CN107254588A - A kind of method that antimony is efficiently removed from high antimony lead - Google Patents
A kind of method that antimony is efficiently removed from high antimony lead Download PDFInfo
- Publication number
- CN107254588A CN107254588A CN201710472940.4A CN201710472940A CN107254588A CN 107254588 A CN107254588 A CN 107254588A CN 201710472940 A CN201710472940 A CN 201710472940A CN 107254588 A CN107254588 A CN 107254588A
- Authority
- CN
- China
- Prior art keywords
- antimony
- lead
- oxide
- efficiently removed
- added
- 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
- C22B13/06—Refining
-
- 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
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of method that antimony is efficiently removed from high antimony lead, this method is that under the conditions of vacuum tightness, lead oxide is added in corundum crucible bottom, and high antimony lead is added on lead oxide, makes Sb at 840 DEG C of temperature 700 DEG C by replacing reaction generation Sb2O3, so as to reach the purpose except antimony.This method under vacuum, the Sb of generation2O3Antimony in highly volatile, high antimony lead is with Sb2O3Form volatilization and on condenser pipe collect, avoid the influence of Pb Sb systems " minus deviation ", reach well remove antimony purpose.The present invention only need a step processing can directly output meet country two grades of lead bullions standard amount containing antimony, the industries such as battery, cable cover(ing), machinery manufacturing industry, shipbuilding, light industry, radiation protection can be used for.Whole technical process is simple, environment-friendly, and the loss of lead is seldom, with considerable industrial application value.
Description
Technical field
The present invention relates to a kind of non-ferrous metal pyrometallurgical smelting method, the separation and purification of lead sb system are particularly suitable for use in.
Background technology
In order to meet the yield of reviver in environment-friendly and plumbing sustainable development requirement, global range, to have accounted for lead total
More than half of yield.With the development of auto industry, lead is also growing in the demand of lead accumulator, while also resulting in big
Scrap lead is measured to produce.These scrap lead are sent to lead smeltery and smelted in reverberatory furnace, produce the different lead of amount containing antimony, it is necessary to further remove
It is miscellaneous directly to apply.Therefore, the antimony removed in lead bullion is significant for the sustainable use of lead resource.However, pin
For high antimony lead except antimony technique is but rarely reported, generally handled by the relatively low refining of lead bullion technique of amount containing antimony.At present, the world
The upper refining of lead bullion uses pyro-refining and electrorefining, and pyro-refining accounts for 70% always refined, only Chinese, Canadian, secret
The technique that Shandong and some smelteries of Japan use electrorefining.
Pyro-refining includes two methods of refinement oxide and basic refining.Although refinement oxide equipment is simple, exist
Lead loss is big, working condition is poor, high energy consumption, the high shortcoming of residual antimony after refining, therefore seldom smeltery can be used now.Basic refining
The loss very little of lead, required temperature is also lower than refinement oxide, and the reaction time is shorter, but weak point be equipment investment compared with
Greatly, the basic slag final treatment techniques for consuming a large amount of alkaline reagents and generation are complicated.In electrorefining, it is desirable to which chloride plate antimony contains
Amount is general in 0.4%-0.7%.When antimony content is higher than 1.2% in positive plate, antimony firmly sticks to setting sun in refining process
On pole plate, the earth of positive pole of generation is difficult to do the wash removal, it is necessary to by machinery or artificial removal.Therefore, before electrorefining, if
Antimony content is too high, it is necessary to reduces antimony content by preliminary fire refining, causes whole refining process flow longer, production cost
It is higher.In addition, also needing to that fluosilicic acid solution is regularly replaced or added into electrolyte in electrolytic process, cause substantial amounts of useless
Liquid is produced, and the production cycle is long, about more than 5 days so that refinery practice energy consumption is big.Present in current refining of lead bullion technique
Antimony content is high in problem, and regeneration leady raw materialses, the characteristics of scope is wide, researchs and develops cleaning close friend, and technique is simple, except antimony effect
Really good, the antimony technique of removing of the high antimony lead raw material of vertical high income is very significant.
The content of the invention
It is an object of the invention to provide a kind of method that antimony is efficiently removed from high antimony lead, labor in pyro-refining can solve the problem that
Dynamic condition is poor, residual antimony is higher after refining, lead loss very big, basic slag is difficult and electrorefining in complex process, cost height,
The problems such as waste liquid is produced.It can be completely separated effectively lead antimony simultaneously, output complies fully with national standard GB 469-83 except antimony lead
The standard amount containing antimony of 2# lead bullions.
The technical solution adopted in the present invention comprises the following steps：
1) load weighted lead oxide is placed in corundum pot bottom.
2) load weighted high antimony lead raw material is added on lead oxide.
3) by described the 2) step corundum pot be placed in reactor, vacuum is 30-2500Pa, and temperature is at 700-840 DEG C
Reaction.
4) after reaction terminates, after temperature drops to room temperature, condensate is collected from condenser.
Wherein, amount containing antimony 2.5% in the high antimony lead.
The reaction time 3) in step was 40-80min.
Reaction 3) occurred in step is as follows：
The essence of the present invention is exactly to remove antimony by above-mentioned vacuum displacement reaction, and specific advantage is：It is direct through this method
What is obtained removes the standard amount containing antimony that antimony lead can reach national 2# lead bullions, and removal efficiency is up to 99.9%.The whole process of the present invention is adopted
With vacuum displacement Reaction Separation lead antimony, the lead sb system of heterogeneity amount containing antimony can be handled, lead loss is small, production process is without harmful
Material is discharged, and environmental protection and energy saving are simple to operate, and the process time is short, better economic benefit, it is adaptable to industrial applications.
Specific embodiment
Following examples are intended to illustrate invention rather than limitation of the invention further.
Embodiment 1
The high antimony leads of 12g (mass percent of metallic antimony is about 2.5%) and 4g lead oxide is taken to be placed in experimental provision, in temperature
60min is reacted under the conditions of 840 DEG C of degree, pressure 30Pa, is measured except the 23ppm of amount containing antimony in antimony lead, except antimony rate is 99.91%.
Embodiment 2
Reaction time in embodiment 1 is set as outside 80min that remaining is constant, measured except the 22ppm of amount containing antimony in antimony lead,
Except antimony rate is 99.91%.From the perspective of energy is saved, the reaction time is unsuitable long.
Embodiment 3
Reaction time in embodiment 1 is set as 40min, remaining is constant, measures except the 53ppm of amount containing antimony in antimony lead, remove
Antimony rate is 99.79%.
From embodiment 1,2 and 3 as can be seen that the reaction time is suitably set as 60min.
Embodiment 4
The high antimony leads of 12g (mass percent of metallic antimony is about 2.5%) and 4g lead oxide is taken to be placed in experimental provision, in temperature
60min is reacted under the conditions of 750 DEG C of degree, pressure 30Pa, is measured except the 55ppm of amount containing antimony in antimony lead, except antimony rate is 99.78%.
Comparative example 1
The high antimony leads of 12g (mass percent of metallic antimony is about 2.5%) and 0g lead oxide is taken to be placed in experimental provision, in temperature
60min is reacted under the conditions of 750 DEG C of degree, pressure 30Pa, is measured except amount containing antimony 2.5% in antimony lead, it is seen then that during without lead oxide,
Even if vacuum, antimony also removes not fall.
Comparative example 2
The high antimony leads of 12g (mass percent of metallic antimony is about 2.5%) and 4g lead oxide is taken to be placed in experimental provision, in temperature
60min is reacted under 750 DEG C of degree, condition of normal pressure, is measured except the 234ppm of amount containing antimony in antimony lead, it is seen then that vacuum condition is to except antimony effect
It is critically important.
Claims (4)
1. a kind of method that antimony is efficiently removed from high antimony lead, it is characterised in that it is 2.5% high antimony lead raw material and oxidation that will contain antimony amount
Lead is placed in corundum pot, under vacuum, is reacted by displacement, obtains removing antimony lead.
2. according to the method described in claim 1, it is characterised in that：The lead oxide is placed in corundum pot bottom, high antimony lead raw material
It is put into corundum pot and is added in above lead oxide.
3. according to the method described in claim 1, it is characterised in that：The reaction time 40-80min, temperature is 700-840
DEG C, it is 30-2500Pa to control vacuum.
4. according to the method described in claim 1, it is characterised in that：After the reaction terminates, the complete lead oxide of unreacted is floated
It is recyclable to be continuing with except the surface of antimony lead；Condensate is collected from condenser, can be used as producing the quality raw materials of stibium trioxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710472940.4A CN107254588A (en) | 2017-06-21 | 2017-06-21 | A kind of method that antimony is efficiently removed from high antimony lead |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710472940.4A CN107254588A (en) | 2017-06-21 | 2017-06-21 | A kind of method that antimony is efficiently removed from high antimony lead |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107254588A true CN107254588A (en) | 2017-10-17 |
Family
ID=60024152
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710472940.4A Pending CN107254588A (en) | 2017-06-21 | 2017-06-21 | A kind of method that antimony is efficiently removed from high antimony lead |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107254588A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108149031A (en) * | 2018-01-11 | 2018-06-12 | 中南大学 | A kind of new method of crude pb-sb alloy separation antimony |
| CN108539315A (en) * | 2018-05-30 | 2018-09-14 | 中南大学 | A kind of waste lead accumulator lead plaster recovery process |
| CN108707760A (en) * | 2018-05-30 | 2018-10-26 | 中南大学 | A kind of new method of lead-antimony raw alloy separation antimony |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1644719A (en) * | 2005-03-01 | 2005-07-27 | 张传银 | Method for fire refining lead |
| CN101886174A (en) * | 2010-06-23 | 2010-11-17 | 郴州雄风稀贵金属材料股份有限公司 | Process for refining high-purity bismuth from bismuth-containing material generated from anode mud recovery |
| US20120227544A1 (en) * | 2006-12-05 | 2012-09-13 | Stannum Group LLC | Process for refining lead bullion |
-
2017
- 2017-06-21 CN CN201710472940.4A patent/CN107254588A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1644719A (en) * | 2005-03-01 | 2005-07-27 | 张传银 | Method for fire refining lead |
| US20120227544A1 (en) * | 2006-12-05 | 2012-09-13 | Stannum Group LLC | Process for refining lead bullion |
| CN101886174A (en) * | 2010-06-23 | 2010-11-17 | 郴州雄风稀贵金属材料股份有限公司 | Process for refining high-purity bismuth from bismuth-containing material generated from anode mud recovery |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108149031A (en) * | 2018-01-11 | 2018-06-12 | 中南大学 | A kind of new method of crude pb-sb alloy separation antimony |
| CN108539315A (en) * | 2018-05-30 | 2018-09-14 | 中南大学 | A kind of waste lead accumulator lead plaster recovery process |
| CN108707760A (en) * | 2018-05-30 | 2018-10-26 | 中南大学 | A kind of new method of lead-antimony raw alloy separation antimony |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101660054B (en) | Method for extracting metal indium from waste residues generated from lead and zinc smelting | |
| CN103184338B (en) | Recovery method of copper indium gallium selenide thin-film solar panel | |
| CN102766765B (en) | Zinc oxide powder recycling method | |
| CN101012514A (en) | Method for producing metallic lead and zinc by using lead-zinc containing waste slag or lead-zinc monoxide mine | |
| CN101307385A (en) | Method for treating indium stannum smoke raw material | |
| CN102618884A (en) | Lead regeneration method for recovering lead paste from waste lead acid storage battery by wet method | |
| CN102634659B (en) | Process for recycling gallium from gallium and germanium contained concentrate | |
| CN102140580A (en) | Multi-metal recycling method of electric furnace tin-smelting dust | |
| CN107254588A (en) | A kind of method that antimony is efficiently removed from high antimony lead | |
| CN110016566A (en) | A method of recycling indium in discarded photovoltaic module | |
| CN103243349A (en) | Comprehensive zinc hydrometallurgy recovery system technique | |
| CN103290429A (en) | Method for electrolyzing high-content low-grade lead bullion | |
| CN101974765A (en) | Comprehensive method for separating stibium from materials containing stibium, tin and lead | |
| CN105274359A (en) | Method for extracting and separating valuable metals from secondary lead smelting slag | |
| CN102839391A (en) | Preparation method of high-purity indium | |
| CN104894387A (en) | Technological method for extracting antimony and bismuth from rare and noble metallurgical slag | |
| CN106400051A (en) | Method for achieving copper, nickel and tin separation through low-copper, high-nickel and high-tin anode electrolysis | |
| CN102002584A (en) | Method of recovering manganese, lead and silver from zinc electrolyzed anode mud by utilizing acid-making tail gas | |
| CN102912155A (en) | Recovery processing process of stanniferous electrofacing sludge | |
| CN102978411A (en) | Comprehensive recycling method for crude indium casting slag | |
| CN101333605A (en) | Technology for extracting indium from indium-rich bottom lead | |
| CN104947146A (en) | Method for electrolyzing and recycling valuable metal from high-bismuth lead bullion | |
| CN104087971B (en) | Method for treating lead matte | |
| CN106282588A (en) | Alkali regeneration method in reviver refine alkaline residue | |
| CN106086414B (en) | A method of recycling lead from waste lead acid battery lead cream |
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: 20171017 |
|
| WD01 | Invention patent application deemed withdrawn after publication |