CN101392325B - Method for extracting gold from waste printed circuit board - Google Patents
Method for extracting gold from waste printed circuit board Download PDFInfo
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- CN101392325B CN101392325B CN2008102014200A CN200810201420A CN101392325B CN 101392325 B CN101392325 B CN 101392325B CN 2008102014200 A CN2008102014200 A CN 2008102014200A CN 200810201420 A CN200810201420 A CN 200810201420A CN 101392325 B CN101392325 B CN 101392325B
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- iodine
- printed circuit
- circuit board
- gold
- solution
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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
Abstract
The invention provides a method for leaching gold from a deserted printed circuit board. The method comprises the specified steps: Step 1: the deserted printed circuit board is crushed and smashed to separate metals and plastics; Step 2: the metals obtained from the Step 1 are mixed with nitric acid solution, stirring and reaction are carried out for 1h to 6h at the constant temperature of 10 DEG C to 80 DEG C, products are filtered, copper is leached from the filtrate, and the filter residue is washed and dried; Step 3: the filter residue obtained from the Step 2 is added into the blended solution of first iodine solution and a pro-oxidant, a reaction pH value is controlled at 3 to 9 by an inorganic acid and alkaline solution, reaction is carried out for 2h to 5h in a constant temperature oscillator at the temperature of 10 DEG C to 60 DEG C; and Step 4: products obtained from the Step 3 are filtered, with the filtrate fed into the cathode region of an electrobath, second iodine solution composed of iodine, water-soluble iodide and water is used as the electrolyte and fed into the anode region of the electrobath, electrolysis is carried out, the solution at the cathode region is filtered, then the filter residue obtained is gold mud, and the second iodine solution at the anode region is recovered. The method has high gold leaching ratio, low cost and less environmental pollution.
Description
Technical field
The present invention relates to a kind of method of from abandoned printed circuit board, extracting gold, be specifically related to a kind of novel environment friendly, efficient, the economic method of from abandoned printed circuit board, extracting gold.
Background technology
Along with constantly upgrading and the social continual renovation to electrical type consuming product demand of electronic industry state of the art, electronic product is eliminated and depleted speed is more and more faster, quantity is more and more.As the important component part of electronic product, the discarded amount of printed-wiring board (PWB) (Printed Circuit Board) also grows with each passing day.Abandoned printed circuit board belongs to danger wastes, and the growth of its quantity brings great pressure to environment, becomes urgent problem in the Economic development so it is reasonably handled and dispose.
In the composition of printed-wiring board (PWB) except containing a large amount of plastics (Resins, epoxy etc.) and base metal (copper, lead, zinc etc.), also generally contain rare precious metal (gold and silver, platinum etc.), wherein Jin content reaches 80g/t, is higher than the gold grade in the general gold mine ore far away.Reclaim so abandoned printed circuit board is carried out resource utilization, not only can obtain valuable rare precious metal resource, can also prevent that the heavy metal in the abandoned printed circuit board from producing severe contamination to environment.
Now mainly contain the method that mechanical treatment, pyrometallurgy, hydrometallurgy or several technology combine for the most frequently used recovery technology of abandoned printed circuit board.But mechanical treatment only can be realized separating of metal and plastics, and the metallic particles body that obtains after the processing also needs further processing just can obtain the precious metals such as gold of enrichment.Pyrometallurgy and hydrometallurgical technology are then non-heavy serious to the pollution of environment, traditional cyanide gold-leaching technology in the hydrometallurgical processes especially, because prussiate is a highly toxic substance, its environmental pollution that causes is very serious.
Therefore, in today that nonferrous metal resource shortage, price rise steadily and the abandoned printed circuit board environmental pollution is serious, develop and a kind ofly from abandoned printed circuit board, can extract metal efficiently, economically, can reduce environmental hazard again, nontoxic processing method has become a kind of exigence.
Summary of the invention
The purpose of this invention is to provide a kind of method of from abandoned printed circuit board, extracting gold, it can overcome, and the metal recovery rate that exists in the existing recovery technology is low, environmental pollution serious and medicament has shortcomings such as toxicity, can extract metal efficiently, economically, can reduce again environmental hazard.
In order to achieve the above object, technical scheme of the present invention provides a kind of method of extracting gold from abandoned printed circuit board, it is characterized in that concrete steps are:
The first step: with abandoned printed circuit board fragmentation, pulverizing, separating metal and plastics;
Second step: the metal that the first step is obtained and mass concentration are that 15%～25% salpeter solution is that mix 1:1～45 by mass ratio, stirring reaction 1～6h under 10～80 ℃ of constant temperatures, product is filtered, from filtrate, extract copper, residue washing is dried with ion-exchange membrane electrolysis;
The 3rd step: is that 1:1～25 are added in the mixed solution of the first iodine liquid be made up of iodine, water-soluble iodate thing and water and pro-oxidant with second filter residue that obtain of step by mass ratio, with mineral acid and basic solution control pH value in reaction is 3～9, in 10～60 ℃ of constant temperature oscillators, react 2～5h, wherein, the mass concentration of pro-oxidant is 0.1%～10% in the mixed solution of the first iodine liquid and pro-oxidant, iodine is 1:1～13 with water-soluble iodate amount ratio in the first iodine liquid, and the mass concentration of iodine is 0.2%～2.0%;
The 4th step: the product in the 3rd step is filtered, filtrate is put into the cathodic area of electrolyzer, will be by iodine, the second iodine liquid that water-soluble iodate thing and water are formed is put into the positive column as ionogen, electrolysis, filtering cathode district solution, the filter residue that obtains is gold mud, wherein, iodine is 1:1～13 with water-soluble iodate amount ratio in the described second iodine liquid, and the mass concentration of iodine is 0.1%～2.0%, and it is negative electrode that described electrolyzer adopts carbon-point, the titanium plate, the titanium net, stainless steel plate, stainless (steel) wire, platinum titanium plate or platinum titanium net are anode, bath voltage is 1～20V, and strength of current is 0.01～0.4A, and current density is 5～200A/m
2, temperature of reaction is 20～30 ℃, electrolysis time is 0.25h～5h.
Further, in the described the first step printed-wiring board (PWB) is crushed to granularity and is preferably 0.5-1mm.
Pro-oxidant is preferably hydrogen peroxide in described the 3rd step.
Mineral acid is preferably hydrochloric acid in described the 3rd step, and basic solution is preferably sodium hydroxide solution.
Electric tank cathode district and positive column are preferably separated by anion-exchange membrane in described the 4th step.Described anion-exchange membrane is homogeneous-phase anion exchange film or out-phase anion-exchange membrane.
In described the 4th step in the electric tank cathode district mass concentration of gold be preferably 1～90ppm.
Water-soluble iodate thing is preferably potassiumiodide, sodium iodide or iodate ammonia respectively in the described first iodine liquid and the second iodine liquid.
The present invention be adopt the iodine liquid of non-cyanogen leaching from printed-wiring board (PWB) gold lixiviation, again with the electrolysis deposited gold and reclaim the method for iodine, principle of work of the present invention is as follows:
The present invention utilizes other base metals of parcel gold in the nitric acid oxidation dissolving wiring board earlier; The iodine liquid selectivity that re-uses nontoxic non-cyanogen leaching leaches precious metals such as gold and silver, palladium, realizes separating fully of metal and indifferent oxide and separating of base metals such as precious metals such as gold and silver, palladium and copper; At last lixivium is adopted metals such as electrolytic process deposition gold and silver, palladium, and reclaim simultaneously and obtain iodine liquid and be re-used as ionogen or directly be used for soaking gold.The present invention can eliminate electronic waste and pollute, and improves the resource reutilization rate.
At first, the adding of nitric acid makes the base metal simple substance in the printed-wiring board (PWB) particle form soluble salt with it, and these soluble salts enter the aqueous solution and reached the purpose of separating with other insoluble materials.With copper is example, and following reaction formula is arranged:
3Cu+8HNO
3→3Cu
2++6NO
3 -+4H
2O+2NO↑
Go residue behind the copper through after the washing repeatedly, add water-soluble iodate thing leaching solution of iodo-and pro-oxidant hydrogen peroxide, I
2Elder generation and I
-Reaction generates I
3 -, I then
-, I
3 -React with Au and to form stable AuI
2 -Gold is dissolved in the solution, finishes the golden process of soaking.The pro-oxidant hydrogen peroxide plays and improves the effect of soaking golden efficient.
I
2+I
-——I
3 -
2Au+I
-+I
3-——2AuI
2 -
AuI
2 -+I
3 -——AuI
4 -+I
-
AuI+I
-——AuI
2 -
2Au+4I
-+H
2O
2——2AuI
2 -+2OH
-
The electrolysis lixivium, in the cathodic area, deposition of gold has hydrogen to separate out in the bottom of electrolyzer simultaneously:
AuI
2 -+e——Au+2I
-
2H
2O+2e——H
2+2OH
-
AuI
4 -+3e——Au+4I
-
Deposit in the positive column simultaneously, reclaim iodine, and have oxygen to emit:
2H
2O-4e——O
2+4H
+
2I
--2e——I
2
Printed-wiring board (PWB) of the present invention comprises various types of wiring boards that computer, TV, mobile phone, game machine, electronic cards, main equipment etc. use.
The present invention adopts the water-soluble iodate thing of nontoxic iodo-to soak under the condition of golden agent in lower processing costs, realized the higher golden rate of soaking, and has realized the efficient deposition of gold then by electrolytic reaction, and regeneration, reuse simultaneously soak golden medicament.The present invention can realize innoxious, the minimizing and the resource utilization of electronic waste.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Discarded printed circuit boards is crushed to 0.5mm, separating metal and plastics, in reactor, abandoned printed circuit board metallic particles that separation is obtained and mass concentration are 15% HNO
3Mix and pour in the reactor, the mass ratio of the two is 1:1, stirring reaction 1h under 10 ℃ constant temperature.Post reaction mixture is filtered, and filtrate is extracted copper with ion-exchange membrane electrolysis; Mixed solution with the first iodine liquid and pro-oxidant hydrogen peroxide after the reaction residues washing and drying mixes by mass ratio 1:1.The massfraction of iodine is 0.2% in the first iodine liquid, and iodine and potassiumiodide mass ratio are 1:1, and the massfraction of pro-oxidant hydrogen peroxide is 0.1%, is 3 with the pH value of hydrochloric acid and sodium hydrate regulator solution, under 10 ℃, and oscillatory reaction 2h.Wherein, the extraction yield of copper is 32.3%, and soaking golden rate is 5.5%.(carbon-point is made negative electrode to put into electrolyzer with filtrate (golden amount concentration is 1ppm), the titanium plate is made anode) the cathodic area, the second iodine liquid is put in the positive column, and (massfraction of iodine is 0.1%, iodine and potassiumiodide mass ratio are 1:1), cathodic area and positive column homogeneous-phase anion exchange film (membrane material: polymers such as tetrafluoroethylene; Thickness: 0.2mm; Exchange capacity 〉=1.6mol/Kg (doing); Face resistance≤4.0 Ω .cm
2Select transmitance 〉=97%) separate, bath voltage is 1V, and strength of current is 0.01A, and current density is 5A/m
2, temperature of reaction is 20 ℃, and electrolysis time is 0.25h, and the deposition of cathodic area gold is 61.3%, and the iodine liquid of positive column can be brought and do electrolytic next time ionogen, improves its iodine quality mark, final as the purpose of soaking gold once more to reach.
Embodiment 2
Discarded printed circuit boards is crushed to 1mm, separating metal and plastics, in reactor, abandoned printed circuit board metallic particles that separation is obtained and mass concentration are 25% HNO
3Mix and pour in the reactor, the mass ratio of the two is 1:45, stirring reaction 6h under 80 ℃ constant temperature.Post reaction mixture is filtered, and filtrate is extracted copper with ion-exchange membrane electrolysis; Mixed solution with the first iodine liquid and pro-oxidant hydrogen peroxide after the reaction residues washing and drying mixes.Wherein residue is 1:25 with the mass ratio of leaching mixing solutions, the massfraction of iodine is 2.0% in the first iodine liquid, iodine and sodium iodide mass ratio are 1:13, the massfraction of pro-oxidant hydrogen peroxide is 10% in the mixed solution of the first iodine liquid and pro-oxidant hydrogen peroxide, regulating the pH value with the NaOH solution of the HCl and 1% (mass concentration) of 1% (mass concentration) is 9, reacts 5h in 60 ℃ of constant temperature oscillators.Wherein, the extraction yield of copper is 83.5%, and soaking golden rate is 77.2%.(carbon-point is made negative electrode to put into electrolyzer will to soak golden filtrate (golden amount concentration is 90ppm), the titanium net is made anode) the cathodic area, the second iodine liquid is put in the positive column, and (massfraction of iodine is 2.0%, iodine and sodium iodide mass ratio are 1:13), cathodic area and positive column out-phase anion-exchange membrane (membrane material: polymers such as polyethylene; Thickness: 0.42mm; Exchange capacity 〉=1.8mol/Kg (doing); Face resistance≤12 Ω .cm
2Select transmitance 〉=89%) separate, bath voltage is 20V, and strength of current is 0.4A, and current density is 200A/m
2, 30 ℃ of temperature of reaction, electrolysis time is 5h, and the deposition of cathodic area gold is 89.5%, and the iodine liquid of positive column directly is used for soaking once more gold from abandoned printed circuit board, and soaking golden rate is 92.6%.
Embodiment 3
Discarded printed circuit boards is crushed to 0.75mm, separating metal and plastics, in reactor, abandoned printed circuit board metallic particles that separation is obtained and mass concentration are 20% HNO
3Mix and pour in the reactor, the mass ratio of the two is 1:27, stirring reaction 4h under 20 ℃ constant temperature.Post reaction mixture is filtered, and filtrate is extracted copper with ion-exchange membrane electrolysis; Mix with the first iodine liquid and pro-oxidant hydrogen peroxide mixed solution after the reaction residues washing and drying.Wherein residue is 1:10 with the mass ratio of leaching mixing solutions, the massfraction of iodine is 1.2% in the first iodine liquid, iodine and iodate ammonia mass ratio are 1:6, the massfraction of pro-oxidant hydrogen peroxide is 1.0% in the first iodine liquid and the pro-oxidant hydrogen peroxide mixed solution, regulating the pH value with the NaOH solution of the HCl and 1% (mass concentration) of 1% (mass concentration) is 5, reacts 3h in 50 ℃ of constant temperature oscillators.Wherein, the extraction yield of copper is 95.8%, and soaking golden rate is 97.6%.(carbon-point is made negative electrode to put into electrolyzer will to soak golden filtrate (golden amount concentration is 12ppm), stainless steel plate is made anode) the cathodic area, the second iodine liquid is put in the positive column, and (massfraction of iodine is 0.1%, iodine and iodate ammonia mass ratio are 1:2), cathodic area and positive column homogeneous-phase anion exchange film (membrane material: polymers such as tetrafluoroethylene; Thickness: 0.2mm; Exchange capacity 〉=1.6mol/Kg (doing); Face resistance≤4.0 Ω .cm
2Select transmitance 〉=97%) separate, bath voltage is 14.0V, and strength of current is 0.12A, and current density is 60.0A/m
2, electrolysis time is 4h, and the deposition of cathodic area gold is 95.5%, and the iodine liquid of positive column can be brought and do electrolytic next time ionogen, improves its iodine quality mark, final as the purpose of soaking gold once more to reach.
Embodiment 4
Discarded printed circuit boards is crushed to 0.75mm, separating metal and plastics, in reactor, abandoned printed circuit board metallic particles that separation is obtained and mass concentration are 17% HNO
3Mix and pour in the reactor, the mass ratio of the two is 1:22, stirring reaction 2h under 60 ℃ constant temperature.Post reaction mixture is filtered, and filtrate is extracted copper with ion-exchange membrane electrolysis; Mixed solution with the first iodine liquid and pro-oxidant hydrogen peroxide after the reaction residues washing and drying is that 1:12 mixes with the mass ratio.The massfraction of iodine is 1.1% in the first iodine liquid, iodine is 1:10 with water-soluble iodate amount ratio, the massfraction of pro-oxidant hydrogen peroxide is 1.5% in the mixed solution of the first iodine liquid and pro-oxidant hydrogen peroxide, regulating the pH value with the NaOH solution of the HCl and 1% (mass concentration) of 1% (mass concentration) is 6, reacts 5h in 40 ℃ of constant temperature oscillators.Wherein, the extraction yield of copper is 96.2%, and soaking golden rate is 97.0%.(carbon-point is made negative electrode to put into electrolyzer will to soak golden filtrate (golden amount concentration is 50ppm), platinum titanium plate is made anode) the cathodic area, the second iodine liquid is put in the positive column, and (massfraction of iodine is 0.8%, iodine is 1:6 with water-soluble iodate amount ratio), cathodic area and positive column out-phase anion-exchange membrane (membrane material: polymers such as polyethylene; Thickness: 0.42mm; Exchange capacity 〉=1.8mol/Kg (doing); Face resistance≤12 Ω .cm
2Select transmitance 〉=89%) separate, bath voltage is 10.0V, and strength of current is 0.06A, and current density is 30.0A/m
2, electrolysis time is 4h, and the deposition of cathodic area gold is 95.2%, and the iodine liquid of positive column directly is used for soaking once more gold from abandoned printed circuit board, and soaking golden rate is 94.7%.
Claims (7)
1. one kind is extracted golden method from abandoned printed circuit board, it is characterized in that concrete steps are:
The first step: with abandoned printed circuit board fragmentation, pulverizing, separating metal and plastics;
Second step: the metal that the first step is obtained and mass concentration are 15%～25% salpeter solution by mass ratio is 1: 1～45 to mix, stirring reaction 1～6h under 10～80 ℃ of constant temperatures, product is filtered, from filtrate, extract copper, residue washing is dried with ion-exchange membrane electrolysis;
The 3rd step: is 1: 1～25 to be added in the mixed solution of the first iodine liquid be made up of iodine, water-soluble iodate thing and water and pro-oxidant hydrogen peroxide second filter residue that obtain of step by mass ratio, with mineral acid and basic solution control pH value in reaction is 3～9, in 10～60 ℃ of constant temperature oscillators, react 2～5h, wherein, the mass concentration of pro-oxidant hydrogen peroxide is 0.1%～10% in the mixed solution of the first iodine liquid and pro-oxidant hydrogen peroxide, iodine is 1: 1～13 with water-soluble iodate amount ratio in the first iodine liquid, and the mass concentration of iodine is 0.2%～2.0%;
The 4th step: the product in the 3rd step is filtered, filtrate is put into the cathodic area of electrolyzer, will be by iodine, the second iodine liquid that water-soluble iodate thing and water are formed is put into the positive column as ionogen, electrolysis, filtering cathode district solution, the filter residue that obtains is gold mud, wherein, iodine is 1: 1～13 with water-soluble iodate amount ratio in the described second iodine liquid, and the mass concentration of iodine is 0.1%～2.0%, and it is negative electrode that described electrolyzer adopts carbon-point, the titanium plate, the titanium net, stainless steel plate, stainless (steel) wire, platinum titanium plate or platinum titanium net are anode, bath voltage is 1～20V, and strength of current is 0.01～0.4A, and current density is 5～200A/m
2, temperature of reaction is 20～30 ℃, electrolysis time is 0.25h～5h.
2. a kind of method of extracting gold from abandoned printed circuit board as claimed in claim 1 is characterized in that in the described the first step printed-wiring board (PWB) being crushed to granularity is 0.5-1mm.
3. a kind of method of extracting gold from abandoned printed circuit board as claimed in claim 1 is characterized in that, mineral acid is a hydrochloric acid in described the 3rd step, and basic solution is a sodium hydroxide solution.
4. a kind of method of extracting gold from abandoned printed circuit board as claimed in claim 1 is characterized in that, electric tank cathode district and positive column are separated by anion-exchange membrane in described the 4th step.
5. a kind of method of extracting gold from abandoned printed circuit board as claimed in claim 4 is characterized in that described anion-exchange membrane is homogeneous-phase anion exchange film or out-phase anion-exchange membrane.
6. a kind of method of extracting gold from abandoned printed circuit board as claimed in claim 1 is characterized in that, filtrate puts into that the mass concentration of electric tank cathode district gold is 1～90ppm behind the cathodic area of electrolyzer in described the 4th step.
7. a kind of method of from abandoned printed circuit board, extracting gold as claimed in claim 1, it is characterized in that, water-soluble iodate thing is potassiumiodide, sodium iodide or iodate ammonia in the described first iodine liquid, and water-soluble iodate thing is potassiumiodide, sodium iodide or iodate ammonia in the described second iodine liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102014200A CN101392325B (en) | 2008-10-21 | 2008-10-21 | Method for extracting gold from waste printed circuit board |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102014200A CN101392325B (en) | 2008-10-21 | 2008-10-21 | Method for extracting gold from waste printed circuit board |
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| Publication Number | Publication Date |
|---|---|
| CN101392325A CN101392325A (en) | 2009-03-25 |
| CN101392325B true CN101392325B (en) | 2010-08-11 |
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|---|---|---|---|
| CN2008102014200A Expired - Fee Related CN101392325B (en) | 2008-10-21 | 2008-10-21 | Method for extracting gold from waste printed circuit board |
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| CN101928840B (en) * | 2010-08-02 | 2012-05-23 | 惠州Tcl环境科技有限公司 | Method for recovering gold and silver from waste circuit boards |
| CN102329960A (en) * | 2011-08-18 | 2012-01-25 | 华星集团环保产业发展有限公司 | Method for extracting gold from waste and old circuit board |
| CN103540748B (en) * | 2012-07-16 | 2015-10-28 | 中国科学院化学研究所 | A kind of metal of waste printed circuit board substrate and nonmetallic separation method |
| CN103194769B (en) * | 2013-04-22 | 2016-02-17 | 北京工业大学 | A kind of electrolyzer and method thereof reclaiming high purity copper from discarded circuit board |
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| CN105838900B (en) * | 2016-04-11 | 2017-08-25 | 许良秋 | One kind uses I2The method that gold refining is carried out with NaI |
| CN105648232B (en) * | 2016-04-11 | 2017-09-26 | 许良秋 | One kind uses I2The method that gold refining is carried out with KI |
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| CN106086417A (en) * | 2016-06-27 | 2016-11-09 | 南开大学 | A kind of method extracting copper and gold from waste mobile phone circuit board |
| CN106435196B (en) * | 2016-11-30 | 2018-12-18 | 福建工程学院 | A kind of technique of old circuit board Leaching of Gold |
| CN108754554B (en) * | 2018-09-18 | 2019-10-22 | 泉州益丰贵金属科技有限公司 | A kind of gold plating liquid and a kind of gold plating method |
| CN109797407B (en) * | 2019-03-13 | 2020-11-27 | 上海第二工业大学 | Method for recovering gold and copper from waste memory bank through selective electrolytic leaching |
| CN110656251B (en) * | 2019-09-24 | 2021-11-26 | 广东工业大学 | Rapid and environment-friendly circuit board gold stripping liquid, preparation method and application thereof, and gold stripping method |
| CN113046569A (en) * | 2021-03-03 | 2021-06-29 | 南昌航空大学 | Method for selectively recovering gold from waste circuit board |
-
2008
- 2008-10-21 CN CN2008102014200A patent/CN101392325B/en not_active Expired - Fee Related
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|---|---|
| CN101392325A (en) | 2009-03-25 |
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