CN108754129A - A kind of method of waste diachylon segmented desulfurization - Google Patents
A kind of method of waste diachylon segmented desulfurization Download PDFInfo
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- CN108754129A CN108754129A CN201810554054.0A CN201810554054A CN108754129A CN 108754129 A CN108754129 A CN 108754129A CN 201810554054 A CN201810554054 A CN 201810554054A CN 108754129 A CN108754129 A CN 108754129A
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- lead plaster
- desulfurization
- reaction
- filtrate
- desulfurizing agent
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/11—Removing sulfur, phosphorus or arsenic other than by roasting
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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
- C22B13/02—Obtaining lead by dry processes
- C22B13/025—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
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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
- 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
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- General Life Sciences & Earth Sciences (AREA)
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Abstract
Once desulfurization reaction system is added in lead plaster, desulfurizing agent, water by a kind of method of waste diachylon segmented desulfurization, and mixed serum carries out press filtration and obtains first-time filtrate and once desulfurization lead plaster；Detect first-time filtrate concentration and desulfurization lead plaster sulfur content.First-time filtrate concentration is judged, concentration is more than 25 ~ 40% and is recycled into crystal system, and concentration is less than 25 ~ 40% and returns to once desulfurization system；Secondary desulfuration reaction system is added in once desulfurization lead plaster, desulfurizing agent, water；After the completion of reaction, mixed serum carries out press filtration and obtains secondary filtrate and secondary desulfuration lead plaster；Secondary filtrate enters once desulfurization reaction system；Secondary desulfuration lead plaster sulfur content is judged, sulfur content is less than 0.1 ~ 0.5% and enters converter smelting system, and sulfur content is more than 0.1 ~ 0.5% and returns to secondary desulfuration system.For inventive desulfurization agent utilization rate up to 99% or more, lead plaster desulfurization degree is far above industry average level up to 98% or more.
Description
Technical field
The present invention relates to a kind of recovery methods of reviver, belong to waste and old lead acid accumulator reclaiming field.
Background technology
Lead-acid accumulator has been developed more than 160 years, is now widely used in the fields such as passenger car, communication, military affairs, and China is every
The lead-acid accumulator that year scraps reaches 300,000,000, more than 350 ten thousand tons of lead tolerance.Waste and old lead acid accumulator resource reclaim recycles
The important content of recycling economy development can not only recycle the resources such as metallic lead, plastics, sulfuric acid, but also be also environmental protection
It needs, if because lead, sulfuric acid are not recycled effectively, serious influence will be caused on environment.Waste and old lead acid accumulator
Cracking and sorting obtains plastics, sulfuric acid, lead grid, lead plaster etc. and is required for recycling after collection, and lead plaster is main component, accounts for battery
Recycle the 30 ~ 50% of weight.The main component of wherein lead plaster includes：PbSO4（50-60%）,PbO2（20-30%）,PbO（10-15%）
With other substances（0 .5-1%）.Lead sulfate accounts for major part wherein, at the same also contain other sulfide of part and lead, antimony,
The heavy metal substances such as arsenic, zinc.The recovery method of lead plaster mainly has high temperature pyrometallurgical smelting and desulfurization-two kinds of converter low smelting heat, high
Warm fire method recovery process needs carry out in 1100 DEG C or more of high temperature, because its cardinal principle is that the lead sulfate in lead plaster exists
Lead is converted under the action of the reducing agents such as coke, iron filings, this traditional lead plaster smelting process has the following problems：（1）It is required that
Temperature is high, and natural gas, amount of oxygen consumption are big, and production cost is higher；（2）Lead volatility amount increases under high temperature, leads to lead in lead plaster
The rate of recovery reduces；（3）Sulphur in lead plaster is reacted with oxygen generates a large amount of SO2Gas enters in flue gas, and being discharged into air will production
Raw Heavy environmental pollution will consume a large amount of alkali if the method using Alkali absorption carries out desulfurization process, and cost is higher, meanwhile,
The desulfurization wastewater impurity content of generation is high, can not recycle, and results in secondary waste water pollution.The side more praised highly outside Current Domestic
Method is exactly under carbonate effect to convert lead sulfate in lead plaster to ceruse, then by the ceruse after reaction at low temperature into
Row is smelted, and the ceruse decomposition temperature which obtains is very low, and energy consumption can be largely saved compared to high temperature pyrometallurgical smelting.Together
When, into the solid material not sulfur-bearing of smelting furnace, also without or with seldom sulfur dioxide in the flue gas of output.Desulphurization reaction
The method that evaporative crystallization can be used in the sulfate by-products of generation is recycled, and generates certain economic value, which has
Good energy-saving benefit and economic benefit.
Domestic praise highly recycles lead plaster using desulfurization-converter low smelting heat technique at present, domestic large size lead acid storage battery
The most import of pond returned enterprise external advanced lead plaster desulfurization and desulfurizing byproduct reclaimer, but do not obtain practical fortune
With equipment causes huge waste all in idle state.The problem of being primarily present has：（1）Desulfurization degree is low, lead after desulfurization
For cream sulfur content 1 ~ 2%, there are a large amount of lead sulfates not to react completely, causes low smelting heat that can not all be recycled to lead plaster, lead recycling
Rate is low；（2）Desulfurization filter liquor concentration is low, and average 15 ~ 20% or so, cause crystallization removal process to need to evaporate a large amount of water, energy consumption
Height, low production efficiency；（3）Desulfurizing agent is not sufficiently reacted, and causes desulfurization degree low, while desulfurizing agent enters in desulfurization filtrate, is taken off
Sulphur filtrate pure cannot be recycled, and desulfurizing agent is caused to waste, and production cost increases.
Invention content
The object of the present invention is to provide a kind of methods of efficient waste diachylon segmented desulfurization, by using segmentation
Formula desulfurization method improves lead plaster desulfurization degree, meanwhile, desulfurization filtrate cycle utilizes, and improves filter liquor concentration and sorbent utilization,
The energy consumption cost and material cost for greatly reducing production process, make desulfurization technology that can actually be promoted the use.
Technical program of the present invention lies in the method includes the steps of：
（1）Waste and old lead acid accumulator obtains lead plaster by cracking and sorting, is sampled detection sulfur content；
（2）Once desulfurization reaction system is added in the lead plaster, desulfurizing agent, water；Cation and sulphur in lead plaster in the desulfurizing agent
The molar ratio of element is 1.5 ~ 2:1, desulphurization reaction liquid-solid ratio mass ratio is 1 ~ 2:1, addition sequence is water, lead plaster, desulfurizing agent, is taken off
Reaction of Salmon-Saxl temperature is 20 ~ 30 DEG C, and the reaction time is 30 ~ 60min；
The desulfurizing agent is NH4HCO3、Na2CO3、(NH4)2 CO3、NaHCO3；
（3）Step（2）Middle once desulfurization reaction system includes：Lead plaster, desulfurizing agent, water carry out solid-liquid reaction；After the completion of reaction,
Mixed serum progress press filtration is obtained into first-time filtrate and once desulfurization lead plaster；
（4）First-time filtrate concentration is judged, concentration is more than 30% ~ 40% and is recycled into crystal system, and concentration is less than 30%
~ 40% returns to once desulfurization reaction system；
（5）Secondary desulfuration reaction system is added in the once desulfurization lead plaster, desulfurizing agent, water；In the desulfurizing agent cation with
The molar ratio of element sulphur is 7.5 ~ 10 in once desulfurization lead plaster:1, desulphurization reaction liquid-solid ratio mass ratio is 1 ~ 2:1, addition sequence is
Water, lead plaster, desulfurizing agent, desulfurization reaction temperature are 20 ~ 30 DEG C, reaction time 10-30min；The desulfurizing agent is NH4HCO3、
Na2CO3、(NH4)2 CO3、NaHCO3,；
（6）Step（5）Middle secondary desulfuration reaction system includes：Once desulfurization lead plaster, desulfurizing agent, pure water carry out solid-liquid reaction；Instead
After the completion of answering, mixed serum carries out press filtration and obtains secondary filtrate and secondary desulfuration lead plaster；
（7）Secondary filtrate enters once desulfurization reaction system；
（8）Secondary desulfuration lead plaster sulfur content is judged, sulfur content is less than 0.1% ~ 0.5% and enters converter smelting system, and sulphur contains
Amount is more than 0.1% ~ 0.5% and returns to secondary desulfuration reaction system.
Step of the present invention（1）In, lead plaster need to dry 12h at 105 DEG C, and 140 mesh standard sieves are crossed after being fully ground, are taken
Screenings detects sulfur content, and detecting instrument is high frequency infrared ray carbon sulphur analyser.
Step of the present invention（3）In, first-time filtrate detects the concentration of sulfate in filtrate, and once desulfurization lead plaster detects sulphur
Content.
Step of the present invention（6）In in secondary filtrate detection filtrate sulfate concentration, secondary desulfuration lead plaster detects sulphur
Content.
Step of the present invention（2）In water be pure water, first-time filtrate or one kind in secondary filtrate or combination.
Step of the present invention（4）In first-time filtrate concentration is judged, first-time filtrate detection concentration be in filtrate
The concentration of sulfate, the criterion of the concentration of sulfate are that the solubility of the sulfate corresponding to filtrate is formulated.
Step of the present invention（8）In secondary filter liquor concentration is judged, the concentration of secondary filtrate detection is in filtrate
The concentration of sulfate, the criterion of the concentration of sulfate are that the solubility of the sulfate corresponding to filtrate is formulated.
Step of the present invention（8）In, the criterion of secondary desulfuration lead plaster sulfur content is according to converter smelting system pair
What the sulfur content requirement of raw material was formulated.
The beneficial effects of the invention are as follows：（1）First-time filtrate is recycled in once desulfurization reaction system, and it is dense to improve filtrate
Degree, can reduce filtrate cost recovery；（2）Lead plaster is in excessive state in once desulfurization system, and desulfurizing agent can be reacted completely,
It will not be introduced into first-time filtrate, desulfurization utilization rate is high, while the pure recycling of first-time filtrate；（3）Lead plaster carries out multistage desulphurization reaction,
Meanwhile in secondary desulfuration system, desulfurizing agent is in excessive state, and the reactivity of sulphur in lead plaster can be improved, greatly improve desulfurization degree；
（4）Secondary desulfuration filtrate contains a large amount of desulfurizing agents, is utilized again into once desulfurization system, improves the utilization rate of desulfurizing agent.
For inventive desulfurization agent utilization rate up to 99% or more, lead plaster desulfurization degree is far above industry average level up to 98% or more.
Description of the drawings
Fig. 1 is the process flow diagram of the present invention.
Specific implementation mode
Embodiment 1
Waste and old lead acid accumulator is first obtained into lead plaster by cracking and sorting, is sampled detection sulfur content, detects lead plaster sulfur content
It is 6.5%.The present embodiment takes lead plaster 10t to carry out desulphurization reaction according to Fig. 1 technological processes, and detection lead plaster sulfur content is 6.5%, is taken off
Sulphur agent uses NH4HCO3, wherein ammonium ion and element sulphur molar ratio in lead plaster are 1.5:1, react liquid-solid ratio（Mass ratio）For
1.5, reaction temperature is 20 DEG C, reaction time 40min, and after completing once desulfurization reaction, it is 1.6% to detect sulfur content in lead plaster, into
Enter secondary desulfuration system, (NH in first-time filtrate4)2SO4Content is 19.5%, sets concentration criterion as 35%, first-time filtrate is returned
Once desulfurization system is returned, then detects (NH in filtrate after secondary response4)2SO4Content is 37.8%, and judgement is qualified, can enter system of crystallization
System.
Secondary desulfuration system desulfurizing agent is also NH4HCO3, the molar ratio of ammonium ion and sulfur content in once desulfurization lead plaster is
7.5:1, react liquid-solid ratio（Mass ratio）It is 1, reaction temperature is 20 DEG C, reaction time 20min, after completing secondary desulfuration reaction,
It is 0.15% to detect sulfur content in lead plaster, and judgement is qualified, can enter converter smelting system.
Embodiment 2
The present embodiment takes lead plaster 10t to carry out desulphurization reaction according to Fig. 1 technological processes, and detection lead plaster sulfur content is 6.5%, desulfurizing agent
Using NH4HCO3, wherein ammonium ion and element sulphur molar ratio in lead plaster are 1.7:1, react liquid-solid ratio（Mass ratio）It is 1.7, instead
It is 20 DEG C, reaction time 35min to answer temperature, and after completing once desulfurization reaction, it is 1.3% to detect sulfur content in lead plaster, and entrance is secondary
Desulphurization system, (NH in first-time filtrate4)2SO4Content is 20.3%, sets concentration criterion as 35%, filtrate returns to once desulfurization
(NH in filtrate is detected after system, then secondary response4)2SO4Content is 39.5%, and judgement is qualified, can enter crystal system.
Secondary desulfuration system desulfurizing agent is also NH4HCO3, the molar ratio of ammonium ion and sulfur content in once desulfurization lead plaster
It is 8.5:1, react liquid-solid ratio（Mass ratio）It is 1, reaction temperature is 20 DEG C, reaction time 15min, completes secondary desulfuration reaction
Afterwards, it is 0.13% to detect sulfur content in lead plaster, and judgement is qualified, can enter converter smelting system.
Embodiment 3
The present embodiment takes lead plaster 10t to carry out desulphurization reaction according to Fig. 1 technological processes, and detection lead plaster sulfur content is 6.5%, desulfurization
Agent uses Na2CO3, sodium ion is 1.5 with element sulphur molar ratio in lead plaster:1, react liquid-solid ratio（Mass ratio）It is 2, reaction temperature
It it is 30 DEG C, reaction time 40min, after completing once desulfurization reaction, it is 1.1% to detect sulfur content in lead plaster, into secondary desulfuration system
It unites, Na in first-time filtrate2SO4Content is 19.4%, sets concentration criterion as 28%, filtrate returns to once desulfurization system, again
Na in filtrate is detected after reaction2SO4Content is 29.1%, and judgement is qualified, can enter crystal system.
Secondary desulfuration system desulfurizing agent is also Na2CO3, sodium ion and the molar ratio of sulfur content in once desulfurization lead plaster are
7.5:1, react liquid-solid ratio（Mass ratio）It is 1, reaction temperature is 30 DEG C, reaction time 15min, after completing secondary desulfuration reaction,
It is 0.11% to detect sulfur content in lead plaster, and judgement is qualified, can enter converter smelting system.
Embodiment 4
The present embodiment takes lead plaster 10t to carry out desulphurization reaction according to Fig. 1 technological processes, and detection lead plaster sulfur content is 6.6%, desulfurizing agent
Using Na2CO3, sodium ion is 1.7 with element sulphur molar ratio in lead plaster:1, react liquid-solid ratio（Mass ratio）It is 2, reaction temperature is
30 DEG C, reaction time 35min, after completing once desulfurization reaction, it is 0.9% to detect sulfur content in lead plaster, into secondary desulfuration system
It unites, Na in first-time filtrate2SO4Content is 19.8%, sets concentration criterion as 28%, filtrate returns to once desulfurization system, again
Na in filtrate is detected after reaction2SO4Content is 30.5%, and judgement is qualified, can enter crystal system.
Secondary desulfuration system desulfurizing agent is also Na2CO3, sodium ion and the molar ratio of sulfur content in once desulfurization lead plaster are
8.5:1, react liquid-solid ratio（Mass ratio）It is 1, reaction temperature is 30 DEG C, reaction time 15min, after completing secondary desulfuration reaction,
It is 0.1% to detect sulfur content in lead plaster, and judgement is qualified, can enter converter smelting system.
Claims (5)
1. a kind of method of waste diachylon segmented desulfurization, it is characterised in that the method includes the steps of：
（1）Waste and old lead acid accumulator obtains lead plaster by cracking and sorting, is sampled detection sulfur content；
（2）Once desulfurization reaction system is added in the lead plaster, desulfurizing agent, water；Cation and sulphur in lead plaster in the desulfurizing agent
The molar ratio of element is 1.5 ~ 2:1, desulphurization reaction liquid-solid ratio mass ratio is 1 ~ 2:1, addition sequence is water, lead plaster, desulfurizing agent, is taken off
Reaction of Salmon-Saxl temperature is 20 ~ 30 DEG C, and the reaction time is 30 ~ 60min；
The desulfurizing agent is NH4HCO3、Na2CO3、(NH4)2 CO3、NaHCO3；
（3）Step（2）Middle once desulfurization reaction system includes：Lead plaster, desulfurizing agent, water carry out solid-liquid reaction；After the completion of reaction,
Mixed serum progress press filtration is obtained into first-time filtrate and once desulfurization lead plaster；
（4）First-time filtrate concentration is judged, concentration is more than 30% ~ 40% and is recycled into crystal system, and concentration is less than 30%
~ 40% returns to once desulfurization reaction system；
（5）Secondary desulfuration reaction system is added in the once desulfurization lead plaster, desulfurizing agent, water；In the desulfurizing agent cation with
The molar ratio of element sulphur is 7.5 ~ 10 in once desulfurization lead plaster:1, desulphurization reaction liquid-solid ratio mass ratio is 1 ~ 2:1, addition sequence is
Water, lead plaster, desulfurizing agent, desulfurization reaction temperature are 20 ~ 30 DEG C, reaction time 10-30min；The desulfurizing agent is NH4HCO3、
Na2CO3、(NH4)2 CO3、NaHCO3,；
（6）Step（5）Middle secondary desulfuration reaction system includes：Once desulfurization lead plaster, desulfurizing agent, pure water carry out solid-liquid reaction；Instead
After the completion of answering, mixed serum carries out press filtration and obtains secondary filtrate and secondary desulfuration lead plaster；
（7）Secondary filtrate enters once desulfurization reaction system；
（8）Secondary desulfuration lead plaster sulfur content is judged, sulfur content is less than 0.1% ~ 0.5% and enters converter smelting system, and sulphur contains
Amount is more than 0.1% ~ 0.5% and returns to secondary desulfuration reaction system.
2. the method for waste diachylon circulation desulfurization according to claim 1, it is characterised in that：The step（1）In, lead plaster needs
The dry 12h at 105 DEG C crosses 140 mesh standard sieves after being fully ground, extracting screen underflow detects sulfur content, and detecting instrument is that high frequency is red
Outer carbon and sulfur analytical instrument.
3. the method for waste diachylon circulation desulfurization according to claim 1, it is characterised in that：The step（3）In, it is primary to filter
Liquid detects the concentration of sulfate in filtrate, and once desulfurization lead plaster detects sulfur content.
4. the method for waste diachylon circulation desulfurization according to claim 1, it is characterised in that：The step（6）In secondary filter
Liquid detects the concentration of sulfate in filtrate, and secondary desulfuration lead plaster detects sulfur content.
5. the method for waste diachylon circulation desulfurization according to claim 1, it is characterised in that：The step（2）In water be
Pure water, first-time filtrate or one kind in secondary filtrate or combination.
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Cited By (5)
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| CN112176179A (en) * | 2020-09-11 | 2021-01-05 | 安徽华铂再生资源科技有限公司 | Carbonating lead plaster smelting process |
| CN113897489A (en) * | 2021-10-08 | 2022-01-07 | 太和县大华能源科技有限公司 | Sectional type desulfurization process for waste lead plaster for recycling lead-acid batteries |
| CN113912024A (en) * | 2021-10-22 | 2022-01-11 | 昆明理工大学 | Method for removing impurity sulfur from selenium-sulfur slag |
| CN114249478A (en) * | 2021-11-26 | 2022-03-29 | 湖北楚凯冶金有限公司 | Method for treating waste acid water by combining ammonium method desulfurization |
| CN114317947A (en) * | 2021-12-14 | 2022-04-12 | 北京工业大学 | Method and device for two-stage mechanical reinforced desulfurization of waste lead paste |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112176179A (en) * | 2020-09-11 | 2021-01-05 | 安徽华铂再生资源科技有限公司 | Carbonating lead plaster smelting process |
| CN113897489A (en) * | 2021-10-08 | 2022-01-07 | 太和县大华能源科技有限公司 | Sectional type desulfurization process for waste lead plaster for recycling lead-acid batteries |
| CN113912024A (en) * | 2021-10-22 | 2022-01-11 | 昆明理工大学 | Method for removing impurity sulfur from selenium-sulfur slag |
| CN113912024B (en) * | 2021-10-22 | 2024-03-22 | 昆明理工大学 | Method for removing impurity sulfur from selenium-sulfur slag |
| CN114249478A (en) * | 2021-11-26 | 2022-03-29 | 湖北楚凯冶金有限公司 | Method for treating waste acid water by combining ammonium method desulfurization |
| CN114317947A (en) * | 2021-12-14 | 2022-04-12 | 北京工业大学 | Method and device for two-stage mechanical reinforced desulfurization of waste lead paste |
| CN114317947B (en) * | 2021-12-14 | 2023-12-29 | 北京工业大学 | Method and device for mechanically strengthening desulfurization of waste lead plaster in two sections |
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Application publication date: 20181106 |