CN103540748A - Separating method for metals and nonmetals of waste printed circuit board substrate - Google Patents
Separating method for metals and nonmetals of waste printed circuit board substrate Download PDFInfo
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- CN103540748A CN103540748A CN201210246532.4A CN201210246532A CN103540748A CN 103540748 A CN103540748 A CN 103540748A CN 201210246532 A CN201210246532 A CN 201210246532A CN 103540748 A CN103540748 A CN 103540748A
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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 belongs to recycling of waste printed circuit boards and particularly relates to a separating method of metals and nonmetals of a waste printed circuit board substrate. A liquid medium is obtained by preparing organic acid aqueous liquor and an oxidizing agent, copper rivets and surface parts of copper foils on the waste printed circuit board substrate react and dissolve with the liquid medium, so that the copper rivets and the copper foils are separated from a nonmetal material of the waste printed circuit board to obtain treated nonmetal materials of the waste printed circuit board, and copper rivets and copper foils drop from the waste printed circuit board substrate; the used liquid medium can be electrolyzed, copper in the liquid medium can be recycled and the electrolyzed liquid medium can be recycled. The separating method disclosed by the invention is gentle in reaction condition, simple to operate and convenient to control; the liquid medium has no damage to the nonmetal materials of the waste printed circuit board substrate, the copper rivets and the copper foils are completely separated from the nonmetal materials, and no three wastes are exhausted.
Description
Technical field
The invention belongs to the recovery of waste printed circuit board, particularly a kind of metal of waste printed circuit board substrate and nonmetallic separation method.
Background technology
Usage quantity due to global electronic equipment sharply increases in recent years, causes electronic and electrical equipment, as the discarded amount of televisor, computer, mobile phone and electronic amusement apparatus etc. also rapid growth.According to estimates, at present China's generation of main electron wastes year is 1,500,000 tons, account for China's domestic refuse and produce 1% of total amount per year, and with annual 13%～15% speed increment.In electron wastes, the recycling of wiring board is the most complicated, but is also to have most value, because it contains the noble metals such as copper, lead, tin, chromium, cadmium, mercury, nickel, gold and silver, palladium.
Printed-wiring board (PWB) (Printed circuit Bonds, PCBs) is that substrate, the copper rivet on substrate and Copper Foil and the electronic devices and components etc. of being prepared by resin and glass fiber material form.Printed-wiring board (PWB) is widely used in the fields such as information, communication, electronics, military affairs, space flight.Along with the continuous expansion of scientific and technical development and every field demand printed-wiring board (PWB), the also sharp increase of the quantity of the waste printed circuit board producing.Multiple hazardous and noxious substances in waste printed circuit board must be through recycling on the one hand; Heavy metal element in waste printed circuit board substrate has again high resource recycling value on the other hand, is a kind of potential secondary resource.Therefore, rationally effectively reclaiming waste printed circuit board all has great significance to economy and environmental protection.
The recycling of waste printed circuit board general through disassembling, the process of sorting and recycling.First by machinery, disassemble the electronic devices and components on waste printed circuit board are removed from substrate, then the substrate of having disassembled electronic devices and components is carried out to sorting by methods such as physics or chemistry to substrate and copper rivet and Copper Foil, finally each component after sorting is processed and reclaimed.The method of carrying out at present sorting to removing waste printed circuit board substrate after electronic devices and components has the methods such as mechanical physical separation, pyrometallurgy sorting and hydrometallurgy sorting.Mechanical-physical separating method can be separated preferably with nonmetal realization to metal, its flow process is simple, to environment without destruction, but to pulverize waste printed circuit board substrate during sorting, after sorting, the purity of each component of gained is not high, can not directly by industry, be recycled.Pyrometallurgy separating method only has good recovering effect to metal, and under high temperature, non-metallic material are easily decomposed, and the material forming after non-metallic material decomposition has larger harm to human body and environment.The technological principle of hydrometallurgy separating method is to utilize the solution with oxidisability substrate to be dipped in solution under certain condition, the metal ion of then purifying in leach liquor, thus realize the recycling treatment of waste printed circuit board.But while leaching the metal in substrate with the strong acid such as nitric acid, sulfuric acid and hydrogen peroxide, can there is on the one hand oxidation and destroyed in substrate non-metallic material; The metal ion dissolving on the other hand also can destroy the molecular structure of non-metallic material on substrate reduces non-metallic material performance.If while leaching the metal on substrate with ammoniacal liquor, due to ammonia highly volatile, easily cause secondary environmental pollution.When having oxygenant to exist, organic acid at ambient temperature can be optionally and metallic copper generation complex reaction, and do not destroy non-metallic material, obtains the complex solution of single pure copper.Therefore the present invention selects when having oxygenant to exist, copper rivet and Copper Foil with organic acid and on waste printed circuit board substrate react, make the copper rivet on waste printed circuit board substrate separated with non-metallic material with Copper Foil, in its liquid medium, the complex compound of copper can be through electrolytic recovery simultaneously, and the liquid medium after electrolysis can be recycled; Neither destroy non-metallic material, high efficiente callback metallic copper, has avoided again the discharge of " three wastes ", environmental friendliness.
Summary of the invention
The object of the invention is to utilize when having oxygenant to exist, with the copper rivet on aqueous solutions of organic acids and waste printed circuit board substrate and Copper Foil, carry out selectivity partial reaction, make copper rivet separated with the non-metallic material on waste printed circuit board with Copper Foil, thereby provide that a kind of technique is simple, reaction conditions is gentle, the metal of cheap and eco-friendly waste printed circuit board substrate and nonmetallic separation method.
The present invention utilizes when having oxygenant to exist, with organic acid and metallic copper, there is at ambient temperature the character of complex reaction, with aqueous solutions of organic acids and oxygenant, prepare and obtain liquid medium, surface part by the copper rivet on waste printed circuit board substrate and Copper Foil is dissolved and is made copper rivet separated with the non-metallic material of waste printed circuit board with Copper Foil with liquid medium reaction, obtains non-metallic material and the copper rivet coming off from waste printed circuit board substrate and the Copper Foil of treated waste printed circuit board; Liquid medium after electrolysis is used, the copper in recyclable liquid medium; Liquid medium after electrolysis can be recycled.Liquid medium of the present invention is to the non-metallic material of waste printed circuit board substrate without destruction, and copper rivet is completely separated with non-metallic material with Copper Foil, has avoided the discharge of " three wastes " simultaneously.Reaction conditions of the present invention is gentle, simple to operate, is convenient to control, and cost of material is cheap, and liquid medium is reusable, environmental friendliness.
The metal of waste printed circuit board substrate of the present invention and nonmetallic separation method are: the aqueous solutions of organic acids that secure ph is 2-5 in container, is immersed in the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate in described aqueous solutions of organic acids; Under room temperature, lucifuge condition, dropwise add wherein while stirring aqueous oxidizing agent solution or pass into oxidant gas, preparation obtains being soaked with the liquid medium system of waste printed circuit board substrate; On the surface of observing copper rivet and Copper Foil, have after bubble formation, still continue to drip aqueous oxidizing agent solution or pass into oxidant gas, until copper rivet and Copper Foil depart from after waste printed circuit board substrate, stop dripping aqueous oxidizing agent solution or stop passing into oxidant gas; Take out treated waste printed circuit board substrate, isolate the copper rivet and the Copper Foil that in liquid medium, come off.
The described copper rivet that comes off in liquid medium and the liquid medium after Copper Foil isolated, through electrolysis, the copper in recovering liquid medium.
The described liquid medium after the copper in electrolysis recovering liquid medium, the metal for above-mentioned waste printed circuit board substrate capable of circulation and nonmetallic separated use.
Described stirring is one or more in magnetic agitation, mechanical stirring and sonic oscillation, wherein preferably uses sonic oscillation.
Described organic acid is one or more in glycine, citric acid, acetic acid, formic acid, oxalic acid (oxalic acid), propionic acid, propanedioic acid, succsinic acid (succinic acid), tartrate (2,3 dihydroxybutanedioic acid) and butyric acid.
Described aqueous oxidizing agent solution is one or more in aqueous hydrogen peroxide solution, benzoyl peroxide formic acid, peroxidation disuccinic acid, tertbutyl peroxide and the dibenzoyl peroxide aqueous solution.
Described oxidant gas is selected from the mixed gas (wherein the content of ozone is not less than 5mg/L) of mixed gas (wherein the content of oxygen is not less than 400mg/L), ozone and nitrogen of mixed gas (wherein the content of oxygen is not less than 400mg/L), oxygen and carbonic acid gas of mixed gas, oxygen and the nitrogen of oxygen, ozone, oxygen and ozone, one or more in the mixed gas (wherein the content of ozone is not less than 5mg/L) of smelly oxygen and carbon dioxide.
The metal of waste printed circuit board substrate of the present invention and nonmetallic separation method have following features:
(1) agents useful for same is organic acid and oxygenant, chemical property and reaction conditions are gentle, in reaction process, avoided the discharge of " three wastes ", to the non-metallic material on waste printed circuit board substrate, substantially without destroying, copper rivet is easy to separated with Copper Foil and non-metallic material.
(2) whole treating processes does not need non-metallic material to carry out Mechanical Crushing, and equipment therefor is simple, and processing ease is easy to control, with low cost.
(3) liquid medium after use is easy to process, reusable, environmental friendliness.
Embodiment
Embodiment 1
The glycine solution that secure ph is 5 in container, is immersed in the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate in described glycine solution; Under room temperature, lucifuge condition, dropwise add wherein while stirring aqueous hydrogen peroxide solution, preparation obtains being soaked with the liquid medium system of waste printed circuit board substrate; On the surface of observing copper rivet and Copper Foil, have after bubble formation, still continue to drip described aqueous hydrogen peroxide solution, until copper rivet and Copper Foil depart from after waste printed circuit board substrate, stop dripping described aqueous hydrogen peroxide solution; Take out treated waste printed circuit board substrate, isolate the copper rivet and the Copper Foil that in liquid medium, come off.
The described copper rivet that comes off in liquid medium and the liquid medium after Copper Foil isolated, through electrolysis, the copper in recyclable liquid medium.
The described liquid medium after the copper in electrolysis recovering liquid medium, the metal for above-mentioned waste printed circuit board substrate capable of circulation and nonmetallic separated use.
Embodiment 2
The aqueous acetic acid that secure ph is 2 in container, is immersed in the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate in described aqueous acetic acid; Under room temperature, lucifuge condition, dropwise add wherein while stirring benzoyl peroxide aqueous formic acid, preparation obtains being soaked with the liquid medium system of waste printed circuit board substrate; On the surface of observing copper rivet and Copper Foil, have after bubble formation, still continue to drip described benzoyl peroxide aqueous formic acid, until copper rivet and Copper Foil depart from after waste printed circuit board substrate, stop dripping described benzoyl peroxide aqueous formic acid; Take out treated waste printed circuit board substrate, isolate the copper rivet and the Copper Foil that in liquid medium, come off.
The described copper rivet that comes off in liquid medium and the liquid medium after Copper Foil isolated, through electrolysis, the copper in recyclable liquid medium.
The described liquid medium after the copper in electrolysis recovering liquid medium, the metal for above-mentioned waste printed circuit board substrate capable of circulation and nonmetallic separated use.
Embodiment 3
The mixed aqueous solution of the propionic acid that secure ph is 4 in container and oxalic acid (volume ratio is 1:1), is immersed in the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate in the mixed aqueous solution of described propionic acid and oxalic acid; Under room temperature, lucifuge condition, dropwise add wherein while stirring aqueous hydrogen peroxide solution, preparation obtains being soaked with the liquid medium system of waste printed circuit board substrate; On the surface of observing copper rivet and Copper Foil, have after bubble formation, still continue to drip described aqueous hydrogen peroxide solution, until copper rivet and Copper Foil depart from after waste printed circuit board substrate, stop dripping described aqueous hydrogen peroxide solution; Take out treated waste printed circuit board substrate, isolate the copper rivet and the Copper Foil that in liquid medium, come off.
The described copper rivet that comes off in liquid medium and the liquid medium after Copper Foil isolated, through electrolysis, the copper in recyclable liquid medium.
The described liquid medium after the copper in electrolysis recovering liquid medium, the metal for above-mentioned waste printed circuit board substrate capable of circulation and nonmetallic separated use.
Embodiment 4
The aqueous citric acid solution that secure ph is 3 in container, is immersed in the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate in described aqueous citric acid solution; Under room temperature, lucifuge condition, pass into wherein while stirring oxygen, preparation obtains being soaked with the liquid medium system of waste printed circuit board substrate; On the surface of observing copper rivet and Copper Foil, have after bubble formation, still continue to pass into oxygen, until copper rivet and Copper Foil depart from after waste printed circuit board substrate, stop passing into oxygen; Take out treated waste printed circuit board substrate, isolate the copper rivet and the Copper Foil that in liquid medium, come off.
The described copper rivet that comes off in liquid medium and the liquid medium after Copper Foil isolated, through electrolysis, the copper in recyclable liquid medium.
The described liquid medium after the copper in electrolysis recovering liquid medium, the metal for above-mentioned waste printed circuit board substrate capable of circulation and nonmetallic separated use.
Embodiment 5
The oxalic acid aqueous solution that secure ph is 3 in container, is immersed in the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate in described oxalic acid aqueous solution; Under room temperature, lucifuge condition, dropwise add wherein while stirring the mixed aqueous solution of hydrogen peroxide and dibenzoyl peroxide (volume ratio is 1:1), preparation obtains being soaked with the liquid medium system of waste printed circuit board substrate; On the surface of observing copper rivet and Copper Foil, have after bubble formation, still continue to drip described hydrogen peroxide and the mixed aqueous solution of dibenzoyl peroxide, until copper rivet and Copper Foil depart from after waste printed circuit board substrate, stop dripping described hydrogen peroxide and the mixed aqueous solution of dibenzoyl peroxide; Take out treated waste printed circuit board substrate, isolate the copper rivet and the Copper Foil that in liquid medium, come off.
The described copper rivet that comes off in liquid medium and the liquid medium after Copper Foil isolated, through electrolysis, the copper in recyclable liquid medium.
The described liquid medium after the copper in electrolysis recovering liquid medium, the metal for above-mentioned waste printed circuit board substrate capable of circulation and nonmetallic separated use.
Embodiment 6
The aqueous acetic acid that secure ph is 2 in container, is immersed in the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate in described aqueous acetic acid; Under room temperature, lucifuge condition, pass into wherein while stirring ozone and oxygen (volume ratio is 1:1), preparation obtains being soaked with the liquid medium system of waste printed circuit board substrate; On the surface of observing copper rivet and Copper Foil, have after bubble formation, still continue to pass into ozone and oxygen, until copper rivet and Copper Foil depart from after waste printed circuit board substrate, stop passing into ozone and oxygen; Take out treated waste printed circuit board substrate, isolate the copper rivet and the Copper Foil that in liquid medium, come off.
The described copper rivet that comes off in liquid medium and the liquid medium after Copper Foil isolated, through electrolysis, the copper in recyclable liquid medium.
The described liquid medium after the copper in electrolysis recovering liquid medium, the metal for above-mentioned waste printed circuit board substrate capable of circulation and nonmetallic separated use.
Embodiment 7
The aqueous citric acid solution that secure ph is 3 in container, is immersed in the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate in described aqueous citric acid solution; Under room temperature, lucifuge condition, pass into wherein while stirring the mixed gas (wherein the content of oxygen is 400mg/L) of oxygen and nitrogen, preparation obtains being soaked with the liquid medium system of waste printed circuit board substrate; On the surface of observing copper rivet and Copper Foil, have after bubble formation, still continue to pass into the mixed gas of oxygen and nitrogen, until copper rivet and Copper Foil depart from after waste printed circuit board substrate, stop passing into the mixed gas of oxygen and nitrogen; Take out treated waste printed circuit board substrate, isolate the copper rivet and the Copper Foil that in liquid medium, come off.
The described copper rivet that comes off in liquid medium and the liquid medium after Copper Foil isolated, through electrolysis, the copper in recyclable liquid medium.
The described liquid medium after the copper in electrolysis recovering liquid medium, the metal for above-mentioned waste printed circuit board substrate capable of circulation and nonmetallic separated use.
Embodiment 8
The aqueous acetic acid that secure ph is 2 in container, is immersed in the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate in described aqueous acetic acid; Under room temperature, lucifuge condition, pass into wherein while stirring the mixed gas (wherein the content of ozone is 5～8mg/L) of smelly oxygen and carbon dioxide, preparation obtains being soaked with the liquid medium system of waste printed circuit board substrate; On the surface of observing copper rivet and Copper Foil, have after bubble formation, still continue to pass into the mixed gas of smelly oxygen and carbon dioxide, until copper rivet and Copper Foil depart from after waste printed circuit board substrate, stop passing into the mixed gas of smelly oxygen and carbon dioxide; Take out treated waste printed circuit board substrate, isolate the copper rivet and the Copper Foil that in liquid medium, come off.
The described copper rivet that comes off in liquid medium and the liquid medium after Copper Foil isolated, through electrolysis, the copper in recyclable liquid medium.
The described liquid medium after the copper in electrolysis recovering liquid medium, the metal for above-mentioned waste printed circuit board substrate capable of circulation and nonmetallic separated use.
Claims (7)
1. the metal of a waste printed circuit board substrate and nonmetallic separation method, it is characterized in that: the aqueous solutions of organic acids that secure ph is 2-5 in container, is immersed in the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate in described aqueous solutions of organic acids; Under room temperature, lucifuge condition, dropwise add wherein while stirring aqueous oxidizing agent solution or pass into oxidant gas, preparation obtains being soaked with the liquid medium system of waste printed circuit board substrate; On the surface of observing copper rivet and Copper Foil, have after bubble formation, still continue to drip aqueous oxidizing agent solution or pass into oxidant gas, until copper rivet and Copper Foil depart from after waste printed circuit board substrate, stop dripping aqueous oxidizing agent solution or stop passing into oxidant gas; Take out treated waste printed circuit board substrate, isolate the copper rivet and the Copper Foil that in liquid medium, come off.
2. separation method according to claim 1, is characterized in that: the described copper rivet that comes off in liquid medium and the liquid medium after Copper Foil isolated, and through electrolysis, the copper in recovering liquid medium.
3. separation method according to claim 2, is characterized in that: the described liquid medium after the copper in electrolysis recovering liquid medium, and for metal and the nonmetallic separated use of waste printed circuit board substrate.
4. separation method according to claim 1, is characterized in that: described stirring is one or more in magnetic agitation, mechanical stirring and sonic oscillation.
5. separation method according to claim 1, is characterized in that: described organic acid is one or more in glycine, citric acid, acetic acid, formic acid, oxalic acid, propionic acid, propanedioic acid, succsinic acid, tartrate and butyric acid.
6. method according to claim 1, is characterized in that: described aqueous oxidizing agent solution is one or more in aqueous hydrogen peroxide solution, benzoyl peroxide formic acid, peroxidation disuccinic acid, tertbutyl peroxide and the dibenzoyl peroxide aqueous solution.
7. separation method according to claim 1, is characterized in that: described oxidant gas is selected from the mixed gas of mixed gas, ozone and nitrogen of mixed gas, oxygen and carbonic acid gas of mixed gas, oxygen and nitrogen of oxygen, ozone, oxygen and ozone, one or more in the mixed gas of smelly oxygen and carbon dioxide;
Wherein: the content of the oxygen in the mixed gas of oxygen and nitrogen is not less than 400mg/L, the content of the oxygen in the mixed gas of oxygen and carbonic acid gas is not less than 400mg/L, the content of the ozone in the mixed gas of ozone and nitrogen is not less than 5mg/L, and the content of the ozone in the mixed gas of smelly oxygen and carbon dioxide is not less than 5mg/L.
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| CN201210246532.4A CN103540748B (en) | 2012-07-16 | 2012-07-16 | A kind of metal of waste printed circuit board substrate and nonmetallic separation method |
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| CN103894391A (en) * | 2014-03-27 | 2014-07-02 | 宁波同道恒信环保科技有限公司 | Layered peeling method of circuit board |
| CN108018556A (en) * | 2016-10-31 | 2018-05-11 | 易案爱富科技有限公司 | Etch combination |
| CN110629037A (en) * | 2019-10-21 | 2019-12-31 | 西南科技大学 | Method for leaching copper in waste printed circuit board by using glycine solution |
| CN110757682A (en) * | 2019-10-29 | 2020-02-07 | 中国科学院山西煤炭化学研究所 | Method for recycling waste circuit boards in full-component mode through two-step method |
| CN113292498A (en) * | 2021-06-16 | 2021-08-24 | 浙江工业大学 | 3-peroxybenzoic acid-1-methylimidazole chloride salt and preparation and application thereof |
| CN117600203A (en) * | 2024-01-24 | 2024-02-27 | 江苏云洋电力科技有限公司 | Recycling equipment and recycling method for waste electronic components |
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