CN108149031A - A kind of new method of crude pb-sb alloy separation antimony - Google Patents
A kind of new method of crude pb-sb alloy separation antimony Download PDFInfo
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- CN108149031A CN108149031A CN201810024596.7A CN201810024596A CN108149031A CN 108149031 A CN108149031 A CN 108149031A CN 201810024596 A CN201810024596 A CN 201810024596A CN 108149031 A CN108149031 A CN 108149031A
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- antimony
- alloy
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- new 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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/02—Obtaining antimony
-
- 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
-
- 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 kind of new methods of crude pb-sb alloy separation antimony, and this method is to use air as oxidant, and the concentration of oxygen is controlled by the vacuum degree of regulation system, and barium plumbate is carried out to the crude pb-sb alloy containing antimony 42% in a dynamic oxidation process.By controlling vacuum degree 14kPa, 660 DEG C~680 DEG C of vacuum reaction temperature, during 180~240min of vacuum reaction time, obtained steaming thing Sb2O3The content of middle PbO is less than 1%, can be used to produce stibium trioxide, steaming excess lead bullion, less than 1%, can produce lead bullion containing antimony by refining.Compared to existing crude pb-sb alloy atmospheric pressure oxidation method, which has that low energy consumption, and separation is thorough, simple for process, pollution-free.
Description
Technical field
The present invention relates to a kind of new methods of crude pb-sb alloy separation antimony, belong to vacuum technical field of non-ferrous metallurgy.
Background technology
Jamesonite (Pb4FeSb6S14) it is a kind of complicated sulfuration mine for being enriched with the important meals elements such as Pb, Sb and Ag
Object.It, all cannot be by its point using existing beneficiating method since lead and antimony are existed in the form of solid solution in jamesonite
From, it is therefore necessary to their separation is realized by metallurgical process.At present, traditional pyrometallurgy of jamesonite is handled
Journey is broadly divided into following steps：First jamesonite input boiling roaster desulfurization is obtained again through retailoring of blast furnace
It is about 45% lead-antimony alloy containing antimony, this alloy is called crude pb-sb alloy in enterprise.At present, it is thick to handle this lead antimony
Unique current technology of alloy is that this crude pb-sb alloy input reverberatory furnace is carried out oxidation blowing again, realizes point of lead and antimony
From.But this current technology falls behind very much：Blowing temperature is up to 950 DEG C or more, and the separating effect of lead and antimony is very poor；Anti-
It penetrates in the converting process of stove, due to being unevenly distributed for oxygen, leads to a part of metallic antimony far from oxygen lance because lacking oxygen
And cannot be fully oxidized, but the metallic antimony of oxygen lance is proximate to because oxygen is excessively excessively oxidated into the antimony pentoxide of high price；
The sb oxide of high price is since volatility is poor, it is difficult to be volatized into gas phase, the surface of alloy melt can only be floated in the form of slag,
Seriously hamper Sb2O3Volatilization and metallic antimony further oxidation, barium plumbate is caused to be not thorough.In addition, the process can also produce
The raw flue dust being largely harmful to human body and environment.
In order to improve the existing separating technology of lead-antimony alloy, Chinese researchers propose many new methods.For example,
Application No. is CN02139073.8, disclose a kind of method that lead antimony is detached from crude pb-sb alloy, it is based on Pb-Sb binary
Alloy phase diagram is a typical partial miscibility eutectic phasor.Infinitely dissolve during liquid, partial miscibility during solid-state, is melted by a step
Analysis by it is leaded be higher than 62% crude pb-sb alloy output be suitble to electrolysis require it is leaded be higher than 72% lead bullion.Wherein high temperature liquate
At 600~750 DEG C, the temperature of low temperature liquate is controlled at 350~440 DEG C for temperature control, but this method also can only be by antimony except extremely
15% or so and temperature be difficult to control.Application No. is CN88104919.0, disclose a kind of lead-antimony alloy centrifugation segregation separation
Method, this method are the centrifugate that is generated in centrifugal force field by alloy liquid under the collective effect in centrifugal force field and temperature field
Pressure, using the difference in specific gravity of lead and antimony, control temperature makes lead, antimony quickly be segregated separation at 450~500 DEG C.But when this method cools down
Between long, operation interruption, crystal grain and rich lead liquid ingredient fluctuation are big, are extremely difficult to theoretical composition.Also document《Lead-antimony alloy vacuum is steamed
Evaporate Separation Research》In propose and lead-antimony alloy detached, but this method is needed in vacuum using multistage continuous vacuum distillation
It is operated under high temperature, height is required to equipment and materials, cost is also high, and in addition lead antimony Binary Alloy System belongs to minus deviation system, only logical
It is that can not be achieved efficiently separating for lead-antimony alloy to cross vacuum distillation.Therefore, the lead antimony for studying a kind of efficient, low consumption and environmental protection is thick
Alloy separation method is of great significance.
Invention content
For existing crude pb-sb alloy separating technology, there are many deficiencies, and the present invention provides a kind of crude pb-sb alloy point
New method from antimony while realizing crude pb-sb alloy economy, being completely separated, simplifies the technological process of separation.This technology
Invention is realized using following scheme step：
1) a certain amount of crude pb-sb alloy is taken to be placed in vacuum resistance together with material in corundum material boat, then by corundum material boat
It is heated in stove, heating and temperature control is at 660~680 DEG C；
2) vacuum pump is opened, control system pressure is 14kP, and a certain amount of air, oxidation processes are continuously passed through to system
180~240min after reaction, closes vacuum systems.After material completely cooling, take out；
3) the steaming thing Sb obtained in this process2O3The raw material of production stibium trioxide is used as, and steaming excess lead bullion can lead to
It crosses various refining productions and obtains lead bullion.
The present invention's has the prominent advantages that：High-efficiency environment friendly by the antimony content in crude pb-sb alloy be reduced to 1% hereinafter,
Sb2O3It is less than 1% containing PbO.This technology invention process is simple, realizes being completely separated for crude pb-sb alloy at a lower temperature,
It is at low cost, realize that energy-saving and emission-reduction create necessary and sufficient conditions for the follow-up refining of lead bullion.In addition, since this method is in vacuum
It is operated under environment, the flue dust and waste residue being harmful to environment and human body will not be generated.
Specific embodiment
Embodiment 1
It takes 5g containing the crude pb-sb alloy that antimony is 42% in corundum material boat, then places it in vacuum resistance furnace and heat, control
It is 3L/min into system air capacity when vacuum degree processed is 14kPa, reaction temperature is 660 DEG C, reaction time 180min, reaction
After, obtain steaming thing Sb2O3Middle PbO contents are 0.051%, and the antimony content in steaming excess lead bullion is 6.88%.
Embodiment 2
It takes 5g containing the crude pb-sb alloy that antimony is 42% in corundum material boat, then places it in vacuum resistance furnace and heat, control
It is 3L/min into system air capacity when vacuum degree processed is 14kPa, reaction temperature is 680 DEG C, reaction time 180min, reaction
After, obtain steaming thing Sb2O3Middle PbO contents are 0.082%, and the antimony content in steaming excess lead bullion is 2.02%.
Embodiment 3
It takes 5g containing the crude pb-sb alloy that antimony is 42% in corundum material boat, then places it in vacuum resistance furnace and heat, control
It is 3L/min into system air capacity when vacuum degree processed is 14kPa, reaction temperature is 680 DEG C, reaction time 210min, reaction
After, obtain steaming thing Sb2O3Middle PbO contents are 0.12%, and the antimony content in steaming excess lead bullion is 0.30%.
Embodiment 4
It takes 5g containing the crude pb-sb alloy that antimony is 42% in corundum material boat, then places it in vacuum resistance furnace and heat, control
It is 3L/min into system air capacity when vacuum degree processed is 14kPa, reaction temperature is 680 DEG C, reaction time 240min, reaction
After, obtain steaming thing Sb2O3Middle PbO contents are 0.19%, and the antimony content in steaming excess lead bullion is 0.081%.
Claims (4)
1. a kind of new method of crude pb-sb alloy separation antimony, it is characterised in that using containing the crude pb-sb alloy that antimony is 42% as raw material,
At 660 DEG C~680 DEG C, the concentration of oxygen is controlled by the vacuum degree of regulation system, it is real by one step of dynamic oxidation process
Existing lead and antimony efficiently separate.It is as follows：
1) a certain amount of crude pb-sb alloy raw material is taken to be placed in corundum material boat, corundum material boat is then put into homemade resistance furnace
It is interior；
2) different vacuum degrees is controlled, a certain amount of air is continuously passed through to reaction system, is handled under selected temperature condition
For a period of time, after reaction, vacuum systems are closed, are taken out after product cooling, you can obtain steaming thing Sb2O3And steaming excess
Lead bullion.
2. a kind of new method of crude pb-sb alloy separation antimony according to claim 1, lead antimony of the characterization method in 1)
Antimony content is 42% in thick alloy.
A kind of 3. new method of crude pb-sb alloy separation antimony according to claim 1, it is characterised in that the 2) reactant in
System will continuously be passed through a certain amount of air, and for vacuum degree control in 14kPa, temperature is 660~680 DEG C, the time for 180~
240min。
4. the new method of a kind of crude pb-sb alloy separation antimony according to claim 1, which is characterized in that by dynamic oxidation
Separation, the removal rate of antimony have reached more than 99%, and steaming thing Sb2O3The content of middle PbO is also below 1%.
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| CN201810024596.7A CN108149031A (en) | 2018-01-11 | 2018-01-11 | A kind of new method of crude pb-sb alloy separation antimony |
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| CN201810024596.7A CN108149031A (en) | 2018-01-11 | 2018-01-11 | A kind of new method of crude pb-sb alloy separation antimony |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87104574A (en) * | 1987-06-27 | 1988-03-30 | 昆明工学院 | New technique of fire refining method for bullion lead |
| CN101525694A (en) * | 2009-04-17 | 2009-09-09 | 深圳市中金岭南有色金属股份有限公司韶关冶炼厂 | Separation process for material containing lead, antimony, copper, bismuth and silver |
| CN104141152A (en) * | 2014-07-28 | 2014-11-12 | 蒙自矿冶有限责任公司 | Method for recycling tin from lead bullion |
| CN104451188A (en) * | 2014-11-18 | 2015-03-25 | 昆明理工大学 | Method for separating lead and antimony of jamesonite concentrate by virtue of vacuum treatment |
| CN106868314A (en) * | 2016-12-29 | 2017-06-20 | 中南大学 | The technique and device of a kind of lead bullion refinement oxide |
| CN107254588A (en) * | 2017-06-21 | 2017-10-17 | 中南大学 | A kind of method that antimony is efficiently removed from high antimony lead |
| CN107287441A (en) * | 2017-06-21 | 2017-10-24 | 中南大学 | A kind of method that bottom lead depth removes antimony |
-
2018
- 2018-01-11 CN CN201810024596.7A patent/CN108149031A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87104574A (en) * | 1987-06-27 | 1988-03-30 | 昆明工学院 | New technique of fire refining method for bullion lead |
| CN101525694A (en) * | 2009-04-17 | 2009-09-09 | 深圳市中金岭南有色金属股份有限公司韶关冶炼厂 | Separation process for material containing lead, antimony, copper, bismuth and silver |
| CN104141152A (en) * | 2014-07-28 | 2014-11-12 | 蒙自矿冶有限责任公司 | Method for recycling tin from lead bullion |
| CN104451188A (en) * | 2014-11-18 | 2015-03-25 | 昆明理工大学 | Method for separating lead and antimony of jamesonite concentrate by virtue of vacuum treatment |
| CN106868314A (en) * | 2016-12-29 | 2017-06-20 | 中南大学 | The technique and device of a kind of lead bullion refinement oxide |
| CN107254588A (en) * | 2017-06-21 | 2017-10-17 | 中南大学 | A kind of method that antimony is efficiently removed from high antimony lead |
| CN107287441A (en) * | 2017-06-21 | 2017-10-24 | 中南大学 | A kind of method that bottom lead depth removes antimony |
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