CN1948524A - Comprehensive resources treatment method of waste circuit board - Google Patents
Comprehensive resources treatment method of waste circuit board Download PDFInfo
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- CN1948524A CN1948524A CNA200610097382XA CN200610097382A CN1948524A CN 1948524 A CN1948524 A CN 1948524A CN A200610097382X A CNA200610097382X A CN A200610097382XA CN 200610097382 A CN200610097382 A CN 200610097382A CN 1948524 A CN1948524 A CN 1948524A
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Links
- 238000000034 method Methods 0.000 title claims abstract description 45
- 239000002699 waste material Substances 0.000 title claims description 9
- 239000010949 copper Substances 0.000 claims abstract description 59
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 52
- 241000605118 Thiobacillus Species 0.000 claims abstract description 36
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052802 copper Inorganic materials 0.000 claims abstract description 28
- 239000007787 solid Substances 0.000 claims abstract description 25
- 229910052742 iron Inorganic materials 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims description 51
- 241000894006 Bacteria Species 0.000 claims description 31
- 238000000605 extraction Methods 0.000 claims description 23
- 244000005700 microbiome Species 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 238000002386 leaching Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 16
- 241000605008 Spirillum Species 0.000 claims description 15
- 235000015097 nutrients Nutrition 0.000 claims description 14
- 239000011347 resin Substances 0.000 claims description 14
- 229920005989 resin Polymers 0.000 claims description 14
- 238000011081 inoculation Methods 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 13
- 239000001963 growth medium Substances 0.000 claims description 12
- 239000004593 Epoxy Substances 0.000 claims description 10
- 238000013019 agitation Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 241000205091 Sulfolobus solfataricus Species 0.000 claims description 9
- -1 2-hydroxyl-5-dodecyl diphenylketoxime Chemical compound 0.000 claims description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 7
- 238000010276 construction Methods 0.000 claims description 7
- 229910052698 phosphorus Inorganic materials 0.000 claims description 7
- 239000011574 phosphorus Substances 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 239000002054 inoculum Substances 0.000 claims description 6
- 239000002609 medium Substances 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- 238000002255 vaccination Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 238000005868 electrolysis reaction Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 19
- 239000002184 metal Substances 0.000 abstract description 19
- 230000008901 benefit Effects 0.000 abstract description 6
- 238000005272 metallurgy Methods 0.000 abstract description 6
- 238000011084 recovery Methods 0.000 abstract description 4
- 238000004064 recycling Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000002912 waste gas Substances 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 238000007599 discharging Methods 0.000 abstract 1
- 230000000813 microbial effect Effects 0.000 abstract 1
- 230000000717 retained effect Effects 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 8
- 238000009854 hydrometallurgy Methods 0.000 description 6
- 238000011161 development Methods 0.000 description 4
- 238000004070 electrodeposition Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 239000003365 glass fiber Substances 0.000 description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- 230000033116 oxidation-reduction process Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000004566 building material Substances 0.000 description 3
- 239000004568 cement Substances 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 241000605268 Thiobacillus thioparus Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000001580 bacterial effect Effects 0.000 description 2
- 238000009395 breeding Methods 0.000 description 2
- 230000001488 breeding effect Effects 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 238000012258 culturing Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 2
- UKUVVAMSXXBMRX-UHFFFAOYSA-N 2,4,5-trithia-1,3-diarsabicyclo[1.1.1]pentane Chemical compound S1[As]2S[As]1S2 UKUVVAMSXXBMRX-UHFFFAOYSA-N 0.000 description 1
- 241000605272 Acidithiobacillus thiooxidans Species 0.000 description 1
- 241000589158 Agrobacterium Species 0.000 description 1
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- 101100004287 Caenorhabditis elegans best-6 gene Proteins 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910016374 CuSO45H2O Inorganic materials 0.000 description 1
- 235000015076 Shorea robusta Nutrition 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 241001509286 Thiobacillus denitrificans Species 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 230000009615 deamination Effects 0.000 description 1
- 238000006481 deamination reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 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
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000000088 plastic resin Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 229940093916 potassium phosphate Drugs 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000036642 wellbeing Effects 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
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/82—Recycling of waste of electrical or electronic equipment [WEEE]
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method to extract copper from abandoned breadboards and to use remain substance comprehensively recycling by combining techniques of microbe, metallurgy and materials. Based on principles of microbial wet-process metallurgy, Cu is extracted from abandoned breadboards by using iron protoxide thiobacillus. At the same time, the retained solid is recycled to realize the comprehensive treatment of abandoned breadboards. The entire recycled treatment of abandoned breadboards is realized, which guarantees the entirely clean produce without discharging waste water, waster residue and waste gas into the environment. This method has much strongpoint including little investment, low cost, high recovery rate of metal, non-pollution and green zoology etc. It benefits the society, economy and environment.
Description
Technical field
The invention belongs to the changing rejected material to useful resource treatment technology, relate to a kind of in conjunction with microorganism, metallurgy, technology such as material are extracted metallic copper from discarded circuit board, and other surplus materials is carried out the method that comprehensive resource utilizes.
Background technology
The microorganism hydrometallurgy is to utilize oxidation, reduction, dissolving, the absorption effects such as (absorption) to mineral and element of some specific microorganism or its meta-bolites, the molten method of soaking metal or reclaiming (removing) metal from water from ore.
Utilize microorganism to leach and oxidation comes molten lean ore, abandoned mine, mine tailing and Daye slag etc. that contain the valuable and rare metal of tens kinds of copper, gold and silver, manganese, nickel, chromium etc. that soak, reach the purpose that prevents the Mineral resources loss.
At nineteen fifty-five S.R.Zimmerley, D.G.Wilson and J.D.Prater have applied for the patent of biological dump leaching first, and this technology is entrusted to Kennecott copper industry company practice, Canada utilized bacterium leaching uranium research and industrial application to obtain success in 1966, and the modern industry that has begun the microorganism hydrometallurgy is used.The 3rd geologic prospecting party of office and dump leaching center thereof are born in ground, China Shaanxi in 1994, two king's gold mine nine Ping Gou ore deposit sections have been carried out 2000t level technical scale microorganism preoxidation dump leaching test first in Shaanxi, the dump leaching rate of recovery exceeds 32% than conventional dump leaching, and test has obtained good result.
The microorganism hydrometallurgy has that cost is low, less investment, simple to operate, flow process short, advantages of environment protection, and is with fastest developing speed in the mineral engineering subject in recent years, research is the most extensive, its application is also more and more general.In recent years, because the high speed development of national economy, the resource critical shortage has appearred, problems such as environmental degradation, to strengthen major technologies and equipment development and the research of great industrial technology to fields such as biological metallurgies during country's 11th Five-Year, and started the construction of 3 national engineering laboratories such as biological metallurgy in the first batch, with the development that promotes the microorganism hydrometallurgy and the development of cleaner production.
The microorganism that is used for the microorganism hydrometallurgy has a variety of, as thiobacillus thiooxidans, thiobacillus thioparus (T.thioparus), deamination thiobacillus (T.denitrificans) and some heterotrophic bacteriums, thiobacillus ferrooxidant (as bacillus, Agrobacterium) etc.These microorganisms mostly are the chemosynthetic autotroph bacterium, and how acidproof they are generally, even still can survive under the environment of pH＜1.The bacterium energy sulfur oxide and the sulfide that have, Fe
2+Deng therefrom obtaining energy for existence.When cultivating bacterium used in metallurgy, at first should be different with the impurity situation according to ore kind and various component thereof, select suitable bacterial classification.Can make tolerance and molten the soak efficient of bacterial strain enhancing in case of necessity by the method for breeding to full genus.Secondly, preparation suitable culture base is with the required bacterium of enlarged culturing.Because metallurgical bacterium mostly is autotroph, generally need do not add the phosphorus source in the substratum, but need to add sulfuric acid amine or saltpetre, potassiumphosphate, sal epsom, ferric sulfate, sulphur etc. as N and mineral origin.The pH of substratum is advisable with 3～4.Culture temperature is 30 ℃～35 ℃.Must ventilate in the culturing process in order to breeding.
Printed-wiring board (PWB) (PCB) is one of basic element of character of electronic product composition, along with rolling up of electronic product demand, has produced a large amount of abandoned printed circuit boards, and also can produce a large amount of scrap stock in the printed-wiring board (PWB) production process.If these discarded circuit boards do not pass through appropriate processing, after the harmful element that contains when the inside enters environment, will influence local resident's health and wellbeing.Simultaneously contain a large amount of useful resources in the discarded circuit board, contain the metal about 40% usually, about 30% Plastic Resin and about 30% oxide compound (pressing mass ratio).Wherein metal Cu is a major ingredients, can account for 15～25% of discarded circuit board.Therefore the processing to discarded circuit board promptly has good economic benefits, has good society and environmental benefit again.
At present, the treatment process of discarded circuit board mainly contains technology such as mechanical treatment process, method of chemical treatment, pyrogenic attack method, pyrolysis processing method.But the existence that these treatment processs have investment is big, easily produce poisonous, harmful the like waste in the operating process.And all be that metal is recycled usually, and with direct landfill of other residuum or burning, the resource that causes in the discarded circuit board to be contained can not get well utilizing fully.
Therefore each state is all in the active research low cost, the resource recovery processing technique of green ecological.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art, a kind of green ecology synthesis recycling processing method of discarded circuit board is provided.
Purpose of the present invention can reach by following measure:
A kind of comprehensive resources treatment method of waste circuit board may further comprise the steps:
The little spirillum of thiobacillus ferrooxidant, iron protoxide or the sulfolobus solfataricus bacterium liquid of A, inoculation process domestication in culture medium solution, inoculum size is 5～15% of a culture medium solution volume, stir culture is 1～3 day under the speed of 80～120r/min, become reddish-brown until solution, redox potential is 550～650mV, and the amount of surveying microorganism in the bacterium liquid of biomass gained with fat phosphorus method is 2～10nmol P/mL;
After B, the wiring board substrate that will remove various components and parts are pulverized, cultivate the bacterium liquid that obtains to wherein adding above-mentioned steps, agitation leach is 10～15 days under the speed of 120～160r/min, is stabilized between 350～450mV separating liquid and solid to the redox potential of solution;
C, the liquid that above-mentioned steps is obtained extract with copper extractant, with the copper bearing copper extraction liquid that extraction obtains, strip with reverse-extraction agent, and the cupric strip liquor that obtains is carried out electrolytic deposition, get final product metallic copper;
D, the solid that obtains among the step B added Resins, epoxy and the solidifying agent of 5～25wt%, fully be filled in the forming mould behind the stirring and evenly mixing, and apply the compacting of 60～100MPa pressure, and moving in the baking oven and stablize 3～5h under 40～60 ℃, cooling back die sinking promptly obtains the material of construction of moulding.
Every liter of above-mentioned culture medium solution form and content is:
(NH
4)
2SO
4 2.5～3.0g，FeSO
4·7H
2O 10～44.3g，K
2HPO
4 0.2～0.5g，
MgSO
4·7H
2O 0.4～0.5g，Ca(NO
3)
2 0.01～0.02g，KCl 0.05～0.1g，
H
2O 1L。
The pH of above-mentioned culture medium solution is 1.5～2.5, with the H of 5mol/L
2SO
4Regulate.
The little spirillum of thiobacillus ferrooxidant, iron protoxide of above-mentioned process domestication or the acclimation method of sulfolobus solfataricus are: add CuSO earlier in the liquid nutrient medium of having inoculated thiobacillus ferrooxidant, the little spirillum of iron protoxide or sulfolobus solfataricus
45H
2O cultivates, when solution become by blue-greenish colour blackish green after, the bacterium of the above-mentioned domestication of renewed vaccination, and increase CuSO
45H
2The dosage of O shifts domestication repeatedly by above-mentioned steps and cultivates, and can adapt to 6～50gCu until bacterium
2+The culture environment of/L, preferred 6～20gCu
2+/ L, most preferably 6～15gCu
2+The culture environment of/L.
Thiobacillus ferrooxidant, the little spirillum of iron protoxide or the sulfolobus solfataricus temperature when cultivating, taming and leaching is 30 ℃～35 ℃.
Among the above-mentioned steps C, after the liquid that separation obtains extracted with copper extractant, remaining liquid can be used for cultivating in the steps A bacterium of taming.
Described copper extractant is Li * 64 of Henkel Corp., and its main component is 2-hydroxyl-5-dodecyl diphenylketoxime, and strippant is a waste solution of copper electrolysis, is remaining liquid behind the electro deposited copper, mainly is strong acid, and as sulfuric acid, content is more than 200g/L.It can reuse.
Among the above-mentioned steps B, solid that separation obtains and solidifying agent and the Resins, epoxy of 5～25%wt, can also add glue crosslinking agent and cement, after mixing stirs evenly, be filled in the forming mould, and apply the compacting of 60～100MPa pressure, and moving in the baking oven and stablize 3～5h under 40～60 ℃, cooling back die sinking promptly obtains the material of construction of moulding.
Purpose of the present invention specifically can reach by following measure:
A kind of comprehensive resources treatment method of waste circuit board specifically may further comprise the steps:
A. little spirillum of thiobacillus ferrooxidant, iron protoxide or the sulfolobus solfataricus that metal Cu uses in the discarded circuit board leached in domestication, adds CuSO in the liquid nutrient medium of inoculated bacteria
45H
2O, when solution become by blue-greenish colour blackish green after, the bacterium after the renewed vaccination domestication, and increase CuSO
45H
2The dosage of O is cultivated through shifting domestication for several times, makes the bacterium of leaching usefulness to adapt to and contains high density Cu ionic culture environment, as 6～20gCu
2+/ L, best 6～15gCu
2+/ L.
B. fill that inoculation is through the bacterium of domestication in the 1# container of culture medium solution, inoculum size is 5～15% (volume ratios), and solution is stirred, and agitation speed is 80～120r/min, cultivates 2 days, and solution becomes reddish-brown at this moment.Fe in the solution
2+Substantially with Fe
3+Form exist, the amount of microorganism is 2～10n mol P/mL in the bacterium liquid that records with fat phosphorus method, utilizing the redox potential of the solution that oxidation-reduction potentiometer records is 550～650mV;
C. remove the various components and parts on the discarded circuit board, substrate is pulverized, put into the 2# container, the cultured nutrient solution in the 1# container is got in the 2# container with pump.
D.2# the agitation speed of container solution is 120～160r/min, and the residence time is 10～15 days, is stabilized in 350～450mV to the redox potential of solution.
E. with solid and liquid separation in the 2# container, liquid is extracted with copper extractant, with the extraction after the cupric extraction liquid carry out back extraction copper with reverse-extraction agent, the cupric strip liquor is carried out electrolytic deposition, get final product metallic copper.
F. the liquid through after the Cu extraction of 2# container is returned in the 1# container with pump, and the thiobacillus ferrooxidant of inoculation domestication.
G. isolated solid (main component is a fortified resin, glass fibre) adds 5～25% Resins, epoxy, solidifying agent in the 2# container, can also add cementing agent, cement etc., and abundant stirring and evenly mixing.
H. the solid with mixing is filled in the forming mould, and applies the pressure of 60～100MPa, with the solid compacting of mixing.
I. forming mould is put into the baking oven that sets temperature (40～60 ℃) and stablized 3～5 hours, cooling back die sinking and can obtain the material of construction of moulding.
The pH of nutrient solution is 1.5～2.5, with the H of 5mol/L
2SO
4Regulate, the temperature when cultivating thiobacillus ferrooxidant, little spirillum of iron protoxide or sulfolobus solfataricus bacterium liquid and utilizing thiobacillus ferrooxidant bacterium liquid to leach metal Cu in the discarded circuit board remains between 30～35 ℃.
The nutrient solution prescription of thiobacillus ferrooxidant is:
| (NH 4) 2SO 4 | KCl | K 2HPO 4 | MgSO 4·7H 2O | Ca(NO 3) 2 | FeSO 4·7H 2O | H 2O | |
| Nutrient solution | 2.5～3.0g | 0.05～0.1g | 0.2～0.5g | 0.4～0.5g | 0.01～0.02g | 10～44.3g | 1L |
Present method two stages of adopting are leached the metal Cu in the discarded circuit board, and promptly the fs is cultivated thiobacillus ferrooxidant liquid, and thiobacillus ferrooxidant is through domestication, and subordinate phase utilizes thiobacillus ferrooxidant liquid to leach metal Cu in the discarded circuit board.
In leaching discarded circuit board during metal Cu, select suitable extraction agent to extract Cu in the subordinate phase leach liquor in present method
2+, and with extracting Cu
2+After contain Fe
2+, Fe
3+Plasma solution reuse is again cultivated the nutrient solution of thiobacillus ferrooxidant bacterium liquid as the fs.
To add Resins, epoxy and solidifying agent etc. in the residual solids of utilizing after thiobacillus ferrooxidant is leached Cu in present method, by hot-forming manufacturing material of construction, wherein the addition of Resins, epoxy, solidifying agent, cementing agent, cement etc. is moderate, will be to the abundant stirring and evenly mixing of mixture, and under suitable temperature and pressure, keep certain hour hot-forming.
The present invention uses for reference the principle of microorganism hydrometallurgy, utilizes thiobacillus ferrooxidant to leach the metal Cu that reclaims in the discarded circuit board, simultaneously the residual solids behind the leaching Cu is carried out resource utilization, has realized the complete comprehensive resource of discarded circuit board is handled.In treating processes, because the effect of domestication thiobacillus ferrooxidant etc. is with Fe
2+Change Fe into
3+, while Fe
3+Metal Cu in the discarded circuit board is oxidized to Cu
2+Enter into solution, Fe
3+Be reduced to Fe
2+, to leach liquor by extracting-back extraction get-electrodeposition can obtain metal Cu.Through containing required Fe, N, the P plasma of thiobacillus ferrooxidant growth in the solution after the extraction, can after cultivating, can be reused for the metal Cu that leaches in the discarded circuit board again by inoculating the thiobacillus ferrooxidant after domestication.Reach the recycle that contains Fe, N, the isoionic solution of P, need not extraneous pharmaceutical chemicals and the reagent that adds other.Leach the back and in the residual solids of separating, add Resins, epoxy, solidifying agent, cementing agents etc. directly are molded into the material of construction with property.
Present method has realized whole recycling treatment to discarded circuit board, and not to environmental emission waste water, waste residue or waste gas have been realized the cleaner production of whole process.Advantages such as therefore the technology of the present invention has less investment, cost is low, metal recovery rate is high, pollution-free, green ecological have good society, economy and environmental benefit.
Description of drawings
Fig. 1 is a concrete grammar schematic flow sheet of the present invention.
Embodiment
Example 1:
A. the thiobacillus ferrooxidant that metal Cu uses in the discarded circuit board is leached in domestication, adds CuSO in the 9K liquid nutrient medium of the inoculation thiobacillus ferrooxidant substratum of the formulated among the present invention (promptly with)
45H
2O, when solution become by blue-greenish colour blackish green after, the thiobacillus ferrooxidant after the renewed vaccination domestication, and increase CuSO
45H
2The dosage of O is cultivated through shifting domestication for several times, makes the thiobacillus ferrooxidant of leaching usefulness to adapt to and contain high density Cu ionic culture environment that its tolerance degree reaches 6～8gCu
2+/ L.
B. fill that (volume is 4L) inoculation is through the thiobacillus ferrooxidant liquid of domestication in the 1# container of 9K culture medium solution, inoculum size is 10% (volume ratio), and solution is stirred, and agitation speed is 100r/min, cultivates 2 days, and solution becomes reddish-brown at this moment.Iron ion is substantially with Fe in the solution
3+Form exist, the amount of microorganism is 6n mol P/mL in the bacterium liquid that records with fat phosphorus method, utilizes the redox potential of the solution that oxidation-reduction potentiometer records to be 600mV;
C. remove the various components and parts on the discarded circuit board, substrate is pulverized, be weighed as 120g, put into 2# container (volume is 4L), the cultured nutrient solution in the 1# container is got in the 2# container with pump.
D.2# the agitation speed of solution is 120r/min in the container, and the residence time is 14 days, is stabilized in 410～440mV to the redox potential of solution.
E. with solid and liquid separation in the 2# container, be 98.9% through measuring the leaching yield that calculates Cu in the powder.Liquid is extracted with copper extractant, the cupric extraction liquid after the extraction can be obtained metallic copper through back extraction-electrodeposition.
F. will return in the 1# container with pump through the liquid after the Cu extraction in the 2# container.And the thiobacillus ferrooxidant of inoculation domestication.
G. isolated solid (main component is a fortified resin, glass fibre) adds 20g Resins, epoxy and 15g solidifying agent in the 2# container, and abundant stirring and evenly mixing.
H. the solid with mixing is filled in the forming mould, and applies the pressure of 60MPa, with the solid compacting of mixing.
I. forming mould being put into temperature is set is that 45 ℃ baking oven was stablized 3 hours, cools off that die sinking can obtain New Building Materials after 10 hours, and its folding strength has reached 0.71MPa, and ultimate compression strength is 304.3MPa.
Example 2:
A. the thiobacillus ferrooxidant that metal Cu uses in the discarded circuit board is leached in domestication, adds CuSO in the 9K liquid nutrient medium of inoculation thiobacillus ferrooxidant
45H
2O, when solution become by blue-greenish colour blackish green after, thiobacillus ferrooxidant after the renewed vaccination domestication, and the dosage of increase CuSO45H2O, cultivate through shifting domestication for several times, make the thiobacillus ferrooxidant of leaching usefulness to adapt to and contain high density Cu ionic culture environment, its tolerance degree reaches 10～13g Cu
2+/ L.
B. fill that (volume is 4L) inoculation is through the oxidation industry iron thiobacillus liquid of domestication in the 1# container of 9K culture medium solution, inoculum size is 14% (volume ratio), and solution is stirred, and agitation speed is 80r/min, cultivates 1 day, and solution becomes reddish-brown at this moment.Iron ion is substantially with Fe in the solution
3+Form exist, the amount of microorganism is 8n mol P/mL in the bacterium liquid that records with fat phosphorus method, utilizes the redox potential of the solution that oxidation-reduction potentiometer records to be 580mV;
C. remove the various components and parts on the discarded circuit board, substrate is pulverized, be weighed as 160g, put into 2# container (volume is 4L), the cultured nutrient solution among the container 1# is got in the 2# container with pump.
D.2# the agitation speed of container solution is 150r/min, and the residence time is 12 days, is stabilized in 430～450mV to the redox potential of solution.
E. with solid in the 2# container and liquid separation, be 99.5% through measuring the leaching yield that calculates Cu in the powder.Liquid is extracted with copper extractant, the cupric extraction liquid after the extraction can be obtained metallic copper through back extraction-electrodeposition.
F. the liquid through after the Cu extraction of 2# container is returned in the 1# container with pump.And the thiobacillus ferrooxidant of inoculation domestication.
G. isolated solid (main component is a fortified resin, glass fibre) adds 25g Resins, epoxy and 20g solidifying agent in the 2# container, and abundant stirring and evenly mixing.
H. the solid with mixing is filled in the forming mould, and applies the pressure of 70MPa, with the solid compacting of mixing.
I. forming mould being put into temperature is set is that 55 ℃ baking oven was stablized 4 hours, cools off that die sinking can obtain New Building Materials after 10 hours, and its folding strength has reached 0.63MPa, and ultimate compression strength is 260.3MPa.
Example 3:
A. the little spirillum of iron protoxide that metal Cu uses in the discarded circuit board is leached in domestication, adds CuSO in the 9K liquid nutrient medium of the little spirillum of the inoculation iron protoxide substratum of the formulated among the present invention (promptly with)
45H
2O, when solution become by blue-greenish colour blackish green after, the little spirillum of iron protoxide after the renewed vaccination domestication, and increase CuSO
45H
2The dosage of O is cultivated through shifting domestication for several times, makes the little spirillum of iron protoxide of leaching usefulness to adapt to and contain high density Cu ionic culture environment that its tolerance degree reaches 12～15g Cu
2+L.
B. fill that (volume is 4L) inoculation is through the little spirillum bacterium of the iron protoxide liquid of domestication in the 1# container of 9K culture medium solution, inoculum size is 5% (volume ratio), and solution is stirred, and agitation speed is 120r/min, cultivates 3 days, and solution becomes reddish-brown at this moment.Iron ion is substantially with Fe in the solution
3+Form exist, the amount of microorganism is 7n mol P/mL in the bacterium liquid that records with fat phosphorus method, utilizes the redox potential of the solution that oxidation-reduction potentiometer records to be 640mV;
C. remove the various components and parts on the discarded circuit board, substrate is pulverized, be weighed as 110g, put into 2# container (volume is 4L), the cultured nutrient solution in the 1# container is got in the 2# container with pump.
D.2# the agitation speed of solution is 160r/min in the container, and the residence time is 10 days, is stabilized in 360～400mV to the redox potential of solution.
E. with solid and liquid separation in the 2# container, be 99.1% through measuring the leaching yield that calculates Cu in the powder.Liquid is extracted with copper extractant, the cupric extraction liquid after the extraction can be obtained metallic copper through back extraction-electrodeposition.
F. will return in the 1# container with pump through the liquid after the Cu extraction in the 2# container.And the little spirillum of iron protoxide of inoculation domestication.
G. isolated solid (main component is a fortified resin, glass fibre) adds 20g Resins, epoxy, 10g solidifying agent and 5g glue crosslinking agent in the 2# container, and abundant stirring and evenly mixing.
H. the solid with mixing is filled in the forming mould, and applies the pressure of 90MPa, with the solid compacting of mixing.
I. forming mould being put into temperature is set is that 40 ℃ baking oven was stablized 5 hours, cools off that die sinking can obtain New Building Materials after 10 hours, and its folding strength has reached 0.70MPa, and ultimate compression strength is 300.7MPa.
Claims (7)
1, a kind of comprehensive resources treatment method of waste circuit board is characterized in that may further comprise the steps:
The little spirillum of thiobacillus ferrooxidant, iron protoxide or the sulfolobus solfataricus bacterium liquid of A, inoculation process domestication in culture medium solution, inoculum size is 5～15% of a culture medium solution volume, stir culture is 1～3 day under the speed of 80～120r/min, become reddish-brown until solution, between 2～10n mol P/mL, redox potential is 550～650mV to the amount of microorganism in fat phosphorus;
After B, the wiring board substrate that will remove various components and parts are pulverized, cultivate the bacterium liquid that obtains to wherein adding above-mentioned steps, agitation leach is 10～15 days under the speed of 120～160r/min, is stabilized between 350～450mV separating liquid and solid to the redox potential of solution;
C, the liquid that above-mentioned steps is obtained extract with copper extractant, with the copper bearing copper extraction liquid that extraction obtains, strip with reverse-extraction agent, and the cupric strip liquor that obtains is carried out electrolytic deposition, get final product metallic copper;
D, the solid that obtains among the step B added Resins, epoxy and the solidifying agent of 5～25wt%, fully be filled in the forming mould behind the stirring and evenly mixing, and apply the compacting of 60～100MPa pressure, and moving in the baking oven and stablize 3～5h under 40～60 ℃, cooling back die sinking promptly obtains the material of construction of moulding.
2, method according to claim 1 is characterized in that every liter of described culture medium solution forms and content is:
(NH
4)
2SO
4 2.5～3.0g，FeSO
4·7H
2O 10～44.3g，K
2HPO
4 0.2～0.5g，
MgSO
4·7H
2O 0.4～0.5g，Ca(NO
3)
2 0.01～0.02g，KCl 0.05～0.1g，
H
2O 1L。
3, method according to claim 1 and 2, the pH that it is characterized in that described culture medium solution is 1.5～2.5, with the H of 5mol/L
2SO
4Regulate.
4, method according to claim 1 is characterized in that the little spirillum of thiobacillus ferrooxidant, iron protoxide of described process domestication or the acclimation method of sulfolobus solfataricus are: add CuSO earlier in the liquid nutrient medium of having inoculated thiobacillus ferrooxidant, the little spirillum of iron protoxide or sulfolobus solfataricus bacterium liquid
45H
2O cultivates, when solution become by blue-greenish colour blackish green after, the bacterium of the above-mentioned domestication of renewed vaccination, and increase CuSO
45H
2The dosage of O shifts domestication repeatedly by above-mentioned steps and cultivates, and can adapt to 6～20gCu until bacterium
2+The culture environment of/L.
5,, it is characterized in that the temperature of bacterium when cultivating, taming and leaching is 30～35 ℃ according to claim 1 or 4 described methods.
6, method according to claim 1 is characterized in that among the step C, and after the liquid that separation obtains extracted with copper extractant, remaining liquid was used for the bacterium that steps A is cultivated the process domestication.
7, method according to claim 1 is characterized in that described copper extractant is 2-hydroxyl-5-dodecyl diphenylketoxime, and strippant is a waste solution of copper electrolysis.
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|---|---|---|---|
| CNB200610097382XA CN100510126C (en) | 2006-11-02 | 2006-11-02 | Comprehensive resources treatment method of waste circuit board |
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|---|---|---|---|
| CNB200610097382XA CN100510126C (en) | 2006-11-02 | 2006-11-02 | Comprehensive resources treatment method of waste circuit board |
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| CN100510126C CN100510126C (en) | 2009-07-08 |
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| CN102091711A (en) * | 2010-12-14 | 2011-06-15 | 惠州市雄越保环科技有限公司 | Device for recycling waste printed circuit board |
| CN102206751A (en) * | 2011-04-29 | 2011-10-05 | 常州纺织服装职业技术学院 | Method for continuously recovering copper from printed circuit boards by microbial metabolites under action of micro electric field |
| CN102218437A (en) * | 2011-05-05 | 2011-10-19 | 广州有色金属研究院 | Recovery method for waste circuit board |
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| CN105032899A (en) * | 2015-08-07 | 2015-11-11 | 周群刚 | Waste circuit board resource utilization process |
| CN105420500A (en) * | 2015-11-10 | 2016-03-23 | 森蓝环保(上海)有限公司 | Method for separating and extracting all metal components from waste printed circuit boards through wet metallurgy |
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| CN102206751B (en) * | 2011-04-29 | 2013-10-02 | 常州纺织服装职业技术学院 | Method for continuously recovering copper from printed circuit boards by microbial metabolites under action of micro electric field |
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| CN102218437B (en) * | 2011-05-05 | 2013-02-06 | 广州有色金属研究院 | Recovery method for waste circuit board |
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