CN107447112B - A method of the enriched lead from low-grade lead skim - Google Patents
A method of the enriched lead from low-grade lead skim Download PDFInfo
- Publication number
- CN107447112B CN107447112B CN201710681742.9A CN201710681742A CN107447112B CN 107447112 B CN107447112 B CN 107447112B CN 201710681742 A CN201710681742 A CN 201710681742A CN 107447112 B CN107447112 B CN 107447112B
- Authority
- CN
- China
- Prior art keywords
- liquid
- lead
- calcium
- added
- skim
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 75
- 239000002893 slag Substances 0.000 claims abstract description 37
- 239000011777 magnesium Substances 0.000 claims abstract description 29
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 27
- 238000005406 washing Methods 0.000 claims abstract description 27
- UCUJUFDOQOJLBE-UHFFFAOYSA-N [Cl].[Ca] Chemical compound [Cl].[Ca] UCUJUFDOQOJLBE-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 239000007787 solid Substances 0.000 claims abstract description 20
- 239000011575 calcium Substances 0.000 claims abstract description 18
- 239000006210 lotion Substances 0.000 claims abstract description 17
- 239000002253 acid Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 11
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 10
- IHBCFWWEZXPPLG-UHFFFAOYSA-N [Ca].[Zn] Chemical compound [Ca].[Zn] IHBCFWWEZXPPLG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000010792 warming Methods 0.000 claims description 16
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 10
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 10
- 239000001110 calcium chloride Substances 0.000 claims description 10
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 10
- 239000003153 chemical reaction reagent Substances 0.000 claims description 10
- 239000004571 lime Substances 0.000 claims description 10
- 239000000920 calcium hydroxide Substances 0.000 claims description 7
- 239000012047 saturated solution Substances 0.000 claims description 6
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 3
- 238000011084 recovery Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000013019 agitation Methods 0.000 abstract 1
- 231100000693 bioaccumulation Toxicity 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000011701 zinc Substances 0.000 description 23
- 239000000460 chlorine Substances 0.000 description 17
- 229910052725 zinc Inorganic materials 0.000 description 17
- SMBGWMJTOOLQHN-UHFFFAOYSA-N lead;sulfuric acid Chemical compound [Pb].OS(O)(=O)=O SMBGWMJTOOLQHN-UHFFFAOYSA-N 0.000 description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 5
- 229910052801 chlorine Inorganic materials 0.000 description 4
- 239000006071 cream Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 230000001698 pyrogenic effect Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000009858 zinc metallurgy Methods 0.000 description 2
- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical compound [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 description 1
- 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 description 1
- 229910020218 Pb—Zn Inorganic materials 0.000 description 1
- 229910052924 anglesite Inorganic materials 0.000 description 1
- 229910052925 anhydrite Inorganic materials 0.000 description 1
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
-
- 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
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Processing Of Solid Wastes (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of methods of enriched lead from low-grade lead skim, including the following steps: 1) low-grade lead skim is added to liquid after washing calcium chlorine, filter to obtain washing lotion and washery slag；2) washing lotion is heated up and adjusts PH, liquid after zinc calcium and magnesium slag and dezincification calcium and magnesium is filtered to obtain in reaction；3) washery slag is added to liquid after adjusting acid, leachate and leached mud are filtered to obtain in heating stirring；4) leachate is heated up, is stirred, adjusted pH value, obtain liquid and lead skim after de- lead；Liquid and calcium chloride solution adjust PH into after adjusting sour pond together again after de- lead, and liquid after tune acid is made, liquid after acid is adjusted to return step 3) use；5) liquid and a small amount of water after decalcification magnesium is added in the lead skim obtained in the step 4) with liquid-solid ratio 5:1, agitation and filtration obtains high lead slag and washes liquid after calcium chlorine, and liquid PH after calcium chlorine is washed in adjusting, washes liquid after calcium chlorine and returns in step 1) and uses；Invention bioaccumulation efficiency is high, and lead recovery is high；Lead recovery and treatment method after enrichment improves content is more, and technology difficulty is low, and development space is big.
Description
Technical field
The present invention relates to zinc metallurgy recycling fields, more specifically, being a kind of method of enriched lead from low-grade lead skim.
Background technique
Sulfuric acid lead skim is that zinc metallurgy and zinc product produce and use the waste residue being discharged in the process, it is both the nocuousness for polluting environment
Substance is also the secondary resource for extracting valuable constituent, it is therefore necessary to integrated treatment is carried out to it, to reach " increasing income and decreasing expenditure ", prevent
The purpose of pollution.At present to being difficult to ore dressing and complicated component, the lead-containing material for being unsuitable for pyrogenic attack, pyrogenic process directly recycle sky
Gas pollution is big, and energy consumption is high, and employment injuries is also larger, and hydrometallurgic recovery is avoided that the above problem, but technical difficulty is big.
Summary of the invention
In order to make up the above deficiency, the present invention provides a kind of methods of enriched lead from low-grade lead skim.
The scheme of the invention is:
A method of the enriched lead from low-grade lead skim, including the following steps:
1) low-grade lead skim is added to liquid after washing calcium chlorine with liquid-solid ratio 5:1,40~60 DEG C is heated up to, stirs 30 minutes, mistake
Filter to obtain washing lotion and washery slag；
2) washing lotion is warming up to 65~70 DEG C, lime is added and adjusts pH > 12, zinc calcium and magnesium slag and de- is filtered to obtain in reaction for 30 minutes
Liquid after zinc calcium and magnesium；
3) washery slag is added to liquid after adjusting acid with 6~5:1 of liquid-solid ratio, 70~90 DEG C is warming up to, stirs 1 hour, control terminal
PH is 4~4.5, filters to obtain leachate and leached mud；
4) leachate is warming up to 80~90 DEG C or more, be added with stirring purification deleading reagent adjust pH value, half an hour it
Interior adjusting pH to 7, after stablizing 30 minutes, it is 12 that a small amount of deleading reagent, which is added, to adjust pH according to pH value, and reaction is filtered after 30 minutes, is obtained
Liquid and lead skim after de- lead；Liquid and calcium chloride saturated solution add a small amount of HCl adjusting into after adjusting sour pond together after the de- lead
PH is 2~3, liquid after the tune acid is made, liquid returns the use of step 3) extracting stage after the tune acid；
5) liquid and a small amount of water after decalcification magnesium is added in the lead skim obtained in the step 4) with liquid-solid ratio 5:1, stirs 30 minutes,
It filters high lead slag and to wash liquid after calcium chlorine, uses H2SO4It is 3~4 that liquid pH after calcium chlorine is washed in adjusting, and washing liquid after calcium chlorine and returning in step 1) makes
With.
Taking off lead temperature in the step 4) as a preferred technical solution, is 80~90 DEG C, and deleading reagent is various alkalinity examinations
Agent.
Deleading reagent is milk of lime in the step 4) as a preferred technical solution,.
The reaction principle that the invention is related to
PbSO4+CaCl2+ 2NaCl=CaSO4+Na2PbCl4
2Na2PbCl4+Ca(OH)2=2PbClOH+CaCl2+4NaCl
2PbClOH+Ca(OH)2=2PbO+2H2O+CaCl2
By adopting the above-described technical solution, a kind of method of the enriched lead from low-grade lead skim, including the following steps: 1)
Low-grade lead skim is washed into liquid after calcium chlorine with liquid-solid ratio 5:1 addition, 40~60 DEG C is heated up to, stirs 30 minutes, filter washing lotion and
Washery slag；2) washing lotion is warming up to 65~70 DEG C, lime is added and adjusts pH > 12, reaction filters to obtain zinc calcium and magnesium slag and dezincification in 30 minutes
Liquid after calcium and magnesium；3) washery slag is added to liquid after adjusting acid with 6~5:1 of liquid-solid ratio, 70~90 DEG C is warming up to, stirs 1 hour, control terminal
PH is 4~4.5, filters to obtain leachate and leached mud；4) leachate is warming up to 80~90 DEG C or more, it is de- is added with stirring purification
Lead agent adjusts pH value, and pH to 7 is adjusted within half an hour, after stablizing 30 minutes, a small amount of deleading reagent is added according to pH value and adjusts pH
It is 12, reaction is filtered after 30 minutes, obtains liquid and lead skim after de- lead；Liquid and calcium chloride saturated solution enter together after the de- lead adjusts
Adding a small amount of HCl behind sour pond and adjusting pH is 2~3, and liquid after the tune acid is made, and liquid, which returns step 3) extracting stage, after the tune acid makes
With；5) liquid and a small amount of water after decalcification magnesium is added in the lead skim obtained in the step 4) with liquid-solid ratio 5:1, stirs 30 minutes, filtering
It obtains high lead slag and washes liquid after calcium chlorine, use H2SO4Liquid pH is 3~4 after calcium chlorine is washed in adjusting, and liquid returns use in step 1) after washing calcium chlorine；It should
Invention is difficult using original technique and domestic most zinc hydrometallurgy factory present in low-grade lead skim or sulfuric acid lead skim as raw material, use
Cheap industrial chlorinations sodium, calcium chloride and lime carries out desulfurization and enrichment to lead skim by simple process, and entire technique is realized molten
The closed cycle of liquid, three-waste free discharge.In large-scale production, temperature loss is few, and leachate lead concentration is efficiently saved up to 40g/L
Can, environmental protection and economy, product is leaded up to 65%~75%, and impurity is few, and post-processing can use pyrogenic process or wet process.Aftertreatment technology letter
It is single, it is at low cost.This technique also may extend to the recycling industry of waste lead accumulator.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Case study on implementation 1
Sulfuric acid lead skim contains Pb17.5%, Zn8%, Fe3.7%, Mn0.2%, Mg0.38%, S10%.
1, sulfuric acid lead skim is added to liquid after washing calcium chlorine with liquid-solid ratio 5:1,40~50 DEG C is heated up to, stirs 30 minutes, filtering
Washing lotion and washery slag, washing lotion containing Pb < 50mg/L, Zn3.9g/L, Fe0.78g/L, Mn1.36g/L, Mg0.51g/L, Cl3.8g/L,
SO4 2~10g/L, washery slag contain Pb20%.
2, washing lotion is warming up to 70 DEG C, lime is added and adjusts pH > 12, reaction filters to obtain zinc calcium and magnesium slag and dezincification calcium in 30 minutes
Liquid after magnesium.Zinc calcium and magnesium slag contains Pb < 0.1%, Zn 12%, Fe2.4%, Mn2.6%, Mg2.6%, after dezincification calcium and magnesium liquid containing Pb <
150mg/L、Zn<200mg/L、Fe<50mg/L、Mn<50mg/L、Mg200mg/L、Cl17g/L。
3, washery slag is added to liquid (Pb140mg/L, Zn140mg/L, Ca 10g/L, Cl 200g/ after adjusting acid with liquid-solid ratio 5:1
L), 70~80 DEG C are warming up to, is stirred 1 hour, terminal pH about 4.5 is controlled, filters to obtain leachate and leached mud.Leachate contains Pb
30.4g/L, Zn 0.8g/L, Ca 4.1g/L, Cl 198g/L, leached mud contain Pb2.74%, Zn6.8%, and leached mud is again into fuming
Furnace processing.
4, leachate is warming up to 80 DEG C or more, is added with stirring refined lime cream and adjusts pH value, is adjusted within half an hour
PH to 7 is saved, after stablizing 30 minutes, it is 12 that a small amount of milk of lime, which is added, to adjust pH according to pH value, and reaction is filtered after 30 minutes, obtains de- lead
Liquid and lead skim afterwards.Liquid contains Pb144mg/L, Zn147mg/L, Ca7.8g/L, Cl190g/L after de- lead, lead skim containing Pb61.8%,
Zn0.84%, Cl17.6%.Liquid and calcium chloride saturated solution add a small amount of HCl adjusting pH into after adjusting sour pond together after de- lead
It is 2~3, returns extracting stage use.
5, liquid and a small amount of water after decalcification magnesium is added into lead skim with liquid-solid ratio 5:1, stirs 30 minutes, filter high lead slag and
Liquid after calcium chlorine is washed, liquid uses H containing Pb100mg/L, Zn200mg/L, Cl19g/L after washing calcium chlorine2SO4Adjusting pH is 3~4, returns first
Step uses.High lead slag contains Pb72%, Zn1.2%, Cl8%.
Conclusion: technique lead recovery 95%, filter plant uses vertical type blotter press in leaching section, and supplementary product onsumption is few.
Case study on implementation 2
Sulfuric acid lead skim contains Pb27%, Zn10.9%, Fe2.8%, Mn0.3%, Mg0.38%, S11%.
1, sulfuric acid lead skim is added to liquid after washing calcium chlorine with liquid-solid ratio 5:1,50~60 DEG C is heated up to, stirs 30 minutes, filtering
Washing lotion and washery slag are obtained, washing lotion contains Pb179mg/L, Zn3.9g/L, Fe 0.8g/L, Mn1.56g/L, Mg 0.62g/L, Cl 3.8g/
L、SO4 2~11g/L, washery slag contain Pb 34%.
2, washing lotion is warming up to 65 DEG C, lime is added and adjusts pH13~14, zinc calcium and magnesium slag and de- is filtered to obtain in reaction for 30 minutes
Liquid after zinc calcium and magnesium.Zinc calcium and magnesium slag contains Pb < 0.1%, Zn 16.5%, Fe2.4%, Mn2.6%, Mg2.6%, liquid after dezincification calcium and magnesium
Containing Pb < 50mg/L, Zn < 50mg/L, Fe < 50mg/L, Mn < 50mg/L, Mg200mg/L, Cl 25g/L.
3, washery slag is added to liquid (Pb 500mg/L, Zn 300mg/L, Ca 13.5g/L, Cl after adjusting acid with liquid-solid ratio 5:1
210g/L), 80~90 DEG C are warming up to, is stirred 1 hour, terminal pH about 4.0 is controlled, filters to obtain leachate and leached mud.Leachate
40.2g/L containing Pb, Zn0.8g/L, Ca 5.1g/L, Cl 205g/L, leached mud contain Pb1.5%, Zn 5.5%, leached mud again into
Fuming furnace processing.
4, leachate temperature is maintained at 85~90 DEG C, be added with stirring refined lime cream adjust pH value, half an hour it
Interior adjusting pH to 7, after stablizing 30 minutes, it is 12 that a small amount of milk of lime, which is added, to adjust pH according to pH value, and reaction is filtered after 30 minutes, is obtained
Liquid and lead skim after de- lead.Liquid 200mg/L containing Pb, Zn500mg/L, Ca 12.0g/L, Cl 200g/L after de- lead, lead skim contain Pb
65%, Zn 0.65%, Cl 15.6%.Liquid and calcium chloride saturated solution add on a small quantity into after adjusting sour pond together after de- lead
It is 2~3 that HCl, which adjusts pH, returns extracting stage use.
5, liquid and a small amount of water after decalcification magnesium is added into lead skim with liquid-solid ratio 5:1, stirs 30 minutes, filter high lead slag and
Liquid after calcium chlorine is washed, liquid 50mg/L containing Pb, Zn 100mg/L, Cl19g/L after calcium chlorine is washed, uses H2SO4Adjusting pH is 3~4, returns first
Step uses.High lead slag contains Pb75%, Zn1.5%, Cl 6.5%.
Conclusion: when raw material lead content is high, lead concentration is also high in leachate, lead recovery 95%.
Case study on implementation 3
Lead skim contains Pb10%, Zn13%, Fe5%, Mn0.8%, Mg0.4%, S12%.
1, low-grade lead skim is added to liquid after washing calcium chlorine with liquid-solid ratio 5:1,60 DEG C is heated up to, stirs 30 minutes, filter
Washing lotion and washery slag, washing lotion 200mg/L containing Pb, Zn 20g/L, Fe 5g/L, Mn1.3g/L, Mg 0.62g/L, Cl 3.8g/L,
SO4 2~13g/L, washery slag contain Pb 34%.
2, washing lotion is warming up to 65 DEG C, lime is added and adjusts pH13~14, zinc calcium and magnesium slag and de- is filtered to obtain in reaction for 30 minutes
Liquid after zinc calcium and magnesium.Zinc calcium and magnesium slag contains Pb < 0.1%, Zn 16.5%, Fe2.4%, Mn2.6%, Mg2.6%, liquid after dezincification calcium and magnesium
Containing Pb < 50mg/L, Zn < 50mg/L, Fe < 50mg/L, Mn < 50mg/L, Mg200mg/L, Cl 25g/L.
3, washery slag is added to liquid (Pb100mg/L, Zn 100mg/L, Ca 8.1g/L, Cl after adjusting acid with liquid-solid ratio 6:1
180g/L), 80~90 DEG C are warming up to, is stirred 1 hour, terminal pH about 4.0 is controlled, filters to obtain leachate and leached mud.Leachate
Containing Pb15.5g/L, Zn0.3g/L, Ca 5.1g/L, Cl 178g/L, leached mud contains Pb0.75%, Zn 7.5%, leached mud again into
Fuming furnace processing.
4, leachate temperature is maintained at 85~90 DEG C, be added with stirring refined lime cream adjust pH value, half an hour it
Interior adjusting pH to 7, after stablizing 30 minutes, it is 12 that a small amount of milk of lime, which is added, to adjust pH according to pH value, and reaction is filtered after 30 minutes, is obtained
Liquid and lead skim after de- lead.Liquid 200mg/L containing Pb, Zn 200mg/L, Ca 7.1g/L, Cl 175g/L after de- lead, lead skim contain Pb
60.2%, Zn 0.65%, Cl 15.6%.Liquid and calcium chloride saturated solution add on a small quantity into after adjusting sour pond together after de- lead
It is 2~3 that HCl, which adjusts pH, returns extracting stage use.
5, liquid and a small amount of water after decalcification magnesium is added into lead skim with liquid-solid ratio 5:1, stirs 30 minutes, filter high lead slag and
Liquid after calcium chlorine is washed, liquid 20mg/L containing Pb, Zn 500mg/L, Cl 14g/L after calcium chlorine is washed, uses H2SO4Adjusting pH is 3~4, returns the
One step uses.High lead slag contains Pb 65%, Zn 2.5%, Cl 9.5%.
Conclusion: this technique lead recovery is 94.8%, selects washup according to the soluble impurity content of used lead skim
Liquid-solid ratio increases washup number, can promote product quality, improve Pb-Zn separation effect.
The above shows and describes the basic principle, main features and advantages of the invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent circle.
Claims (3)
1. a kind of method of the enriched lead from low-grade lead skim, characterized in that it comprises the following steps:
1) low-grade lead skim is added to liquid after washing calcium chlorine with liquid-solid ratio 5:1,40~60 DEG C is heated up to, stirs 30 minutes, filter
Washing lotion and washery slag；
2) washing lotion is warming up to 65~70 DEG C, lime is added and adjusts pH > 12, reaction filters to obtain zinc calcium and magnesium slag and dezincification in 30 minutes
Liquid after calcium and magnesium；
3) washery slag is added to liquid after adjusting acid with 6~5:1 of liquid-solid ratio, 70~90 DEG C is warming up to, stirs 1 hour, control terminal pH is
4~4.5, filter to obtain leachate and leached mud；
4) leachate is warming up to 80~90 DEG C or more, is added with stirring purification deleading reagent and adjusts pH value, is adjusted within half an hour
PH to 7 is saved, after stablizing 30 minutes, it is 12 that a small amount of deleading reagent, which is added, to adjust pH according to pH value, and reaction is filtered after 30 minutes, is obtained
Liquid and lead skim after de- lead；Liquid and calcium chloride saturated solution add a small amount of HCl adjusting into after adjusting sour pond together after the de- lead
PH is 2~3, liquid after the tune acid is made, liquid returns the use of step 3) extracting stage after the tune acid；
5) liquid and a small amount of water after decalcification magnesium is added in the lead skim obtained in the step 4) with liquid-solid ratio 5:1, stirs 30 minutes, filtering
It obtains high lead slag and washes liquid after calcium chlorine, use H2SO4Liquid pH is 3~4 after calcium chlorine is washed in adjusting, and liquid returns use in step 1) after washing calcium chlorine.
2. a kind of method of the enriched lead from low-grade lead skim as described in claim 1, it is characterised in that: in the step 4)
De- lead temperature is 80~90 DEG C, and deleading reagent is various alkaline reagents.
3. a kind of method of the enriched lead from low-grade lead skim as described in claim 1, it is characterised in that: in the step 4)
Deleading reagent is milk of lime.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710681742.9A CN107447112B (en) | 2017-08-10 | 2017-08-10 | A method of the enriched lead from low-grade lead skim |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710681742.9A CN107447112B (en) | 2017-08-10 | 2017-08-10 | A method of the enriched lead from low-grade lead skim |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107447112A CN107447112A (en) | 2017-12-08 |
| CN107447112B true CN107447112B (en) | 2019-03-01 |
Family
ID=60491706
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710681742.9A Active CN107447112B (en) | 2017-08-10 | 2017-08-10 | A method of the enriched lead from low-grade lead skim |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107447112B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555550A (en) * | 2009-05-22 | 2009-10-14 | 北京科技大学 | Method for recycling lead-tin in silver separating residue of copper anode slime of circuit board |
| CN103194615A (en) * | 2013-03-27 | 2013-07-10 | 云南祥云飞龙有色金属股份有限公司 | Lead hydrometallurgical technology through utilizing lead sulfate |
| CN104532014A (en) * | 2014-12-23 | 2015-04-22 | 东莞市粤威环保科技有限公司 | Innocent treatment of low-grade lead slag |
| CN105907986A (en) * | 2016-06-29 | 2016-08-31 | 江西铜业集团公司 | Extracting method for lead in silver separating residues |
| CN105907974A (en) * | 2016-06-16 | 2016-08-31 | 北京科技大学 | Method of comprehensively recycling valuable metal from lead sulfate slag |
| CN106521169A (en) * | 2016-11-05 | 2017-03-22 | 北京工业大学 | Comprehensive recovery method of silver-containing lead slag |
| CN106939377A (en) * | 2017-04-27 | 2017-07-11 | 中南大学 | A kind of chlorination of sulfur acid lead materials takes off the method that lead liquid is recycled |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005068535A (en) * | 2003-08-28 | 2005-03-17 | Jfe Engineering Kk | Method for processing lead or zinc containing gas or fly ash |
| JP5796716B2 (en) * | 2012-03-17 | 2015-10-21 | 三菱マテリアル株式会社 | Method for removing impurities from cobalt-containing liquid |
-
2017
- 2017-08-10 CN CN201710681742.9A patent/CN107447112B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555550A (en) * | 2009-05-22 | 2009-10-14 | 北京科技大学 | Method for recycling lead-tin in silver separating residue of copper anode slime of circuit board |
| CN103194615A (en) * | 2013-03-27 | 2013-07-10 | 云南祥云飞龙有色金属股份有限公司 | Lead hydrometallurgical technology through utilizing lead sulfate |
| CN104532014A (en) * | 2014-12-23 | 2015-04-22 | 东莞市粤威环保科技有限公司 | Innocent treatment of low-grade lead slag |
| CN105907974A (en) * | 2016-06-16 | 2016-08-31 | 北京科技大学 | Method of comprehensively recycling valuable metal from lead sulfate slag |
| CN105907986A (en) * | 2016-06-29 | 2016-08-31 | 江西铜业集团公司 | Extracting method for lead in silver separating residues |
| CN106521169A (en) * | 2016-11-05 | 2017-03-22 | 北京工业大学 | Comprehensive recovery method of silver-containing lead slag |
| CN106939377A (en) * | 2017-04-27 | 2017-07-11 | 中南大学 | A kind of chlorination of sulfur acid lead materials takes off the method that lead liquid is recycled |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107447112A (en) | 2017-12-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103194615B (en) | Lead hydrometallurgical technology through utilizing lead sulfate | |
| CN101503761B (en) | A method for separating and recovering valuable metals from high-sulfur slag leached by pressure | |
| CN102363522B (en) | Technology for extracting selenium from low-grade selenium-containing material | |
| CN106319233B (en) | The technique of arsenic alkaline slag room temperature wet method harmless treatment | |
| CN101871046A (en) | Method for recycling heavy metal pollution wastes | |
| CN103526017A (en) | Extraction method of valuable elements from acid mud produced in sulfuric acid production by copper smelting flue gas | |
| CN105506294A (en) | Method for comprehensively recovering manganese and lead from electrolytic manganese anode slime | |
| CN101760613B (en) | Method for leaching zinc-containing ores | |
| CN102173547A (en) | Resource recycling process for nickel-containing sludge in electroplating enterprises | |
| CN106011475B (en) | A kind of low concentration arsenic-containing waste residue harmless treatment and the method for arsenic recycling | |
| CN102851707A (en) | Technology for recovering production of electrolytic zinc powder and lead powder from smelting ash through alkali leaching method | |
| JPWO2015162902A1 (en) | Method and facility for recovering valuable components from waste dry batteries | |
| CN101603125B (en) | Method for purification and impurity removal of nickel liquid | |
| CN108384959A (en) | A kind of preparation method of electrolytic zinc | |
| CN108276448A (en) | A kind of method that arsenic-containing material alkali soaks arsenic recycling in dearsenification liquid | |
| Makovskaya et al. | Leaching of non-ferrous metals from galvanic sludges | |
| JP2006198448A (en) | Valuable recovery method from flying ash | |
| CN102002597B (en) | Method for comprehensively recovering valuable metals from low-grade tellurium slag | |
| RU2670117C2 (en) | Process for the selective recovery of lead and silver and carbonate lead and silver concentrate, obtained by the method above | |
| WO2017110572A1 (en) | Method for removing sulfidizing agent | |
| BG113021A (en) | Under pressure oxidative leaching of sulphide raw materials at low solid content and acidity | |
| JP2010196140A (en) | Method for recovering bismuth | |
| KR101470123B1 (en) | Refining method of Tin sludge | |
| CN107447112B (en) | A method of the enriched lead from low-grade lead skim | |
| CN108315565A (en) | A method of the Selectively leaching vulcanized lead from sulfide containing lead material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20221208 Address after: No. 28, Beihou Street, Xiangcheng Town, Xiangyun County, Dali Bai Autonomous Prefecture, Yunnan 672199 Patentee after: Yang Yunting Address before: 671000 Fortune Industrial Park, Xiangcheng Town, Xiangyun County, Dali Bai Autonomous Prefecture, Yunnan Province Patentee before: YUNNAN LONGYUN TECHNOLOGY ENVIRONMENTAL PROTECTION CO.,LTD. |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240616 Address after: Room 401147, Building 1, Time City, No. 409 Jiahong Avenue, Longshan Street, Yubei District, Chongqing, China, Commercial Building 5-9 Patentee after: Chongqing Hongbo New Materials Technology Co.,Ltd. Country or region after: China Address before: No. 28, Beihou Street, Xiangcheng Town, Xiangyun County, Dali Bai Autonomous Prefecture, Yunnan 672199 Patentee before: Yang Yunting Country or region before: China |