CN103898550A - Recovery method of cupper in circuit board - Google Patents
Recovery method of cupper in circuit board Download PDFInfo
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- CN103898550A CN103898550A CN201410147510.1A CN201410147510A CN103898550A CN 103898550 A CN103898550 A CN 103898550A CN 201410147510 A CN201410147510 A CN 201410147510A CN 103898550 A CN103898550 A CN 103898550A
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- copper
- recovery method
- wiring board
- recovery
- bacterium liquid
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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
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Abstract
The invention relates to a recovery method of cupper in a circuit board. The recovery method is a circulating recovery method. Each cycle comprises a biochemical reaction stage, an oxidizing reaction stage and an electrolytic copper recovery stage, wherein the biochemical reaction stage comprises the following step of culturing in a biochemical reaction tank to obtain a ferrous oxide thiobacillus liquid; the oxidizing reaction stage comprises the following steps of contacting the ferrous oxide thiobacillus liquid with circuit board powder in an oxidizing reaction tank and applying a leaching micro-electric field to obtain a lixivium; the electrolytic copper recovery stage comprises the following step of applying an electrolytic micro-electric field to the lixivium to obtain copper and a circulating culture solution. The circulating culture solution is used for continuous culture in the biochemical reaction stage to obtain the ferrous oxide thiobacillus liquid. The method provided by the invention provides a novel path of recycling electronic wastes. Copper in waste circuit boards is continuously recovered by means of microorganisms, so that the method is low in cost, good in extracting effect and little in influence on environment.
Description
Technical field
The present invention relates to the recovery method of copper in a kind of wiring board.
Background technology
At present comprehensively recycling technology of electron wastes mainly contains pyrometallurgy, hydrometallurgy, mechanical treatment process, microbial method and several technology and combines etc.
Pyrometallurgy and hydrometallurgy are mainly used in the recovery of the precious metals such as gold and silver.Pyrometallurgy is owing to containing halogen flame in abandoned printed circuit board, and burning easily causes toxic gas to overflow, and causes secondary pollution, and precious metal is also easily with muriatic form volatilization, causes the loss of metal, and metal recovery rate is reduced; A large amount of nonmetal compositions, as plastics etc. also lose in burning, cause the recyclable wasting of resources, and in addition, strict due to treatment facility is required, it is expensive, thereby processing cost is high.
Wet chemical metallurgical technology comprises pickling, corrosion etc., that abandoned printed circuit board strong acid or strong oxidizer are processed, obtain the throw out of peeling off of precious metal, be reduced into respectively again gold, palladium etc., the waste liquid that contains high concentration ion is other metal values such as recyclable copper, can obtain the non-ferrous metals such as precious metal and copper such as the gold and silver of higher-grade and high-recovery by the method, have the advantages that expense is low.But the leach liquor of the method and residue have corrodibility and toxicity, if deal with improperly, easily cause even more serious secondary pollution; The leaching efficiency of part metals is low, acts on not obviously, and when coating metal lid or while being covered with scolding tin, wrapped precious metal more cannot reclaim, and causes the economic feasibility of this method to reduce.
Summary of the invention
To the object of the invention is the above-mentioned shortcoming existing in copper recovery technology in existing wiring board in order overcoming, the recovery method that a kind of cost is low, pollute copper in wiring board little, that can loop to be provided.
The invention provides the recovery method of copper in a kind of wiring board, wherein, this recovery method is circulation recovery method, and each circulation comprises: biochemical reaction stage, oxidizing reaction stage and electrolytic recovery copper stage;
Wherein, the biochemical reaction stage comprises, cultivates and obtain thiobacillus ferrooxidant bacterium liquid in biochemical reaction groove; The oxidizing reaction stage comprises, in oxidizing reaction groove, thiobacillus ferrooxidant bacterium liquid is contacted with circuit board powder, and applies leaching electric microfield, obtains leach liquor; The electrolytic recovery copper stage comprises, in electrolyzer, leach liquor is applied to electrolysis electric microfield and obtains copper and Cyclic culture liquid; Described Cyclic culture liquid is for continuing to cultivate acquisition thiobacillus ferrooxidant bacterium liquid in the biochemical reaction stage.
The recovery method of copper in wiring board of the present invention, utilizes thiobacillus ferrooxidant to leach the copper in discarded circuit board, makes bacterium liquid obtain recycle, has solved traditional hydrometallurgy and cause the problem of a large amount of difficult sewage; This law only needs the electricity charge of some broken wiring boards and backflow bacterium liquid, and energy-conservation 60% left and right, has overcome the defect that traditional pyrometallurgy needs mass energy compared with traditional method; Utilize this method to be combined with mechanical treatment process, the rate of recovery of copper can reach 99.99%, has made up the deficiency of single mechanical treatment process; In this continuous recovery discarded circuit board, the method for copper is that industrialization is provided convenience.
Embodiment
The invention provides many applicable creative concepts, this creativeness concept can be reflected in a large number of in concrete context.The specific embodiment of describing in following embodiments of the present invention is only as the exemplary illustration of the specific embodiment of the present invention, and do not form limitation of the scope of the invention.
Below in conjunction with concrete embodiment, the invention will be further described.
The invention provides the recovery method of copper in a kind of wiring board, wherein, this recovery method is circulation recovery method, and each circulation comprises: biochemical reaction stage, oxidizing reaction stage and electrolytic recovery copper stage;
Wherein, the biochemical reaction stage comprises, cultivates and obtain thiobacillus ferrooxidant bacterium liquid in biochemical reaction groove; The oxidizing reaction stage comprises, in oxidizing reaction groove, thiobacillus ferrooxidant bacterium liquid is contacted with circuit board powder, and applies leaching electric microfield, obtains leach liquor; The electrolytic recovery copper stage comprises, in electrolyzer, leach liquor is applied to electrolysis electric microfield and obtains copper and Cyclic culture liquid; Described Cyclic culture liquid is for continuing to cultivate acquisition thiobacillus ferrooxidant bacterium liquid in the biochemical reaction stage.
In method provided by the present invention, described thiobacillus ferrooxidant is Gram-negative bacteria thiobacillus ferrooxidant (acidithiobacillus ferrooxidans a.f.).
Described thiobacillus ferrooxidant can be for separating the bacterial strain from active sludge, the method separating can be that the thiobacillus ferrooxidant of this area routine separates acclimation method, the bacterial strain that for example utilizes 9K substratum purifying to obtain, in order to obtain the bacterial strain that there is higher generation and thank ability, can adopt the induction mutation of bacterium method of this area routine, for example, can adopt the method for ultraviolet mutagenesis breeding to obtain the thiobacillus ferrooxidant bacterial strain that is applicable to copper in recovery train plate.
In method provided by the present invention, can adopt 9K substratum is 140-170r/min at rotating speed, temperature is that under 25-30 DEG C, the pH condition that is 2-2.5, concussion is cultivated and obtained thiobacillus ferrooxidant bacterium liquid, and in described bacterium liquid, the density of thiobacillus ferrooxidant is 6.5-7.0 × 10
7individual/ml, pH value is 2-2.5, Fe
3+concentration be 10-30mol/L, Fe
2+concentration lower than 0.05mol/L.In preferred situation, in described bacterium liquid, the density of thiobacillus ferrooxidant is 6.6-6.8 × 10
7individual/ml, pH value is 2.2-2.4, Fe
3+concentration be 15-25mol/L, Fe
2+concentration lower than 0.04mol/L.
The biochemical reaction stage of the present invention carries out in biochemical reaction groove, the present invention has no particular limits for the setting of biochemical reaction groove, preferably, described biochemical reaction groove disposes the delivery port can convenient bacteria liquid flowing out and the input aperture that can facilitate Cyclic culture liquid to reclaim.
In the present invention, kind for wiring board has no particular limits, it can be any pending wiring board that contains copper in this area, before carrying out copper reclaimer, need to carry out pre-treatment step to wiring board, pre-treatment step can complete in such a way: first pending wiring board being crushed to particle diameter in pulverizer is 60-80 order, then is placed in vacuum drying oven dries 0.8-1.2h at 105-120 DEG C, oven dry is sieved after finishing, and obtaining particle diameter is 60-80 object circuit board powder.
In method provided by the present invention, with respect to the described circuit board powder of 100g, the consumption of the thiobacillus ferrooxidant bacterium liquid being in contact with it is 300-500ml, in preferred situation, with respect to the described circuit board powder of 100g, the consumption of the thiobacillus ferrooxidant bacterium liquid being in contact with it is 350-450ml.
In method provided by the present invention, need to apply electric microfield to thiobacillus ferrooxidant bacterium liquid in leaching stage, the intensity of described leaching electric microfield is 10-30mA, in preferred situation, the intensity of described leaching electric microfield is 15-25mA.
In method provided by the present invention, the condition that thiobacillus ferrooxidant bacterium liquid contacts with circuit board powder is: at 25-30 DEG C, stir contact 3-30h with the speed of turn/min of 100-140.In preferred situation, the condition that thiobacillus ferrooxidant bacterium liquid contacts with circuit board powder is: at 25-28 DEG C, stir contact 5-25h with the speed of turn/min of 120-130.
Described contact reacts is carried out in oxidizing reaction groove, utilizes thiobacillus ferrooxidant meta-bolites Fe
3+carry out the principle of oxidizing reaction with the copper in circuit board powder and see formula (1)
The present inventor finds, in leaching process, along with nutraceutical consumption and Cu
2+concentration increases, and the nectar degree in thiobacillus ferrooxidant bacterium liquid can present overall downward trend.Leach the efficiency of copper in discarded circuit board but can effectively improve thiobacillus ferrooxidant under the electric field action of some strength, thereby continue to leach the copper in circuit board powder.Suitable strength of electric field is conducive to maintain Cu in thiobacillus ferrooxidant leach liquor
2+concentration.Under additional 10-30mA strength of electric field, can extend the logarithmic phase of thiobacillus ferrooxidant, one of them reason may be can effectively keep Fe under extra electric field environment
2+concentration; Suitable strength of current can increase the generation of thiobacillus ferrooxidant intracellular protein effectively, because thiobacillus ferrooxidant intracellular protein total amount reaches 2-3 times while not applying electric field in the time applying 10-30mA; In addition, suitable extra electric field can obviously increase the permeability of thiobacillus ferrooxidant film, is conducive to bacterium and extraneous exchange of substance, thereby improves its metaboilic level; And make single thalline volume become large, cytolemma also has the sign of thickening, this all can improve thiobacillus ferrooxidant in the oxidizing reaction stage leaching effect to copper.
In method provided by the present invention, have no particular limits for the specification of oxidizing reaction groove, as long as can be used in the copper in sufficient lixiviate oxidizing reaction system and reclaim leach liquor.
In the electrolytic recovery copper stage, the intensity of described electrolysis electric microfield is 10-20mA, and in preferred situation, the intensity of described electrolysis electric microfield is 12-18mA.
The described electrolytic recovery copper stage carries out in electrolyzer, and the kind for electrolyzer in the present invention has no particular limits, as long as be applicable to utilize bacterium liquid to obtain copper by electrolytic reaction on negative electrode.
By apply electrolysis electric microfield in leach liquor, on the negative electrode of electrolyzer, there is electro deposited copper reaction, formula (2), Fe are shown in electro deposited copper reaction
3+be reduced into Fe
2+see formula (3), also have a small amount of O simultaneously
2generate.
In the electrolytic recovery copper stage, the Cu in leach liquor
2+and Fe
3+concentration reduces, as the Cu in leach liquor
2+concentration be 0.4g/L, Fe
2+concentration while being 0.1mol/L, stop electrolytic process, reclaim and obtain the copper and the remaining circulation bacterium liquid that on negative electrode, adhere to.
In one embodiment of the invention, described circulation bacterium liquid can continue on for the oxidizing reaction stage after recovery, obtains thiobacillus ferrooxidant bacterium liquid by cultivation.Wherein, described circulation bacterium liquid can directly apply to the oxidizing reaction stage, also can replenish after fresh 9K substratum for the oxidizing reaction stage, and method provided by the present invention has realized the recycle of material by recycling circulation bacterium liquid.
The present invention is described further for the following examples.In following examples, circuit board powder makes in such a way:
Discarded household electrical appliances and other various discarded electronic products are carried out to craft after by Mechanical Crushing more tentatively to be disassembled, wiring board fragment after disassembling is sent into and in tilting high speed Universalpulverizer, is crushed to 70 orders and is placed in vacuum drying oven, under the high temperature of 105 DEG C, dry 1 hour, adopt top to hit formula vibration screening machine above-mentioned dry cooling powder is sieved, obtain 70 object circuit board powders.
Thiobacillus ferrooxidant bacterial strain obtains in such a way:
To be configured to bacterium liquid by separating the thiobacillus ferrooxidant bacterial strain obtaining in active sludge, get this bacterium liquid of 50ml in culture dish, stir and make bacteria suspension with magnetic stirrer simultaneously, bacteria suspension is placed in to ultraviolet mutagenesis instrument, making electric power is the ultraviolet lamp of 30W, with the about 30cm of bacterium liquid distance, regulate irradiation time (time gradient is 60s, 100s, 150s, 200s, 250s, controls mutagenesis dosage with this).After mutagenesis finishes, be inoculated in rapidly in previously prepd 9K substratum, and be placed in the cultivation of constant temperature air bath shaking culture case lucifuge, sampling in every 12 hours is measured wherein Fe with potassium dichromate process
2+concentration and with microscopic examination nectar degree, choose the strongest bacterial strain of anti-copper ability for subsequent use.
Embodiment 1
This embodiment is for illustrating the recovery method of wiring board copper of the present invention.
In 9K substratum, be that 160r/min, temperature are that on the constant-temperature table of 30 DEG C, concussion is cultivated by thiobacillus ferrooxidant bacterial strain according to 10% inoculum size at rotating speed, obtaining nectar degree is 7.0 × 10
7individual/ml, pH value is 2.2, Fe
3+the concentration bacterium liquid that is 20mg/L.
In oxidizing reaction groove, 500g circuit board powder is stirred and contacts 20h with the speed of 120 turn/min at 25 DEG C with 2000ml bacterium liquid, and in contact process, apply the leaching electric microfield of 20mA, detect and leach Cu in 20min, 40min, 60min, 80min, 100min, 120min, 140min, 160min and 180min leach liquor
2+concentration list in table 1.
Leach liquor is transferred in electrolyzer, at 25 DEG C, applies the electrolysis electric microfield 3h of 15mA.
After electrolysis finishes, on electric tank cathode, collect copper products, and remaining circulation bacterium liquid is reclaimed.
Embodiment 2
This embodiment is for illustrating the recovery method of wiring board copper of the present invention.
Adopt the copper in the method recovery train plate identical with embodiment 1, different, the consumption of thiobacillus ferrooxidant bacterium liquid is 1500ml.
Detect and leach Cu in 20min, 40min, 60min, 80min, 100min, 120min, 140min, 160min and 180min leach liquor
2+concentration list in table 1.
Embodiment 3
This embodiment is for illustrating the recovery method of wiring board copper of the present invention.
Adopt the copper in the method recovery train plate identical with embodiment 1, different, the consumption of thiobacillus ferrooxidant bacterium liquid is 2500ml.
Detect and leach Cu in 20min, 40min, 60min, 80min, 100min, 120min, 140min, 160min and 180min leach liquor
2+concentration list in table 1.
Embodiment 4
This embodiment is for illustrating the recovery method of wiring board copper of the present invention.
Adopt the copper in the method recovery train plate identical with embodiment 1, different, the intensity that leaches electric microfield is 10mA.
Detect and leach Cu in 20min, 40min, 60min, 80min, 100min, 120min, 140min, 160min and 180min leach liquor
2+concentration list in table 1.
Embodiment 5
This embodiment is for illustrating the recovery method of wiring board copper of the present invention.
Adopt the copper in the method recovery train plate identical with embodiment 1, different, the intensity that leaches electric microfield is 30mA.
Detect and leach Cu in 20min, 40min, 60min, 80min, 100min, 120min, 140min, 160min and 180min leach liquor
2+concentration list in table 1.
Comparative example 1
This embodiment is for illustrating the recovery method of wiring board copper of the present invention.
Adopt the copper in the method recovery train plate identical with embodiment 1, different, the consumption of the thiobacillus ferrooxidant bacterium liquid using is 1000ml.
Detect and leach Cu in 20min, 40min, 60min, 80min, 100min, 120min, 140min, 160min and 180min leach liquor
2+concentration list in table 1.
Comparative example 2
This embodiment is for illustrating the recovery method of wiring board copper of the present invention.
Adopt the copper in the method recovery train plate identical with embodiment 1, different, the intensity that leaches electric microfield is 35mA.
Detect and leach Cu in 20min, 40min, 60min, 80min, 100min, 120min, 140min, 160min and 180min leach liquor
2+concentration list in table 1.
Comparative example 3
This embodiment is for illustrating the recovery method of wiring board copper of the present invention.
Adopt the copper in the method recovery train plate identical with embodiment 1, different, do not apply leaching electric field.
Detect and leach Cu in 20min, 40min, 60min, 80min, 100min, 120min, 140min, 160min and 180min leach liquor
2+concentration list in table 1.
Table 1
Can find out from the measurement result shown in table 1, method provided by the invention is the copper in recovery train plate effectively, particularly when bacterium liquid consumption, leach electric microfield intensity all within the scope of the invention time, can effectively leach the Cu existing in circuit board powder
2+.
By comparative example 1 and the result of embodiment 1 are compared and can be found out, in the time that the consumption of bacterium liquid is in scope provided by the present invention, Cu
2+leaching effect better.
By the result of comparative example 2,3 and embodiment 1 is compared and can be found out, when leaching the intensity of electric field in scope provided by the present invention time, Cu
2+leaching effect better.
Method provided by the present invention provides the new way of recycling electron wastes.Creatively reclaim continuously the copper in discarded circuit board by utilizing microorganism to reclaim the electric field biotechnology of metal in electron wastes, be that a kind of cost is low, extraction effect good, the method little to environmental influence.
Claims (10)
1. a recovery method for copper in wiring board, is characterized in that, this recovery method is circulation recovery method, and each circulation comprises: biochemical reaction stage, oxidizing reaction stage and electrolytic recovery copper stage;
Wherein, the biochemical reaction stage comprises, cultivates and obtain thiobacillus ferrooxidant bacterium liquid in biochemical reaction groove; The oxidizing reaction stage comprises, in oxidizing reaction groove, thiobacillus ferrooxidant bacterium liquid is contacted with circuit board powder, and applies leaching electric microfield, obtains leach liquor; The electrolytic recovery copper stage comprises, in electrolyzer, leach liquor is applied to electrolysis electric microfield and obtains copper and Cyclic culture liquid; Described Cyclic culture liquid is for continuing to cultivate acquisition thiobacillus ferrooxidant bacterium liquid in the biochemical reaction stage.
2. the recovery method of copper in wiring board according to claim 1, wherein, in described thiobacillus ferrooxidant bacterium liquid, nectar degree is 6.5-7.0 × 10
7individual/ml, pH value is 2-2.5, Fe
3+concentration be 10-30mg/L.
3. the recovery method of copper in wiring board according to claim 2, wherein, with respect to the described circuit board powder of 100g, the consumption of thiobacillus ferrooxidant bacterium liquid is 300-500ml.
4. according to the recovery method of copper in the wiring board described in any one in claim 1-3, wherein, the intensity of described leaching electric microfield is 10-30mA.
5. the recovery method of copper in wiring board according to claim 4, wherein, the intensity of described leaching electric microfield is 15-20mA.
6. the recovery method of copper in wiring board according to claim 5, wherein, the condition of contact is: at 25-30 DEG C, stir contact 3-30h with the speed of turn/min of 100-140.
7. according to the recovery method of copper in the wiring board described in any one in claim 1-3,5 and 6, wherein, in the electrolytic recovery copper stage, the intensity of described electrolysis electric microfield is 10-20mA.
8. according to the recovery method of copper in the wiring board described in any one in claim 1-3,5 and 6, wherein, the particle diameter of described circuit board powder is 60-80 order.
9. according to the recovery method of copper in the wiring board described in any one in claim 1-3, wherein, the method of cultivating acquisition thiobacillus ferrooxidant bacterium liquid is that the ratio taking 10% in the 9K substratum in pH as 2-3, is shaken thiobacillus ferrooxidant inoculation and cultivated 4-5 days at 25-30 DEG C.
10. according to the recovery method of copper in the wiring board described in any one in claim 1-3,5 and 6, wherein, Cu in described Cyclic culture liquid
2+concentration be 0.4-0.5g/L, Fe
2+concentration be 6-9g/L.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410147510.1A CN103898550A (en) | 2014-04-14 | 2014-04-14 | Recovery method of cupper in circuit board |
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|---|---|---|---|
| CN201410147510.1A CN103898550A (en) | 2014-04-14 | 2014-04-14 | Recovery method of cupper in circuit board |
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ID=50990114
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| ES2707353A1 (en) * | 2018-04-25 | 2019-04-03 | Univ Catalunya Politecnica | METHOD FOR THE BIOLOGICAL RECOVERY OF METALS IN ELECTRICAL AND ELECTRONIC WASTE (Machine-translation by Google Translate, not legally binding) |
| CN110863110A (en) * | 2019-12-09 | 2020-03-06 | 阳新鹏富矿业有限公司 | Copper, gold, silver and palladium cooperative recycling method |
| CN113308605A (en) * | 2021-05-19 | 2021-08-27 | 上海第二工业大学 | Method for strengthening leaching of copper and gold in waste circuit board by phanerochaete chrysosporium by using micro-electric field |
| WO2022162252A1 (en) | 2021-01-28 | 2022-08-04 | Universitat Politecnica De Catalunya | Method for biological recovery of metals from electrical and electronic waste |
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| CN110863110A (en) * | 2019-12-09 | 2020-03-06 | 阳新鹏富矿业有限公司 | Copper, gold, silver and palladium cooperative recycling method |
| WO2022162252A1 (en) | 2021-01-28 | 2022-08-04 | Universitat Politecnica De Catalunya | Method for biological recovery of metals from electrical and electronic waste |
| CN113308605A (en) * | 2021-05-19 | 2021-08-27 | 上海第二工业大学 | Method for strengthening leaching of copper and gold in waste circuit board by phanerochaete chrysosporium by using micro-electric field |
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Application publication date: 20140702 |