CN108277357A - A kind of method of steel works sintering head dedusting ash separation and recovery silver and lead - Google Patents
A kind of method of steel works sintering head dedusting ash separation and recovery silver and lead Download PDFInfo
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- CN108277357A CN108277357A CN201810099938.1A CN201810099938A CN108277357A CN 108277357 A CN108277357 A CN 108277357A CN 201810099938 A CN201810099938 A CN 201810099938A CN 108277357 A CN108277357 A CN 108277357A
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- 229910052709 silver Inorganic materials 0.000 title claims abstract description 48
- 239000004332 silver Substances 0.000 title claims abstract description 48
- 238000005245 sintering Methods 0.000 title claims abstract description 44
- 238000000926 separation method Methods 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000011084 recovery Methods 0.000 title claims abstract description 28
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 24
- 239000010959 steel Substances 0.000 title claims abstract description 24
- 238000002386 leaching Methods 0.000 claims abstract description 46
- 239000007788 liquid Substances 0.000 claims abstract description 43
- 238000002156 mixing Methods 0.000 claims abstract description 26
- 239000002893 slag Substances 0.000 claims abstract description 26
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 22
- LWUVWAREOOAHDW-UHFFFAOYSA-N lead silver Chemical compound [Ag].[Pb] LWUVWAREOOAHDW-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000010413 mother solution Substances 0.000 claims abstract description 18
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 claims abstract description 16
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000004064 recycling Methods 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 11
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 11
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 11
- 239000011701 zinc Substances 0.000 claims abstract description 11
- 238000002425 crystallisation Methods 0.000 claims abstract description 10
- 230000003647 oxidation Effects 0.000 claims abstract description 10
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 9
- 239000011591 potassium Substances 0.000 claims abstract description 9
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 9
- 239000011734 sodium Substances 0.000 claims abstract description 9
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 235000012501 ammonium carbonate Nutrition 0.000 claims abstract description 8
- 238000006073 displacement reaction Methods 0.000 claims abstract description 8
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims abstract description 7
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 43
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 38
- 229910052742 iron Inorganic materials 0.000 claims description 19
- 230000035484 reaction time Effects 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- 239000000908 ammonium hydroxide Substances 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 239000012295 chemical reaction liquid Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000460 chlorine Substances 0.000 abstract description 6
- 229910052801 chlorine Inorganic materials 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 6
- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 abstract description 3
- 230000002411 adverse Effects 0.000 abstract description 3
- PRKQVKDSMLBJBJ-UHFFFAOYSA-N ammonium carbonate Chemical class N.N.OC(O)=O PRKQVKDSMLBJBJ-UHFFFAOYSA-N 0.000 abstract description 3
- 235000011162 ammonium carbonates Nutrition 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 abstract description 3
- RYZCLUQMCYZBJQ-UHFFFAOYSA-H lead(2+);dicarbonate;dihydroxide Chemical compound [OH-].[OH-].[Pb+2].[Pb+2].[Pb+2].[O-]C([O-])=O.[O-]C([O-])=O RYZCLUQMCYZBJQ-UHFFFAOYSA-H 0.000 abstract description 3
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 abstract description 3
- 229910001958 silver carbonate Inorganic materials 0.000 abstract description 3
- 230000001131 transforming effect Effects 0.000 abstract description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 5
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 4
- 150000001340 alkali metals Chemical class 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- 239000004568 cement Substances 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 235000015096 spirit Nutrition 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- IWLXWEWGQZEKGZ-UHFFFAOYSA-N azane;zinc Chemical compound N.[Zn] IWLXWEWGQZEKGZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- -1 cuprammonium Chemical compound 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 238000005406 washing Methods 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
- C22B7/02—Working-up flue dust
-
- 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
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention relates to a kind of methods of steel works sintering head dedusting ash separation and recovery silver and lead, belong to resource comprehensive utilization technical field.Sintering machine head end dedusting ash is uniformly mixed with ammonium carbonate first, adds water to size mixing and is leached to obtain lead silver enrichment slag；Ammonium chloride is added into obtained lead silver enrichment slag, and sodium chlorate or hypochlorite oxidation agent carry out two sections of counter flow oxidations and leach, one section of obtained leachate is using metallic lead displacement recycling silver, output sponge silver and displaced liquid, for displaced liquid using crystallisation by cooling output lead chloride, crystalline mother solution returns to two sections of leachings；Two sections are leached two sections of obtained leachates and return to one section of leaching.The invention firstly uses ammonium carbonates as transforming agent and leaching agent, by in material lead and silver be converted into ceruse and silver carbonate, simultaneously by the harmful elements separated and dissolved such as soluble zinc, potassium, sodium and chlorine, adverse effect of these foreign ions to lead silver package etc. is avoided, and these impurity is avoided to be enriched in leaching finishing slag.
Description
Technical field
The present invention relates to a kind of methods of steel works sintering head dedusting ash separation and recovery silver and lead, belong to resource comprehensive and return
Receive technical field.
Background technology
The steel and iron industry production in China mainly uses " blast furnace ironmaking-oxygen top blown converter steel making " technological process.Iron ore
Sintering is the important link in steel production.Sintering machine head end dedusting ash is that the sintering flue gas of iron ore sintering head output passes through electricity
The dust that deduster is collected, yield account for about the 2% ~ 4% of Sintering Yield, the annual resulting dedusting ash total amount in the whole nation
It is 15,000,000 tons or so.The pollution control of sintering machine head end dedusting ash and valuable resource synthetical recovery are major iron and steel enterprise's energy-saving and emission-reduction
Important topic.
Currently, most of steel plant are directly incorporated sintering feed again using sintering flue gas dedusting ash as Iron Ore Powder.This method
Iron in it can utilize dedusting ash and carbon realize the synthetical recovery of iron and carbon, but valuable metal lead and silver cannot be returned
It receives；Simultaneously because not carrying out separating treatment to the harmful element of blast furnace to zinc contained therein, alkali metal, chlorine element etc. so that
Continuous circulation collection during the sintering of these objectionable impurities elements and blast furnace ironmaking, influences the normal production of iron and steel enterprise, together
When also bring new environmental issue.
Currently, the method for recycling valuable metal in the slave sintering machine head end dedusting ash reported and detaching harmful element is mainly
Recycle the elements such as potassium, sodium and iron." the side of sintering machine head end dedusting ash extraction k-na salt that patent application 201410397569.6 provides
Method " is to mix sintering machine head end ash with distilled water, and suds are added and are disperseed, by leaching, removal of impurities, filtering is evaporated
Etc. processes, obtain k-na salt.This method is simple for process, but is unable to comprehensive recovery of lead and silver.Patent application 201410248826.X
" a kind of technique and system removing alkali metal in smelting iron and steel dedusting ash " provided, is to mix smelting iron and steel dedusting ash with water
It sizes mixing, carries out water logging, recycle the existing concentration in ore dressing plant and filter plant to carry out thickening filtration, it is former to obtain 12% ~ 15% sintering
Material.This method can effectively remove the alkali metal in dedusting ash, but lead silver cannot recycle.Patent application 201610791064.7
There is provided " a method of recycling iron ore concentrate and non-ferrous metal using sintering machine head end ash ", it is that sintering machine head end ash is sized mixing with water,
By gravity separation, low intensity magnetic separation, closed circuit flotation, lead concentrate and non-ferrous metal enriched substance are obtained.This method can recycle
Iron ore concentrate, and the enriched substance of non-ferrous metal is obtained, but it is unable to output nonferrous metal product.Patent application 201410048263.X is public
Open " from steel works sintering dust recycle silver, copper and zinc method ", be will be sintered ash carry out first washing remove it is therein can
Molten alkali metal, then using ammonium hydroxide complexing extraction, obtained argentiferous ammonia, cuprammonium, zinc ammonia complex mixed solution use formaldehyde again
Or acetaldehyde reduction recycling silver.This method can realize the synthetical recovery of silver, copper and zinc, but it is complexed under conditions of pH is 10 ~ 13
Extraction, ammonia volatilization is serious, severe operational environment, and as reducing agent, there are security risks using formaldehyde or acetaldehyde.
Therefore, new technique and technological process are developed, realize the synthetical recovery of lead silver in sintering machine head end dedusting ash and is harmful to
The separation of element, it has also become the important technology problem that iron and steel enterprise faces.
Invention content
The problem of existing for the above-mentioned prior art and deficiency, the present invention provide a kind of steel works sintering head dust setting ash
Method from recycling silver and lead.The invention firstly uses ammonium carbonates as transforming agent and leaching agent, by the lead and silver turn in material
Ceruse and silver carbonate are turned to, while by the harmful elements separated and dissolved such as soluble zinc, potassium, sodium and chlorine, avoiding these impurity
The adverse effect of ion pair lead silver package etc., and these impurity is avoided to be enriched in leaching finishing slag, leaching finishing slag can return
Sintered material.High, the high feature of product purity with lead silver comprehensive recovery.The invention is realized by the following technical scheme.
A kind of method of steel works sintering head dedusting ash separation and recovery silver and lead, specific steps include：It will burn first
Knot head dedusting ash is uniformly mixed with ammonium carbonate, is added water to size mixing and is leached to obtain lead silver enrichment slag；To obtained lead silver enrichment
Ammonium chloride and sodium chlorate are added in slag or hypochlorite oxidation agent carries out two sections of counter flow oxidations and leaches, one section of obtained leaching
Liquid is using metallic lead displacement recycling silver, output sponge silver and displaced liquid, displaced liquid using crystallisation by cooling output lead chloride,
Crystalline mother solution returns to two sections of leachings；Two sections are leached two sections of obtained leachates and return to one section of leaching.
It is as follows：
Step 1, alkaline leaching：It is 1 in mass ratio by sintering machine head end dedusting ash and ammonium carbonate:1 ~ 4 be uniformly mixed obtain mixture
Material is 1 by solid-to-liquid ratio:2 ~ 8g/mL adds water to size mixing, and is 25 DEG C ~ 95 DEG C in temperature, speed of agitator is 100r/min ~ 600r/min
Under conditions of leached, control reaction time 60min ~ 300min, slurry pH be 7.5 ~ 9.8, after reaction liquid divide admittedly
It is enriched with slag and alkaline leaching liquid from lead silver is obtained；
Step 2, one section of leaching：The lead silver enrichment slag that step 1 is obtained is 1 in mass ratio with ammonium chloride:1 ~ 4 is uniformly mixed, and presses
Solid-to-liquid ratio is 1:Two sections of leachates that step 3 output is added in 3 ~ 15g/mL are sized mixing, and are 60 DEG C ~ 120 DEG C in temperature, speed of agitator is
Leached under conditions of 100r/min ~ 600r/min, the control reaction time be 120min ~ 300min, slurry pH be 1.5 ~
6.8, after reaction solid-liquor separation obtain one section of leachate and one section of leached mud；
Step 3, two sections of leachings：It is in mass ratio with sodium chlorate or hypochlorite oxidation agent by one section of leached mud that step 2 obtains
30~100:1 is mixed, and is 1 by solid-to-liquid ratio:The crystalline mother solution that step 5 output is added in 3 ~ 15g/mL is sized mixing, and is 50 DEG C in temperature
~ 90 DEG C, speed of agitator be 100r/min ~ 600r/min under conditions of leached, the control reaction time for 120min ~
300min, slurry pH are 1.0 ~ 6.0, and solid-liquor separation obtains two sections of leachates and leaches finishing slag after reaction, two sections of leachings
Liquid return to step 2 recycles；
Step 4, displacement recycling silver：Lead flake will be added in one section of leachate that step 3 obtains, the item for being 60 DEG C ~ 100 DEG C in temperature
60min ~ 300min, solid-liquor separation output sponge silver and displaced liquid are reacted under part；
Step 5, crystallisation by cooling recycle lead：The displaced liquid that step 4 obtains is cooled, lead chloride crystal seed is added, in temperature
It is stopped 2 ~ 8 hours under the conditions of being 15 DEG C ~ 40 DEG C, solid-liquor separation obtains lead chloride and crystalline mother solution, and crystalline mother solution return to step 3 is followed
Ring uses.
20 ~ 45wt% of sintering machine head end dedusting ash iron content in the step 1, containing 0.1 ~ 3wt% of zinc, containing 3 ~ 20wt% of potassium, contain sodium
0.3 ~ 5wt%, 100 ~ 800g/t of argentiferous and leaded 3 ~ 22wt%.
The step 2 is added when leaching for the first time into 4 ~ 6mol/L ammonium chloride solutions, and follow-up leach is added the two of step 3 output
Section leachate is sized mixing.
The step 2 and step 3 pH values of pulp are regulated and controled using hydrochloric acid and ammonium hydroxide.
Lead flake addition is the 3 ~ 10 of the Theoretical Mass for cementing out the silver in one section of leachate completely in the step 4
Times.
The beneficial effects of the invention are as follows：
（1）The invention firstly uses ammonium carbonates as transforming agent and leaching agent, by material lead and silver be converted into ceruse and
Silver carbonate, while by the harmful elements separated and dissolved such as soluble zinc, potassium, sodium and chlorine, these foreign ions are avoided to lead silver packet
The adverse effect wrapped up in etc., and these impurity is avoided to be enriched in leaching finishing slag, sintered material can be returned to by leaching finishing slag.Have
Lead silver comprehensive recovery is high, the high feature of product purity.
（2）The present invention realizes the efficiently leaching of lead and silver in the condition less than 120 DEG C using two sections of counter flow oxidation leaching-out techniques
Go out, while the lead controlled in rational temperature gradient crystallisation by cooling recycling solution has energy consumption without traditional evaporative crystallization steps
Low, at low cost, lead recovery is high, the feature that process cleans are efficient, environmental-friendly.
Description of the drawings
Fig. 1 is present invention process flow chart.
Specific implementation mode
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
As shown in Figure 1, the method for the steel works sintering head dedusting ash separation and recovery silver and lead, is as follows：
Step 1, alkaline leaching：By sintering machine head end dedusting ash（Sintering machine head end dedusting ash iron content 25.3wt%, 0.5wt% containing zinc, contain potassium
11.2wt%, 0.7wt% containing sodium, argentiferous 421g/t and leaded 5.8wt%）It is 1 in mass ratio with ammonium carbonate:1 is mixed
Material is closed, is 1 by solid-to-liquid ratio:2g/mL adds water to size mixing, and is 60 DEG C in temperature, speed of agitator carries out under conditions of being 400r/min
It leaches, controls reaction time 120min, slurry pH is 9.2 ~ 9.5（It is adjusted using a concentration of 8mol/L ammonia spirits）, reaction
After solid-liquor separation obtain lead silver enrichment slag and alkaline leaching liquid；
Step 2, one section of leaching：The lead silver enrichment slag that step 1 is obtained is 1 in mass ratio with ammonium chloride:2 are uniformly mixed, by solid
Liquor ratio is 1:Two sections of leachates that step 3 output is added in 3g/mL are sized mixing, and are 90 DEG C in temperature, speed of agitator is 300r/min's
Under the conditions of leached, the control reaction time be 180min, slurry pH 3.5（PH values of pulp uses a concentration of 8mol/L hydrochloric acid
It adjusts）, after reaction solid-liquor separation obtain one section of leachate and one section of leached mud；4mol/L chlorine is added when wherein leaching for the first time
Change ammonium salt solution, dosage is identical as two sections of leachate dosages of step 3 output, follow-up to leach two sections of leachings that step 3 output is added
Liquid is sized mixing；
Step 3, two sections of leachings：One section of leached mud that step 2 is obtained is 100 in mass ratio with hypochlorite oxidation agent:1 carries out
Mixing is 1 by solid-to-liquid ratio:The crystalline mother solution that step 5 output is added in 3g/mL is sized mixing, and is 60 DEG C in temperature, speed of agitator is
It is leached under conditions of 300r/min, the control reaction time is 180min, slurry pH 2.0（PH values of pulp is using a concentration of
8mol/L hydrochloric acid is adjusted）, after reaction solid-liquor separation obtain two sections of leachates and leach finishing slag, two sections of leachate return to step
2 recycle；
Step 4, displacement recycling silver：Lead flake will be added in one section of leachate that step 3 obtains（Lead flake addition is to leach one section
5 times of the Theoretical Mass that silver in liquid cements out completely）, react 180min, solid-liquor separation under conditions of temperature is 70 DEG C
Output sponge silver and displaced liquid；
Step 5, crystallisation by cooling recycle lead：The displaced liquid that step 4 obtains is cooled, 10g lead chloride crystal seeds are added, in temperature
Degree stops 5 hours under the conditions of being 20 DEG C, and solid-liquor separation obtains lead chloride and crystalline mother solution, and the cycle of crystalline mother solution return to step 3 makes
With.
The rear silver-colored rate of recovery is 87.3% after testing for above-mentioned sponge silver, lead chloride, and the rate of recovery of lead is 93.7%.
Embodiment 2
As shown in Figure 1, the method for the steel works sintering head dedusting ash separation and recovery silver and lead, is as follows：
Step 1, alkaline leaching：By sintering machine head end dedusting ash（Sintering machine head end dedusting ash iron content 45wt%, 0.1wt% containing zinc, contain potassium
3wt%, 5wt% containing sodium, argentiferous 800g/t and leaded 3wt%）It is 1 in mass ratio with ammonium carbonate:4 be uniformly mixed obtain mixed material,
It is 1 by solid-to-liquid ratio:8g/mL adds water to size mixing, and is 25 DEG C in temperature, speed of agitator is leached under conditions of being 100r/min, is controlled
Reaction time 300min processed, slurry pH 7.5（It is adjusted using a concentration of 8mol/L ammonia spirits）, after reaction liquid divide admittedly
It is enriched with slag and alkaline leaching liquid from lead silver is obtained；
Step 2, one section of leaching：The lead silver enrichment slag that step 1 is obtained is 1 in mass ratio with ammonium chloride:1 is uniformly mixed, by solid
Liquor ratio is 1:Two sections of leachates that step 3 output is added in 6g/mL are sized mixing, and are 60 DEG C in temperature, speed of agitator is 100r/min's
Under the conditions of leached, the control reaction time be 300min, slurry pH 1.5（PH values of pulp uses a concentration of 8mol/L hydrochloric acid
It adjusts）, after reaction solid-liquor separation obtain one section of leachate and one section of leached mud；6mol/L chlorine is added when wherein leaching for the first time
Change ammonium salt solution, dosage is identical as two sections of leachate dosages of step 3 output, follow-up to leach two sections of leachings that step 3 output is added
Liquid is sized mixing；
Step 3, two sections of leachings：One section of leached mud that step 2 is obtained is 30 in mass ratio with sodium chlorate oxidant:1 is mixed
It closes, is 1 by solid-to-liquid ratio:The crystalline mother solution that step 5 output is added in 10g/mL is sized mixing, and is 50 DEG C in temperature, speed of agitator 100r/
It is leached under conditions of min, the control reaction time is 300min, slurry pH 1.0（PH values of pulp uses a concentration of 8mol/L
Hydrochloric acid is adjusted）, after reaction solid-liquor separation obtain two sections of leachates and leach finishing slag, two sections of leachate return to step 2 recycle
It uses；
Step 4, displacement recycling silver：Lead flake will be added in one section of leachate that step 3 obtains（Lead flake addition is to leach one section
3 times of the Theoretical Mass that silver in liquid cements out completely）, react 300min, solid-liquor separation under conditions of temperature is 60 DEG C
Output sponge silver and displaced liquid；
Step 5, crystallisation by cooling recycle lead：The displaced liquid that step 4 obtains is cooled, 10g lead chloride crystal seeds are added, in temperature
Degree stops 8 hours under the conditions of being 15 DEG C, and solid-liquor separation obtains lead chloride and crystalline mother solution, and the cycle of crystalline mother solution return to step 3 makes
With.
The rear silver-colored rate of recovery is 90.2% after testing for above-mentioned sponge silver, lead chloride, and the rate of recovery of lead is 87.8%.
Embodiment 3
As shown in Figure 1, the method for the steel works sintering head dedusting ash separation and recovery silver and lead, is as follows：
Step 1, alkaline leaching：By sintering machine head end dedusting ash（Sintering machine head end dedusting ash iron content 20wt%, 3wt% containing zinc, contain potassium
20wt%, 0.3wt% containing sodium, argentiferous 100g/t and leaded 22wt%）It is 1 in mass ratio with ammonium carbonate:2 are mixed
Material is 1 by solid-to-liquid ratio:6g/mL adds water to size mixing, and is 95 DEG C in temperature, speed of agitator is soaked under conditions of being 600r/min
Go out, controls reaction time 60min, slurry pH 8.2（It is adjusted using a concentration of 8mol/L ammonia spirits）, liquid after reaction
Gu isolated lead silver enrichment slag and alkaline leaching liquid；
Step 2, one section of leaching：The lead silver enrichment slag that step 1 is obtained is 1 in mass ratio with ammonium chloride:4 are uniformly mixed, by solid
Liquor ratio is 1:Two sections of leachates that step 3 output is added in 15g/mL are sized mixing, and are 120 DEG C in temperature, speed of agitator 600r/min
Under conditions of leached, the control reaction time be 120min, slurry pH 6.8（PH values of pulp uses a concentration of 8mol/L ammonia
Water is adjusted）, after reaction solid-liquor separation obtain one section of leachate and one section of leached mud；5mol/L is added when wherein leaching for the first time
Ammonium chloride solution, dosage is identical as two sections of leachate dosages of step 3 output, follow-up to leach two sections of leachings that step 3 output is added
Go out liquid to size mixing；
Step 3, two sections of leachings：One section of leached mud that step 2 is obtained is 80 in mass ratio with sodium chlorate oxidant:1 is mixed
It closes, is 1 by solid-to-liquid ratio:The crystalline mother solution that step 5 output is added in 15g/mL is sized mixing, and is 90 DEG C in temperature, speed of agitator 600r/
It is leached under conditions of min, the control reaction time is 120min, slurry pH 6.0（PH values of pulp uses a concentration of 8mol/L
Ammonium hydroxide is adjusted）, after reaction solid-liquor separation obtain two sections of leachates and leach finishing slag, two sections of leachate return to step 2 recycle
It uses；
Step 4, displacement recycling silver：Lead flake will be added in one section of leachate that step 3 obtains（Lead flake addition is to leach one section
10 times of the Theoretical Mass that silver in liquid cements out completely）, react 60min, solid-liquor separation under conditions of temperature is 100 DEG C
Output sponge silver and displaced liquid；
Step 5, crystallisation by cooling recycle lead：The displaced liquid that step 4 obtains is cooled, 10g lead chloride crystal seeds are added, in temperature
Degree stops 2 hours under the conditions of being 40 DEG C, and solid-liquor separation obtains lead chloride and crystalline mother solution, and the cycle of crystalline mother solution return to step 3 makes
With.
The rear silver-colored rate of recovery is 82.7% after testing for above-mentioned sponge silver, lead chloride, and the rate of recovery of lead is 94.2%.
The specific implementation mode of the present invention is explained in detail above in association with attached drawing, but the present invention is not limited to above-mentioned
Embodiment within the knowledge of a person skilled in the art can also be before not departing from present inventive concept
Put that various changes can be made.
Claims (6)
1. a kind of method of steel works sintering head dedusting ash separation and recovery silver and lead, it is characterised in that specific steps include：It is first
Sintering machine head end dedusting ash is uniformly mixed with ammonium carbonate first, adds water to size mixing and is leached to obtain lead silver enrichment slag；To obtained lead
Ammonium chloride and sodium chlorate are added in silver enrichment slag or hypochlorite oxidation agent carries out two sections of counter flow oxidations and leaches, one obtained
Section leachate is using metallic lead displacement recycling silver, output sponge silver and displaced liquid, and displaced liquid is using crystallisation by cooling output
Lead chloride, crystalline mother solution return to two sections of leachings；Two sections are leached two sections of obtained leachates and return to one section of leaching.
2. the method for steel works sintering head dedusting ash separation and recovery silver and lead according to claim 1, it is characterised in that
It is as follows：
Step 1, alkaline leaching：It is 1 in mass ratio by sintering machine head end dedusting ash and ammonium carbonate:1 ~ 4 be uniformly mixed obtain mixture
Material is 1 by solid-to-liquid ratio:2 ~ 8g/mL adds water to size mixing, and is 25 DEG C ~ 95 DEG C in temperature, speed of agitator is 100r/min ~ 600r/min
Under conditions of leached, control reaction time 60min ~ 300min, slurry pH be 7.5 ~ 9.8, after reaction liquid divide admittedly
It is enriched with slag and alkaline leaching liquid from lead silver is obtained；
Step 2, one section of leaching：The lead silver enrichment slag that step 1 is obtained is 1 in mass ratio with ammonium chloride:1 ~ 4 is uniformly mixed, and presses
Solid-to-liquid ratio is 1:Two sections of leachates that step 3 output is added in 3 ~ 15g/mL are sized mixing, and are 60 DEG C ~ 120 DEG C in temperature, speed of agitator is
Leached under conditions of 100r/min ~ 600r/min, the control reaction time be 120min ~ 300min, slurry pH be 1.5 ~
6.8, after reaction solid-liquor separation obtain one section of leachate and one section of leached mud；
Step 3, two sections of leachings：It is in mass ratio with sodium chlorate or hypochlorite oxidation agent by one section of leached mud that step 2 obtains
30~100:1 is mixed, and is 1 by solid-to-liquid ratio:The crystalline mother solution that step 5 output is added in 3 ~ 15g/mL is sized mixing, and is 50 DEG C in temperature
~ 90 DEG C, speed of agitator be 100r/min ~ 600r/min under conditions of leached, the control reaction time for 120min ~
300min, slurry pH are 1.0 ~ 6.0, and solid-liquor separation obtains two sections of leachates and leaches finishing slag after reaction, two sections of leachings
Liquid return to step 2 recycles；
Step 4, displacement recycling silver：Lead flake will be added in one section of leachate that step 3 obtains, the item for being 60 DEG C ~ 100 DEG C in temperature
60min ~ 300min, solid-liquor separation output sponge silver and displaced liquid are reacted under part；
Step 5, crystallisation by cooling recycle lead：The displaced liquid that step 4 obtains is cooled, lead chloride crystal seed is added, in temperature
It is stopped 2 ~ 8 hours under the conditions of being 15 DEG C ~ 40 DEG C, solid-liquor separation obtains lead chloride and crystalline mother solution, and crystalline mother solution return to step 3 is followed
Ring uses.
3. the method for steel works sintering head dedusting ash separation and recovery silver and lead according to claim 2, it is characterised in that：
20 ~ 45wt% of sintering machine head end dedusting ash iron content in the step 1, containing 0.1 ~ 3wt% of zinc, containing 3 ~ 20wt% of potassium, containing 0.3 ~ 5wt% of sodium,
100 ~ 800g/t of argentiferous and leaded 3 ~ 22wt%.
4. the method for steel works sintering head dedusting ash separation and recovery silver and lead according to claim 2, it is characterised in that：
4 ~ 6mol/L aqueous ammonium chloride solutions are added when the step 2 leaches for the first time, it is follow-up to leach two sections of leachates that step 3 output is added
It sizes mixing.
5. the method for steel works sintering head dedusting ash separation and recovery silver and lead according to claim 2, it is characterised in that：
The step 2 and step 3 pH values of pulp are regulated and controled using hydrochloric acid and ammonium hydroxide.
6. the method for steel works sintering head dedusting ash separation and recovery silver and lead according to claim 2, it is characterised in that：
Lead flake addition is by 3 ~ 10 times of the silver-colored Theoretical Mass cemented out completely in one section of leachate in the step 4.
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