stirring 1h, must soak antimony liquid and leaching antimony slag, soak antimony
Slag send noble metal to reclaim, separation of solid and liquid behind leaching antimony liquid hydrogenation sodium hydroxide solution regulation pH=1.0, obtains liquid after antimony slag and antimony hydrolysis,
Liquid continues to be hydrogenated with separation of solid and liquid behind sodium hydroxide solution regulation pH=3.0 after antimony hydrolysis, liquid after bismuth slag and bismuth hydrolysis is obtained, after bismuth hydrolysis
Liquid returns to antimony bismuth and leached.Copper leaching liquid makees separation of solid and liquid after adding soda ash solid regulation pH value of solution=3.5, obtains scum and except iron liquid, removes
Iron liquid adds zinc powder in 60 DEG C and enters line replacement, obtains copper sponge and displaced liquid, copper recovery 99.2%.Liquid after reduction and it will put
Change rear liquid to merge, condensing crystallizing obtains white vitriol product and crystalline mother solution, and crystalline mother solution send wastewater treatment.
Embodiment 2
Take 300g crushing grindings to cross the copper and zinc bulk concentrate of 50 mesh sieves, be after 110g/L sodium hydroxide solutions are sized mixing with 2.4L concentration
Pour into compressive reaction kettle, kettle opens stirring after installing, rotating speed 500r/min, be filled with oxygen and be depressed into after 0.85MPa and be warming up to 135
DEG C, stagnation pressure is 1.35MPa, and kettle discharging is unloaded after reaction 4.5h, alkali immersion liquid and alkali phase analysis is filtered to obtain.Alkali immersion liquid adds sulfuric acid to adjust to pH
=3, filtering obtains lead sulfate precipitation and heavy lead liquid, lead sulfate precipitation dries to obtain lead sulfate product after being washed with dilute sulfuric acid, heavy lead liquid
70 DEG C are heated to, reaction solution current potential is monitored when adding sodium sulfite, stops adding when reaction solution current potential is 550mV, filtering
Liquid after impure selenium powder and selenium reduction is obtained, liquid continuously adds sodium sulfite after being heated to 75 DEG C after selenium reduction, until reaction solution current potential is
Stop during 220mV, filter, obtain liquid after coarse tellurium powder and reduction.Alkali phase analysis presses liquid-solid ratio 8.0:1 and 210g/L sulfuric acid solution is mixed
Close, be warming up to separation of solid and liquid after 60 DEG C, stirring 1.5h, obtain copper leaching liquid and leaching copper ashes.Soak copper ashes and press liquid-solid ratio 10.0:1 with containing
The solution mixing of 230g/L sodium chloride and 180g/L sulfuric acid, is warming up to separation of solid and liquid after 55 DEG C, stirring 2h, must soak antimony liquid and leaching antimony
Slag, leaching antimony slag send noble metal to reclaim, separation of solid and liquid behind leaching antimony liquid hydrogenation sodium hydroxide solution regulation pH=1.5, obtains antimony slag and antimony water
Liquid after solution, liquid continues to be hydrogenated with separation of solid and liquid behind sodium hydroxide solution regulation pH=4.0 after antimony hydrolysis, obtains liquid, bismuth after bismuth slag and bismuth hydrolysis
Liquid returns to antimony bismuth and leached after hydrolysis.Copper leaching liquid makees separation of solid and liquid after adding piece alkali regulation pH value of solution=3.0, obtains scum and except iron liquid,
Enter line replacement except iron liquid adds zinc powder in 75 DEG C, obtain copper sponge and displaced liquid, copper recovery 99.4%.Will reduction after liquid and
Displaced liquid merges, and condensing crystallizing obtains white vitriol product and crystalline mother solution, zinc recovery 92.7%, and crystalline mother solution send useless
Water process.
Claims (6)
1. the technique that a kind of Whote-wet method reclaims valuable element in complicated low-grade sulphide ore, it is characterised in that including next coming in order
Progress the step of：
Step 1：50 mesh sieves are crossed after raw material stoving is ground；
Step 2：Raw material after sieving pours into progress pressure oxidation leaching in reactor after being sized mixing with sodium hydroxide solution, obtain alkali leaching
Liquid and alkali phase analysis；
Step 3：Sulfuric acid is added into alkali immersion liquid to pH value of solution≤7, lead sulfate precipitation and heavy lead liquid is obtained, lead sulfate precipitation is with dilute
Dry, sold as lead sulfate product after sulfuric acid scrubbing；The reducing agent without heavy metal element is added in heavy lead liquid, and controls electricity
Position carries out step-by-step reduction, obtains liquid after impure selenium powder, coarse tellurium powder and reduction；
Step 4：Alkali phase analysis soaks copper with sulfuric acid solution, obtains copper leaching liquid and leaching copper ashes；
Step 5：The acid immersion antimony bismuth of copper ashes chloride ion-containing is soaked, leaching antimony liquid is obtained and soaks antimony slag, soak antimony liquid sodium hydroxide
Solution adjusted stepwise pH obtains liquid after antimony slag, bismuth slag and bismuth are hydrolyzed, and antimony slag and bismuth slag send antimony bismuth to extract, and liquid returns to antimony after bismuth hydrolysis
Bismuth is leached, and leaching antimony slag send noble metal to reclaim；
Step 6：Copper leaching liquid adjusts pH to 3 ~ 4 with alkaline matter, obtains scum and except iron liquid, scum is sent as wastewater treatment additive
Go out, copper sponge and displaced liquid are obtained except iron liquid adds zinc dust precipitation；
Step 7：Displaced liquid in liquid and step 6 after reduction in step 3 is merged, condensing crystallizing obtains white vitriol production
Product, crystalline mother solution send wastewater treatment.
2. technique according to claim 1, it is characterised in that：The complicated low-grade sulphide ore be copper and zinc bulk concentrate,
Lead copper matte, bismuth matte, setting form, antimony matte or matte iron.
3. technique according to claim 1, it is characterised in that：In the step 2 pressure oxidation leach liquid-solid ratio be 4.0 ~
20.0:1, reaction temperature is 100 ~ 160 DEG C, 2.0 ~ 8.0h of reaction time, 0.15 ~ 0.95MPa of partial pressure of oxygen, stagnation pressure 1.05 ~
1.35MPa, 200 ~ 700r/min of speed of agitator, concentration of sodium hydroxide solution are 70 ~ 140g/L.
4. technique according to claim 1, it is characterised in that：Reduction temperature is 50 ~ 90 DEG C in the step 3, and a step is also
Former controlling potential is 450 ~ 650mV, obtains impure selenium powder, two steps reduction controlling potential is 160 ~ 350mV, obtains coarse tellurium powder；Be free of
The reducing agent of heavy metal element is sodium sulfite, sodium hydrogensulfite, sodium pyrosulfite, pyrosulfurous acid hydrogen sodium, sulfur dioxide and grass
One or more of combinations in acid.
5. technique according to claim 1, it is characterised in that：Liquid-solid ratio 5.0 ~ 15.0 in the step 5:1, temperature 40 ~
90 DEG C, 0.5 ~ 4.0h of time, a step section pH is 0.5 ~ 2.5, obtains antimony slag, and two step section pH are 3.0 ~ 5.0, obtain bismuth slag, described
The Acidic Liquid of chloride ion-containing is the solution of 30 ~ 220g/L hydrochloric acid solutions and/or 50 ~ 350g/L sodium chloride and 50 ~ 300g/L sulfuric acid.
6. technique according to claim 1, it is characterised in that：Step 6 neutral and alkali material is sodium hydrate solid, hydroxide
One or more of combinations in sodium solution, sodium carbonate, sodium carbonate liquor, milk of lime, zinc dust precipitation temperature is 30 ~ 90 DEG C.
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| CN113148963A (en) * | 2021-03-15 | 2021-07-23 | 广东先导稀贵金属材料有限公司 | Method for separating and recovering tellurium and selenium |
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