CN105039706B - The enrichment of nickel element and separation method in many metal mixed resources of waste printed circuit board - Google Patents
The enrichment of nickel element and separation method in many metal mixed resources of waste printed circuit board Download PDFInfo
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- CN105039706B CN105039706B CN201510402109.2A CN201510402109A CN105039706B CN 105039706 B CN105039706 B CN 105039706B CN 201510402109 A CN201510402109 A CN 201510402109A CN 105039706 B CN105039706 B CN 105039706B
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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
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Abstract
The invention belongs to complicated secondary nonferrous metal resource synthesis cycling and reutilization technology, the enrichment of nickel element and separation method in specially a kind of many metal mixed resources of waste printed circuit board.First, waste printed circuit board obtains the multi-metal complex mixture containing nickel element after broken+sorting, trapping agent is added in multi-metal complex mixture, the multi-metal complex mixture that will have been configured is placed in the graphite crucible of vacuum drying oven, after many metal mixtures are completely melt, by adding micro pregnant solution silicon or titanium elements, the separation rate of both regulation liquid copper and liquid iron, nickel element is set to be enriched in iron liquid phase, it is that liquid iron and lower floor are the separation melt of liquid copper to form upper strata, the upper strata liquid iron for trapping nickel element is poured out, nickel element is separated from waste printed circuit board multi-metal complex mixture, and it is able to cycling and reutilization.The present invention it is simple and easy, with low cost, comprehensive high-efficiency, it is pollution-free the features such as.
Description
Technical field
The invention belongs to complicated secondary nonferrous metal resource synthesis cycling and reutilization technology, specially a kind of waste printed circuit board
The enrichment of nickel element and separation method in many metal mixed resources, are related to carry out electron wastes in environmental protection technical field
Reclaim, regenerate and comprehensive high-efficiency resource technology, help and solve the problems, such as electron wastes to the harm of ecological environment and alleviate me
The pressure of state's non-ferrous metal shortage of resources.
Background technology
With the update constantly brought forth new ideas with electric equipment products of science and technology, a large amount of waste electric products have turned into
Growth rate most fast and most intractable class solid waste.Electron wastes are also known as electronic waste, including various waste and old electricity
Brain, communication equipment, household electrical appliance and the precision electronic device instrument that is eliminated etc..According to statistics, every thousand people is put down in the whole world in 2002
Computer owning amount is about 100, and has ever-increasing trend.The social recoverable amount of domestic television machine is more than 3.7 within 2010
Hundred million, computer, refrigerator and washing machine are respectively more than 80,000,000,1.5 hundred million and 1.9 hundred million.In general, refrigerator, wash
The average life of clothing machine in 8 to 10 years, television set average life in 4 to 6 years, as the faster computer that updates
With superseded cycle of mobile phone in 1 to 3 year, especially mobile phone is even shorter.Estimate according to United Nations Environment Programme, the whole world is often produced per year
Raw about 4000~60,000,000 tons of electronic wastes, wherein US and European accounts for 1/3 and 1/4 respectively.China is only second to the U.S.
Second largest electron wastes producing country.Additionally, the electronic waste of foreign countries continually pours into China.It is reported that the whole world 90%
" electronic waste " enters Asia, wherein about 80% enters China's Mainland.In all kinds of electron wastes, wherein waste printed circuit board
Averagely account for the 4% of total amount.However, being eliminated or the electronic product such as panel computer, notebook computer, mobile phone that turnover rate is high
In, circuit board proportion is up to 40%.
Used as the important composition part of electron wastes, waste printed circuit board (WCB) but contains substantial amounts of metals resources, gold
Category accounts for the 40% of circuit board gross weight.By weight percentage, 0.5 is included in waste printed circuit board multi-metal complex mixture
~6.0% aluminium, 1%~2.5% silicon, 0.1%~1.0% chromium, 0.05%~1.0% manganese, 5.0%~10% iron, 0.05%~
1.0% cobalt, 1.5%~3.0% nickel, 60%~80% bronze medal, 0.5%~1.5% zinc, 0.05%~0.1% silver medal, 0.05%~
1.0% cadmium, 5.0%~8.0% tin, 0.5%~1.0% antimony, 0.05%~0.1% gold medal, 2.0%~5.0% lead, 0.5%~
The metallic elements such as 1.0% bismuth.It can be seen that, the metal contained in waste printed circuit board is tens times or even hundred times of native deposits, it
Be both environmentally hazardous rubbish, be again valuable resource.
The recycling technology of metals resources is broadly divided into mechanical-physical treatment, hydrometallurgy, biology in waste printed circuit board
Metallurgy, pyrometallurgy etc. or several treatment technologies are combined：
1. mechanical-physical treatment (《The process for breaking, separating and recovering and its device therefor of printed circuit board (PCB)》, referring to middle promulgated by the State Council
Bright patent (patent 99102862.7, publication number CN1238244A)；《The broken and high-pressure electrostatic separation method of waste and old circuit board》,
Referring to Chinese invention patent (patent No. 200510023785.5, publication number CN1313208A)；《Metal enrichment in waste printed circuit board
The physiochemical mutagens technique of body》, referring to Chinese invention patent (patent No. 200410014582.5, publication number CN1563440A)).Should
Method is that discarded circuit board first is ground into particle using plant equipment, then recycles each component physical property (such as：Density, conduction
Property etc.) difference, realize that metal is separated with nonmetallic.Using mechanical-physical facture, more than 95% gold in waste printed circuit board
Category material can be recycled.But, the metal of separation is the complicated secondary metals resource that Determination of multiple metal elements is mixed,
Many metal mixtures must be separated and cycling and reutilization, metals resources could be realized.
2. hydrometallurgy (《The method of valuable metal in the separation and recovery many metal enrichment powder of waste printed circuit board》, referring to China
Patent of invention (patent No. 201210267821.2, publication number CN102747229A)；《A kind of Selectively leaching separates discarded circuit
The method of tin, lead and copper in plate》, referring to Chinese invention patent (patent No. 200910082443.9, publication number
CN101864519A)).The method is that waste printed circuit board is placed in strong acid solution, and metallics occurs chemical reaction and dissolves,
Then metallic element is reclaimed from solution.However, the method is low to the leaching efficiency of part metals, act on limited, especially by
The metallic element being wrapped in ceramics cannot be reclaimed；The technology especially weak point is that chemical reagent consumption amount is big, while producing
It is a large amount of to contain waste liquid and the waste residue being corrosive with toxicity and heavy metal ion, easily cause secondary pollution.
3. biological metallurgy (《The waste printed circuit board method for recovering precious metals of joint physical separation and Bioleaching》, in
State's application for a patent for invention (application number 201310262065.9, publication number CN103320618A)；《Copper reclaims system in waste printed circuit board
System》, referring to Chinese utility model patent (patent No. 201220074426.8, publication number CN202519343U)；《Biological wet method smelting
Technology for gold reclaims the progress of valuable metal in discarded circuit board》, non-ferrous metal scientific and engineering, 1 phase in 2013).The skill
Art is interacted with the metallic element in waste printed circuit board using certain microorganism or its metabolite, produce oxidation, reduction,
The reactions such as absorption, dissolving, it is so as to realize the recovery of metallic element in waste printed circuit board but limited due to being currently known strain, and
It is difficult industrialization and amplifies culture, the leaching velocity of metal is slower, and the production cycle of removal process is long, low production efficiency.
4. pyrometallurgy.The technology be by smelting furnace under oxygen-enriched environment high-temperature heating waste printed circuit board, peel off non-gold
Category material, and the metallics for melting flows out in alloy melt, then metallic element is reclaimed by refining and being electrolysed treatment, but
Nonmetallic substance can produce volume of smoke or toxic gas in combustion, have harm to air ecological environment.
As can be seen here, during recycling treatment waste printed circuit board metallic element, prior art also exist limitation or
It is not enough.Reclaimed or recycling method currently without to nickel element proposition is rational in many metal mixtures of waste printed circuit board.
If nickel element is dealt with improperly in many metal mixtures of waste printed circuit board, on the one hand, cause high risks to the mankind and animals and plants,
Such as nickel salt or NICKEL CARBONYL POISONING；On the other hand, valuable secondary nonferrous metal resource cannot be reclaimed and cycling and reutilization, be caused
The wasting of resources.
The content of the invention
It is an object of the invention to overcome prior art not enough, there is provided a kind for the treatment of by stages, technique are simple and direct, high efficiency,
The enrichment of nickel element and separation method in low emission, many metal mixed resources of environmentally friendly waste printed circuit board, by nickel element from
Separated in hybrid metal, realize the recovery to metallic nickel in waste printed circuit board and recycling treatment.
In order to realize this purpose, the metallurgy feature and metallic element present invention utilizes metal liquid-liquid separation are in liquid
Selectivity distribution behavior and its control technology in phase-separation system are different by the micro- and use for adding different
Technological parameter, apportionment ratio of the regulation and control metallic element in liquid-phase separating system, makes the Biosorption of Metal Elements being recovered and is fixed on
In predetermined liquid phase, so as to realize that be recovered metallic element is separated from each other with many metal mixtures of waste printed circuit board, is finally reached
Green reclaim and cycling and reutilization.
For the separation of nickel element in many metal mixtures of waste printed circuit board, the present invention through broken+sorting first to giving up
Abandoning multi-metal complex mixture of the circuit board containing nickel element carries out chemical analysis, then adds trapping agent in many metal mixtures
And pregnant solution, the metal mixture that will be prepared is placed in and fusing heated in vacuum furnace, and modulation process parameter occurs melt
Thus liquid-liquid separation, metal nickel element selective enrichment, nickel element is isolated from many metal mixtures in iron liquid phase
Come, specifically include following steps：
Step 1) waste printed circuit board is carried out to crush+sort, the metal in waste printed circuit board is isolated from nonmetallic
Come, obtain the multi-metal complex mixture containing nickel element；
Step 2 carries out chemical composition analysis to multi-metal complex mixture, measures copper, the quality of iron in many metal mixtures
Content；
Step 3 adds trapping agent ferro element in multi-metal complex mixture, ferro element is matched in many metal mixtures
In shared mass fraction be 35%~50%, the multi-metal complex mixture that will have been configured is placed in the graphite earthenware of vacuum furnace
In pot；
Start vacuum-pumping system after the sealing of step 4 vacuum furnace, then start vacuum furnace power supply, be heated to
1350~1450 DEG C, after many metal mixtures in graphite crucible are completely melt, and it is incubated 5~10min；
Step 5 reduction melt temperature to 1150~1250 DEG C, in making the matrix liquid phase with copper as essential element, isolate with
Iron is the second liquid phase of essential element；
Step 6 keeps melt temperature in 1150~1250 DEG C, and pregnant solution silicon or titanium elements are added in the melt, regulates and controls liquid
The separation rate of state copper and liquid iron two-phase, makes nickel element selectivity fast enriching in iron liquid phase；
Step 7 keeps melt temperature in 1150~1250 DEG C, and liquid copper is mixed with liquid iron in mechanical agitation graphite crucible
Close 10~15min of melt；
Step 8 keeps melt temperature in 1150~1250 DEG C, 10~30min of melt is stood, due to liquid iron and liquid
There is density contrast between copper, under gravity melt separation in crucible, form upper strata for liquid iron and lower floor are liquid copper
Melt is separated, the upper strata liquid iron that will trap nickel element is poured out；
The mass content of nickel element in step 9 detection upper strata liquid iron, if nickel mass content is less than 15%, liquid iron is returned
Recycling in step 3 is returned to, nickel in many metal mixed resources of waste printed circuit board of next batch is used for as trapping agent ferro element
The multi-cycle separation of element and extraction.
The enrichment of nickel element and separation method in many metal mixed resources of described waste printed circuit board, what step 3 was added catches
Collection agent ferro element is mainly derived from the ferrous metal that electron wastes are dismantled, and obtains the metallic element in electron wastes
Comprehensive cyclic utilization.
The enrichment of nickel element and separation method in many metal mixed resources of described waste printed circuit board, in step 6, pregnant solution
Silicon or titanium elements are with the ferro-silicium of silicon mass content 50~60% or the ferro-titanium with titanium mass content 65~75%
What form was added.
The enrichment of nickel element and separation method in many metal mixed resources of described waste printed circuit board, step 8 is when in iron liquid
When the mass fraction of nickel element is less than 15%, the upper strata liquid iron return to step 3 that can will have trapped metal nickel element is circulated again
Utilize, as trapping agent ferro element be used for next batch many metal mixed resources of waste printed circuit board in nickel element separation with carry
Take.
The enrichment of nickel element and separation method, catch in step 8 crucible in many metal mixed resources of described waste printed circuit board
The upper strata liquid iron of metal nickel element is collected, has been reached or close to after 15% after the nickel element mass content in iron liquid, will directly fall
What is gone out has trapped the upper strata liquid iron of nickel element, is sent to steel mill, and stainless steel or the middle conjunction as steel alloy are manufactured after refining
Gold etc., thus, nickel element is separated from waste printed circuit board multi-metal complex mixture and is able to cycling and reutilization.
Advantages of the present invention and beneficial effect are：
1st, the present invention utilizes the metallurgy feature and metallic element of metal itself liquid-liquid separation in liquid-phase separating system
Selectivity distribution behavior and its control technology, by adding the elements such as different trapping agent and pregnant solutions and using different
Technological parameter, apportionment ratio of the regulation and control metallic element in liquid-phase separating system, makes the Biosorption of Metal Elements being recovered and is fixed on
In predetermined liquid phase, so as to realize that be recovered metallic element is separated from each other with many metal mixtures of waste printed circuit board, is finally able to
Green reclaim and cycling and reutilization.The separation of nickel element and recycling method letter in many metal mixed resources of waste printed circuit board
It is single easy, with comprehensive high-efficiency, low cost, it is environment-friendly the features such as；The trapping agent ferro element of addition is because useless from electronics
Gurry, can make the major metal iron of electron wastes obtain comprehensive high-efficiency cycling and reutilization；The upper strata liquid of nickel element is trapped
Iron can be recycled, and nickel element in many metal mixed resources of waste printed circuit board of next batch is used for as trapping agent ferro element
Separate and extract；After the nickel element mass content in iron liquid reaches predetermined value such as 15%, directly nickel unit has been trapped by what is poured out
The liquid iron of element is sent to steel mill, and stainless steel or the intermediate alloy as steel alloy etc. are manufactured after refining；In crucible it is remaining under
Layer liquid copper continues on for other, and there is targetedly metallic element to separate and cycling and reutilization.With hydrometallurgy and extensive fire
The method that method metallurgy etc. reclaims valuable metal in waste printed circuit board is compared, and the present invention is reducing the side such as secondary pollution, energy saving
Face and metals resources comprehensive high-efficiency recycling aspect substantially have bigger advantage.
2nd, containing substantial amounts of ferrous metal, non-ferrous metal, rare precious metal etc. in circuit board, waste printed circuit board of the invention is more
The separation of metal mixed resource and recycling method, help efficiently to recycle non-ferrous metal secondary resource, alleviate China
The pressure of nonferrous metal resource shortage, it is ensured that China's sustainable economic development.Additionally, many metals of waste printed circuit board of the invention are mixed
The separation in joint source and recycling method, because its separation process occurs in vacuum furnace, it is to avoid because of waste gas and
Secondary pollution caused by discharge of wastewater, the characteristics of possess environment-friendly.Therefore, many metal mixeds of waste printed circuit board of the invention
The separation of resource has economy and environment double benefit with recycling method.
Specific embodiment
In a specific embodiment, the separation the invention provides waste printed circuit board mixing multiple metallic element is sharp again with circulation
With method, the specifically selectivity using the metallurgy feature and metallic element of metal liquid-liquid separation in liquid-phase separating system
Distribution behavior and its control, by adding different trapping agents and pregnant solution element and the different technological parameter of use, regulation and control
Apportionment ratio of the metallic element in liquid-phase separating system, makes the Biosorption of Metal Elements being recovered and is fixed in trapping agent liquid phase,
So as to realize that be recovered metallic element separates from many metal mixtures of waste printed circuit board, finally it is able to green reclaim and follows
Ring is recycled.
For the separation of nickel element in many metal mixtures of waste printed circuit board, and contain in view of each metal in various boards
The difference of amount, the present invention is first to multi-metal complex mixture of the waste printed circuit board containing nickel element through broken+sorting
Credit is analysed, and mainly grasps copper and weight of iron content in many metal mixtures.And then, trapping is added in multi-metal complex mixture
Agent ferro element, it is 35%~50% ferro element is matched the mass fraction accounted in many metal mixtures, the gold more that will have been configured
Category complex mixture is placed in the graphite crucible of vacuum furnace.After sealing vacuum furnace, start vacuum-pumping system, then
Start vacuum furnace power supply, be heated to 1350~1450 DEG C, after many metal mixtures in graphite crucible are completely melt, and
5~10min of insulation；Then, melt temperature is reduced to 1150~1250 DEG C, is made in the matrix liquid phase with copper as essential element, divide
Separate out the second liquid phase with iron as essential element.Keep melt temperature constant at 1150~1250 DEG C, add in the melt micro
Pregnant solution silicon or titanium elements, make pregnant solution be 0.5%~5% in the mass fraction shared by melt, regulate and control liquid copper and liquid iron
The separation rate of two-phase, makes nickel element selectivity fast enriching in iron liquid phase.In 1150~1250 DEG C, using mechanical agitation skill
Art, liquid copper and liquid iron blend melt about 10~15min in stirring graphite crucible.Then, melt stands about at this temperature
10~30min, due to there is density contrast between liquid iron and liquid copper, melt separation in crucible under gravity, in formation
Layer is that liquid iron and lower floor are the separation melt of liquid copper, and the upper strata liquid iron that will trap nickel element is poured out, and detects liquid
Nickel element mass content in iron, if nickel mass content is less than 15%, liquid iron is recycled in returning to piece-rate system, as catching
Collection agent ferro element is used for the multi-cycle separation of nickel element and extraction in many metal mixed resources of waste printed circuit board of next batch.Treat iron
Nickel element mass content in liquid reaches or close to after 15%, does not return again to piece-rate system, is routed directly to steel mill, is manufactured after refining
Stainless steel or the intermediate alloy as steel alloy etc., thus, nickel element divides from waste printed circuit board multi-metal complex mixture
Separate out and, and be able to cycling and reutilization.Remaining lower floor's liquid copper continues on for other in crucible has targetedly metal unit
Element is separated and cycling and reutilization.
Below, technical scheme is further described by embodiment.
Embodiment 1
In the present embodiment, for the separation of nickel element in many metal mixtures of waste printed circuit board, confirmatory reality is carried out to it
Test.Chemical analysis is carried out to multi-metal complex mixture of the waste printed circuit board containing nickel element through broken+sorting first, it is measured
Middle copper and weight of iron content are respectively~75% and~4.3%.Added in multi-metal complex mixture and torn open from electron wastes
The ferrous metal that solution is got off as trapping agent ferro element, after adding iron, make weight of iron content in many metal mixtures reach~
40%.The multi-metal complex mixture that will have been configured is placed in the graphite crucible of vacuum furnace, seals vacuum furnace, is started
Vacuum-pumping system.Then, start vacuum furnace power supply, heating melting furnace in many metal mixtures, until temperature to~
1350 DEG C, it is incubated 5min.Afterwards, reduce heating power, reduce melt temperature to~1250 DEG C.At the same time, siliceous amount is added
Content is~55% ferro-silicium pregnant solution, accumulation rate of the regulation and control nickel element in iron liquid phase.Liquid copper mixes with liquid iron
After melt is through mechanical agitation 10min, 10min is stood at~1250 DEG C.Separate in crucible the liquid iron that forms upper lower leaf and
Liquid copper.The upper strata liquid iron that nickel element will have been trapped is poured out, and thus, nickel element divides from many metal mixtures of waste printed circuit board
Separate out and.Remaining lower floor's liquid copper continues on for other in crucible has targetedly separation and cycling and reutilization.Chemistry point
Analysis result shows, after once trapping nickel element, the nickel element mass content in the iron liquid of upper strata has reached~3.5%, and under
Nickel element mass content in layer copper liquid is~0.17%, the nickel element overwhelming majority point in many metal mixtures of waste printed circuit board
From being enriched in iron liquid phase.
Embodiment 2
In the present embodiment, for the separation of nickel element in many metal mixtures of waste printed circuit board, confirmatory reality is carried out to it
Test.Chemical analysis is carried out to multi-metal complex mixture of the waste printed circuit board containing nickel element through broken+sorting first, it is measured
Middle copper and weight of iron content respectively may be about~79% and~4.3%.Added in multi-metal complex mixture from electron wastes
The ferrous metal for dismantling as trapping agent ferro element, after adding iron, make weight of iron content in many metal mixtures reach~
40%.The multi-metal complex mixture that will have been configured is placed in the graphite crucible of vacuum furnace, seals vacuum furnace, is started
Vacuum-pumping system.Then, start vacuum furnace power supply, heat many metal mixtures in melting furnace up to~1350 DEG C,
Insulation 5min.Afterwards, reduce heating power, reduce melt temperature to~1200 DEG C.At the same time, addition titanium mass content for~
70% ferro-titanium pregnant solution, accumulation rate of the regulation and control nickel element in iron liquid phase.Liquid copper is with liquid iron blend melt through machine
After tool stirring 10min, melt is incubated standing 10min at~1200 DEG C.Melt separation in crucible, the liquid of lower leaf in formation
Iron and liquid copper.The upper strata liquid iron that nickel element will have been trapped is poured out, and thus, nickel element is from many metal mixtures of waste printed circuit board
In separate.Remaining lower floor's liquid copper continues on for other in crucible has targetedly separation and cycling and reutilization.Change
Learn analysis result and show that after once trapping nickel element, the nickel element mass content in the iron liquid of upper strata has reached~3.8%,
And the nickel element mass content in lower floor's copper liquid is~0.175%, the nickel element in many metal mixtures of waste printed circuit board is big absolutely
It is partially separated and is enriched in iron liquid phase.
Embodiment 3
In the present embodiment, for the separation of nickel element in many metal mixtures of waste printed circuit board, confirmatory reality is carried out to it
Test.Chemical analysis is carried out to multi-metal complex mixture of the waste printed circuit board containing nickel element through broken+sorting first, it is measured
Middle copper and weight of iron content respectively may be about~77% and~4.3%.Added in multi-metal complex mixture from electron wastes
The ferrous metal for dismantling as trapping agent ferro element, after adding iron, make weight of iron content in many metal mixtures reach~
40%.The multi-metal complex mixture that will have been configured is placed in the graphite crucible of vacuum furnace, seals vacuum furnace, is started
Vacuum-pumping system.Then, start vacuum furnace power supply, heat many metal mixtures in melting furnace up to~1350 DEG C,
Insulation 5min.Afterwards, reduce heating power, reduce melt temperature to~1150 DEG C.At the same time, addition titanium mass content is
~70% ferro-titanium pregnant solution, accumulation rate of the regulation and control nickel element in iron liquid phase.Liquid copper is passed through with liquid iron blend melt
After mechanical agitation 15min, melt is incubated standing 30min at~1150 DEG C.Melt is separated in crucible, lower leaf in formation
Liquid iron and liquid copper.The upper strata liquid iron that nickel element will have been trapped is poured out, and thus, nickel element is from many metals of waste printed circuit board
Separated in mixture.Remaining lower floor's liquid copper continues on for other in crucible has targetedly separation sharp again with circulation
With.Chemical analysis results show, the nickel element mass content in the iron liquid of upper strata has reached~4.3%, and the nickel in lower floor's copper liquid
Element mass content is~0.176%, the nickel element overwhelming majority separation and concentration in many metal mixtures of waste printed circuit board to iron
In liquid phase.
Embodiment 4
In the present embodiment, for the separation of nickel element in many metal mixtures of waste printed circuit board, confirmatory reality is carried out to it
Test.Chemical analysis is carried out to multi-metal complex mixture of the waste printed circuit board containing nickel element through broken+sorting first, it is measured
Middle copper and weight of iron content respectively may be about~79% and~4.1%.Through one in embodiment 3 being added in multi-metal complex mixture
The iron liquid of secondary trapping nickel element, weight of iron content reaches~40% in making many metal mixtures.The multi-metal complex that will have been configured
Mixture is placed in the graphite crucible of vacuum furnace, seals vacuum furnace, starts vacuum-pumping system.Then, start true
Empty heating furnace power supply, many metal mixtures in heating melting furnace are until~1350 DEG C, insulation 5min.Afterwards, heating work(is reduced
Rate, reduces melt temperature to~1150 DEG C.Addition titanium mass content is~70% ferro-titanium pregnant solution, and regulation and control nickel element exists
Accumulation rate in iron liquid phase.With liquid iron blend melt after mechanical agitation 15min, melt is incubated liquid copper at~1150 DEG C
Stand 30min.Melt is separated in crucible, the liquid iron of lower leaf and liquid copper in formation.The upper of nickel element will be trapped
Layer liquid iron is poured out, and thus, nickel element is separated from many metal mixtures of waste printed circuit board.Remaining subnatant in crucible
State copper continues on for other has targetedly separation and cycling and reutilization.Chemical analysis results show, by 2 trapping nickel units
After element, the nickel element mass content in the iron liquid of upper strata has reached~8.3%, and nickel element mass content in lower floor's copper liquid for~
0.197%, in nickel element in many metal mixtures of waste printed circuit board overwhelming majority separation and concentrations to iron liquid phase.
Embodiment 5
In the present embodiment, for the separation of nickel element in many metal mixtures of waste printed circuit board, confirmatory reality is carried out to it
Test.Chemical analysis is carried out to multi-metal complex mixture of the waste printed circuit board containing nickel element through broken+sorting first, it is measured
Middle copper and weight of iron content respectively may be about~78% and~4.2%.Through two in embodiment 4 being added in multi-metal complex mixture
The iron liquid of secondary trapping nickel element, weight of iron content reaches~40% in making many metal mixtures.The multi-metal complex that will have been configured
Mixture is placed in the graphite crucible of vacuum furnace, seals vacuum furnace, starts vacuum-pumping system.Then, start true
Empty heating furnace power supply, many metal mixtures in heating melting furnace are until~1350 DEG C, insulation 5min.Afterwards, heating work(is reduced
Rate, reduces melt temperature to~1150 DEG C.Addition titanium mass content is~70% ferro-titanium pregnant solution, and regulation and control nickel element exists
Accumulation rate in iron liquid phase.With liquid iron blend melt after mechanical agitation 15min, melt is incubated liquid copper at~1150 DEG C
Stand 30min.Melt is separated in crucible, the liquid iron of lower leaf and liquid copper in formation.The upper of nickel element will be trapped
Layer liquid iron is poured out, and thus, nickel element is separated from many metal mixtures of waste printed circuit board.Remaining subnatant in crucible
State copper continues on for other has targetedly separation and cycling and reutilization.Chemical analysis results show, by 3 trapping nickel units
After element, the nickel element mass content in the iron liquid of upper strata has reached~12.7%, and the nickel element mass content in lower floor's copper liquid is
~0.211%, in nickel element in many metal mixtures of waste printed circuit board overwhelming majority separation and concentrations to iron liquid phase.
Claims (4)
1. the enrichment of nickel element and separation method in a kind of many metal mixed resources of waste printed circuit board, it is characterised in that using gold
Belong to selectivity distribution behavior and its control of the metallurgy feature and metallic element of liquid-liquid separation in liquid-phase separating system, lead to
Cross and add different trapping agents and pregnant solution element and the different technological parameter of use, regulation and control metallic element is in liquid phase separation system
Apportionment ratio in system, makes the Biosorption of Metal Elements being recovered and is fixed in trapping agent liquid phase, so as to realize being recovered metal unit
Element is separated from many metal mixtures of waste printed circuit board, is finally able to green reclaim and cycling and reutilization, including following step
Suddenly：
Step 1 is carried out crushing+sorting to waste printed circuit board, and the metal in waste printed circuit board is separated from nonmetallic, is obtained
Multi-metal complex mixture that must be containing nickel element；
Step 2 carries out chemical composition analysis to multi-metal complex mixture, measures copper in many metal mixtures, the quality of iron and contains
Amount；
Step 3 adds trapping agent ferro element in multi-metal complex mixture, ferro element is matched the institute in many metal mixtures
The mass fraction for accounting for is 35%~50%, and the multi-metal complex mixture that will have been configured is placed in the graphite crucible of vacuum furnace；
Start vacuum-pumping system after the sealing of step 4 vacuum furnace, then start vacuum furnace power supply, it is heated to 1350~
1450 DEG C, after many metal mixtures in graphite crucible are completely melt, and it is incubated 5~10min；
Step 5 reduction melt temperature in making the matrix liquid phase with copper as essential element, is isolated and is with iron to 1150~1250 DEG C
The second liquid phase of essential element；
Step 6 keeps melt temperature in 1150~1250 DEG C, and pregnant solution titanium elements are added in the melt, regulates and controls liquid copper and liquid
The separation rate of state iron two-phase, makes nickel element selectivity fast enriching in iron liquid phase；
Step 7 keeps melt temperature in 1150~1250 DEG C, and liquid copper mixes molten with liquid iron in mechanical agitation graphite crucible
10~15min of body；
Step 8 keeps melt temperature in 1150~1250 DEG C, stands 10~30min of melt, due to liquid iron and liquid copper it
Between there is density contrast, melt separation in crucible under gravity forms upper strata for liquid iron and lower floor are the separation of liquid copper
Melt, the upper strata liquid iron that will trap nickel element is poured out；
The mass content of nickel element in step 9 detection upper strata liquid iron, if nickel mass content is less than 15%, liquid iron is returned to
Recycled in step 3, nickel element in many metal mixed resources of waste printed circuit board of next batch is used for as trapping agent ferro element
Multi-cycle separation with extract.
2. the enrichment according to nickel element in many metal mixed resources of waste printed circuit board described in claim 1 and separation method, its
It is characterised by：In step 3, the trapping agent ferro element of addition is mainly derived from the ferrous metal that electron wastes are dismantled, and makes
The metal of electron wastes obtains comprehensive cyclic utilization.
3. the enrichment according to nickel element in many metal mixed resources of waste printed circuit board described in claim 1 and separation method, its
It is characterised by：In step 6, pregnant solution titanium elements are added in the ferro-titanium form of titanium mass content 65~75%.
4. the enrichment according to nickel element in many metal mixed resources of waste printed circuit board described in claim 1 and separation method, its
It is characterised by：In step 8, that pours out has trapped the upper strata liquid iron of nickel element, is routed directly to steel mill, and stainless steel is manufactured after refining
Or the intermediate alloy as steel alloy, thus, nickel element is separated from waste printed circuit board multi-metal complex mixture, and
It is able to cycling and reutilization.
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