CN105331823A - Lead waste residue recycling method - Google Patents
Lead waste residue recycling method Download PDFInfo
- Publication number
- CN105331823A CN105331823A CN201510935345.0A CN201510935345A CN105331823A CN 105331823 A CN105331823 A CN 105331823A CN 201510935345 A CN201510935345 A CN 201510935345A CN 105331823 A CN105331823 A CN 105331823A
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- China
- Prior art keywords
- lead
- plumbous
- waste residue
- solution
- recovery method
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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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
- C22B13/045—Recovery from waste materials
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- 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
Abstract
The invention discloses a lead waste residue recycling method. The method comprises the steps that 1, calcination is carried out, wherein lead waste residues are placed into a calcining furnace for calcination, and powder produced through calcination is collected; 2, the powder produced through calcination is completely dissolved in an excessive amount of a salpeter solution to form a nitrate solution; 3, an excessive amount of a sodium chloride solution is added into the nitrate solution, and lead chloride crystals are separated out under the low temperature; 4, the lead chloride crystals obtained in the step 3 are placed in hot water and stirred to be completely dissolved; 5, an excessive amount of carbon dioxide gas or a sodium carbonate solution are introduced into a lead chloride solution obtained in the step 4, and filtering is carried out to obtain lead carbonate crystals; 6, the lead carbonate crystals obtained in the step 5 are heated and decomposed to obtain lead oxide; 7, the lead oxide is restored to obtain elemental lead; 8, the elemental lead is molten into a lead ingot. According to the lead waste residue recycling method, the characteristic that the lead chloride is slightly dissolved in water, can separate out crystals at low temperature and can be dissolved in hot water is ingeniously utilized, and the high-purity elemental lead is obtained.
Description
Technical field
The present invention relates to a kind of recovery method of plumbous waste residue.
Background technology
From 1859 by since the special invention lead-acid cell in French slip-stick artist Pulan, lead-acid cell with its cheap price and reliable stability in secondary cell market, particularly automobile battery and electric bicycle market in occupation of important position.Show according to battery statistics, within 2012, Chinese lead bullion total quantity consumed is more than 464.6 ten thousand tons, and wherein lead-acid cell consumption is 3,300,000 tons, accounts for 71% of plumbous total quantity consumed.Due to the fast development of China's automobile consumption, can predict a very long time from now on is still faced with plumbous consumption sustainable growth and lead resource problem day by day in short supply.The major way of current plumbous scale operation is pyrometallurgical smelting.Statistic data according to Yu Guangdeng enterprise shows, is mingled with a small amount of leaded dust in the stack gas generally produced in pyrometallurgical smelting process, and these leaded dust particles, after electric field or cloth bag absorption dedusting, account for the 7-12% of plumbous output usually.Therefore one is produced per year to the Lian Qian enterprise of 400,000 tons, mean the leaded flue dust needing to process nearly 40,000 tons every year.Similarly, in existing lead-acid cell manufacturing enterprise, the brush earrings joint of the Shimadzu ball milling operation of lead powder, polar plate plaster coating operation, battery pole ear and the welding sequence of pole plate all can produce a large amount of containing plumbous oxide waste material, therefore, reclaim the method containing plumbous oxide waste material that smeltery and lead-acid cell production link produce with finding a kind of efficient, economic and environmental protection become resources effective utilization problem urgently to be resolved hurrily.
In a large amount of leaded flue dust that the pyrometallurgical smelting process of existing lead bullion produces, the general plumbous oxide containing 30-70%, the metallic compound such as iron, copper, tin simultaneously containing a small amount of silicon-dioxide, aluminum oxide and trace.The processing mode of existing leaded flue dust is divided into pyrogenic process and wet method two kinds.Wherein, leaded flue dust is used as refining leady raw materials by pyrogenic process exactly.Particularly, in leaded flue dust, generally add the materials such as a small amount of water glass or milk of lime pre-bonded is carried out to leaded flue dust, thus reduce the airborne dust produced in smelting process, improve plumbous organic efficiency.Although hydrometallurgic recovery plumbous oxide is considered to the recovery plumbous oxide mode more clean than pyrogenic process, but analyze situation according to available data to show, the hydrometallurgic recovery plumbous oxide of current report substantially all belongs to expendable and reclaims, not namely set out based on atomic economy reaction in removal process, build zero raw material consumption that atomic economy reaction and Cycling And Utilizing Patterns realize leaching process.Because existing most recovery plumbous oxide needs a large amount of chemical feedstocks to realize the recovery of plumbous oxide, in removal process, therefore not only bring the cost recovery of great number, and bring secondary lead pollution to environment.
Summary of the invention
The technical problem to be solved in the present invention overcomes the deficiencies in the prior art, provides a kind of recovery method of simple to operate, plumbous waste residue that organic efficiency is high.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is: a kind of recovery method of plumbous waste residue, comprise the following steps: 1) calcine, plumbous waste residue is put into calcining furnace and carry out calcining and the powder collecting calcining generation, the gas that calcining produces is discharged after sodium hydroxide solution process;
2) powder that calcining produces is dissolved in completely in excessive salpeter solution and forms nitrate solution;
3) in nitrate solution, add excessive sodium chloride solution and separate out lead chloride crystal at the temperature of-5-5 degree Celsius;
4) the lead chloride crystal in step 3 is placed in the hot water of 100-150 degree Celsius, stirs and make it dissolve completely;
5) in the lead chloride solution of step 4), pass into excessive carbon dioxide or add sodium carbonate solution, filtering the crystal obtaining lead carbonate;
6) the lead carbonate heating crystals obtained in step 5) is obtained plumbous oxide to 350-400 degree Celsius of decomposition;
7) plumbous oxide and carbon simple substance, carbon monoxide or hydrogen are carried out being obtained by reacting plumbous simple substance;
8) lead pig is cast in plumbous simple substance thawing.
The recovery method of above-mentioned plumbous waste residue, preferably, the concentration of described salpeter solution is 5-10%.
The recovery method of above-mentioned plumbous waste residue, preferably, the concentration of described hydrochloric acid is 3-10%.
The recovery method of above-mentioned plumbous waste residue, preferably, in step 5), the mol ratio of lead chloride and sodium carbonate is 2:3-1:2.
The recovery method of above-mentioned plumbous waste residue, preferably, the temperature of reaction in step 5) is 100-200 degree Celsius.
First carried out by plumbous waste residue in plumbous waste residue recovery method of the present invention calcining and the sulphur in plumbous waste residue, carbon, nitrogen element etc. carried out burning and form complicated metal oxide powder, metal oxide mainly contains the oxide compound of iron, copper, tin, aluminium; Be dissolved in by metal oxide powder in nitric acid, then add sodium chloride solution, now lead chloride meeting in the environment of low temperature is separated out with the form of crystal and other metal chloride can not be separated out.Lead chloride crystal can be dissolved in the hot water of 100-150 degree Celsius, and logical as carbon dioxide or the crystal adding excessive sodium carbonate solution Formed lead plumbate, and lead carbonate decomposition, reduction can be obtained simple substance lead.
The recovery method of plumbous waste residue of the present invention make use of cleverly lead chloride be slightly soluble in water at low temperatures can crystallization, and the characteristic can dissolved in the hot water, separates out lead element with the form of lead carbonate, decomposes and reduces that to obtain highly purified simple substance plumbous.
Embodiment
For the ease of understanding the present invention, hereafter will do to describe more comprehensively, meticulously to the present invention in conjunction with preferred embodiment, but protection scope of the present invention is not limited to following specific embodiment.
It should be noted that, when a certain element is described on " be fixed on, be fixed in, be connected to or be communicated in " another element, it can be directly fixing, affixed, connect or be communicated with on another element, also can be by other intermediate connectors indirectly fixing, affixed, connection or connection on another element.
Unless otherwise defined, hereinafter used all technical terms are identical with the implication that those skilled in the art understand usually.The object of technical term used herein just in order to describe specific embodiment is not be intended to limit the scope of the invention.
Embodiment 1
A recovery method for plumbous waste residue, comprises the following steps: 1) calcine, and plumbous waste residue is put into calcining furnace and carry out calcining and the powder collecting calcining generation, the gas that calcining produces is discharged after sodium hydroxide solution process;
2) powder that calcining produces is dissolved in completely in excessive salpeter solution and forms nitrate solution;
3) in nitrate solution, add excessive sodium chloride solution and separate out lead chloride crystal at the temperature of-5-5 degree Celsius;
4) the lead chloride crystal in step 3 is placed in the hot water of 100-150 degree Celsius, stirs and make it dissolve completely;
5) in the lead chloride solution of step 4), pass into excessive carbon dioxide or add sodium carbonate solution, filtering the crystal obtaining lead carbonate;
6) the lead carbonate heating crystals obtained in step 5) is obtained plumbous oxide to 350-400 degree Celsius of decomposition;
7) plumbous oxide and carbon simple substance, carbon monoxide or hydrogen are carried out being obtained by reacting plumbous simple substance;
8) lead pig is cast in plumbous simple substance thawing.
In the present embodiment, the concentration of salpeter solution is 5-10%.The concentration of hydrochloric acid is 3-10%.In step 5), the mol ratio of lead chloride and sodium carbonate is 2:3-1:2; Temperature of reaction is 100-200 degree Celsius.
First carried out by plumbous waste residue in the plumbous waste residue recovery method of the present embodiment calcining and the sulphur in plumbous waste residue, carbon, nitrogen element etc. carried out burning and form complicated metal oxide powder, metal oxide mainly contains the oxide compound of iron, copper, tin, aluminium; Be dissolved in by metal oxide powder in nitric acid, then add sodium chloride solution, now lead chloride meeting in the environment of low temperature is separated out with the form of crystal and other metal chloride can not be separated out.Lead chloride crystal can be dissolved in the hot water of 100-150 degree Celsius, and logical as carbon dioxide or the crystal adding excessive sodium carbonate solution Formed lead plumbate, and lead carbonate decomposition, reduction can be obtained simple substance lead.
The plumbous organic efficiency of the recovery method of the plumbous waste residue of the present embodiment is high, effectively can alleviate the problem of Lead contamination.
Claims (5)
1. a recovery method for plumbous waste residue, is characterized in that, comprises the following steps: 1) calcine, and plumbous waste residue is put into calcining furnace and carry out calcining and the powder collecting calcining generation, the gas that calcining produces is discharged after sodium hydroxide solution process;
2) powder that calcining produces is dissolved in completely in excessive salpeter solution and forms nitrate solution;
3) in nitrate solution, add excessive sodium chloride solution and separate out lead chloride crystal at the temperature of-5-5 degree Celsius;
4) the lead chloride crystal in step 3 is placed in the hot water of 100-150 degree Celsius, stirs and make it dissolve completely;
5) in the lead chloride solution of step 4), pass into excessive carbon dioxide or sodium carbonate solution, filter the crystal obtaining lead carbonate;
6) the lead carbonate heating crystals obtained in step 5) is obtained plumbous oxide to 350-400 degree Celsius of decomposition;
7) plumbous oxide and carbon simple substance, carbon monoxide or hydrogen are carried out being obtained by reacting plumbous simple substance;
8) lead pig is cast in plumbous simple substance thawing.
2. the recovery method of plumbous waste residue according to claim 1, is characterized in that: the concentration of described salpeter solution is 5-10%.
3. the recovery method of plumbous waste residue according to claim 1, is characterized in that: the concentration of described hydrochloric acid is 3-10%.
4. the recovery method of plumbous waste residue according to claim 1, is characterized in that: in step 5), the mol ratio of lead chloride and sodium carbonate is 2:3-1:2.
5. the recovery method of plumbous waste residue according to claim 4, is characterized in that: the temperature of reaction in step 5) is 100-200 degree Celsius.
Priority Applications (1)
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| CN201510935345.0A CN105331823A (en) | 2015-12-15 | 2015-12-15 | Lead waste residue recycling method |
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| CN201510935345.0A CN105331823A (en) | 2015-12-15 | 2015-12-15 | Lead waste residue recycling method |
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| CN105331823A true CN105331823A (en) | 2016-02-17 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106834721A (en) * | 2017-01-04 | 2017-06-13 | 长沙汇聚环境技术有限公司 | A kind of its recovery method as resource of the leaded zinc powder dirt of blast furnace |
| CN110137452A (en) * | 2019-04-26 | 2019-08-16 | 浙江工业大学 | A kind of preparation method and application of Nanometer sized lead oxide/carbon composite |
| CN110791661A (en) * | 2019-09-18 | 2020-02-14 | 超威电源集团有限公司 | Waste lead paste recovery treatment method |
Citations (5)
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| CN1065885A (en) * | 1992-06-05 | 1992-11-04 | 孙午伯 | The method that scrap battery lead reclaims |
| CN101768668A (en) * | 2010-01-07 | 2010-07-07 | 株洲冶炼集团股份有限公司 | Method for comprehensive recovery of lead and tin from alkaline refining slag of lead |
| CN103290225A (en) * | 2013-06-20 | 2013-09-11 | 长沙华明复合材料科技有限公司 | Method for recovering lead from lead-containing solid wastes |
| CN104178631A (en) * | 2013-07-22 | 2014-12-03 | 天能电池(芜湖)有限公司 | Lead recycling technology of lead pollution for storage battery |
| CN104726718A (en) * | 2015-04-07 | 2015-06-24 | 杨秋良 | Method for producing high-purity discandium trioxide from alkali fusion separated anode slime/silver separating residue by use of total wet process |
-
2015
- 2015-12-15 CN CN201510935345.0A patent/CN105331823A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1065885A (en) * | 1992-06-05 | 1992-11-04 | 孙午伯 | The method that scrap battery lead reclaims |
| CN101768668A (en) * | 2010-01-07 | 2010-07-07 | 株洲冶炼集团股份有限公司 | Method for comprehensive recovery of lead and tin from alkaline refining slag of lead |
| CN103290225A (en) * | 2013-06-20 | 2013-09-11 | 长沙华明复合材料科技有限公司 | Method for recovering lead from lead-containing solid wastes |
| CN104178631A (en) * | 2013-07-22 | 2014-12-03 | 天能电池(芜湖)有限公司 | Lead recycling technology of lead pollution for storage battery |
| CN104726718A (en) * | 2015-04-07 | 2015-06-24 | 杨秋良 | Method for producing high-purity discandium trioxide from alkali fusion separated anode slime/silver separating residue by use of total wet process |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106834721A (en) * | 2017-01-04 | 2017-06-13 | 长沙汇聚环境技术有限公司 | A kind of its recovery method as resource of the leaded zinc powder dirt of blast furnace |
| CN110137452A (en) * | 2019-04-26 | 2019-08-16 | 浙江工业大学 | A kind of preparation method and application of Nanometer sized lead oxide/carbon composite |
| CN110791661A (en) * | 2019-09-18 | 2020-02-14 | 超威电源集团有限公司 | Waste lead paste recovery treatment method |
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