CN105695764A - Method for separating lead from lead-containing alkaline leaching liquor by oxidizing and precipitating - Google Patents

Method for separating lead from lead-containing alkaline leaching liquor by oxidizing and precipitating Download PDF

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Publication number
CN105695764A
CN105695764A CN201610115959.9A CN201610115959A CN105695764A CN 105695764 A CN105695764 A CN 105695764A CN 201610115959 A CN201610115959 A CN 201610115959A CN 105695764 A CN105695764 A CN 105695764A
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China
Prior art keywords
lead
precipitating
alkali
alkali immersion
heavy
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CN201610115959.9A
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Chinese (zh)
Inventor
陈永明
杨声海
薛浩天
李云
林文荣
刘恒
郭路路
刘南南
唐朝波
宣曹成
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Central South University
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Central South University
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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
    • 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
    • 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
    • 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
    • C22B7/008—Wet processes by an alkaline or ammoniacal leaching
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (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)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention provides a method for separating lead from lead-containing alkaline leaching liquor by oxidizing and precipitating. The method comprises the following steps: firstly, adding HNO3 or NaOH with concentration being 10-20% into the alkaline leaching liquor to regulate the pH value of a system to be 11-13.9; then, adding Na2S2O8 or H2O2 with a coefficient of excess being 1.2-1.8 as an oxidant, carrying out mechanical stirring reaction for 30-120 minutes at a temperature of 20-50 DEG C, thereby precipitating and separating lead in the alkaline leaching liquor in the form of PbO2; and carrying out reductive smelting on precipitated lead slag obtained by liquid-solid separation to produce crude lead, wherein liquor obtained by oxidizing and carrying out lead precipitation on H2O2 can be directly returned to an alkaline leaching for being recycled. The method has the advantages of a simple process, a high pH value of the lead precipitates, a low lead precipitating temperature, a high lead separating rate, less reagent consumption, capacity of treating various kinds of lead-containing alkaline leaching liquor, and the like. The defects that a conventional sulfuric acid neutralizing and lead-precipitating process is great in acid and alkaline consumption, and is difficult to recycle lead-removed liquor are overcome, and the defects that in a conventional vulcanizing and lead-precipitating process, Na2S is liable to oxidize into polysulfide, Na2S consumption is great, acid mists are liable to generate, an operation environment is severe and the like are also overcome.

Description

A kind of method of leaded alkali immersion oxidation precipitation separation of lead
Technical field
The present invention provides a kind of method of oxidation precipitation separation of lead in alkali immersion, belongs to metallurgical and chemical technology field, is specifically related to the purification deleading technology of alkaline leaching liquid。
Background technology
In the oxidation alkaline pretreatment dearsenization process of zinc oxide ore, NaOH alkaline leaching containing Pb-Zn dust and lead anode slurry, owing to lead is amphoteric metal, the lead in raw material also can be extracted into alkali immersion to some extent。
At present for removing the lead in alkali immersion in production practices, sulfuric acid solution can be added to turn down system pH, make-Lead in alkali immersion is with PbSO4With Pb (OH)2Form is precipitated out。The method existing problems are that after heavy lead, the pH value of liquid is reduced to about neutrality from high alkalinity, cause whole system acid, quantity of alkali consumption very big。After gained deleading, liquid is also difficult to the effect recycled。
Zhu Youzhen, Zhao Youcai is at document " lead in sulphide precipitation Selective Separation Alkaline Zinc solution " (Shanghai Institute Of Technology's journal (natural science edition), 2001, 1(1): 59～63) and document " leaching with sodium hydroxide two-step precipitation prepares lead and zinc concentrate new technology " (hydrometallurgy, 2010, propose to add sodium sulfide in 29(1): 33～36) in the alkali immersion of zincy lead, when sodium sulfide and plumbous weight ratio are when 1.7～1.9, lead can separate by quantitative deposition from alkaline solution, pollution or co-precipitation without zinc, the purity of the vulcanized lead obtained reaches 95～98%, can as the raw material being directly produced metallic lead or other purposes。" a kind of leaching from lead anode slurry alkali removes method plumbous, antimony dearsenization liquid " (patent No. CN102690951B) of Li Dong, Qin little Long et al. invention soaks after dearsenization filtrate for raw material with lead anode slurry alkali, by adopting diluted acid to control solution ph 3～10, reaction temperature 30～80 DEG C, when stirring reaction time 0.5～2h, add appropriate reducing agent and sulfide precipitation agent by lead adjoint in solution, antimony ion selective precipitation, enrichment, thus having reached the purpose separating and reclaiming arsenic with plumbous antimony。The subject matter that sulfide precipitation technique exists is that sodium sulfide is easily oxidized to polysulfide in alkaline solution, and sodium sulfide consumption is relatively big, and can produce acid mist in heavy plumbous process, and operating environment is comparatively severe。
Summary of the invention
For the problems that above-mentioned technology exists, the present invention provides a kind of method of oxidation precipitation separation of lead in alkali immersion, to replace traditional sulphuric acid neutralization precipitation and sulfide precipitation method。First in alkali immersion, add HNO3Or NaOH regulation system pH value, add Na2S2O8Or H2O2As oxidant, wherein, when the control of oxidant coefficient of excess is 1.2 ~ 1.8, it is possible to fully make the lead in alkali immersion be oxidized to PbO2Form precipitate and separate, but reagent consumption is moderate, and the heavy lead skim that solid-liquor separation obtains can output lead bullion through reduction melting。
The inventive method step is as follows:
(1) in reaction alkali in groove immersion, HNO is added3Or NaOH regulation system pH value is 11 ~ 13.9；
(2) alkali immersion heated and maintain in 20 ~ 50 DEG C of temperature ranges；
(3) adding coefficient of excess under certain mixing speed is the Na of 1.2 ~ 1.82S2O8Or H2O2Carry out aoxidizing heavy lead:
Na2S2O8+Na2PbO2=PbO2↓+2Na2SO4
H2O2+Na2PbO2=PbO2↓+2NaOH
(4) carrying out solid-liquid separation after reaction 30 ~ 120min, the filtering residue obtained is mainly PbO2, adopt simple reduction melting can realize the synthetical recovery of lead, H2O2After the heavy lead of oxidation, liquid can directly return alkali leaching operation and recycles。
The method have the advantages that technique is simple, plumbous precipitation pH value high (11 ~ 13.9), heavy plumbous temperature is low, and plumbous precipitate and separate rate is high, and reagent consumption is few, it is possible to process the advantages such as multiple leaded alkali immersion, in particular by H2O2As oxidant, after deleading, liquid can directly return alkali leaching operation and recycles after reclaiming other valuable metal, and system acid when overcoming tradition with sulphuric acid for pH value regulator, quantity of alkali consumption are big, and after deleading, liquid is difficult to the shortcoming recycled。Meanwhile, this technique is with Na2S2O8Or H2O2Carry out aoxidizing heavy lead, overcome tradition Na2Na in the heavy splicer's skill of S sulfuration2S is easily oxidized to polysulfide, Na2S consumption is big, is easily generated acid mist, the shortcomings of severe operational environment。
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention；
Fig. 2 is with Na2S2O8The XRD diffracting spectrum of heavy lead skim during for oxidant；
Fig. 3 is with H2O2The XRD diffracting spectrum of heavy lead skim during for oxidant。
Detailed description of the invention
Further illustrate the flesh and blood of the present invention below with example, but protection scope of the present invention is not limited to this。
Embodiment 1
A kind of method of oxidation precipitation separation of lead in alkali immersion, alkali immersion used is Refractory ore NaOH leachate, and it mainly comprises as (g/L): Zn29.63, Pb7.28, As0.07, Cu0.14, Cd0.002, Al0.03, Si0.65。First in alkali immersion, rare HNO is added3Solution regulation system pH value is 13, alkali immersion is heated and maintains 30 DEG C, and adding coefficient of excess under certain mixing speed is the Na of 1.22S2O8Carry out aoxidizing heavy lead, after reaction 120min, carry out solid-liquid separation。Being computed heavy plumbous rate is 96.21%, and content plumbous in liquid after deleading is about 0.268g/L。
Embodiment 2
A kind of method of oxidation precipitation separation of lead in alkali immersion, alkali immersion used is the NaOH leachate containing Pb-Zn dust, and it mainly comprises as (g/L): Zn38.83, Pb10.31, As0.95, Cu0.22, Al0.29, Fe0.05, Si0.22。First in alkali immersion, rare HNO is added3Solution regulation system pH value is 12, alkali immersion is heated and maintains 40 DEG C, and adding coefficient of excess under certain mixing speed is the H of 1.62O2Carry out aoxidizing heavy lead, after reaction 60min, carry out solid-liquid separation。Being computed heavy plumbous rate is 95.85%, and content plumbous in liquid after deleading is about 0.309g/L。
Embodiment 3
A kind of method of oxidation precipitation separation of lead in alkali immersion, alkali immersion used is the oxidation alkaline pretreatment dearsenization liquid of lead anode slurry, and it mainly comprises as (g/L): Pb5.79, As4.67, Cu0.36, Sb0.70, Bi0.26。First adding dilute NaOH solution regulation system pH value in alkali immersion is 13.5, alkali immersion is heated and maintains 50 DEG C, and adding coefficient of excess under certain mixing speed is the H of 1.42O2Carry out aoxidizing heavy lead, after reaction 90min, carry out solid-liquid separation。Being computed heavy plumbous rate is 97.82%, and content plumbous in liquid after deleading is about 0.126g/L。
Embodiment 4
A kind of method of oxidation precipitation separation of lead in alkali immersion, alkali immersion used is the NaOH leachate of copper metallurgy industry flue dust, and it mainly comprises as (g/L): Zn25.88, Pb9.64, As8.62, Cu0.85, Sb0.61, Bi0.35。First in alkali immersion, rare HNO is added3Solution regulation system pH value is 11.5, and adding coefficient of excess at 20 DEG C of temperature is the Na of 1.82S2O8Carry out aoxidizing heavy lead, after mechanic whirl-nett reaction 30min, carrying out solid-liquid separation。Being computed heavy plumbous rate is 95.63%, and content plumbous in liquid after deleading is about 0.411g/L。
Obviously, the above embodiment of the present invention is only for clearly demonstrating the citing that the present invention does, and is not the restriction to embodiments of the present invention。For those of ordinary skill in the field, other multi-form change and variations can also be made on the basis of the above description。Here without also cannot all of detailed description of the invention be given exhaustive。And these belong to apparent change that technical scheme amplified out and the variation row still in protection scope of the present invention。

Claims (3)

1. the method for a leaded alkali immersion oxidation precipitation separation of lead, it is characterised in that comprise the following steps:
(1) adding concentration in alkali immersion is the pH value regulator of 10% ~ 20%, and regulation system pH value is in the scope of 11 ~ 13.9, and pH value regulator is HNO3Or NaOH；
(2) alkali immersion heated and maintain in the temperature range of 20 ~ 50 DEG C；
(3) adding the oxidant that coefficient of excess is 1.2 ~ 1.8 under mechanical agitation to carry out aoxidizing heavy lead, described oxidant is Na2S2O8Or H2O2；
(4) carrying out solid-liquid separation after reaction 30 ~ 120min, obtain heavy lead skim, heavy lead skim gets final product output lead bullion through simple reduction melting, it is achieved plumbous synthetical recovery。
2. the method for leaded alkali immersion oxidation precipitation separation of lead according to claim 1, it is characterized in that alkali immersion described in step (1) be zinc oxide ore NaOH leachate, the alkali oxide leaching dearsenization liquid of NaOH leachate containing Pb-Zn dust or lead anode slurry, lead content is 4 ~ 15%。
3. the method for a kind of leaded alkali immersion oxidation precipitation separation of lead according to claim 1, it is characterised in that oxidant Na described in step (3)2S2O8Or H2O2, in the heavy lead reaction of lead oxidation it is:
Na2S2O8+Na2PbO2=PbO2↓+2Na2SO4
H2O2+Na2PbO2=PbO2↓+2NaOH
The heavy lead skim obtained is mainly composed of PbO2, H2O2After the heavy lead of oxidation, liquid directly returns alkali leaching operation and recycles。
CN201610115959.9A 2016-03-02 2016-03-02 Method for separating lead from lead-containing alkaline leaching liquor by oxidizing and precipitating Pending CN105695764A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106167856A (en) * 2016-08-25 2016-11-30 安徽华铂再生资源科技有限公司 Reviver refine alkaline residue leaches process of tin
CN106282588A (en) * 2016-08-25 2017-01-04 安徽华铂再生资源科技有限公司 Alkali regeneration method in reviver refine alkaline residue
KR20190037038A (en) * 2017-09-28 2019-04-05 (주) 대건산업기계 Method for producing potassium chloride using cement bypass dust

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0575768A1 (en) * 1992-05-27 1993-12-29 Nikolai Vladimirovich Khodov Method of recovering lead from recycable lead-containing raw material
CN1456692A (en) * 2003-05-24 2003-11-19 北京科技大学 Wet process sulfide mineral leaching-out method
CN102242269A (en) * 2011-06-30 2011-11-16 长春黄金研究院 Method for selectively recovering lead from pregnant solution containing cyanides and heavy metals
CN102586604A (en) * 2011-01-18 2012-07-18 郴州市金贵银业股份有限公司 Technology for wet-processing anode mud containing arsenic and lead
CN105274359A (en) * 2015-10-21 2016-01-27 北京矿冶研究总院 Method for extracting and separating valuable metals from secondary lead smelting slag

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0575768A1 (en) * 1992-05-27 1993-12-29 Nikolai Vladimirovich Khodov Method of recovering lead from recycable lead-containing raw material
CN1456692A (en) * 2003-05-24 2003-11-19 北京科技大学 Wet process sulfide mineral leaching-out method
CN102586604A (en) * 2011-01-18 2012-07-18 郴州市金贵银业股份有限公司 Technology for wet-processing anode mud containing arsenic and lead
CN102242269A (en) * 2011-06-30 2011-11-16 长春黄金研究院 Method for selectively recovering lead from pregnant solution containing cyanides and heavy metals
CN105274359A (en) * 2015-10-21 2016-01-27 北京矿冶研究总院 Method for extracting and separating valuable metals from secondary lead smelting slag

Non-Patent Citations (1)

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Title
薛光等: ""从含铜、铅金精矿焙砂中综合回收金、银、铜、铅、铁的试验研究", 《中国有色金属》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106167856A (en) * 2016-08-25 2016-11-30 安徽华铂再生资源科技有限公司 Reviver refine alkaline residue leaches process of tin
CN106282588A (en) * 2016-08-25 2017-01-04 安徽华铂再生资源科技有限公司 Alkali regeneration method in reviver refine alkaline residue
KR20190037038A (en) * 2017-09-28 2019-04-05 (주) 대건산업기계 Method for producing potassium chloride using cement bypass dust
KR101968111B1 (en) * 2017-09-28 2019-08-13 성신양회 주식회사 Method for producing potassium chloride using cement bypass dust

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