CN106834734A - A kind of agitating ball mill high-efficiency desulfurization method - Google Patents
A kind of agitating ball mill high-efficiency desulfurization method Download PDFInfo
- Publication number
- CN106834734A CN106834734A CN201710162410.XA CN201710162410A CN106834734A CN 106834734 A CN106834734 A CN 106834734A CN 201710162410 A CN201710162410 A CN 201710162410A CN 106834734 A CN106834734 A CN 106834734A
- Authority
- CN
- China
- Prior art keywords
- ball mill
- agitating ball
- desulfurization
- lead plaster
- medium
- 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.)
- Pending
Links
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
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Crushing And Grinding (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention relates to lead plaster desulfurization technology, particularly a kind of agitating ball mill high-efficiency desulfurization method.The present invention is first to the medium ball that a diameter of 5 12mm is added in agitating ball mill, medium sphere volume pack completeness is set to reach 40 60%, and then the lead plaster ore pulp that mass concentration is 20 70% is added, one or more compounds make C/S mol ratios reach 1.1 1.5/1 as desulfurizing agent in being subsequently adding sodium carbonate or potassium carbonate, sodium acid carbonate or saleratus, ammonium hydrogencarbonate；Agitating ball mill cover being fixed again, and setting reaction temperature as 25 50 DEG C, in 15 60min, regulation agitating ball mill speed of agitator is 400 700r/min, until desulphurization reaction terminates for reaction time control.Ore pulp after inventive desulfurization is by after washing, filtering, desulfurization degree reaches more than 95.5%；The recovery utilization rate of lead plaster is drastically increased, environmental pollution is eliminated.
Description
Technical field
The present invention relates to lead plaster desulfurization technology, particularly a kind of agitating ball mill high-efficiency desulfurization method.
Background technology
Lead-acid accumulator is widely used in the fields such as motor vehicle, mobile communication base station, defence equipment.In recent years, with
The sustained and rapid development of lead-acid accumulator industry, China has turned into the producing country and country of consumption of lead-acid accumulator the biggest in the world.
China's lead-acid accumulator yield accounts for the 1/3 of Gross World Product, and the lead-acid accumulator scrapped in use every year is more than 300
Ten thousand tons.Lead plaster in waste lead acid battery contains a large amount of sulphur lead compounds, it is necessary to properly recycle, and the difficult point that lead is reclaimed is
The desulfurization of content highest lead sulfate in lead plaster.At present, the recovery method of waste lead acid battery lead plaster mainly has pyrogenic process, wet method and wet
Method-pyrogenic process joint smelting.Pyrometallurgical smelting process needs 1300 DEG C of high temperature, there is the lead dust two for producing sulfur dioxide and high temperature
Secondary pollutant, and its relative energy consumption is higher, the more low defect of utilization rate.Typical wet method smelting process includes Solid phase electrolysis
Reducing process, directly leachings-strike and desulfurization conversion-strike, production process pollution are lacked, be easily controlled and
Accuracy is high, but flow is relative complex.Wet method-pyrogenic process combined recovery technique is by the sulfuric acid in scrap lead cream by chemical method
Lead is converted into the carbonic acid lead compound (desulfurization stage) for being easy to low-temperature decomposition, then carries out low smelting heat (about 350 DEG C), obtain lead or
Lead oxide.The technique combines the advantage of wet method and pyrometallurgical smelting, but desulfurized effect is unsatisfactory, the final material after desulfurization
Sulfur-bearing rate be difficult to reach the level less than 0.5%, be not suitable for carrying out low smelting heat.Therefore, the desulfurization degree of raising scrap lead cream is
Reclaim the important channel of lead in economical and efficient ground.
The content of the invention
It is an object of the invention to provide a kind of agitating ball mill high-efficiency desulfurization method, it is intended to solve lead plaster desulfurization degree low
Problem.
What the present invention was realized in：
A kind of agitating ball mill high-efficiency desulfurization method, first to the medium ball that a diameter of 5-12mm is added in agitating ball mill,
Medium sphere volume pack completeness is set to reach 40-60%, it is the lead plaster ore pulp of 20-70% and then to add mass concentration, is subsequently adding
One or more compounds make as desulfurizing agent in sodium carbonate or potassium carbonate, sodium acid carbonate or saleratus, ammonium hydrogencarbonate
C/S mol ratios reach 1.1-1.5/1；Agitating ball mill cover is fixed again, and sets reaction temperature as 25-50 DEG C, the reaction time
In 15-60min, regulation agitating ball mill speed of agitator is 400-700r/min, until desulphurization reaction terminates for control.
Ore pulp after inventive desulfurization is by after washing, filtering, desulfurization degree reaches more than 95.5%；Realize the height of lead plaster
Effect desulfurization, drastically increases the recovery utilization rate of lead plaster, eliminates environmental pollution, and technological process is simple.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
The medium ball of a diameter of 12mm is first added to agitating ball mill, medium sphere volume pack completeness is reached 40%, immediately
The lead plaster ore pulp for adding mass concentration to be 20%, sodium carbonate is subsequently adding as desulfurizing agent, C/S mol ratios is reached 1.1/1.
After installing material and medium, fixed agitating ball mill cover, and reaction temperature to 25 DEG C is set, regulation speed of agitator is 700r/
Min, starts reaction, and the reaction time is controlled in 30min.After reaction terminates, by the ore pulp after desulfurization by three washings, filtering
Afterwards, desulfurization Analysis are carried out.By analysis, the desulfurization degree of lead plaster reaches 95.66%.
Embodiment 2
The medium ball of a diameter of 10mm is first added to agitating ball mill, medium sphere volume pack completeness is reached 50%, immediately
The lead plaster ore pulp for adding mass concentration to be 30%, sodium carbonate and potassium carbonate mixtures is subsequently adding as desulfurizing agent (wherein carbon
Sour sodium is 4 with the mol ratio of potassium carbonate:1) C/S mol ratios, are made to reach 1.2/1.After installing material and medium, fixed stirring ball-milling
Machine cover, and reaction temperature to 35 DEG C is set, regulation speed of agitator is 500r/min, starts reaction, and reaction time control exists
15min.After reaction terminates, by the ore pulp after desulfurization by after three washings, filtering, carrying out desulfurization Analysis.By analysis, lead plaster
Desulfurization degree reach 96.12%.
Embodiment 3
The medium ball of a diameter of 8mm is first added to agitating ball mill, medium sphere volume pack completeness is reached 40%, and then
The lead plaster ore pulp for adding mass concentration to be 40%, is subsequently adding sodium carbonate and ammonium hydrogencarbonate mixture as desulfurizing agent (wherein carbon
Sour sodium is 4 with the mol ratio of ammonium hydrogencarbonate:1) C/S mol ratios, are made to reach 1.2/1.After installing material and medium, fixed stirring ball
Grinding machine cover, and reaction temperature to 40 DEG C is set, regulation speed of agitator is 400r/min, starts reaction, and reaction time control exists
25min.After reaction terminates, by the ore pulp after desulfurization by after three washings, filtering, carrying out desulfurization Analysis.By analysis, lead plaster
Desulfurization degree reach 96.68%.
Embodiment 4
The medium ball of a diameter of 8mm is first added to agitating ball mill, medium sphere volume pack completeness is reached 50%, and then
The lead plaster ore pulp for adding mass concentration to be 50%, is subsequently adding potassium carbonate as desulfurizing agent, C/S mol ratios is reached 1.3/1.Dress
After good material and medium, fixed agitating ball mill cover, and reaction temperature to 25 DEG C is set, regulation speed of agitator is 600r/
Min, starts reaction, and the reaction time is controlled in 50min.After reaction terminates, by the ore pulp after desulfurization by three washings, filtering
Afterwards, desulfurization Analysis are carried out.By analysis, the desulfurization degree of lead plaster reaches 96.39%.
Embodiment 5
The medium ball of a diameter of 5mm is first added to agitating ball mill, medium sphere volume pack completeness is reached 60%, and then
The lead plaster ore pulp for adding mass concentration to be 60%, is subsequently adding sodium carbonate as desulfurizing agent, C/S mol ratios is reached 1.4/1.Dress
After good material and medium, fixed agitating ball mill cover, and reaction temperature to 50 DEG C is set, regulation speed of agitator is 500r/
Min, starts reaction, and the reaction time is controlled in 40min.After reaction terminates, by the ore pulp after desulfurization by three washings, filtering
Afterwards, desulfurization Analysis are carried out.By analysis, the desulfurization degree of lead plaster reaches 96.88%.
Embodiment 6
The medium ball of a diameter of 6mm is first added to agitating ball mill, medium sphere volume pack completeness is reached 60%, and then
The lead plaster ore pulp for adding mass concentration to be 70%, is subsequently adding sodium carbonate and sodium bicarbonate mixture as desulfurizing agent (wherein carbon
Sour sodium is 9 with the mol ratio of sodium acid carbonate:1) C/S mol ratios, are made to reach 1.5/1.After installing material and medium, fixed stirring ball
Grinding machine cover, and reaction temperature to 40 DEG C is set, regulation speed of agitator is 400r/min, starts reaction, and reaction time control exists
60min.After reaction terminates, by the ore pulp after desulfurization by after three washings, filtering, carrying out desulfurization Analysis.By analysis, lead plaster
Desulfurization degree reach 96.68%.
Claims (2)
1. a kind of agitating ball mill high-efficiency desulfurization method, it is characterized in that：First to adding a diameter of 5-12mm's in agitating ball mill
Medium ball, makes medium sphere volume pack completeness reach 40-60%, and it is the lead plaster ore pulp of 20-70% and then to add mass concentration, so
One or more compounds are used as de- in adding sodium carbonate or potassium carbonate, sodium acid carbonate or saleratus, ammonium hydrogencarbonate afterwards
Sulphur agent, makes C/S mol ratios reach 1-1.5/1；Agitating ball mill cover is fixed again, and sets reaction temperature as 25-50 DEG C, react
In 15-60min, regulation agitating ball mill speed of agitator is 400-700r/min to time control, until desulphurization reaction terminates.
2. a kind of agitating ball mill high-efficiency desulfurization method according to claim 1, it is characterized in that：It is embodied as：First to
The medium ball of a diameter of 6mm is added in agitating ball mill, medium sphere volume pack completeness is reached 60%, and then add quality dense
The lead plaster ore pulp for 70% is spent, sodium carbonate and sodium bicarbonate mixture is subsequently adding as desulfurizing agent, sodium carbonate and sodium acid carbonate
Mol ratio be 9:1, C/S mol ratios is reached 1.5/1；Agitating ball mill cover is fixed again, and sets reaction temperature to 40 DEG C,
Regulation speed of agitator is 400r/min, and the reaction time is controlled in 60min；After reaction terminates, by the ore pulp after desulfurization by three times
After washing, filtering, desulfurization Analysis are carried out, the desulfurization degree of lead plaster reaches 96.68%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710162410.XA CN106834734A (en) | 2017-03-18 | 2017-03-18 | A kind of agitating ball mill high-efficiency desulfurization method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710162410.XA CN106834734A (en) | 2017-03-18 | 2017-03-18 | A kind of agitating ball mill high-efficiency desulfurization method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106834734A true CN106834734A (en) | 2017-06-13 |
Family
ID=59145211
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710162410.XA Pending CN106834734A (en) | 2017-03-18 | 2017-03-18 | A kind of agitating ball mill high-efficiency desulfurization method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106834734A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101608264A (en) * | 2009-06-30 | 2009-12-23 | 张天任 | A kind of waste lead recovering method for lead-acid storage batteries |
| CN103060569A (en) * | 2013-01-15 | 2013-04-24 | 浙江汇同电源有限公司 | Process of recovering lead from pasty fluid of waste lead-acid storage battery |
| CN103540741A (en) * | 2013-11-05 | 2014-01-29 | 湖南江冶机电科技股份有限公司 | Forcible wet desulphurization process for lead plaster |
| CN104263944A (en) * | 2014-09-29 | 2015-01-07 | 湖南江冶机电科技股份有限公司 | Lead paste desulfurization method based on grinding mechanism |
| CN106337112A (en) * | 2016-08-25 | 2017-01-18 | 安徽华铂再生资源科技有限公司 | Wet low-liquid-solid-ratio desulfurization process for waste lead-acid storage battery lead plaster |
| CN106435194A (en) * | 2016-09-30 | 2017-02-22 | 刘振 | Efficient desulfurization technology for waste lead-acid cell lead plaster |
-
2017
- 2017-03-18 CN CN201710162410.XA patent/CN106834734A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101608264A (en) * | 2009-06-30 | 2009-12-23 | 张天任 | A kind of waste lead recovering method for lead-acid storage batteries |
| CN103060569A (en) * | 2013-01-15 | 2013-04-24 | 浙江汇同电源有限公司 | Process of recovering lead from pasty fluid of waste lead-acid storage battery |
| CN103540741A (en) * | 2013-11-05 | 2014-01-29 | 湖南江冶机电科技股份有限公司 | Forcible wet desulphurization process for lead plaster |
| CN104263944A (en) * | 2014-09-29 | 2015-01-07 | 湖南江冶机电科技股份有限公司 | Lead paste desulfurization method based on grinding mechanism |
| CN106337112A (en) * | 2016-08-25 | 2017-01-18 | 安徽华铂再生资源科技有限公司 | Wet low-liquid-solid-ratio desulfurization process for waste lead-acid storage battery lead plaster |
| CN106435194A (en) * | 2016-09-30 | 2017-02-22 | 刘振 | Efficient desulfurization technology for waste lead-acid cell lead plaster |
Non-Patent Citations (1)
| Title |
|---|
| 边文璟: "基于粒子研磨作用的废铅膏脱硫新方法实验研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101609888B (en) | Method for preparing battery level lithium carbonate by using lithium chloride solution | |
| CN105280976A (en) | Environmental-friendly and high-efficiency processing method of waste lead-acid storage battery | |
| CN103526016B (en) | A kind of method of raw material containing lead hydrometallurgic recovery | |
| CN106587142B (en) | A kind of method that 4BS is prepared using waste lead acid battery lead cream | |
| CN110459828B (en) | Comprehensive recovery method of waste lithium iron phosphate battery positive electrode material | |
| CN104208992A (en) | Method for desulfurizing acid gas containing hydrogen sulfide and recycling sulfur | |
| CN107394300A (en) | A kind of sulfur method of waste lead acid battery lead cream | |
| CN112723330B (en) | Preparation method and application of iso-phospho-ferromanganese iron phosphate | |
| CN105858716A (en) | Novel method for directly regenerating waste lead-acid battery into lead powders | |
| CN102424431A (en) | Method for preparing nickel oxide, magnesium oxide and silicon oxide products from laterite-nickel ore | |
| CN105420489A (en) | Diachylon desulphurization method based on throttling self-collision | |
| CN102352442B (en) | Waste lead acid storage battery lead paste desulfurization method | |
| CN108754129A (en) | A kind of method of waste diachylon segmented desulfurization | |
| CN104975168A (en) | Method for rapidly desulfurizing lead-sulfate-containing substances | |
| CN108565419A (en) | A kind of regenerative lithium ion anode material and preparation method thereof | |
| CN112582606B (en) | Preparation method and device of lead-acid storage battery positive electrode material | |
| CN106222425A (en) | The sulfur method of lead plaster in a kind of waste and old lead acid accumulator | |
| CN107586951A (en) | A kind of method that manganese, iron isochronous resources utilize in low-grade manganese carbonate ore | |
| CN106834734A (en) | A kind of agitating ball mill high-efficiency desulfurization method | |
| CN106450540A (en) | Lead paste recycling method by atomic economic method | |
| CN109599602A (en) | The method that the waste and old positive electrode of a kind of pair of lithium battery carries out resource utilization | |
| CN102851486A (en) | Pyrite cinder treatment method | |
| CN109585962A (en) | A kind of method of the waste and old positive electrode of resource utilization lithium battery | |
| CN105149105B (en) | A kind of method of fluorite concentrate desulfurization purifying | |
| CN202778263U (en) | System for recovering sulfur dioxide in smoke |
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 | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170613 |
|
| WD01 | Invention patent application deemed withdrawn after publication |