CN105039710B - Enrichment and separation method of cadmium in waste circuit board multi-metal hybrid resources - Google Patents
Enrichment and separation method of cadmium in waste circuit board multi-metal hybrid resources Download PDFInfo
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- CN105039710B CN105039710B CN201510404232.8A CN201510404232A CN105039710B CN 105039710 B CN105039710 B CN 105039710B CN 201510404232 A CN201510404232 A CN 201510404232A CN 105039710 B CN105039710 B CN 105039710B
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 134
- 239000002184 metal Substances 0.000 title claims abstract description 102
- 239000002699 waste material Substances 0.000 title claims abstract description 92
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 86
- 238000000926 separation method Methods 0.000 title claims abstract description 48
- 239000007788 liquid Substances 0.000 claims abstract description 132
- 239000000203 mixture Substances 0.000 claims abstract description 77
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 57
- 229910052802 copper Inorganic materials 0.000 claims abstract description 57
- 239000010949 copper Substances 0.000 claims abstract description 57
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 26
- 239000010439 graphite Substances 0.000 claims abstract description 26
- 239000007791 liquid phase Substances 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 17
- 230000001351 cycling effect Effects 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 13
- 229910052782 aluminium Inorganic materials 0.000 claims description 12
- 238000013019 agitation Methods 0.000 claims description 11
- 239000004411 aluminium Substances 0.000 claims description 10
- 230000005484 gravity Effects 0.000 claims description 7
- 238000003723 Smelting Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000000956 alloy Substances 0.000 claims description 5
- 239000010813 municipal solid waste Substances 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 4
- 239000002023 wood Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 3
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000002955 isolation Methods 0.000 claims description 2
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- 125000004122 cyclic group Chemical group 0.000 claims 1
- 239000007789 gas Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 30
- 238000005516 engineering process Methods 0.000 abstract description 12
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- 230000008569 process Effects 0.000 description 9
- 150000002739 metals Chemical class 0.000 description 8
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 6
- 229910052571 earthenware Inorganic materials 0.000 description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 5
- 229910052737 gold Inorganic materials 0.000 description 5
- 239000010931 gold Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000005272 metallurgy Methods 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 239000010793 electronic waste Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000009854 hydrometallurgy Methods 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 238000009853 pyrometallurgy Methods 0.000 description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 3
- 229910001948 sodium oxide Inorganic materials 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
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- 230000007613 environmental effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 229910000906 Bronze Inorganic materials 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- FAWGZAFXDJGWBB-UHFFFAOYSA-N antimony(3+) Chemical compound [Sb+3] FAWGZAFXDJGWBB-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 239000010974 bronze Substances 0.000 description 1
- PLZFHNWCKKPCMI-UHFFFAOYSA-N cadmium copper Chemical compound [Cu].[Cd] PLZFHNWCKKPCMI-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910000960 colored gold Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000003471 mutagenic agent Substances 0.000 description 1
- 231100000707 mutagenic chemical Toxicity 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- 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
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention belongs to the technology of comprehensive recycling of complex nonferrous metal secondary resources, and particularly relates to an enrichment and separation method of cadmium in waste circuit board multi-metal hybrid resources. The method includes the steps that firstly, a multi-metal complex mixture containing cadmium is obtained from a waste circuit board through smashing and sorting; a separating agent is added into the multi-metal complex mixture; the prepared multi-metal complex mixture is placed in a graphite crucible of a vacuum furnace; after the metal mixture is completely melted, trapping agent lead and a trace enrichment reagent are added; and cadmium is selectively enriched in a lead liquid phase, a separation melt with liquid copper on the upper layer and liquid lead on the lower layer is formed, and the liquid copper on the upper layer and the liquid lead trapping cadmium on the lower layer are poured out respectively. Thus, cadmium is separated from the multi-metal complex mixture of the waste circuit board and is further recycled. The method is simple and easy to implement and has the characteristics of being low in cost, comprehensive, efficient, free of pollution and the like.
Description
Technical field
The invention belongs to complicated non-ferrous metal secondary resource synthesis cycling and reutilization technology, specially a kind of waste printed circuit board
The enrichment of cadmium element and separation method in many metal mixed resource, are related in environmental protection technical field, electron wastes be carried out
Reclaim, regenerate and comprehensive high-efficiency resource technology, help and solve the problems, such as that 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 scientific and technical update constantly brought forth new ideas with electric equipment products, a large amount of waste electric products become
Growth rate is the fastest and a most intractable class solid waste.Electron wastes 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 are 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 in 2010 is more than 3.7
Hundred million, computer, electric refrigerator and washing machine are respectively more than 80,000,000,1.5 hundred million and 1.9 hundred million.In general, electric refrigerator, wash
The average life of clothing machine in 8 to 10 years, television set average life in 4 to 6 years, as update faster computer
With superseded cycle of mobile phone in 1 to 3 year, especially mobile phone is even shorter.Estimate, the whole world is often produced per year according to United Nations Environment Programme
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 manufacturing country.Additionally, external electronic waste continually pours into China.It is reported that, the whole world 90%
" electronic waste " enters Asia, and 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 that turnover rate is high, notebook computer, mobile phone
In, circuit board proportion is up to 40%.
As the important composition part of electron wastes, waste printed circuit board (wcb) but contains substantial amounts of metals resources, gold
Belong to and account for the 40% of circuit board gross weight.By weight percentage, include 0.5 in waste printed circuit board multi-metal complex mixture
～6.0% aluminum, 1%～2.5% silicon, 0.1%～1.0% chromium, 0.05%～1.0% manganese, 5.0%～10% ferrum, 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% stannum, 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 containing in waste printed circuit board is tens times or even hundred times of native deposits, it
Be environmentally hazardous rubbish, be valuable resource again.
In waste printed circuit board, the recycling technology of metals resources is broadly divided into mechanical-physical process, hydrometallurgy, biology
Metallurgy, pyrometallurgy etc. or several treatment technology combine:
1. (" process for breaking, separating and recovering of printed circuit board (PCB) and its device therefor ", referring to middle promulgated by the State Council for mechanical-physical process
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 first discarded circuit board to be ground into granule using plant equipment, then recycles each component physical property (such as: density, conduction
Property etc.) difference, realize metal and separate with nonmetallic.Using mechanical-physical facture, more than 95% gold in waste printed circuit board
Belong to material can be recycled.But, detached metal is the complicated secondary metals resource that Determination of multiple metal elements mixes,
Many metal mixtures must be carried out separating and cycling and reutilization, just enable metals resources.
2. (" method of valuable metal in separation and recovery waste printed circuit board many metal enrichments powder ", referring to China for hydrometallurgy
Patent of invention (patent No. 201210267821.2, publication number cn102747229a)；" a kind of Selectively leaching separates discarded circuit
The method of stannum, 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 metallicses occur chemical reaction to dissolve,
Then reclaim metallic element from solution.However, the method is low to the leaching efficiency of part metals, limited use, especially by
The metallic element being wrapped in pottery cannot reclaim；This technology especially weak point is that chemical reagent consumption amount is big, produces simultaneously
Contain waste liquid and the waste residue being corrosive with toxicity and heavy metal ion in a large number, easily cause secondary pollution.
3. biological metallurgy (" joint physical separation and Bioleaching waste printed circuit board method for recovering precious metals ", referring in
State's application for a patent for invention (application number 201310262065.9, publication number cn103320618a)；" in waste printed circuit board, copper reclaims system
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).This skill
Art is to be 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, thus realizing the recovery of metallic element in waste printed circuit board, but limited due to being currently known strain, and
It is difficult industrialization amplification culture, the leaching velocity of metal is slower, and the production cycle of removal process is long, low production efficiency.
4. pyrometallurgy.This technology be by smelting furnace under oxygen enriched environment high-temperature heating waste printed circuit board, peel off non-gold
Belong to material, and the metallicses melting are in alloy melt outflow, then recovery metallic element is processed by refine and electrolysis, but right and wrong
Metallicses can produce volume of smoke or toxic gas in combustion, has 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
Not enough.Although having developed sealing-off technology during electron wastes are disassembled (referring to " circuit board element and solder separation and recovery
Method and device ", Chinese invention patent, patent No. cn200710201532.1, publication number cn101112728), but, at present
In many metal mixtures to waste printed circuit board, cadmium element does not propose rational enrichment, separates and recycling method.Weight
The toxicity of cadmium metal and its compound is very big.Propose rational currently without cadmium element in metal mixtures many to waste printed circuit board
Reclaim or recycling method.If in the many metal mixtures of waste printed circuit board, cadmium element is dealt with improperly, on the one hand, to the mankind
Cause high risks with animals and plants, such as the cadmium in subsoil water, soil, food etc. is exceeded；On the other hand, the secondary of preciousness has coloured gold
Belong to resource cannot reclaim and cycling and reutilization, cause the wasting of resources.
Content of the invention
It is an object of the invention to overcoming prior art not enough, provide that a kind for the treatment of by stages, technique be simple and direct, high efficiency,
The enrichment of cadmium element and separation method in low emission, environmentally friendly waste printed circuit board many metal mixed resource, by cadmium element from
Separate in hybrid metal, realize the recovery to cadmium metal in waste printed circuit board and recycling treatment.
In order to realize this purpose, present invention utilizes metal liquid-liquid detached metallurgy feature and metallic element are in liquid
Selectivity distribution behavior in phase-separation system and its control technology, by adding different trace element and adopting different
Technological parameter, regulates and controls apportionment ratios in liquid-phase separating system for the metallic element, makes the Biosorption of Metal Elements being recovered and be fixed on
In predetermined liquid phase, thus realization is recovered metallic element and separates from the many metal mixtures of waste printed circuit board, final
With green reclaim and cycling and reutilization.
For the separation of cadmium element in the many metal mixtures of waste printed circuit board, first, waste printed circuit board is after broken+sorting
Obtain the multi-metal complex mixture containing cadmium element, multi-metal complex mixture adds separating medium, trapping agent, enrichment
Agent, the metal mixture preparing is placed in heating fusing, modulation process parameter in the graphite crucible of vacuum furnace, so that melt is sent out
Give birth to liquid-liquid separation, cadmium element selective enrichment, in lead liquid phase, due to there is density contrast between liquid copper and liquid lead, is weighing
Under power effect, there is stratified liquid in melt in crucible, and forming upper strata is the liquid copper and lower floor separation melt for liquid lead.By
This, cadmium element is separated from waste printed circuit board multi-metal complex mixture, and is recycled, and specifically includes following step
Rapid:
Step 1 carries out crushing+sorting to waste printed circuit board, and the metal in waste printed circuit board is isolated from nonmetallic
Come, obtain the multi-metal complex mixture containing cadmium element；
Step 2 adds separating medium aluminium element in multi-metal complex mixture, makes aluminium element proportioning in many metal mixtures
In shared mass fraction be 10%～20%, the multi-metal complex having configured mixture is placed in the graphite earthenware of vacuum furnace
In pot；
After the sealing of step 3 vacuum furnace, start vacuum-pumping system, after vacuum is less than 1pa, be filled with high pure nitrogen
Air pressure is made to reach 0.05mpa～0.1mpa, to reduce the volatilization of low-melting-point metal element and to avoid metal to aoxidize；
Step 4 starts vacuum furnace power supply, is heated to 1150～1200 DEG C, treats the many metal mixtures in graphite crucible
After being completely melt, mechanical agitation 5 minutes, and it is incubated 5～10min；
Step 5 reduces melt temperature to 1050～1100 DEG C, and adds trapping agent lead element, makes lead element proportioning in graphite
In crucible melt, shared mass fraction is 40%～60%, and melt liquid-liquid separation becomes liquid copper and liquid lead；
Step 6 reduces melt temperature to 1000～1050 DEG C, adds pregnant solution, and regulation and control liquid copper is biphase with liquid lead
Separation rate, makes cadmium element selectivity fast enriching in lead liquid phase；
Step 7 keeps melt temperature at 1000～1050 DEG C, and in mechanical agitation graphite crucible, liquid copper is mixed with liquid lead
Melt 10～15min；
Step 8 melt temperature stands 10～30min at 1000～1050 DEG C, because there is density between liquid lead and liquid copper
Difference, the melt in crucible is layered under gravity, is formed upper strata for liquid copper and lower floor for liquid lead layering melt,
Upper strata liquid copper is poured out, continues on for other and there is targetedly metallic element separation and cycling and reutilization；
Then the lower floor's liquid lead having trapped cadmium element remaining in crucible is poured out by step 9, and detects cadmium in liquid lead
The mass content of element, if cadmium element mass content is less than 6%, liquid lead returns in step 5 and recycles, as trapping agent
Lead element be used for next batch waste printed circuit board many metal mixed resource in cadmium element enrichment with separate.
The enrichment of cadmium element and separation method in described waste printed circuit board many metal mixed resource, in step 2, addition
Separating medium aluminium element is mainly derived from the aluminum metal that electron wastes dismantle, and makes the metal of electron wastes obtain synthesis
Recycle.
The enrichment of cadmium element and separation method in described waste printed circuit board many metal mixed resource, in step 6, addition
Pregnant solution is mainly the oxide of alkali metal (such as: sodium, potassium etc.).
In described waste printed circuit board many metal mixed resource, the enrichment of cadmium element and separation method, in step 9, pour out
Trap lower floor's liquid lead of cadmium element, be cooled to 350～450 DEG C, in melt, separated out a small amount of In Crystal Solid Copper, then using centrifugation point
From or solid-liquid filtration isolation technics, liquid lead can be separated further with copper, if the cadmium element mass content in liquid lead
Now reach predetermined value, be sent to coloured smelting factory, after refine, manufacture wood's alloy material.Thus, cadmium element is from discarded
Separate in circuit board multi-metal complex mixture, and recycled.
Advantages of the present invention and beneficial effect are:
1st, the present invention utilizes the metallurgy feature of metal itself liquid-liquid separation and metallic element in liquid-phase separating system
Selectivity distribution behavior and its control technology, by adding element and the employings such as different separating mediums, trapping agent and pregnant solution
Different technological parameters, regulates and controls apportionment ratios in liquid-phase separating system for the metallic element, make the Biosorption of Metal Elements that is recovered and
It is fixed in predetermined liquid phase, thus realization is recovered metallic element, and many metal mixtures are separated from each other, with waste printed circuit board
It is able to green reclaim and cycling and reutilization eventually.In waste printed circuit board many metal mixed resource of the present invention the enrichment of cadmium element with separate
Method is simple, has the features such as comprehensive high-efficiency, low cost, environmental friendliness.By liquid-liquid layering formed upper strata liquid copper and
Lower floor's liquid lead is poured out respectively, and upper strata liquid copper continues on for other and has targetedly metallic element separation and extraction, traps
Lower floor's liquid lead of cadmium element can recycle, and be used for waste printed circuit board many metals of next batch as trapping agent lead element
In mixing resource, the separation of cadmium element and extraction, after the cadmium element mass content in lead liquid reaches predetermined value, are sent to coloured smelting
Refinery, manufactures wood's alloy material after refine.Reclaim in waste printed circuit board with hydrometallurgy and extensive pyrometallurgy etc.
The method of valuable metal is compared, and the present invention is sharp again at the aspects such as reduction secondary pollution, energy saving and metals resources comprehensive high-efficiency
With aspect, substantially there is bigger advantage.
2nd, substantial amounts of ferrous metal, non-ferrous metal, rare precious metal etc. are contained in circuit board, the waste printed circuit board of the present invention is many
The separation of metal mixed resource and recycling method, contribute to efficiently recycling non-ferrous metal secondary resource, alleviate China
The pressure of nonferrous metal resource shortage is it is ensured that China's sustainable economic development.Additionally, the many metals of the waste printed circuit board of the present invention mix
The separation in joint source and recycling method, because its separation process occurs in the vacuum or anaerobic heating furnace, it is to avoid because
Waste gas and discharge of wastewater and the secondary pollution that leads to, possess eco-friendly feature.Therefore, how golden the waste printed circuit board of the present invention is
The separation belonging to mixing resource has economy and environment double benefit with recycling method.
Specific embodiment
In a specific embodiment, the invention provides the separation of waste printed circuit board mixing multiple metallic element and circulation are sharp again
With method, specifically utilize the metal liquid-liquid detached metallurgy feature and metallic element selectivity in liquid-phase separating system
Distribution behavior and its control, by adding different separating mediums, trapping agent and pregnant solution element and adopting different technique ginsengs
Number, regulates and controls apportionment ratios in liquid-phase separating system for the metallic element, makes the Biosorption of Metal Elements being recovered and be fixed on trapping agent
In liquid phase, thus realization is recovered metallic element and separates from the many metal mixtures of waste printed circuit board, finally it is able to green
Reclaim and cycling and reutilization.
For cadmium element in the many metal mixtures of waste printed circuit board enrichment with separate, first waste printed circuit board is broken
Broken+sorting, the metal in waste printed circuit board is separated from nonmetallic, obtains the mixing of the multi-metal complex containing cadmium element
Thing.Add separating medium aluminum in multi-metal complex mixture, the quality making aluminium element proportioning shared in many metal mixtures is divided
Number is 10%～20%, and the multi-metal complex having configured mixture is placed in the black-fead crucible of vacuum furnace.Heating in vacuum
After stove sealing, start vacuum-pumping system, be then charged with nitrogen, to reduce the volatilization of low-melting-point metal element and to avoid metal oxygen
Change.Then, start vacuum furnace power supply, be heated to 1150～1200 DEG C, treat that the many metal mixtures in graphite crucible are complete
After fusing, mechanical agitation 5 minutes, and it is incubated 5～10min.Reduce melt temperature, and add trapping agent lead element, make lead element
The shared mass fraction in graphite crucible melt of proportioning is 40%～60%, and melt liquid-liquid separation becomes liquid copper and liquid lead.
Afterwards, reduce melt temperature further, and add micro pregnant solution, make mass fraction shared by graphite crucible melt for the pregnant solution
For 0.5%～3%, regulate and control the liquid copper separation rate biphase with liquid lead, make cadmium element selectivity fast enriching in lead liquid phase.
In mechanical agitation graphite crucible, liquid copper and liquid lead blend melt about 10～15min, stand 10～30min.Liquid lead and liquid
Because there is density contrast between state copper, the melt in crucible is layered under gravity, and forming upper strata is liquid copper and lower floor
For the layering melt of liquid lead, the melt of upper lower leaf is poured out respectively.The upper strata liquid copper poured out, continues on for other and has
Targetedly metallic element separates and cycling and reutilization；Trap in lower floor's liquid lead of cadmium element, if the quality of cadmium element
Content is less than 6%, and liquid lead can return to recycle in piece-rate system, is used for the discarded electricity of next batch as trapping agent lead element
The multi-cycle separation of antimony element and extraction in the plate many metal mixed resource of road.Treat that the cadmium element mass content in lead liquid reaches or close
After 6%, do not return again to piece-rate system, be sent to coloured smelting factory, after refine, manufacture wood's alloy material.Thus, cadmium element
Separate from waste printed circuit board multi-metal complex mixture, and be able to cycling and reutilization.
Below, by embodiment, technical scheme is further described.
Embodiment 1
In the present embodiment, for cadmium element in the many metal mixtures of waste printed circuit board enrichment with separate, it is carried out and tests
The experiment of card property.First waste printed circuit board is carried out crushing+sorting, the metal in waste printed circuit board is isolated from nonmetallic
Come, obtain the multi-metal complex mixture containing cadmium element.Multi-metal complex mixture adds from electric garbage is disassembled
The aluminum metal separating medium coming, makes the shared mass fraction in many metal mixtures of aluminium element proportioning be 10%, will configure
Multi-metal complex mixture be placed in the black-fead crucible of vacuum furnace.Then, seal vacuum furnace, start vacuum suction
System, when vacuum < after 1pa, is filled with high pure nitrogen in heating furnace nacelle, makes air pressure reach 0.07mpa, to reduce low melting point
The volatilization of metallic element and avoid METAL HEATING PROCESS process aoxidize.Start vacuum furnace power supply, be heated to 1180 DEG C, treat graphite earthenware
After many metal mixtures in crucible are completely melt, mechanical agitation 5min, and it is incubated 5min.Then, reduce melt temperature to 1100
DEG C, add trapping agent lead, make the shared mass fraction in graphite crucible melt of lead element proportioning be 50%, melt liquid-liquid is divided
From one-tenth liquid copper and liquid lead.Reduce melt temperature further to 1050 DEG C, and add micro pregnant solution sodium oxide, regulate and control liquid
The copper separation rate biphase with liquid lead, cadmium element selectivity fast enriching is in lead liquid phase.In 1050 DEG C of melt temperature, machinery stirs
Mix liquid copper and liquid lead blend melt about 10min in graphite crucible, subsequently stand 10min.Between liquid lead and liquid copper because
There is density contrast, the melt in crucible is layered under gravity, formed upper strata be liquid copper and lower floor be liquid lead
Layering melt, the melt of upper lower leaf is poured out respectively.Thus, cadmium element is isolated from the many metal mixtures of waste printed circuit board
Come.Upper strata liquid copper continues on for other and has targetedly metallic element separation and cycling and reutilization.Chemical analysis results table
Bright, after once trapping cadmium element, the cadmium element mass content in lower floor's lead liquid has reached 0.07%, and the cadmium in liquid copper
Element mass content is negligible, and the cadmium element overwhelming majority separation and concentration in the many metal mixtures of waste printed circuit board is to lead liquid
Xiang Zhong.
Embodiment 2
In the present embodiment, for cadmium element in the many metal mixtures of waste printed circuit board enrichment with separate, it is carried out and tests
The experiment of card property.First waste printed circuit board is carried out crushing+sorting, the metal in waste printed circuit board is isolated from nonmetallic
Come, obtain the multi-metal complex mixture containing cadmium element.Multi-metal complex mixture adds from electric garbage is disassembled
The aluminum metal separating medium coming, makes the shared mass fraction in many metal mixtures of aluminium element proportioning be 15%, will configure
Multi-metal complex mixture be placed in the black-fead crucible of vacuum furnace.Then, seal vacuum furnace, start vacuum suction
System, when vacuum < after 1pa, is filled with high pure nitrogen in heating furnace nacelle, makes air pressure reach 0.07mpa, to reduce low melting point
The volatilization of metallic element and avoid METAL HEATING PROCESS process aoxidize.Start vacuum furnace power supply, be heated to 1150 DEG C, treat graphite earthenware
After many metal mixtures in crucible are completely melt, mechanical agitation 5min, and it is incubated 5min.Then, reduce melt temperature to 1100
DEG C, add trapping agent lead, make the shared mass fraction in graphite crucible melt of lead element proportioning be 50%, melt liquid-liquid is divided
From one-tenth liquid copper and liquid lead.Reduce melt temperature further to 1050 DEG C, and add micro pregnant solution sodium oxide, regulate and control liquid
The copper separation rate biphase with liquid lead, cadmium element selectivity fast enriching is in lead liquid phase.In 1050 DEG C of melt temperature, machinery stirs
Mix liquid copper and liquid lead blend melt about 10min in graphite crucible, subsequently stand 10min.Between liquid lead and liquid copper because
There is density contrast, the melt in crucible is layered under gravity, formed upper strata be liquid copper and lower floor be liquid lead
Layering melt, the melt of upper lower leaf is poured out respectively.Thus, cadmium element is isolated from the many metal mixtures of waste printed circuit board
Come.Upper strata liquid copper continues on for other and has targetedly metallic element separation and cycling and reutilization.Chemical analysis results table
Bright, after once trapping cadmium element, the cadmium element mass content in lower floor's lead liquid has reached 0.09%, and the cadmium in liquid copper
Element mass content is negligible, and the cadmium element overwhelming majority separation and concentration in the many metal mixtures of waste printed circuit board is to lead liquid
Xiang Zhong.
Embodiment 3
In the present embodiment, for cadmium element in the many metal mixtures of waste printed circuit board enrichment with separate, it is carried out and tests
The experiment of card property.First waste printed circuit board is carried out crushing+sorting, the metal in waste printed circuit board is isolated from nonmetallic
Come, obtain the multi-metal complex mixture containing cadmium element.Multi-metal complex mixture adds from electric garbage is disassembled
The aluminum metal separating medium coming, makes the shared mass fraction in many metal mixtures of aluminium element proportioning be 20%, will configure
Multi-metal complex mixture be placed in the black-fead crucible of vacuum furnace.Then, seal vacuum furnace, start vacuum suction
System, when vacuum < after 1pa, is filled with high pure nitrogen in heating furnace nacelle, makes air pressure reach 0.07mpa, to reduce low melting point
The volatilization of metallic element and avoid METAL HEATING PROCESS process aoxidize.Start vacuum furnace power supply, be heated to 1100 DEG C, treat graphite earthenware
After many metal mixtures in crucible are completely melt, mechanical agitation 5min, and it is incubated 5min.Then, reduce melt temperature to 1050
DEG C, add trapping agent lead, make the shared mass fraction in graphite crucible melt of lead element proportioning be 50%, melt liquid-liquid is divided
From one-tenth liquid copper and liquid lead.Reduce melt temperature further to 1000 DEG C, and add micro pregnant solution sodium oxide, regulate and control liquid
The copper separation rate biphase with liquid lead, cadmium element selectivity fast enriching is in lead liquid phase.In 1000 DEG C of melt temperature, machinery stirs
Mix liquid copper and liquid lead blend melt about 15min in graphite crucible, subsequently stand 30min.Between liquid lead and liquid copper because
There is density contrast, the melt in crucible is layered under gravity, formed upper strata be liquid copper and lower floor be liquid lead
Layering melt, the melt of upper lower leaf is poured out respectively.Thus, cadmium element is isolated from the many metal mixtures of waste printed circuit board
Come.Upper strata liquid copper continues on for other and has targetedly metallic element separation and cycling and reutilization.Chemical analysis results table
Bright, after once trapping cadmium element, the cadmium element mass content in lower floor's lead liquid has reached 0.105%, and in liquid copper
Cadmium element mass content is negligible, and the cadmium element overwhelming majority separation and concentration in the many metal mixtures of waste printed circuit board is to lead
In liquid phase.
Embodiment 4
In the present embodiment, for cadmium element in the many metal mixtures of waste printed circuit board enrichment with separate, it is carried out and tests
The experiment of card property.First waste printed circuit board is carried out crushing+sorting, the metal in waste printed circuit board is isolated from nonmetallic
Come, obtain the multi-metal complex mixture containing cadmium element.Multi-metal complex mixture is placed in the graphite earthenware of vacuum furnace
In pot.Then, seal vacuum furnace, start vacuum-pumping system, when vacuum < after 1pa, is filled with height in heating furnace nacelle
Pure nitrogen gas, make air pressure reach 0.07mpa, to reduce the volatilization of low-melting-point metal element and to avoid METAL HEATING PROCESS process to aoxidize.Open
Dynamic vacuum furnace power supply, is heated to 1100 DEG C, after the many metal mixtures in graphite crucible are completely melt, mechanical agitation
5min, and it is incubated 5min.Then, reduce melt temperature to 1050 DEG C, add the lead after once trapping in embodiment 3, make lead
The shared mass fraction in graphite crucible melt of element proportioning is 50%, and melt liquid-liquid separation becomes liquid copper and liquid lead.Enter
One step reduces melt temperature to 1000 DEG C, the regulation and control liquid copper separation rate biphase with liquid lead, and cadmium element selective enrichment is to lead
In liquid phase.In 1000 DEG C of melt temperature, liquid copper and liquid lead blend melt about 15min in mechanical agitation graphite crucible, subsequently
Standing 30min.Because there is density contrast between liquid lead and liquid copper, the melt in crucible is layered under gravity, shape
One-tenth upper strata is liquid copper and lower floor is the layering melt of liquid lead, and the melt of upper lower leaf is poured out respectively.Thus, cadmium element from
Separate in the many metal mixtures of waste printed circuit board.Upper strata liquid copper continues on for other and has targetedly metallic element dividing
From with cycling and reutilization.Chemical analysis results show, after 2 trapping cadmium elements, the cadmium element quality in lower floor's lead liquid contains
Amount has reached 0.171%, and the cadmium element mass content in liquid copper is negligible, in the many metal mixtures of waste printed circuit board
Cadmium element the overwhelming majority separation and concentration in lead liquid phase.
Claims (4)
1. in a kind of waste printed circuit board many metal mixed resource the enrichment of cadmium element and separation method it is characterised in that following walk
Rapid:
Step 1 carries out crushing+sorting to waste printed circuit board, the metal in waste printed circuit board is separated from nonmetallic, obtains
Obtain the multi-metal complex mixture containing cadmium element；
Step 2 adds separating medium aluminium element in multi-metal complex mixture, makes aluminium element proportioning institute in many metal mixtures
The mass fraction accounting for is 10%～20%, the multi-metal complex having configured mixture is placed in the black-fead crucible of vacuum furnace
In；
After the sealing of step 3 vacuum furnace, start vacuum-pumping system, after vacuum is less than 1pa, being filled with high pure nitrogen makes gas
Pressure reaches 0.05mpa～0.1mpa, to reduce the volatilization of low-melting-point metal element and to avoid metal to aoxidize；
Step 4 starts vacuum furnace power supply, is heated to 1150～1200 DEG C, treats that the many metal mixtures in graphite crucible are complete
After fusing, mechanical agitation 5 minutes, and it is incubated 5～10min；
Step 5 reduces melt temperature to 1050～1100 DEG C, and adds trapping agent lead element, makes lead element proportioning in graphite crucible
In melt, shared mass fraction is 40%～60%, and melt liquid-liquid separation becomes liquid copper and liquid lead；
Step 6 reduces melt temperature to 1000～1050 DEG C, adds pregnant solution, and liquid copper is biphase with liquid lead separates for regulation and control
Rate, makes cadmium element selectivity fast enriching in lead liquid phase, the pregnant solution of addition is the oxide of alkali metal；
Step 7 keeps melt temperature at 1000～1050 DEG C, liquid copper and liquid lead blend melt in mechanical agitation graphite crucible
10～15min；
Step 8 melt temperature stands 10～30min at 1000～1050 DEG C, because there is density contrast between liquid lead and liquid copper,
Melt in crucible is layered under gravity, forms the layering melt that upper strata is that liquid copper and lower floor are liquid lead, will
Upper strata liquid copper is poured out, and continues on for other and has targetedly metallic element separation and cycling and reutilization；
Then the lower floor's liquid lead having trapped cadmium element remaining in crucible is poured out by step 9, and detects cadmium element in liquid lead
Mass content, if cadmium element mass content be less than 6%, liquid lead return in step 5 recycle, as trapping agent lead unit
Element for next batch waste printed circuit board many metal mixed resource in cadmium element enrichment with separate.
2. according to enrichment and the separation method of cadmium element in the waste printed circuit board many metal mixed resource described in claim 1, its
It is characterised by: in step 2, the aluminum metal that the separating medium aluminium element of addition dismantles from electron wastes, make electronics
The metal of garbage obtains comprehensive cyclic utilization.
3. according to enrichment and the separation method of cadmium element in the waste printed circuit board many metal mixed resource described in claim 1, its
It is characterised by: in step 9, the lower floor's liquid lead having trapped cadmium element poured out, it is cooled to 350～450 DEG C, separate out few in melt
Amount In Crystal Solid Copper, then adopts centrifugation or solid-liquid filtration isolation technics, liquid lead is separated further with copper；Thus, cadmium
Element is separated from waste printed circuit board multi-metal complex mixture, and is recycled.
4. according to enrichment and the separation method of cadmium element in the waste printed circuit board many metal mixed resource described in claim 3, its
It is characterised by: if the cadmium element mass content in liquid lead has now reached predetermined value, be sent to coloured smelting factory, make after refine
Make wood's alloy material.
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| GB461222A (en) * | 1936-03-21 | 1937-02-12 | Cie Metaux Doverpelt Lommel | Process for purifying metallic cadmium |
| CN101629241A (en) * | 2009-08-04 | 2010-01-20 | 齐大全 | Method for extracting noble metals from circuit boards by using lead, tin and alloys of lead and tin as capturing agents |
| CN104313332A (en) * | 2014-10-15 | 2015-01-28 | 中国科学院金属研究所 | Self-assembly separation and resource recycling method for multi-metal components in electronic waste |
| CN104328281A (en) * | 2014-10-15 | 2015-02-04 | 中国科学院金属研究所 | Method for efficient separation and recycling of precious metals in waste circuit board |
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2015
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB461222A (en) * | 1936-03-21 | 1937-02-12 | Cie Metaux Doverpelt Lommel | Process for purifying metallic cadmium |
| CN101629241A (en) * | 2009-08-04 | 2010-01-20 | 齐大全 | Method for extracting noble metals from circuit boards by using lead, tin and alloys of lead and tin as capturing agents |
| CN104313332A (en) * | 2014-10-15 | 2015-01-28 | 中国科学院金属研究所 | Self-assembly separation and resource recycling method for multi-metal components in electronic waste |
| CN104328281A (en) * | 2014-10-15 | 2015-02-04 | 中国科学院金属研究所 | Method for efficient separation and recycling of precious metals in waste circuit board |
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