CN108441647A - A kind of method that pyrogenic process recycles noble metal platinum in automobile dead catalyst - Google Patents
A kind of method that pyrogenic process recycles noble metal platinum in automobile dead catalyst Download PDFInfo
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- CN108441647A CN108441647A CN201810185054.8A CN201810185054A CN108441647A CN 108441647 A CN108441647 A CN 108441647A CN 201810185054 A CN201810185054 A CN 201810185054A CN 108441647 A CN108441647 A CN 108441647A
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- dead catalyst
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- platinum
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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
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
- C22B11/021—Recovery of noble metals from waste materials
- C22B11/026—Recovery of noble metals from waste materials from spent catalysts
- C22B11/028—Recovery of noble metals from waste materials from spent catalysts using solid sorbents, e.g. getters or catchment gauzes
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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
- C22B7/001—Dry processes
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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 kind of methods that pyrogenic process recycles noble metal platinum in automobile dead catalyst, including：（1）Automobile dead catalyst is pre-processed, is then sealed dead catalyst spare；（2）It will be through step（1）Obtained automobile dead catalyst is mixed in a certain ratio uniformly with carbonaceous reducing agent, trapping agent and slag forming material and block-like mixture is made；（3）It will be through step（2）Obtained mixture is broken into pieces, is placed in direct current electric arc furnace and is carried out high melt, obtains molten liquid；（4）It will be through step（3）The upper layer slag liquid of obtained molten liquid is poured out, and is made glassy state or tiny bead, and the alloy of lower layer's platinum containing noble metal natural cooling at room temperature.This method is applicable not only to high-grade material and can also be directed to carry out recycling noble metal platinum compared with low-grade material, simple for process, the period is short.
Description
Technical field
The invention belongs to metallurgical technology fields, and in particular to a kind of pyrogenic process recycles the side of noble metal platinum in automobile dead catalyst
Method.
Background technology
Noble metal platinum is widely used in agricultural, oil industry, military project, new and high technology due to its good physical-chemical property
Etc. industries.In particular with fast development scientific and technological in recent years, noble metal platinum increases severely in the demand of every profession and trade with day.In existing rank
Section, the main source of noble metal platinum have two kinds of approach of mineral resources and secondary resource.And the mineral resources of noble metal platinum extremely have
Limit, platinum grade is low in raw ore and mostly mineral intergrowth in addition, causes to extract noble metal platinum with mineral resources to meet the development of society
Demand has showed situation hard to carry on.For that purpose it is necessary to which the secondary resource to platinum carries out effective recycling, with slow
Solving noble metal platinum, supply falls short of demand and the poor present situation of mineral resources.All the time, noble metal platinum is widely used in automobile catalysis
In agent.In recent years since, due to the fast development of China's economy, the total vehicle in China rises year by year, for automobile catalyst
Noble metal platinum demand is also substantially increased.With the failure of automobile catalyst and " poisoning " and and automobile scrap, annual generation
A large amount of automobile dead catalyst；In addition, automobile dead catalyst has been cited as danger wastes, it is necessary to and being pocessed could abandon,
Achieve the purpose that environmental protection with this.So recycling the noble metal platinum in these automobile dead catalyst, noble metal platinum is realized again
It utilizes, is not only of great significance to the difficult present situation for alleviating noble metal platinum supply and demand, but also also have actively for the protection of environment
Meaning.
At this stage, mainly there are two methods of wet method and pyrogenic process to the recycling of noble metal platinum in automobile dead catalyst.Due to wet
Method is very high to the grade requirement of noble metal platinum in raw material, and to different carrier technique also difference, and wet processing has stream
Noble metal platinum content is high in journey length, residue, generates the shortcomings of waste water and dregs are more, since society gets on the car the day of dead catalyst quantity
Benefit increases, noble metal platinum grade is low and national to requirements such as the raisings of environmental requirement in automobile dead catalyst, and hydrometallurgic recovery is
The technological requirement that existing automobile waste catalyst recovery cannot be met needs to seek a kind of more effective, environmental protection recovery method and compels
In the eyebrows and eyelashes.Pyrogenic process with trapping agent in fusion process by going trapping noble metal platinum to be settled down to bottom, and base metal in raw material
Platinum floats on top with slag former slag making, to realize that slag gold detaches, achievees the purpose that extract noble metal platinum.Pyrogenic process has to raw material
Middle noble metal platinum grade requirement is not high, recyclable low-grade raw material, to the dead catalyst of different carriers only need suitably increase or
It reduces slag former type or quantity, generate the advantages that waste water and dregs are few, from the technique for recycling noble metal platinum in dead catalyst,
It is a kind of very promising method.
The method one of which that pyrogenic process recycles noble metal platinum is exactly metal traps method, the trapping metal master used in the method
Have tetra- kinds of metals of Fe, Cu, Pb, Ni, Pb due to its it is volatile and it is toxic do not used now, Ni is since itself value is high
Expensive and scarcity of resources also and non-optimal trapping metal.The metal of metal method of trapping is mostly based on Fe and Cu at this stage.
It is by the method main problem of trapping agent of Cu：The melting later stage obtains gold in turn to the reprocessing of Pt-Cu alloys
The process of category platinum generally has two methods of oxidation blowing and electrolytic anode copper to obtain metal platinum, but both methods has increasing
The cost of extraction metal platinum increases entire extracting cycle and the shortcomings of waste residue and the waste liquid subsequently generated be disposable.
For Cu, Fe is presently the most main trapping metal, and Fe also has Cu as all of trapping metal
More advantages；And for Cu, Fe has the further advantages such as wide, at low cost, the follow-up alloy in source is disposable.But it is existing at present with
Fe, which is trapping agent, mainly following deficiency：(1) existing method mostly uses greatly metallic iron as trapping agent, and metallic iron density is larger,
And the platinum in dead catalyst is mostly compound containing platinum, and compound containing platinum needs to be reduced into metal platinum just by reducing agent
Alloy can be formed with trapping agent, in existing method preparation process, since the density of iron is larger, when the compound of platinum is also not converted into
When metal platinum, has part or even major part Fe is sink to melt bottom, so as to cause the waste of trapping agent Fe and to dead catalyst
The trapping of middle platinum is insufficient；(2) existing using Fe as in the method for trapping agent, the smelting equipment of use is mostly resistance furnace, induction
Stove etc., it is longer that resistance furnace, induction furnace reach smelting temperature (1600 DEG C~2000 DEG C) used time, when being melted so as to cause mixed material
Between it is longer, cause the requirement that cannot reach slag gold quick separating in the melting viscosity short time so that slag gold disengaging time is longer, with
To the cycle stretch-out of entire extraction metal platinum, the cost of extraction process is increased；(3) existing using Fe as the method for trapping agent, production
Raw waste residue cannot be discarded directly, it is necessary to can be discarded after doing further processing, increase process costs, extend extraction week
Phase.
Invention content
For insufficient existing for above-mentioned prior art, noble metal in a kind of pyrogenic process recycling automobile dead catalyst of present invention offer
The method of platinum.
The present invention is achieved by the following technical solutions.
The method of noble metal platinum in a kind of pyrogenic process recycling automobile dead catalyst, which is characterized in that the method step includes：
(1) automobile dead catalyst is pre-processed, is then sealed automobile dead catalyst spare；
It (2) will be through the automobile dead catalyst that step (1) obtains and carbonaceous reducing agent, oxides-containing iron trapping agent and slag making object
Material is mixed in a certain ratio uniformly and block-like mixture is made；
(3) mixture obtained through step (2) is broken into pieces, is placed in direct current electric arc furnace and carries out high melt, is melted
Liquid；
(4) the upper layer slag liquid of the molten liquid obtained through step (3) is poured out, the alloy of lower layer's platinum containing noble metal is at room temperature
Natural cooling.
According to above-mentioned method, which is characterized in that the step (1) pre-processes automobile dead catalyst, is to pass through
Automobile dead catalyst is placed in air dry oven, processing is dried, drying temperature is 150 DEG C, and drying time is more than or equal to
14h。
According to above-mentioned method, which is characterized in that automobile dead catalyst, carbonaceous reducing agent, iron content oxidation in the step (2)
Object trapping agent, slag forming material in mass ratio 100：1~5：2~5.5：36~50 are mixed.
According to above-mentioned method, which is characterized in that carbonaceous reducing agent is smelter coke or coal dust in the step (2).
According to above-mentioned method, which is characterized in that slag forming material is CaO, Al in the step (2)2O3、MgO、SiO2In
One or more.
According to above-mentioned method, which is characterized in that oxides-containing iron trapping agent is Fe in the step (2)3O4。
According to above-mentioned method, which is characterized in that CaO, Al is added when simultaneously in the step (2)2O3、MgO、SiO2With
Fe3O4When, Fe3O4Reduction obtains FeO under carbonaceous reducing agent, wherein a small amount of FeO and CaO, Al2O3、MgO、SiO2Form SiO2-
CaO-Al2O3Five yuan of slag systems of-MgO-FeO, the SiO2、CaO、Al2O3, the quality of MgO and FeO respectively in five yuan of slag systems accounts for
Than for：SiO2It is 21% -30%, Al for 48% -55%, CaO2O3For 10%-20%, MgO be 0% -5%, FeO is
1% -6%.
According to above-mentioned method, which is characterized in that the mixture broken into pieces is placed in the stone of direct current electric arc furnace by the step (3)
High melt is carried out in black crucible, 1600 DEG C -2000 DEG C of smelting temperature after material melts completely, is kept molten by 2h.
According to above-mentioned method, which is characterized in that natural cooling forms glass to step (4) upper layer slag liquid at normal temperatures
State forms bead by water quenching.
The advantageous effects of the present invention, (1) this method are directed to the grade of the recycling of noble metal platinum in automobile dead catalyst
Range is wider with respect to hydrometallurgic recovery, and the low-grade ore that wet method cannot leach can also be carried out in smelt stage by trapping metal
Trapping, for main platiniferous and few palladium, rhodium using cordierite as the automobile dead catalyst of carrier in noble metal platinum return
It receives better；(2) utilize oxides-containing iron trapping agent as noble metal platinum trapping agent, by by oxides-containing iron trapping agent by
Step is reduced into simple substance Fe, and the trapping metal Fe for keeping density high has enough time trapping noble metal platinum in infall process, makes
Noble metal platinum in dead catalyst is captured more complete, is trapped to noble metal platinum when avoiding using fe as trapping agent
Insufficient problem；(3) instantaneous high-temperature (1600 DEG C -2000 DEG C) improved by direct current electric arc furnace allows material when extremely short
Interior fusing, material viscosity are reduced to 1PaS in a short time hereinafter, slag liquid and alloy is made faster, preferably to detach, are protecting
Smelting time is shortened under the premise of card noble metal platinum high-recovery, reduces smelting cost；(4) make full use of the composition of raw material special
Point, it is this kind of by SiO by the way that additional slag making materials and the Related Component slag making in dead catalyst are added2、Al2O3、MgO、CaO、FeO
The slag density of composition is smaller, is detached with the very big slag gold easy to implement of the density variation of alloy, by slag liquid system after the completion of melting
Tiny glass marble is made at glassy state or by carrying out water quenching to slag liquid, this processing method of slag liquid is environmentally friendly, reduces
Subsequent processing cost, it is easy to accomplish industrialization；(5) pass through the alloy impurity content of the noble metal platinum-iron obtained after melting
Few, subsequent processing is easy, by that can make water purification agent to base-metal solution of the noble metal platinum-ferroalloy acid after molten or trapping agent is made
Other use such as recycle；(6) the method is under the premise of ensureing the rate of recovery to noble metal platinum Pt 99% or more, significantly
Ground, which shortens, to be smelted the short time, reduces smelting cost.The method compared to wet method and other pyrogenic processes have the process time it is short, at
Sheet is low, environmental-friendly, is easily industrialized the advantages of big production.
Description of the drawings
The process flow diagram of Fig. 1 present invention.
Specific implementation mode
Further more detailed description is done to the present invention below in conjunction with experiment attached drawing and specific embodiment.
After multiple experiment, the experimental result of selected part of the present invention is used as with reference to example so that the present invention will be further described
And verification.
A kind of method that pyrogenic process recycles noble metal platinum in automobile dead catalyst, step include：
(1) automobile dead catalyst is pre-processed, to remove moisture content and the partial organic matter in automobile dead catalyst,
Automobile dead catalyst is sealed again spare, pretreatment is done by the way that automobile dead catalyst to be placed in air dry oven
Dry processing, drying temperature are 150 DEG C, and drying time is more than or equal to 14h；
It (2) will be through the automobile dead catalyst that step (1) obtains and carbonaceous reducing agent, oxides-containing iron trapping agent and slag making object
Material in mass ratio 100：1~5：2~5.5：36~50 are uniformly mixed and block-like mixture are made；Wherein carbonaceous reducing agent is metallurgy
Coke or coal dust；The preferred Fe of oxides-containing iron trapping agent3O4, Fe3O4Mostly as the trapping agent of noble metal platinum, wherein on a small quantity
Fe3O4It can also be used for slag making；Slag forming material is CaO, Al2O3、MgO、SiO2One or more of；When simultaneously be added CaO,
Al2O3、MgO、SiO2And Fe3O4When, Fe3O4Reduction obtains FeO under carbonaceous reducing agent, wherein a small amount of FeO and CaO, Al2O3、
MgO、SiO2Form SiO2-CaO-Al2O3Five yuan of slag systems of-MgO-FeO, SiO2、CaO、Al2O3, MgO and FeO be respectively at this five yuan
Quality accounting in slag system is：SiO2It is 21% -30%, Al for 48% -55%, CaO2O3It is for 10%-20%, MgO
0% -5%, FeO is 1% -6%；
(3) mixture obtained through step (2) is broken into pieces, granularity has no too big requirement, only nature is needed to break into pieces, will strike
Mixture after broken is placed in the black-fead crucible of direct current electric arc furnace (model Samsung/GT250, power 200KVA -500KVA) and carries out
High melt, obtains molten liquid, and 1600 DEG C -2000 DEG C of smelting temperature after material melts completely, is kept molten by 2h；It is molten
1600 DEG C -2000 DEG C of temperature of refining is reached by direct current electric arc furnace by moment, so that slag system has lower fusion temperature and suitable
Viscosity is conducive to shorten the heat and faster slag gold separating rate；Pass through high temperature slagging process, trapping agent Fe3O4Also by carbon
Former agent is gradually reduced into fe, and then the alloy for trapping noble metal platinum formation noble metal platinum-iron is sink to graphite crucible bottom, and
In raw material base metal platinum ingredient by with additional slag forming material slag making, since the density variation with alloy floats on the upper of melt
Portion, to realize the extraction of the noble metal platinum from automobile dead catalyst by the separation of molten condition slag gold；
(4) the upper layer slag liquid of the molten liquid obtained through step (3) is poured onto in pre-prepd graphite crucible, lower layer contains
The alloy of noble metal platinum natural cooling at room temperature；Natural cooling forms glassy state or passes through water quenching shape upper layer slag liquid at normal temperatures
At tiny bead.
Embodiment 1
Refering to attached drawing 1, first spent auto catalysts are pre-processed, then weigh the pretreated automobile dead catalyst of 10kg
(wherein SiO260%, Al2O312%, Pt700g/t) and the slag former 4.31kg by being dried (wherein CaO 3.1kg,
Al2O30.81kg, MgO 0.4kg) and Fe3O4The smelter coke of 0.35kg and 0.2kg (wherein fixed carbon content is 80%)
It is uniformly mixed, and clamp dog, in being then added to direct current electric arc furnace after physics is broken, in 1600 DEG C of height in direct current electric arc furnace
The lower melting 2h of temperature.By slagging process slag due to the smaller automatic upper layer for floating on melt of density, the alloy of platiniferous is then because larger
Density be sink to the bottom of melt, be slag liquid to which entire melt is divided into two parts i.e. upper layer, lower layer is containing platinum alloy.Wait for melting
After the completion, the part of the upper layer slag liquid in graphite crucible is poured onto in pre-prepd graphite crucible, remaining melt is gradually
It is cooled to room temperature so that slag liquid is cooled and solidified and then detached with alloy molten solution, and what can finally be enriched with contains platinum alloy and slag.
Then platinum content in the slag liquid and alloy toppled over is detected respectively, obtains in slag platinum containing amount in 5~15g/t, automobile waste
The rate of recovery of platinum is more than 99% in catalyst.
Embodiment 2
Refering to attached drawing 1, processing first is dried to spent auto catalysts, drying temperature is 150 DEG C, drying time 14h, then
Weigh dead catalyst (wherein SiOs of the 5kg through drying process260%, Al2O312%, Pt700g/t) and by drying process
Slag former 2.22kg (wherein CaO 1.61kg, Al2O30.41kg, MgO 0.2kg) and Fe3O40.18kg's and 0.15kg
Smelter coke (wherein fixed carbon content is 80%) is uniformly mixed, and clamp dog, is then added to direct current after physics is broken
In arc stove, in direct current electric arc furnace under 2000 DEG C of high temperature melting 2h.By slagging process slag due to the smaller automatic floating of density
In the upper layer of melt, the alloy of platiniferous is then because larger density is sink to the bottom of melt, to which entire melt is divided into two parts i.e.
Upper layer is slag liquid, and lower layer is containing platinum alloy.After the completion of waiting for melting, the part of the upper layer slag liquid in graphite crucible is poured onto in advance
In the graphite crucible of preparation, remaining melt is gradually cooled to room temperature so that and slag liquid is cooled and solidified and then is detached with alloy molten solution,
What can finally be enriched with contains platinum alloy and slag.Then platinum content in the slag liquid and alloy toppled over is detected respectively,
The rate of recovery for obtaining platinum containing amount platinum in 5~15g/t, automobile dead catalyst in slag is more than 99%.
Embodiment 3
Refering to attached drawing 1, processing first is dried to spent auto catalysts, drying temperature is 150 DEG C, drying time 16h, then
Weigh dead catalyst (wherein SiOs of the 7kg through drying process260%, Al2O312%, Pt700g/t) and by drying process
Slag former 3.05kg (wherein CaO 2.2kg, Al2O30.57kg, MgO 0.28kg) and Fe3O40.25kg's and 0.18kg
Smelter coke (wherein fixed carbon content is 80%) is uniformly mixed, and clamp dog, is then added to direct current after physics is broken
In arc stove, in direct current electric arc furnace under 1800 DEG C of high temperature melting 2h.By slagging process slag due to the smaller automatic floating of density
In the upper layer of melt, the alloy of platiniferous is then because larger density is sink to the bottom of melt, to which entire melt is divided into two parts i.e.
Upper layer is slag liquid, and lower layer is containing platinum alloy.After the completion of waiting for melting, the part of the upper layer slag liquid in graphite crucible is poured onto in advance
In the graphite crucible of preparation, remaining melt is gradually cooled to room temperature so that and slag liquid is cooled and solidified and then is detached with alloy molten solution,
What can finally be enriched with contains platinum alloy and slag.Then platinum content in the slag liquid and alloy toppled over is detected respectively,
The rate of recovery for obtaining platinum containing amount platinum in 5~15g/t, automobile dead catalyst in slag is more than 99%.
Above-described is only presently preferred embodiments of the present invention, not limitation invention.It should be understood that for the general of this field
For logical technical staff, under technical inspiration provided by the present invention, other equivalent improvement can also be made, this may be implemented
The purpose of invention, is regarded as protection scope of the present invention.
Claims (9)
1. the method for noble metal platinum in a kind of pyrogenic process recycling automobile dead catalyst, which is characterized in that the method step includes：
（1）Automobile dead catalyst is pre-processed, is then sealed automobile dead catalyst spare；
（2）It will be through step（1）Obtained automobile dead catalyst and carbonaceous reducing agent, oxides-containing iron trapping agent and slag forming material by
Certain proportion is uniformly mixed and block-like mixture is made；
（3）It will be through step（2）Obtained mixture is broken into pieces, is placed in direct current electric arc furnace and is carried out high melt, obtains molten liquid；
（4）It will be through step（3）The upper layer slag liquid of obtained molten liquid is poured out, and the alloy of lower layer's platinum containing noble metal is natural at room temperature
It is cooling.
2. according to the method described in claim 1, it is characterized in that, the step（1）Automobile dead catalyst is pre-processed,
It is that processing is dried by the way that automobile dead catalyst to be placed in air dry oven, drying temperature is 150 DEG C, and drying time is more than
Equal to 14h.
3. according to the method described in claim 1, it is characterized in that, the step（2）Middle automobile dead catalyst, carbonaceous reducing agent,
Oxides-containing iron trapping agent, slag forming material in mass ratio 100：1~5：2~5.5：36~50 are mixed.
4. according to the method described in claim 1, it is characterized in that, the step（2）Middle carbonaceous reducing agent is smelter coke or coal
Powder.
5. according to the method described in claim 1, it is characterized in that, the step（2）Middle slag forming material is CaO, Al2O3、MgO、
SiO2One or more of.
6. according to the method described in claim 1, it is characterized in that, the step（2）Middle oxides-containing iron trapping agent is Fe3O4。
7. according to the method described in claim 6, it is characterized in that, the step（2）CaO, Al is added when simultaneously2O3、MgO、
SiO2And Fe3O4When, Fe3O4Reduction obtains FeO under carbonaceous reducing agent, wherein a small amount of FeO and CaO, Al2O3、MgO、SiO2It is formed
SiO2-CaO-Al2O3Five yuan of slag systems of-MgO-FeO, the SiO2、CaO、Al2O3, MgO and FeO be respectively in five yuan of slag systems
Quality accounting is：SiO2It is 21% -30%, Al for 48% -55%, CaO2O3It is 0% -5% for 10%-20%, MgO, FeO is 1% -
6%。
8. according to the method described in claim 1, it is characterized in that, the step（3）The mixture broken into pieces is placed in direct current
High melt is carried out in the graphite crucible of arc stove, 1600 DEG C -2000 DEG C of smelting temperature keeps melting after material melts completely
State 2h.
9. according to the method described in claim 1, it is characterized in that, the step（4）Upper layer slag liquid natural cooling at normal temperatures
It forms glassy state or bead is formed by water quenching.
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| CN115323188A (en) * | 2022-07-27 | 2022-11-11 | 中南大学 | Method for trapping platinum group metal in spent catalyst by copper |
| CN116043028A (en) * | 2022-12-29 | 2023-05-02 | 东北大学 | Method for recycling platinum group metals in automobile waste catalyst by taking ferronickel tailings as flux |
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