CN104726714B - Method for leaching copper in waste printed circuit board by using mixed bacteria - Google Patents
Method for leaching copper in waste printed circuit board by using mixed bacteria Download PDFInfo
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- 239000010949 copper Substances 0.000 title claims abstract description 75
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 57
- 241000894006 Bacteria Species 0.000 title claims abstract description 56
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 49
- 238000002386 leaching Methods 0.000 title claims abstract description 38
- 239000002699 waste material Substances 0.000 title abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 81
- 150000003071 polychlorinated biphenyls Chemical class 0.000 claims abstract description 73
- 241000605222 Acidithiobacillus ferrooxidans Species 0.000 claims abstract description 13
- 238000007792 addition Methods 0.000 claims description 38
- 235000015097 nutrients Nutrition 0.000 claims description 37
- 239000007788 liquid Substances 0.000 claims description 18
- 239000002054 inoculum Substances 0.000 claims description 16
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 14
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 12
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 10
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 8
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 8
- 238000004070 electrodeposition Methods 0.000 claims description 8
- 238000011084 recovery Methods 0.000 claims description 8
- 239000010865 sewage Substances 0.000 claims description 8
- 230000001580 bacterial effect Effects 0.000 claims description 7
- 239000001103 potassium chloride Substances 0.000 claims description 7
- 235000011164 potassium chloride Nutrition 0.000 claims description 7
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- 238000005273 aeration Methods 0.000 claims description 6
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 6
- 239000001110 calcium chloride Substances 0.000 claims description 6
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 6
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims description 6
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 6
- 239000010802 sludge Substances 0.000 claims description 6
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 241000266272 Acidithiobacillus Species 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000012263 liquid product Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 238000011534 incubation Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims 2
- 230000012010 growth Effects 0.000 abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 8
- 241000605272 Acidithiobacillus thiooxidans Species 0.000 abstract description 7
- 230000005764 inhibitory process Effects 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 19
- 229910052751 metal Inorganic materials 0.000 description 10
- 239000002184 metal Substances 0.000 description 10
- 238000000605 extraction Methods 0.000 description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000011575 calcium Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- FRXSZNDVFUDTIR-UHFFFAOYSA-N 6-methoxy-1,2,3,4-tetrahydroquinoline Chemical compound N1CCCC2=CC(OC)=CC=C21 FRXSZNDVFUDTIR-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 241001052560 Thallis Species 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000011953 bioanalysis Methods 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229910000396 dipotassium phosphate Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229910052564 epsomite Inorganic materials 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 235000016709 nutrition Nutrition 0.000 description 2
- 230000001698 pyrogenic effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- -1 2- hydroxyl -5- dodecyl diphenyl-ketoximes Chemical class 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 241000605008 Spirillum Species 0.000 description 1
- 241000205091 Sulfolobus solfataricus Species 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 238000012364 cultivation method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000010792 electronic scrap Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012737 fresh medium Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910052603 melanterite Inorganic materials 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000011548 physical evaluation Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 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
- Micro-Organisms Or Cultivation Processes Thereof (AREA)
- Purification Treatments By Anaerobic Or Anaerobic And Aerobic Bacteria Or Animals (AREA)
Abstract
The invention discloses a method for leaching copper in a waste printed circuit board by using mixed bacteria, which comprises the steps of pretreating the waste Printed Circuit Board (PCBs) for later use, respectively carrying out copper-resistant domestication culture on acidithiobacillus ferrooxidans and acidithiobacillus thiooxidans, and then carrying out mixed culture in a mixed bacteria culture solution; and (3) beginning to add PCBs powder when the culture time reaches 40-55 h, and then adding PCBs powder point by point at other time points for bioleaching. The mixed bacteria can grow evenly without adjusting the pH value of the culture solution during culture, and simultaneously, a large amount of sulfuric acid and Fe are generated during growth of the two bacteria3+The method is used for leaching copper in the later-stage waste PCBs powder, the efficiency of the whole process is high, and energy is saved. By adopting a mode of multi-point addition with low front and high back, on the basis of increasing the addition of the waste PCBs powder, the copper leaching rate is obviously improved, and the inhibition degree of the thallus growth is relatively small.
Description
The application is Application No. 201310457250.3, and the applying date is September in 2013 30, and invention and created name is
The divisional application of the application for a patent for invention of " method of copper in Mixed Microbes leaching discarded printed circuit boards ".
Technical field
The present invention relates to a kind of recovery method of copper in discarded printed circuit boards, and in particular to a kind of Mixed Microbes leaching is discarded
The method of copper in printed circuit board (PCB).
Background technology
With information technology fast development, electron wastes (Waste Electric and Electronic
Equipment, WEEE) yield constantly rises, and discarded printed circuit boards (Printed Circuit Boards, PCBs) are made
It is WEEE important components, usually contains 40% or so metal, wherein metallic copper is main composition, and content is up to 20%~30%.
According to estimates, China needs treatment PCBs to increase about more than 500,000 tons and with 22% speed every year.If realizing discarded PCB
Treatment and recovery, can solve problem of environmental pollution, can realize that metal is effectively reclaimed again, by holding to China's PCBs industries
Supervention opens up important in inhibiting.
The method for extracting copper from discarded printed circuit boards at present mainly has Physical, chemical method and bioanalysis.Physical
Evaluation index is higher in terms of regenerated resources effect, the friendly property of environment, commercial Application rate, but the plant equipment for being used is invested
Greatly, energy-output ratio is high, maintenance cost is high, thus economic feasibility is relatively poor；And be difficult between metal separate in product.
Chemical method is broadly divided into pyrogenic process and wet method, although pyrogenic process has the advantages that simple, the convenient and rate of recovery is high, can produce simultaneously
The shortcomings of evil gas, discharge a large amount of scum silica frost；Wet method have waste gas discharge it is few, extract copper after residue be easily handled and technique letter
Single the advantages of, but copper extraction rate is low and leachate and residue have toxicity.Therefore will pollution less, low cost, reaction condition temperature
The bioanalysis of sum has unique advantage in being applied to discarded printed circuit boards metal recovery.
The features such as copper in bioleaching PCBs has safe and clean, efficient, it has also become domestic and international study hotspot.At present
Using most common microorganism be Acidithiobacillus thiooxidans (A.t) and Thiobacillus ferrooxidans (A. f)。
Such as Zhou Peiguo etc.（The such as Zhou Peiguo, Zheng Zheng, Peng Xiaocheng copper leaching from printed circuit board by Thiobacillus ferrooxidans and process
The Changeement of middle iron《Environmental Pollution and Control》；2007（02）：119~122）It is discarded using Thiobacillus ferrooxidans leaching
Circuit board powder（Copper mass fraction is 10.4%）In copper, when waste printed circuit board powder addition be 100 g/L when, 15d or so
Copper extraction rate is about 90%.
The A of Chinese patent literature CN 1948524（Application number 200610097382.X）Disclose a kind of waste printed circuit board comprehensive
Close recycling processing method, in culture medium solution be inoculated with by domestication Thiobacillus ferrooxidans, the micro- spirillum of ferrous oxide or
Sulfolobus solfataricus bacterium solution is cultivated, and after eliminating the circuit board substrate crushing of various components, is added thereto to culture and is obtained
Bacterium solution, leaching 10~15 days under the speed of 120~160r/min, separate liquid and solid；Liquid copper extractant
Extracted, then be stripped and electrolytic deposition obtains metallic copper.
The above method is to carry out bioleaching using single microorganism, and its metal extraction time is long, and leaching efficiency is low.
Research shows that copper is current most efficient method in Mixed Microbes leaching PCBs.
Such as SADIA etc.（ Sadia I, Munir AA, Shahida BN, Afzal Ghauri M.
Bioleaching of metals from electronic scrap by moderately thermophilic
acidophilic bacteria. Hydrometallurgy 2007;88:180–8.）It is useless using the leaching of middle temperature acidophilus Mixed Microbes
Abandon circuit board powder（Copper mass fraction is 8.5%）In metal, when waste printed circuit board powder addition be 10g/L when, after 18d
The extraction rate of copper is 89%.But although the Mixed Microbes leaching method has used Mixed Microbes, but leaching time is long, extraction rate not
Such as a kind of efficiency high of bacterial leaching.When this is due to multi strain co cultivation, there is provided which type of nutritional substrate and external condition make
Mixed Microbes energy uniform growth, is suppressed phenomenon most important from another bacterium without a kind of excessive multiplication.Additionally, thin
Bacterium leaching copper ability is closely related with its own growth metabolism, bacteria growing inhibiting is understood in PCBs adding procedures and then causes copper to soak
Ability decline is taken, thus how to optimize PCBs addition manners is the another key factor for realizing copper in the efficient leaching PCBs of Mixed Microbes
One of.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of multi strain co cultivation method and discarded print are efficiently leached with it
The method of copper in printed circuit board.
The technical scheme for realizing the object of the invention is a kind of method of copper in Mixed Microbes leaching discarded printed circuit boards, including
Following steps：
1. the pretreatment of discarded printed circuit boards；The discarded printed circuit boards PCBs that electronic component will have been removed is crushed and ground
Clay into power, the discarded printed circuit boards powder sieving that grinding is obtained, collection is treated by the discarded printed circuit boards powder of sieve aperture
Treatment.
2. tamed strain；By Acidithiobacillus ferrooxidans strain GFA.ferrooxidansAnd Acidithiobacillus thiooxidansA.thiooxidansResistance to Cu is carried out respectively2+Domestication culture, domestication end respectively obtain resistance to 100~200mmol/L Cu2+Ring
BorderA.ferrooxidansWithA.thiooxidansIt is stand-by.
3. multi strain co cultivation；2. step is tamed what is obtained after cultivatingA.ferrooxidansWithA.thiooxidansPress
Multi strain co cultivation is carried out in multi strain co cultivation liquid for 1: 1.5~2.5 according to inoculum concentration, and it is 1.5~1.8 to cultivate initial pH, is mixed
It is the 10%~20% of multi strain co cultivation liquid product to close bacterium inoculum concentration.
4. the addition of discarded printed circuit boards powder；Treat that 3. the multi strain co cultivation time reaches 40~55 hours, first to step
It is secondary add step 1. to pre-process the discarded PCBs powder for obtaining in the multi strain co cultivation system of 40~55 hours to have cultivated, then
Every 20~25 hours again to multi strain co cultivation system in add step 1. to pre-process the discarded PCBs powder that obtains, after once
The discarded PCBs powder for adding once increases by 1~3g/L, the discarded PCBs powder added in 1L multi strain co cultivation systems compared to preceding
The gross mass at end is 28g~36g；When discarded PCBs powder finishes bacterium incubation time arrival 175h~200h to be mixed, Mixed Microbes
Leaching reaction terminates；Reacted mixed material is centrifuged, upper strata leachate is collected.
5. post-process；The leachate that 4. step obtains is extracted with copper extractant, for the cupric extract for obtaining,
It is stripped with strippant；Then the cupric strip liquor that will be obtained is transferred in electrolytic cell and carries out electrodeposition and obtain copper, completes
The recovery of copper in discarded printed circuit boards.
Above-mentioned steps 3. multi strain co cultivation when, the content of each component is in multi strain co cultivation liquid used：Elemental sulfur 4.0~
6.5g/L, 3.5~4.5g/L of ammonium sulfate, the g/L of dipotassium hydrogen phosphate 0.45~0.65, bitter salt 0.45~0.65
G/L, the g/L of potassium chloride 0.1~0.15, calcium nitrate 0.008~0.015 g/L, 15~18g/L of green vitriol, chlorine
Change the g/L of calcium 0.10~0.18；Multi strain co cultivation liquid solute is water.
As preferred, step 3. multi strain co cultivation when, the content of each component is in multi strain co cultivation liquid used：Simple substance
5.2~5.6g/L of sulphur, 3.5~4.5g/L of ammonium sulfate, the g/L of dipotassium hydrogen phosphate 0.45~0.65, bitter salt 0.45
~0.65 g/L, the g/L of potassium chloride 0.1~0.15, the g/L of calcium nitrate 0.008~0.015, green vitriol 17~
17.5g/L, the g/L of calcium chloride 0.10~0.18；Multi strain co cultivation liquid solute is water.
When 4. above-mentioned steps discard the addition of PCBs powder, treat that 3. the multi strain co cultivation time reaches 40~55 hours step, to
1. addition step pre-processes the discarded PCBs powder for obtaining in having cultivated the multi strain co cultivation system of 40~55 hours, the mixing per 1L
The discarded PCBs powder of 4g~6g is added in bacterium cultivating system, the discarded PCBs powder of addition proceeds by Mixed Microbes leaching reaction；
After bacterium to be mixed continues to cultivate 20~25 hours, the discarded PCBs for obtaining 1. is pre-processed to second addition step in cultivating system
Powder, per 1L multi strain co cultivation systems in add the discarded PCBs powder of 6g~8g, the discarded PCBs powder of addition proceeds by mixed
Close bacterium leaching reaction；After bacterium to be mixed continues to cultivate 20~25 hours, 1. pre-processed to step is added in cultivating system for the third time
The discarded PCBs powder for obtaining, adds the discarded PCBs powder of 8g~10g, the discarded PCBs of addition in every 1L multi strain co cultivation systems
Powder proceeds by Mixed Microbes leaching reaction；After bacterium to be mixed continues to cultivate 20~25 hours, add to the 4th time in cultivating system
Plus 1. step pre-processes the discarded PCBs powder for obtaining, the discarded PCBs powder of 10g~12g is added in every 1L multi strain co cultivation systems
End, discarded PCBs powder addition is finished.
Above-mentioned steps are 2.A.ferrooxidansWhen carrying out domestication culture, will be carried from the aeration tank of municipal sewage plant
The sludge enrichment culture for taking, is then peeled off purifying and obtainingA.ferrooxidans；WillA.ferrooxidansIn 9K nutrient solutions
It is middle to cultivate to logarithmic phase；It is 10%~20% according to strain inoculum concentration（Volume ratio v/v）, draw above-mentioned bacterium solution and be transferred to Cu2+It is dense
Spend in the nutrient solution for 10mmol/L；It is 10%~20% according to strain inoculum concentration after culture to logarithmic phase（Volume ratio v/v）, inhale
Take above-mentioned bacterium solution and be transferred to Cu2+Concentration for 20mmol/L nutrient solution in cultivate to logarithmic phase；Aforesaid operations are repeated, is often increased
The domestication of generation bacterial strain, Cu in nutrient solution used2+Concentration increase 10mmol/L compared to previous generation, so as to obtaining 100~
200mmol/L Cu2+Cultivated in environment to logarithmic phaseA.ferrooxidans。
Above-mentioned steps are 2.A.thiooxidansWhen carrying out domestication culture, will be carried from the aeration tank of municipal sewage plant
The sludge enrichment culture for taking, is then peeled off purifying and obtainingA.thiooxidans；WillA.thiooxidansTrained in nutrient solution
Support to logarithmic phase；It is 10%~20% according to strain inoculum concentration（Volume ratio v/v）, draw above-mentioned bacterium solution and be transferred to Cu2+Concentration be
In the nutrient solution of 10mmol/L；It is 10%~20% according to strain inoculum concentration after culture to logarithmic phase（Volume ratio v/v）, in absorption
State bacterium solution and be transferred to Cu2+Concentration for 20mmol/L nutrient solution in cultivate to logarithmic phase；Aforesaid operations are repeated, often increases a generation
The domestication of bacterial strain, Cu in nutrient solution used2+Concentration increase 10mmol/L compared to previous generation, so as to obtaining 100~
200mmol/L Cu2+Cultivated in environment to logarithmic phaseA.thiooxidans。
The present invention has positive effect：
（1）The nutritional substrate and condition of culture of offer make Acidithiobacillus ferrooxidans strain GF when the present invention carries out multi strain co cultivation
(Acidithiobacillus.ferrooxidans, A.ferrooxidans) and Acidithiobacillus thiooxidans
(Acidithiobacillus. thiooxidans, A.thiooxidans) two kinds of bacterium energy uniform growths, it is a kind of without occurring
Bacterium excessive multiplication and another bacterium is suppressed phenomenon.Additionally, present invention optimizes the addition manner of discarded PCBs powder, using preceding
The mode of low rear multiple spot addition high, on the basis of discarded PCBs additions are improved, copper extraction rate is significantly improved and thalli growth
Suppressed degree is relatively small.
（2）The present invention uses multi strain co cultivation, and two kinds of bacterium of pH of nutrient solution need not be adjusted during culture with regard to energy uniform growth,
Simultaneously a large amount of sulfuric acid and Fe are generated during two kinds of bacteria growings3+For the leaching of copper in later stage discarded PCBs powder, whole process efficiency
High, save energy.
（3）The present invention is right before bioleaching is carried outA.ferrooxidansWithA.thiooxidansCarry out at resistance to copper
Reason, significantly improves two kinds of resistance to copper of bacterium, promotes the leaching of copper in discarded PCBs powder.
（4）) whole process process is simple of the invention, economy, environmental protection, the need for meeting recycling economy development, with good
Good prospects for commercial application.
Specific embodiment
（Embodiment 1）
The method of copper is comprised the following steps in the Mixed Microbes leaching discarded printed circuit boards of the present embodiment：
1. the pretreatment of discarded printed circuit boards.The discarded printed circuit boards PCBs that electronic component will have been removed is crushed and ground
Clay into power, the discarded PCBs powder that grinding is obtained crosses 100 μm~200 μm of sieve aperture（What grinding was obtained in the present embodiment is discarded
Printed circuit board (PCB) powder crosses 100 μm of sieve aperture）, collect pending by the discarded PCBs powder of sieve aperture.
After the ground sievings of discarded PCBs of the present embodiment treatment, its major metal content is analyzed,
Major metal content is as shown in table 1 below：
Major metal content in the discarded printed circuit boards powder of table 1
2. tamed strain.
（1）Acidithiobacillus ferrooxidans strain GF（A.ferrooxidans）Domestication.By from the aeration of municipal sewage plant
The sludge enrichment culture extracted in pond, is then peeled off purifying and obtainingA.ferrooxidans；WillA.ferrooxidansIn 9K
Cultivated in nutrient solution to logarithmic phase, now bacteria concentration rises to 10 in bacterium solution7Cell/mL.
9K nutrient solutions used include per 1L：44.7g FeSO4·7H2O, 3.0g (NH4)2SO4, 0.5g K2HPO4,
0.5g MgSO4·7H2O, 0.1g KCl, 0.01g Ca (NO3)2, the pH value of nutrient solution is 2.00.
It is 10%~20% according to strain inoculum concentration（Volume ratio v/v）, draw above-mentioned bacterium solution and be transferred to and added 100mL fresh
In the 250mL conical flasks of nutrient solution, in 32 DEG C of temperature, shaking speed is 120~200r/min（It is 150 r/ in the present embodiment
min）Under the conditions of cultivate to logarithmic phase complete the first generation domestication.First generation domestication is usedA.fNutrient solution remaining cultivated with above-mentioned 9K
Liquid phase is same, and difference is that increased Cu in nutrient solution2+, Cu in nutrient solution2+Concentration be 10mmol/L.
It is 10%~20% according to strain inoculum concentration（Volume ratio v/v）, draw the bacterium solution after the domestication of the above-mentioned first generation to fresh
Cultivated in nutrient solution to logarithmic phase, Cu in this nutrient solution used2+Concentration rise to 20mmol/L.
Repeat aforesaid operations, bacterium solution is transferred to successively containing 30,40,50,60,70,80,90,100,110,120,130,
140th, 150,160,170,180,190 and 200mmol/L Cu2+Fresh medium in tame culture, culture terminate after, centrifugation
Removal supernatant, collects the Cu for being resistant to 200 mmol/L2+The thalline of concentration to put refrigerator stand-by.
During above-mentioned domestication, often increase the domestication of generation bacterial strain, Cu in nutrient solution used2+Concentration compare previous generation
Increase 10mmol/L.Due to Cu2+Concentration is raised, so cultivating to logarithmic phase（Bacteria concentration is 107Cell/mL）Required time meeting
It is more and more long.According to treatment powder situation, by Acidithiobacillus ferrooxidans strain GF 100 mmol/L Cu2+Concentration under cultivate
Domestication can also be stopped after to logarithmic phase, so as to obtain the Cu of resistance to 100 mmol/L2+ConcentrationA.ferrooxidans。
（2）Acidithiobacillus thiooxidans（A.thiooxidans）Domestication.By from the aeration tank of municipal sewage plant
The sludge enrichment culture of extraction（Sewage Plant processes sewage using A2/O）, it is then peeled off purifying and obtainingA.thiooxidans；WillA.thiooxidansCultivated in nutrient solution to logarithmic phase, now bacteria concentration rises to 10 in bacterium solution7Cell/mL.
Nutrient solution used includes per 1L：10.0g S0, 0.5g (NH4)2SO4, 0.25g K2HPO4, 0.25g
MgSO4·7H2O, 0.02g CaCl2·2H2O；The pH value of nutrient solution is 4.00.
It is 10%~20% according to strain inoculum concentration（Volume ratio v/v）, draw above-mentioned bacterium solution and be transferred to and added 100mL fresh
In the 250mL conical flasks of nutrient solution, in 32 DEG C of temperature, shaking speed is 120~200r/min（It is 150 r/ in the present embodiment
min）Under the conditions of cultivate to logarithmic phase obtain the first generation domestication Acidithiobacillus thiooxidans.
First generation domestication is usedA.tRemaining is identical with above-mentioned nutrient solution for nutrient solution, and difference is first generation domestication institute
WithA.tCu is increased in nutrient solution2+, Cu in nutrient solution2+Concentration be 10mmol/L.
According to（1）Middle Acidithiobacillus ferrooxidans strain GF（A.f）Acclimation method, bacterium solution is transferred to successively containing 20,30,40,
50th, 60,70,80,90,100,110,120,130,140,150,160,170,180,190 and 200mmol/L Cu2+It is fresh
Culture to logarithmic phase is tamed in nutrient solution, after culture terminates, centrifugation removal supernatant collects the Cu for being resistant to 200 mmol/L2+'s
It is stand-by that the thalline of concentration puts refrigerator.
According to the powder situation for the treatment of, willA.thiooxidansIn the Cu of 100 mmol/L2+Concentration under cultivate to logarithm
Domestication can also be stopped after phase, so as to obtain the Cu of resistance to 100 mmol/L2+ConcentrationA.thiooxidans。
During i.e. above-mentioned domestication, often increase the domestication of generation bacterial strain, Cu in nutrient solution used2+Concentration compare upper one
In generation, increases 10mmol/L.Due to Cu2+Concentration is raised, so cultivating to logarithmic phase（Bacteria concentration is 107Cell/mL）Required time
Can be more and more long.
3. multi strain co cultivation.2. step is tamed what is obtained after cultivatingA.ferrooxidansWithA.thiooxidansPress
According to inoculum concentration is 1: 1.5~2.5（It is 1: 2 in the present embodiment）Multi strain co cultivation is carried out in multi strain co cultivation liquid, culture is just
Beginning pH is 1.5~1.8（It is 1.6 in the present embodiment）, Mixed Microbes inoculum concentration is the 10%~20% of multi strain co cultivation liquid product.Mixing
32 DEG C of temperature is controlled when bacterium is cultivated, shaking speed is 120~200r/min（It is 150 r/min in the present embodiment）.
The content of each component is in multi strain co cultivation liquid：4.0~6.5g/L of elemental sulfur, 3.5~4.5g/L of ammonium sulfate,
The g/L of dipotassium hydrogen phosphate 0.45~0.65, the g/L of bitter salt 0.45~0.65, the g/L of potassium chloride 0.1~0.15, nitre
Sour calcium 0.008~0.015 g/L, 15~18g/L of green vitriol, the g/L of calcium chloride 0.10~0.18；Multi strain co cultivation
Liquid solute is water, and pH is 1.5~1.8.
The content of each component is in multi strain co cultivation liquid used in the present embodiment：Elemental sulfur 5.5g/L, ammonium sulfate 4.0
G/L, the g/L of dipotassium hydrogen phosphate 0.5, the g/L of bitter salt 0.5, the g/L of potassium chloride 0.1, calcium nitrate 0.01 g/L, seven
The g/L of ferrous sulfate hydrate 17.2, calcium chloride 0.13 g/L, pH are 1.6.
4. the addition of discarded printed circuit boards powder.Treat that 3. the multi strain co cultivation time reaches 48 hours step, to culture
Step is added 1. to pre-process the discarded PCBs powder for obtaining in the multi strain co cultivation system of 48 hours, per 1L multi strain co cultivation systems
The discarded PCBs powder of middle addition 4g, the discarded PCBs powder of addition proceeds by Mixed Microbes leaching reaction.
Bacterium to be mixed is cultivated during to 72 hours, continues 1. to pre-process the discarded PCBs for obtaining to addition step in cultivating system
Powder, adds the discarded PCBs powder of 6g in every 1L multi strain co cultivation systems, the discarded PCBs powder of addition proceeds by Mixed Microbes
Leaching reaction.
Bacterium to be mixed is cultivated during to 96 hours, continues 1. to pre-process the discarded PCBs for obtaining to addition step in cultivating system
Powder, adds the discarded PCBs powder of 8g in every 1L multi strain co cultivation systems, the discarded PCBs powder of addition proceeds by Mixed Microbes
Leaching reaction.
Bacterium to be mixed is cultivated during to 120 hours, continues 1. to pre-process obtain discarded to adding step in cultivating system
PCBs powder, per 1L multi strain co cultivation systems in add the discarded PCBs powder of 10g, the discarded PCBs powder of addition proceeds by mixed
Close bacterium leaching reaction.
Bacterium to be mixed continues to cultivate to 175h~200h（It is 180h in the present embodiment）When, Mixed Microbes leaching reaction terminates；
Cu, Ni, Zn, Pb leaching rate are respectively 97.3%, 92.5%, 93.4%, 89.6% in measuring discarded printed circuit boards powder.
Reacted mixed material is centrifuged, upper strata leachate is collected.Lower floor's solid can conduct after treatment
Construction material.
5. post-process.The leachate that 4. step obtains is extracted with copper extractant, for the cupric extract for obtaining,
It is stripped with strippant；Then the cupric strip liquor that will be obtained is transferred in electrolytic cell and carries out electrodeposition and obtain copper, completes
The recovery of copper in discarded printed circuit boards.
Anode is done using titanium plate during electrodeposition, copper coin does negative electrode.Control voltage is 2.0V, and current density is 350A/m2, pH value
It is 3, pole span is 1cm, the time is 3h, and temperature is 10 DEG C.
Copper extractant used is 2- hydroxyl -5- dodecyl diphenyl-ketoximes, and strippant is waste solution of copper electrolysis.
The rate of recovery of electro deposited copper is 99%.Reclaim copper and can reach national GB/T 6516-1997 standards.
In order to keep the basicly stable of electrodeposition condition, electrodeposition solution will constantly be circulated.The present embodiment is done using titanium plate
Anode can expeditiously deliver current to electrolyte and for anion electric discharge so that electrodeposition efficiency is improved.In addition, electrodeposition
The sulfuric acid produced during copper, recyclable recycling.
Two kinds of bacterium of pH of nutrient solution need not be adjusted during multi strain co cultivation of the present invention with regard to energy uniform growth, while two kinds of bacterium lifes
A large amount of sulfuric acid and Fe are generated when long3+For the leaching of copper in later stage discarded PCBs powder, whole process efficiency high, save energy.
In addition, present invention optimizes the addition manner of discarded PCBs powder, it is discarded improving by the way of the addition of low early and high after multiple spot
On the basis of PCBs powder additions, copper extraction rate is significantly improved and the suppressed degree of thalli growth is relatively small.
（Embodiment 2 is to embodiment 6）
In embodiment 2 to the Mixed Microbes leaching discarded printed circuit boards of embodiment 6 method of copper remaining with the phase of embodiment 1
Together, difference is：Step 3. multi strain co cultivation when multi strain co cultivation liquid used in each component content and step 4.
The addition time of discarded printed circuit boards powder and addition, are specifically shown in table 2 below and table 3.
The step of table 2 3. multi strain co cultivation when multi strain co cultivation liquid used in each component content
The step of table 3 4. the addition time of discarded printed circuit boards powder and addition
Note：Added described in upper table the time refer to after cultivating since the step 3. Mixed Microbes how many hours when carry out powder addition
Time；The addition refers to the weight of the discarded printed circuit boards powder added in every 1L multi strain co cultivations system, single
Position for gram.
Claims (4)
1. a kind of method that Mixed Microbes leach copper in discarded printed circuit boards, it is characterised in that comprise the following steps：
1. the pretreatment of discarded printed circuit boards；The discarded printed circuit boards PCBs that electronic component will have been removed is crushed and ground to form
Powder, the discarded printed circuit boards powder sieving that grinding is obtained, collects pending by the discarded printed circuit boards powder of sieve aperture；
2. tamed strain；By Acidithiobacillus ferrooxidans strain GFA.ferrooxidansAnd Acidithiobacillus thiooxidansA.thiooxidansResistance to Cu is carried out respectively2+Domestication culture, domestication end respectively obtain resistance to 100~200mmol/L Cu2+Ring
BorderA. ferrooxidansWithA.thiooxidansIt is stand-by；
A. ferrooxidansWhen carrying out domestication culture, the sludge enrichment that will be extracted from the aeration tank of municipal sewage plant
Culture, is then peeled off purifying and obtainingA. ferrooxidans；WillA. ferrooxidansCultivated in 9K nutrient solutions to right
The number phase；It is 10%~20% according to strain inoculum concentration（Volume ratio v/v）, draw above-mentioned bacterium solution and be transferred to Cu2+Concentration be 10mmol/
In the nutrient solution of L；It is 10%~20% according to strain inoculum concentration after culture to logarithmic phase（Volume ratio v/v）, draw above-mentioned bacterium solution and turn
Move on to Cu2+Concentration for 20mmol/L nutrient solution in cultivate to logarithmic phase；Aforesaid operations are repeated, often increases taming and dociling for generation bacterial strain
Change, Cu in nutrient solution used2+Concentration compared to previous generation increase 10mmol/L, so as to obtain in 100~200mmol/L Cu2 +Cultivated in environment to logarithmic phaseA.ferrooxidans；
A.thiooxidansWhen carrying out domestication culture, the sludge that will be extracted from the aeration tank of municipal sewage plant is enriched with training
Support, be then peeled off purifying and obtainingA.thiooxidans；WillA.thiooxidansCultivated in nutrient solution to logarithmic phase；According to
Strain inoculum concentration is 10%~20%（Volume ratio v/v）, draw above-mentioned bacterium solution and be transferred to Cu2+Concentration for 10mmol/L nutrient solution
In；It is 10%~20% according to strain inoculum concentration after culture to logarithmic phase（Volume ratio v/v）, draw above-mentioned bacterium solution and be transferred to Cu2+'s
Concentration for 20mmol/L nutrient solution in cultivate to logarithmic phase；Aforesaid operations are repeated, often increases the domestication of generation bacterial strain, it is used
Cu in nutrient solution2+Concentration compared to previous generation increase 10mmol/L, so as to obtain in 100~200mmol/L Cu2+Trained in environment
Support to logarithmic phaseA.Thiooxidans；
3. multi strain co cultivation；2. step is tamed what is obtained after cultivatingA. ferrooxidansWithA.thiooxidansAccording to connecing
The ratio between amount is planted for 1: 1.5~2.5 carry out multi strain co cultivation in multi strain co cultivation liquid, it is 1.5~1.8 to cultivate initial pH, mixing
Bacterium inoculum concentration is the 10%~20% of multi strain co cultivation liquid product；
4. the addition of discarded printed circuit boards powder；Treat step 3. the multi strain co cultivation time reach 40~55 hours, for the first time to
Cultivated and add in the multi strain co cultivation system of 40~55 hours step and 1. pre-process the discarded PCBs powder for obtaining, then every
20~25 hours again to adding step 1. to pre-process the discarded PCBs powder that obtains in multi strain co cultivation system, after once add
Discarded PCBs powder compared to it is preceding once increase by 1~3g/L, the discarded PCBs powder added in 1L multi strain co cultivation systems
Gross mass is 28g~36g；When discarded PCBs powder finishes bacterium incubation time arrival 175h~200h to be mixed, Mixed Microbes leaching
Reaction terminates；Reacted mixed material is centrifuged, upper strata leachate is collected；
5. post-process；The leachate that 4. step obtains is extracted with copper extractant, for the cupric extract for obtaining, with anti-
Extractant is stripped；Then the cupric strip liquor that will be obtained is transferred in electrolytic cell and carries out electrodeposition and obtain copper, completes discarded
The recovery of copper in printed circuit board (PCB).
2. the method that Mixed Microbes according to claim 1 leach copper in discarded printed circuit boards, it is characterised in that：Step is 3.
During multi strain co cultivation, the content of each component is in multi strain co cultivation liquid used：4.0~6.5g/L of elemental sulfur, ammonium sulfate 3.5
~4.5g/L, the g/L of dipotassium hydrogen phosphate 0.45~0.65, the g/L of bitter salt 0.45~0.65, potassium chloride 0.1~
0.15 g/L, calcium nitrate 0.008~0.015 g/L, 15~18g/L of green vitriol, the g/ of calcium chloride 0.10~0.18
L；Multi strain co cultivation liquid solvent is water.
3. the method that Mixed Microbes according to claim 2 leach copper in discarded printed circuit boards, it is characterised in that：Step is 3.
During multi strain co cultivation, the content of each component is in multi strain co cultivation liquid used：5.2~5.6g/L of elemental sulfur, ammonium sulfate 3.5
~4.5g/L, the g/L of dipotassium hydrogen phosphate 0.45~0.65, the g/L of bitter salt 0.45~0.65, potassium chloride 0.1~
0.15 g/L, calcium nitrate 0.008~0.015 g/L, 17~17.5g/L of green vitriol, calcium chloride 0.10~0.18
g/L；Multi strain co cultivation liquid solvent is water.
4. the method that Mixed Microbes according to claim 1 leach copper in discarded printed circuit boards, it is characterised in that：Step is 4.
When discarded PCBs powder is added, treat that 3. the multi strain co cultivation time reaches 40~55 hours step, to having cultivated 40~55 hours
Add step 1. to pre-process the discarded PCBs powder for obtaining in multi strain co cultivation system, 4g is added in every 1L multi strain co cultivation systems
The discarded PCBs powder of~6g, the discarded PCBs powder of addition proceeds by Mixed Microbes leaching reaction；Bacterium to be mixed continues to cultivate 20
After~25 hours, the discarded PCBs powder for obtaining 1. is pre-processed to second addition step in cultivating system, per the training of 1L Mixed Microbes
The discarded PCBs powder of 6g~8g is added in the system of supporting, the discarded PCBs powder of addition proceeds by Mixed Microbes leaching reaction；Wait to mix
Close after bacterium continues to cultivate 20~25 hours, the discarded PCBs powder that obtains 1. is pre-processed to step is added in cultivating system for the third time
End, adds the discarded PCBs powder of 8g~10g in every 1L multi strain co cultivation systems, the discarded PCBs powder of addition proceeds by mixing
Bacterium leaching reaction；After bacterium to be mixed continues to cultivate 20~25 hours, 1. pre-processed to the 4th addition step in cultivating system
The discarded PCBs powder for arriving, adds the discarded PCBs powder of 10g~12g, discarded printed circuit boards in every 1L multi strain co cultivation systems
Powder addition is finished.
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