CN104630488B - A kind of nitrogen-doped carbon nanometer pipe is utilized to improve the technique of copper Bioleaching efficiency in abandoned printed circuit board - Google Patents
A kind of nitrogen-doped carbon nanometer pipe is utilized to improve the technique of copper Bioleaching efficiency in abandoned printed circuit board Download PDFInfo
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- CN104630488B CN104630488B CN201510051041.8A CN201510051041A CN104630488B CN 104630488 B CN104630488 B CN 104630488B CN 201510051041 A CN201510051041 A CN 201510051041A CN 104630488 B CN104630488 B CN 104630488B
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Abstract
The invention belongs to nonferrous metals recycling technical field, a kind of utilize nitrogen-doped carbon nanometer pipe to improve the technique of copper Bioleaching efficiency in abandoned printed circuit board.This technique uses the mode adding CNTs in the reactor of Acidithiobacillus ferrooxidans strain GF and abandoned printed circuit board powder effect, carries out the Bioleaching of copper in abandoned printed circuit board.Present invention process is simple, it is little and environmentally friendly to invest, and can improve Acidithiobacillus ferrooxidans strain GF and leach the efficiency of copper from abandoned printed circuit board, and expand nanometer technology application in microorganism ecology field.
Description
Technical field
The present invention relates to one utilizes nitrogen-doped carbon nanometer pipe (CNTs) to improve copper leaching in microorganism abandoned printed circuit board
The technique going out efficiency, belongs to solid waste resource recovery and new material is developed jointly and utilized and nonferrous metals recycling technology neck
Territory.
Background technology
The method utilizing microorganism ecology extracts the research of copper from abandoned printed circuit board to be had a lot, and application is at most
Bacterial classification be Acidithiobacillus ferrooxidans strain GF, but common problem the highest and the prolonging along with extraction time that be leaching efficiency
Long, the leaching efficiency of metallic copper promotes the most notable.There is scholar to improve Acidithiobacillus ferrooxidans strain GF from waste print circuit
Plate leaches the efficiency of copper, attempts by the method adding surfactant, chemical agent in the reactor, but the effect of test
Preferable not to the utmost.Reason is that copper is different with the existing forms in ore at printed substrate, be applicable to before improve addicted to
In acid oxidase ferrous iron bioleaching ore, the method for copper efficiency can not solve copper Bioleaching effect in abandoned printed circuit board
The problem that rate is low.Along with the quantity of abandoned printed circuit board is increasing and the worsening shortages of metals resources, utilize biology
It is considered as technology a kind of green, reliable that the method for hydrometallurgy extracts metal from abandoned printed circuit board.Therefore, anxious
Need to find and a kind of can improve the technique that Acidithiobacillus ferrooxidans strain GF leaches copper efficiency from abandoned printed circuit board.
CNTs has the ability of catalytic reaction, great specific surface area, good conduction and heat conductivility so that it is being urged
Change field is with a wide range of applications.But so far, also do not have document announcement to cross its application shape in field of hydrometallurgy
Condition.
Leach the efficiency of copper in abandoned printed circuit board to improve Acidithiobacillus ferrooxidans strain GF further and make
CNTs is applied in Biohydrometallurgy field, and the present invention intends by Acidithiobacillus ferrooxidans strain GF and waste print circuit
The reactor of plate powder adds the mode of CNTs to improve the bacterium leaching efficiency to zerovalent copper.
Summary of the invention
It is an object of the invention to provide one utilizes nitrogen-doped carbon nanometer pipe to improve copper biology leaching in abandoned printed circuit board
The technique going out efficiency, this technique is simple, it is little and environmentally friendly to invest, and does not the most introduce impurity, and the CNTs added can lead to
Later continuous acid treatment recycling；A certain amount of CNTs can improve Acidithiobacillus ferrooxidans strain GF from waste print circuit
Plate leaches the efficiency of copper, is that a kind of Acidithiobacillus ferrooxidans strain GF that improves leaches having of copper efficiency from abandoned printed circuit board
Efficacious prescriptions method, it also allows the CNTs application in Biohydrometallurgy field and is possibly realized, and provides practice for research further
Basis.
To achieve these goals, the present invention takes following design:
A kind of utilize nitrogen-doped carbon nanometer pipe to improve the technique of copper Bioleaching efficiency in abandoned printed circuit board, specifically walk
Rapid as follows:
(1) Acidithiobacillus ferrooxidans strain GF through acclimation is inoculated into equipped with in the reactor of metal concentrate,
Add CNTs the most in the reactor；The addition of CNTs is 0.6-1.2g/L；Wherein: described metal concentrate is by discarding printing
Circuit board powder is through coarse crushing fine crushing two-stage break process, and enters, with saturated aqueous common salt, the fine crushing product obtained
Row sorting obtains；
(2) 25-30 DEG C of temperature, under 120-150 r/min rotating speed, shaking table is cultivated 3-6 days, during monitor in nutrient solution
pH、Fe2+, ORP with the situation of change of incubation time, after reaction terminates, reacted nutrient solution is filtered, filtrate and filter residue is divided
Open collection；
(3) with extractant RE609, step (2) is obtained the copper ion in filtrate and carry out extracting and enriching, logical extra electric field pair
Solution rich in copper ion is electrolysed, and returns recycling as back washing agent after adding sulfuric acid for lean copper electrolyte；
(4) utilize chloroazotic acid that step (2) is obtained filter residue to soak, remove thalline remaining in filter residue and metabolism is produced
Thing, refilters collection CNTs, and deionized water is washed, until pH is between 6.8～7.5；CNTs circulation after recycling washing is real
Execute step (1)-(3), carry out the copper bioleaching process in abandoned printed circuit board.
In the present invention, in step (1), Acidithiobacillus ferrooxidans strain GF is carried out acclimation step as follows, step up
The concentration of copper ion in nutrient solution, filters out the Acidithiobacillus ferrooxidans strain GF high to copper ion tolerance.
In the present invention, in step (1), described CNTs carries out pretreatment ultrasonic, dry before using, specifically comprise the following steps that and adopt
With ultrasonic wave, CNTs is carried out ultrasonically treated, strengthens the specific surface area of CNTs, processed be put in baking oven carry out drying, standby.
In the present invention, inoculation Acidithiobacillus ferrooxidans strain GF uses 9K culture medium, and it is by FeSO4•7H2O、(NH4)2SO4、
K2HPO4、KCl、MgSO4•7H2O、Ca(NO3)2 Form with deionized water.
In the present invention, in step (4), utilizing chloroazotic acid step (2) to obtain filter residue when carrying out immersion treatment, temperature is 85-
95 DEG C, soak time is 1h～3h.
It is an advantage of the current invention that: CNTs has the ability of catalytic oxidation, big specific surface area and good leading
Electricity, heat conductivility, in addition to can strengthening Acidithiobacillus ferrooxidans strain GF and abandoned printed circuit board powdered reaction contact area,
May also speed up electron transfer rate in solution, thus improve zero-valent metal copper and become the efficiency of copper ion.Contained according to obtaining
The ICP-AES of copper ion solution analyzes and understands, and a certain amount of CNTs can improve Acidithiobacillus ferrooxidans strain GF from discarded printing
Wiring board leaches the efficiency of copper.
Present invention process is simple, it is little and environmentally friendly to invest, and improves Acidithiobacillus ferrooxidans strain GF from discarded printing
Wiring board leaches the efficiency of copper, but also has expanded CNT application in microorganism ecology field.The present invention
Technical scheme and the blank group contrast being not added with CNTs, Acidithiobacillus ferrooxidans strain GF leaches the efficiency of copper in abandoned printed circuit board
Obtain a certain degree of raising；The CNTs that after reaction, the filter residue Han CNTs reclaims after peracid treatment, it improves addicted to acid oxidase ferrous
Thiobacillus leaches the efficiency of copper from abandoned printed circuit board a certain degree of weakening, but inconspicuous, illustrates through peracid treatment
CNTs can recycle, environmental protection, reduce cost.
Accompanying drawing explanation
Fig. 1: CNTs improves the process schematic representation of copper Bioleaching efficiency in abandoned printed circuit board.
Fig. 2: CNTs surface SEM figure, wherein Fig. 2 a is not-acidified process CNTs surface SEM figure；Fig. 2 b is that Bioleaching is anti-
Should scheme by CNTs surface SEM afterwards；Fig. 2 c is SEM figure in CNTs surface after acidification.
Detailed description of the invention
Being illustrated in figure 1 the present invention utilizes CNTs to improve the technological process of copper Bioleaching efficiency in abandoned printed circuit board
Schematic diagram.CNTs is self-control, and its method is with reference to (2007) " Chinese Journal of Inorganic Chemistry " 23(6 such as Wang Lijun): 1035-1039；Now tie
Close accompanying drawing technological process is described below:
(1) Acidithiobacillus ferrooxidans strain GF used is carried out acclimation
Stepping up the concentration of copper ion in nutrient solution and reach about 20g/L, acclimation and screening obtains copper ion tolerance high
Acidithiobacillus ferrooxidans strain GF；
(2) broken, the sorting of abandoned printed circuit board
Utilize Large Crusher that abandoned printed circuit board first carries out coarse crushing, thicker by obtain with water-cooled disintegrating machine
Crushed product carries out fine crushing, obtains the particle diameter product at about 1mm；Finally with the saturated aqueous common salt fine crushing product to obtaining
Sort, finally give the metal concentrate containing a small amount of impurity；
(3) CNTs pre-treatment
Use ultrasonic wave to carry out ultrasonically treated to CNTs, strengthen the specific surface area of CNTs, processed to be put in baking oven and carry out
Dry, standby；
(4) CNTs and Acidithiobacillus ferrooxidans strain GF act on abandoned printed circuit board jointly
The Acidithiobacillus ferrooxidans strain GF that (1) processes is inoculated into containing the reaction of abandoned printed circuit board powder in (2)
In device, add a small amount of CNTs processed through (3) the most in the reactor；
(5) Bioleaching a period of time
At 25-30 DEG C, under the conditions of 120～150 r/min, shaking table is cultivated 5 days, during monitor pH, Fe in nutrient solution2+、
ORP etc. are with the situation of change of incubation time；(6) quantitative filter paper filters
Reacted nutrient solution quantitative filter paper is filtered, to filtrate and filter residue separate collection；
(7) enrichment of copper ion and electrolysis in filtrate
With extractant RE609, the copper ion in filtrate is carried out extracting and enriching, molten to rich in copper ion of logical extra electric field
Liquid is electrolysed, and returns recycling as back washing agent after adding sulfuric acid for lean copper electrolyte；
(8) recovery of CNTs in filter residue
After utilizing chloroazotic acid to react Bioleaching, filter residue soaks, and quantitative filter paper is collected by filtration CNTs；
(9) the recycling of CNT
It is washed with deionized water in (8) CNTs collected, repeats step (3).
Below in conjunction with embodiment, the present invention is further elaborated.
Embodiment 1
Preparation 9K fluid nutrient medium, its component content: FeSO4•7H2O is 40g/L, (NH4)2SO4For 3g/L, K2HPO4For
0.5g/L, KCL are 0.1g/L, MgSO4•7H2O is 0.5g/L, Ca (NO3)2For 0.01g/L, remaining is deionized water.Will domestication
The Acidithiobacillus ferrooxidans strain GF crossed is inoculated in reactor by inoculum concentration 10%, forms leaching liquid with culture medium, discarding of input
Printed substrate powder (＜ 1mm) and the ratio of leaching liquid, i.e. solid-to-liquid ratio is 1: 20.Add CNTs amount be respectively 0g/L,
0.6g/L, under the conditions of 120r/min, after cultivating 5 days, has added the experimental group of CNTs by 28 DEG C, and its copper leaching rate is 85.2%；It is not added with
The control group of CNTs, its copper leaching rate is 76.1%；After Bioleaching reaction terminates, process the filter residue containing CNTs with chloroazotic acid, collect
Obtaining CNTs, the CNTs of acidifying carries out identical Bioleaching experiment again, the leaching rate obtaining copper is 83.7%.
Embodiment 2
Preparation 9K fluid nutrient medium, its component content: FeSO4•7H2O is 40g/L, (NH4)2SO4For 3g/L, K2HPO4For
0.5g/L, KCL are 0.1g/L, MgSO4•7H2O is 0.5g/L, Ca (NO3)2For 0.01g/L, remaining is deionized water.Will domestication
The Acidithiobacillus ferrooxidans strain GF crossed is inoculated in reactor by inoculum concentration 10%, forms leaching liquid with culture medium, discarding of input
Printed substrate powder (＜ 1mm) and the ratio of leaching liquid, i.e. solid-to-liquid ratio is 1: 30.Add CNTs amount be respectively 0g/L,
0.8g/L, under the conditions of 125r/min, after cultivating 6 days, has added the experimental group of CNTs by 25 DEG C, and its copper leaching rate is 95.1%；It is not added with
The control group of CNTs, its copper leaching rate is 88.4%；After Bioleaching reaction terminates, process the filter residue containing CNTs with chloroazotic acid, collect
Obtaining CNTs, the CNTs of acidifying carries out identical Bioleaching experiment again, the leaching rate obtaining copper is 94.6%.
Embodiment 3
Preparation 9K fluid nutrient medium, its component content: FeSO4•7H2O is 40g/L, (NH4)2SO4For 3g/L, K2HPO4For
0.5g/L, KCL are 0.1g/L, MgSO4•7H2O is 0.5g/L, Ca (NO3)2For 0.01g/L, remaining is deionized water.Will domestication
The Acidithiobacillus ferrooxidans strain GF crossed is inoculated in reactor by inoculum concentration 10%, forms leaching liquid with culture medium, discarding of input
Printed substrate powder (＜ 1mm) and the ratio of leaching liquid, i.e. solid-to-liquid ratio is 1: 40.Add CNTs amount be respectively 0g/L,
0.4g/L, under the conditions of 150r/min, after cultivating 3 days, has added the experimental group of CNTs by 30 DEG C, and its copper leaching rate is 92.3%；It is not added with
The control group of CNTs, its copper leaching rate is 84.2%；After Bioleaching reaction terminates, process the filter residue containing CNTs with chloroazotic acid, collect
Obtaining CNTs, the CNTs of acidifying carries out identical Bioleaching experiment again, the leaching rate obtaining copper is 90.4%.
Claims (6)
1. utilizing nitrogen-doped carbon nanometer pipe to improve a technique for copper Bioleaching efficiency in abandoned printed circuit board, its feature exists
In, specifically comprise the following steps that
(1) Acidithiobacillus ferrooxidans strain GF through acclimation is inoculated into equipped with in the reactor of metal concentrate, then
Add CNTs in the reactor；The addition of CNTs is 0.6-1.2g/L；Wherein: described metal concentrate is by waste print circuit
Plate powder is through coarse crushing fine crushing two-stage break process, and carries out the fine crushing product obtained point with saturated aqueous common salt
Choosing obtains；
(2) 25-30 DEG C of temperature, under 120-150 r/min rotating speed, shaking table is cultivated 3-6 days, during monitor pH in nutrient solution,
Fe2+, ORP with the situation of change of incubation time, after reaction terminates, reacted nutrient solution is filtered, by filtrate and filter residue separately
Collect；
(3) step (2) obtained after the copper ion in filtrate carries out extracting and enriching with extractant RE609, through back extraction obtain rich in
The solution of copper ion, then lead to extra electric field the solution rich in copper ion is electrolysed, and sulfuric acid is added for lean copper electrolyte
Recycling is returned afterwards as back washing agent；
(4) utilize chloroazotic acid that step (2) is obtained filter residue to soak, remove thalline remaining in filter residue and metabolite thereof, then
CNTs is collected by filtration, and deionized water is washed, until pH is between 6.8～7.5；Step is implemented in CNTs circulation after recycling washing
(1)-(3), carry out the copper bioleaching process in abandoned printed circuit board.
2. technique as claimed in claim 1, it is characterised in that: in step (1), Acidithiobacillus ferrooxidans strain GF is tamed
Process step is as follows, steps up the concentration of copper ion in nutrient solution, filters out high sub-addicted to acid oxidase of copper ion tolerance
Iron Thiobacillus.
3. technique as claimed in claim 1, it is characterised in that: in step (1), through acclimation addicted to acid oxidase ferrous iron sulphur
The inoculum concentration of bacillus is 10%.
4. technique as claimed in claim 1, it is characterised in that: in step (1), described CNTs carries out ultrasonic, dry before using
Pretreatment, specifically comprises the following steps that CNTs is carried out ultrasonically treated by employing ultrasonic wave, strengthens the specific surface area of CNTs, processed and put
Carry out drying in baking oven, standby.
5. technique as claimed in claim 1, it is characterised in that: in step (1), inoculation Acidithiobacillus ferrooxidans strain GF uses 9K
Culture medium.
6. technique as claimed in claim 1, it is characterised in that: in step (4), utilize chloroazotic acid that step (2) is obtained filter residue and enter
During row immersion treatment, temperature is 85-95 DEG C, and soak time is 1h～3h.
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| CN105483375B (en) * | 2015-12-11 | 2018-03-13 | 上海第二工业大学 | A kind of method for improving copper efficiency in Microorganism Leaching printed substrate using NCNTs modification carbon electrodes |
| CN105506281B (en) * | 2015-12-11 | 2017-09-19 | 上海第二工业大学 | A kind of method that utilization NCNTs modifications carbon cloth electrode improves copper efficiency in Microorganism Leaching printed substrate |
| CN105734284A (en) * | 2016-03-10 | 2016-07-06 | 中国科学院城市环境研究所 | High-efficiency bioleaching technology of metal copper in printed circuit board |
| CN105886774B (en) * | 2016-04-12 | 2017-11-10 | 上海第二工业大学 | The method for improving metallic copper in Microorganism Leaching old circuit board using the carbon electrode system of graphene modified |
| CN105886775A (en) * | 2016-04-14 | 2016-08-24 | 上海第二工业大学 | Method for improving microbial leaching of metal copper in waste circuit board through graphene modified carbon cloth electrode system |
| CN107881825B (en) * | 2017-11-17 | 2019-10-18 | 苏州博进生物技术有限公司 | The microbial treatment method of scrap based on fireworks firecracker firing generation rubbish |
| CN109680153B (en) * | 2019-01-28 | 2021-06-22 | 东北大学 | Method for improving metal biological leaching rate in waste printed circuit board by using graphite |
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| JP2007308762A (en) * | 2006-05-18 | 2007-11-29 | Osaka Univ | Low environmental load type metal recovery method using cyanogen formation and decomposition bacteria |
| CN101477105B (en) * | 2009-01-16 | 2012-01-25 | 淮阴工学院 | Rapid measuring method for high-salt industrial waste water BOD |
| CN101935759A (en) * | 2009-07-03 | 2011-01-05 | 惠州市雄越保环科技有限公司 | Method for recycling and treating waste circuit board |
| CN103484680B (en) * | 2013-09-30 | 2015-04-08 | 江苏理工学院 | Method for leaching copper in waste printed circuit boards (PCBs) by mixed bacteria |
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