CN103667704B - The metal of separating waste, worn printed wiring base board and nonmetallic method - Google Patents
The metal of separating waste, worn printed wiring base board and nonmetallic method Download PDFInfo
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- CN103667704B CN103667704B CN201210344906.6A CN201210344906A CN103667704B CN 103667704 B CN103667704 B CN 103667704B CN 201210344906 A CN201210344906 A CN 201210344906A CN 103667704 B CN103667704 B CN 103667704B
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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 belongs to the recovery of waste printed circuit board, relate to the metal of separating waste, worn printed wiring base board and nonmetallic method.The present invention utilizes when there being oxygenant to exist, the character of complex reaction is there is at ambient temperature with organic amine and metallic copper, carry out preparation with the organic amine aqueous solution and oxygenant and obtain liquid medium, to be reacted with liquid medium by the surface portion of the copper rivet on waste printed circuit board substrate and Copper Foil and dissolve and copper rivet and Copper Foil are separated with the non-metallic material of waste printed circuit board, obtain the non-metallic material of treated waste printed circuit board and the copper rivet come off from waste printed circuit board substrate and Copper Foil; Liquid medium after electrolysis uses, the copper in recyclable liquid medium, the liquid medium after electrolysis can be recycled.Reaction conditions of the present invention is gentle, simple to operate, is convenient to control; Liquid medium to the non-metallic material of waste printed circuit board substrate without destruction, without the discharge of " three wastes ".
Description
Technical field
The invention belongs to the recovery of waste printed circuit board, particularly the metal of separating waste, worn printed wiring base board and nonmetallic method.
Background technology
In recent years because the usage quantity of global electronic equipment sharply increases, cause electronic and electrical equipment, as the discarded amount also rapid growth of televisor, computer, mobile phone and electronic amusement apparatus etc.According to estimates, current China primary electron waste year generation is 1,500,000 tons, account for that China domestic refuse produces total amount per year 1%, and with annual 13% ~ 15% speed increment.In electron wastes, the recycling of printed-wiring board (PWB) is the most complicated, but is also the valuable property of most, 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, copper rivet on substrate and Copper Foil and the electronic devices and components etc. prepared by resin and glass fiber material are formed.Printed-wiring board (PWB) is widely used in the fields such as information, communication, electronics, military affairs, space flight.Along with the development of science and technology and the continuous expansion of every field demand printed-wiring board (PWB), the quantity also sharp increase of the waste printed circuit board produced.Multiple hazardous and noxious substances on the one hand in waste printed circuit board has to pass through recycling; Heavy metal element on the other hand in waste printed circuit board substrate has again high resource recycling and is worth, and is a kind of potential secondary resource.Therefore, rationally the effective waste printed circuit board that reclaims all has great significance to economy and environmental protection.
The recycling of waste printed circuit board generally through disassembling, the process of sorting and recycling.First disassembled by machinery and the electronic devices and components on waste printed circuit board are removed from substrate, then to substrate and copper rivet and Copper Foil, sorting is carried out by the method such as physics or chemistry to the substrate disassembling electronic devices and components, finally each component after sorting is processed and reclaimed.At present there are the methods such as mechanical physical separation, pyrometallurgy sorting and hydrometallurgy sorting to the method that the waste printed circuit board substrate after removing electronic devices and components carries out sorting.Mechanical-physical separating method can be separated with nonmetal realization preferably to metal, its flow process is simple, to environment without destruction, but will pulverize waste printed circuit board substrate during sorting, after sorting, the purity of each component of gained is not high, can not directly be recycled by industry.Pyrometallurgy separating method only has good recovering effect to metal, and under high temperature, non-metallic material are easily decomposed, and the material formed after non-metallic material decomposition has larger harm to human body and environment.The technological principle of hydrometallurgy separating method utilizes the solution with oxidisability to be dipped in solution by substrate under certain condition, the metal ion then in purification leach liquor, thus realize the recycling treatment of waste printed circuit board.But when leaching the metal in substrate with the strong acid such as nitric acid, sulfuric acid and hydrogen peroxide, can there is oxidation and be destroyed in substrate non-metallic material on the one hand; The metal ion dissolved on the other hand also can destroy the molecular structure of non-metallic material on substrate makes non-metallic material performance reduce.When there being oxygenant to exist, organic amine at ambient temperature can optionally with metallic copper generation complex reaction, and do not destroy non-metallic material, obtain the complex solution of single pure copper.Therefore the present invention selects when there being oxygenant to exist, come to react with the copper rivet on waste printed circuit board substrate and Copper Foil with organic amine, copper rivet on waste printed circuit board substrate is separated with non-metallic material with Copper Foil, in its liquid medium, the complex compound of copper can through electrolytic recovery simultaneously, and the liquid medium after electrolysis can be recycled; Neither destroy non-metallic material, high efficiente callback metallic copper, turn avoid the discharge of " three wastes ", environmental friendliness.
Summary of the invention
The object of the invention is to utilize when there being oxygenant to exist, selectivity partial reaction is carried out with the copper rivet on the organic amine aqueous solution and waste printed circuit board substrate and Copper Foil, copper rivet is separated with the non-metallic material on waste printed circuit board with Copper Foil, thus provide that a kind of technique is simple, reaction conditions is gentle, cheap and the metal of eco-friendly separating waste, worn printed wiring base board and nonmetallic method.
The present invention utilizes when there being oxygenant to exist, the character of complex reaction is there is at ambient temperature with organic amine and metallic copper, carry out preparation with the organic amine aqueous solution and oxygenant and obtain liquid medium, to be reacted with liquid medium by the surface portion of the copper rivet on waste printed circuit board substrate and Copper Foil and dissolve and copper rivet and Copper Foil are separated with the non-metallic material of waste printed circuit board, obtain the non-metallic material of treated waste printed circuit board and the copper rivet come off from waste printed circuit board substrate and Copper Foil; Liquid medium after electrolysis uses, 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 separated with non-metallic material completely with Copper Foil, avoids the discharge of " three wastes " simultaneously.Reaction conditions of the present invention is gentle, simple to operate, is convenient to control, and low in raw material price, liquid medium is reusable, environmental friendliness.
Metal and the nonmetallic method of separating waste, worn printed wiring base board of the present invention are: secure ph is the organic amine aqueous solution of 9-12 in a reservoir, the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate are immersed in the described organic amine aqueous solution; Under room temperature, lucifuge condition, dropwise add aqueous oxidizing agent solution while stirring wherein or pass into oxidant gas, preparation obtains being soaked with the single layer substrate of waste printed circuit board substrate and/or the liquid medium systems of multilager base plate; After there is bubble formation on the surface observing copper rivet and Copper Foil, still continue drip aqueous oxidizing agent solution or pass into oxidant gas, until after copper rivet and Copper Foil depart from waste printed circuit board substrate, stop dripping aqueous oxidizing agent solution or stopping passes into oxidant gas; Take out treated waste printed circuit board substrate, isolate the copper rivet and Copper Foil that come off in liquid medium.
Described isolate the liquid medium after the copper rivet and Copper Foil come off in liquid medium, through electrolysis, the copper in recovering liquid medium.
Liquid medium after described copper through electrolysis and in recovering liquid medium, the metal for above-mentioned waste printed circuit board substrate capable of circulation is separated use with nonmetallic.
Described stirring is selected from one or more in magnetic agitation, mechanical stirring and sonic oscillation, wherein preferably uses sonic oscillation.
Described organic amine is selected from one or more in n-Butyl Amine 99, TERTIARY BUTYL AMINE, isobutylamine, quadrol, Monoethanolamine MEA BASF, diethanolamine, trolamine, α-amino isopropyl alcohol, N, N dimethylethanolamine and triethylamine.
Described aqueous oxidizing agent solution is selected from one or more in aqueous hydrogen peroxide solution, the tertbutyl peroxide aqueous solution and the dibenzoyl peroxide aqueous solution.
Described oxidant gas is selected from one or more in the mixed gas (wherein the content of ozone is not less than 5mg/L) of the mixed gas (wherein the content of oxygen is not less than 400mg/L) of the mixed gas (wherein the content of oxygen is not less than 400mg/L) of the mixed gas of oxygen, ozone, oxygen and ozone, oxygen and nitrogen, oxygen and carbonic acid gas, ozone and the mixed gas (wherein the content of ozone is not less than 5mg/L) of nitrogen, smelly oxygen and carbon dioxide.
Metal and the nonmetallic method of separating waste, worn printed wiring base board of the present invention have following features:
(1) agents useful for same is organic amine and oxygenant, chemical property and reaction conditions gentleness, avoid the discharge of " three wastes " in reaction process, to the non-metallic material on waste printed circuit board substrate substantially without destruction, copper rivet is easy to be separated with Copper Foil and non-metallic material.
(2) whole treating processes does not need to carry out Mechanical Crushing to non-metallic material, and equipment therefor is simple, processing ease, is easy to control, with low cost.
(3) liquid medium after using is easy to process, reusable, environmental friendliness.
Embodiment
Embodiment 1
In a reservoir by n-Butyl Amine 99 and water mixing, secure ph is the n-Butyl Amine 99 aqueous solution of 9, the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate is immersed in the described n-Butyl Amine 99 aqueous solution; Under room temperature, lucifuge condition, magnetic agitation limit, limit dropwise adds aqueous hydrogen peroxide solution wherein, and preparation obtains being soaked with the single layer substrate of waste printed circuit board substrate and/or the liquid medium systems of multilager base plate; After there is bubble formation on the surface observing copper rivet and Copper Foil, still continue the aqueous hydrogen peroxide solution described in dripping, until after copper rivet and Copper Foil depart from waste printed circuit board substrate, stop the aqueous hydrogen peroxide solution described in dripping; Take out treated waste printed circuit board substrate, isolate the copper rivet and Copper Foil that come off in liquid medium.
Described isolate the liquid medium after the copper rivet and Copper Foil come off in liquid medium, through electrolysis, the copper in recyclable liquid medium.
Liquid medium after described copper through electrolysis and in recovering liquid medium, the metal for above-mentioned waste printed circuit board substrate capable of circulation is separated use with nonmetallic.
Embodiment 2
In a reservoir by quadrol and water mixing, secure ph is the ethylenediamine solution of 12, the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate is immersed in described ethylenediamine solution; Under room temperature, lucifuge condition, mechanical stirring limit, limit dropwise adds the benzoyl peroxide aqueous solution wherein, and preparation obtains being soaked with the single layer substrate of waste printed circuit board substrate and/or the liquid medium systems of multilager base plate; After there is bubble formation on the surface observing copper rivet and Copper Foil, still continue the dibenzoyl peroxide aqueous solution described in dripping, until after copper rivet and Copper Foil depart from waste printed circuit board substrate, stop the dibenzoyl peroxide aqueous solution described in dripping; Take out treated waste printed circuit board substrate, isolate the copper rivet and Copper Foil that come off in liquid medium.
Described isolate the liquid medium after the copper rivet and Copper Foil come off in liquid medium, through electrolysis, the copper in recyclable liquid medium.
Liquid medium after described copper through electrolysis and in recovering liquid medium, the metal for above-mentioned waste printed circuit board substrate capable of circulation is separated use with nonmetallic.
Embodiment 3
In a reservoir by TERTIARY BUTYL AMINE and isobutylamine (volume ratio is 1:1) and water mixing, secure ph is the TERTIARY BUTYL AMINE of 10 and the mixed aqueous solution of isobutylamine, the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate is immersed in the mixed aqueous solution of described TERTIARY BUTYL AMINE and isobutylamine; Under room temperature, lucifuge condition, magnetic agitation limit, limit dropwise adds aqueous hydrogen peroxide solution wherein, and preparation obtains being soaked with the single layer substrate of waste printed circuit board substrate and/or the liquid medium systems of multilager base plate; After there is bubble formation on the surface observing copper rivet and Copper Foil, still continue the aqueous hydrogen peroxide solution described in dripping, until after copper rivet and Copper Foil depart from waste printed circuit board substrate, stop the aqueous hydrogen peroxide solution described in dripping; Take out treated waste printed circuit board substrate, isolate the copper rivet and Copper Foil that come off in liquid medium.
Described isolate the liquid medium after the copper rivet and Copper Foil come off in liquid medium, through electrolysis, the copper in recyclable liquid medium.
Liquid medium after described copper through electrolysis and in recovering liquid medium, the metal for above-mentioned waste printed circuit board substrate capable of circulation is separated use with nonmetallic.
Embodiment 4
In a reservoir by N, N dimethylethanolamine and water mixing, secure ph is the N of 11, N aqueous dimethylethanolamine, the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate are immersed in described N, in N aqueous dimethylethanolamine; Under room temperature, lucifuge condition, sonic oscillation limit, limit passes into oxygen wherein, and preparation obtains being soaked with the single layer substrate of waste printed circuit board substrate and/or the liquid medium systems of multilager base plate; After there is bubble formation on the surface observing copper rivet and Copper Foil, still continue to pass into oxygen, until after copper rivet and Copper Foil depart from waste printed circuit board substrate, stop passing into oxygen; Take out treated waste printed circuit board substrate, isolate the copper rivet and Copper Foil that come off in liquid medium.
Described isolate the liquid medium after the copper rivet and Copper Foil come off in liquid medium, through electrolysis, the copper in recyclable liquid medium.
Liquid medium after described copper through electrolysis and in recovering liquid medium, the metal for above-mentioned waste printed circuit board substrate capable of circulation is separated use with nonmetallic.
Embodiment 5
In a reservoir by diethanolamine and water mixing, secure ph is the diethanolamine aqueous solution of 9, the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate is immersed in the described diethanolamine aqueous solution; Under room temperature, lucifuge condition, magnetic agitation limit, limit dropwise adds the mixed aqueous solution of hydrogen peroxide and tertbutyl peroxide (volume ratio is 1:1) wherein, and preparation obtains being soaked with the single layer substrate of waste printed circuit board substrate and/or the liquid medium systems of multilager base plate; After there is bubble formation on the surface observing copper rivet and Copper Foil, still continue the hydrogen peroxide described in dripping and the mixed aqueous solution of tertbutyl peroxide, until after copper rivet and Copper Foil depart from waste printed circuit board substrate, stop the mixed aqueous solution of hydrogen peroxide described in dripping and tertbutyl peroxide; Take out treated waste printed circuit board substrate, isolate the copper rivet and Copper Foil that come off in liquid medium.
Described isolate the liquid medium after the copper rivet and Copper Foil come off in liquid medium, through electrolysis, the copper in recyclable liquid medium.
Liquid medium after described copper through electrolysis and in recovering liquid medium, the metal for above-mentioned waste printed circuit board substrate capable of circulation is separated use with nonmetallic.
Embodiment 6
In a reservoir by triethylamine and water mixing, secure ph is the triethylamine aqueous solution of 12, the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate is immersed in described triethylamine aqueous solution; Under room temperature, lucifuge condition, sonic oscillation limit, limit passes into ozone and oxygen (volume ratio is 1:1) wherein, and preparation obtains being soaked with the single layer substrate of waste printed circuit board substrate and/or the liquid medium systems of multilager base plate; After there is bubble formation on the surface observing copper rivet and Copper Foil, still continue to pass into ozone and oxygen, until after copper rivet and Copper Foil depart from waste printed circuit board substrate, stop passing into ozone and oxygen; Take out treated waste printed circuit board substrate, isolate the copper rivet and Copper Foil that come off in liquid medium.
Described isolate the liquid medium after the copper rivet and Copper Foil come off in liquid medium, through electrolysis, the copper in recyclable liquid medium.
Liquid medium after described copper through electrolysis and in recovering liquid medium, the metal for above-mentioned waste printed circuit board substrate capable of circulation is separated use with nonmetallic.
Embodiment 7
In a reservoir by α-amino isopropyl alcohol and water mixing, secure ph is the α-amino isopropyl alcohol aqueous solution of 10, the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate is immersed in the described α-amino isopropyl alcohol aqueous solution; Under room temperature, lucifuge condition, sonic oscillation limit, limit passes into the mixed gas (wherein the content of oxygen is 400mg/L) of oxygen and nitrogen wherein, and preparation obtains being soaked with the single layer substrate of waste printed circuit board substrate and/or the liquid medium systems of multilager base plate; After there is bubble formation on the surface observing copper rivet and Copper Foil, still continue the mixed gas passing into oxygen and nitrogen, until after copper rivet and Copper Foil depart from waste printed circuit board substrate, stop the mixed gas passing into oxygen and nitrogen; Take out treated waste printed circuit board substrate, isolate the copper rivet and Copper Foil that come off in liquid medium.
Described isolate the liquid medium after the copper rivet and Copper Foil come off in liquid medium, through electrolysis, the copper in recyclable liquid medium.
Liquid medium after described copper through electrolysis and in recovering liquid medium, the metal for above-mentioned waste printed circuit board substrate capable of circulation is separated use with nonmetallic.
Embodiment 8
In a reservoir by quadrol and water mixing, secure ph is the ethylenediamine solution of 11, the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate is immersed in described ethylenediamine solution; Under room temperature, lucifuge condition, sonic oscillation limit, limit passes into the mixed gas (wherein the content of ozone is 5 ~ 8mg/L) of smelly oxygen and carbon dioxide wherein, and preparation obtains being soaked with the single layer substrate of waste printed circuit board substrate and/or the liquid medium systems of multilager base plate; After there is bubble formation on the surface observing copper rivet and Copper Foil, still continue the mixed gas passing into smelly oxygen and carbon dioxide, until after copper rivet and Copper Foil depart from waste printed circuit board substrate, stop the mixed gas passing into smelly oxygen and carbon dioxide; Take out treated waste printed circuit board substrate, isolate the copper rivet and Copper Foil that come off in liquid medium.
Described isolate the liquid medium after the copper rivet and Copper Foil come off in liquid medium, through electrolysis, the copper in recyclable liquid medium.
Liquid medium after described copper through electrolysis and in recovering liquid medium, the metal for above-mentioned waste printed circuit board substrate capable of circulation is separated use with nonmetallic.
Claims (7)
1. the metal of a separating waste, worn printed wiring base board and nonmetallic method, it is characterized in that: secure ph is the organic amine aqueous solution of 9-12 in a reservoir, the single layer substrate of the waste printed circuit board with copper rivet and Copper Foil and/or multilager base plate are immersed in the described organic amine aqueous solution; Under room temperature, lucifuge condition, dropwise add aqueous oxidizing agent solution while stirring wherein or pass into oxidant gas, preparation obtains being soaked with the single layer substrate of waste printed circuit board substrate and/or the liquid medium systems of multilager base plate; After there is bubble formation on the surface observing copper rivet and Copper Foil, still continue drip aqueous oxidizing agent solution or pass into oxidant gas, until after copper rivet and Copper Foil depart from waste printed circuit board substrate, stop dripping aqueous oxidizing agent solution or stopping passes into oxidant gas; Take out treated waste printed circuit board substrate, isolate the copper rivet and Copper Foil that come off in liquid medium.
2. method according to claim 1, is characterized in that: described isolate the liquid medium after the copper rivet and Copper Foil come off in liquid medium, through electrolysis, and the copper in recovering liquid medium.
3. method according to claim 2, is characterized in that: the liquid medium after described copper through electrolysis and in recovering liquid medium, the metal for waste printed circuit board substrate is separated use with nonmetallic.
4. method according to claim 1, is characterized in that: described stirring is selected from one or more in magnetic agitation, mechanical stirring and sonic oscillation.
5. method according to claim 1, it is characterized in that: described organic amine is selected from one or more in n-Butyl Amine 99, TERTIARY BUTYL AMINE, isobutylamine, quadrol, Monoethanolamine MEA BASF, diethanolamine, trolamine, α-amino isopropyl alcohol, N, N dimethylethanolamine and triethylamine.
6. method according to claim 1, is characterized in that: described aqueous oxidizing agent solution is selected from one or more in aqueous hydrogen peroxide solution, the tertbutyl peroxide aqueous solution and the dibenzoyl peroxide aqueous solution.
7. method according to claim 1, is characterized in that: described oxidant gas is selected from one or more in the mixed gas of the mixed gas of the mixed gas of the mixed gas of oxygen, ozone, oxygen and ozone, oxygen and nitrogen, oxygen and carbonic acid gas, ozone and the mixed gas of nitrogen, 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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| Application Number | Priority Date | Filing Date | Title |
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| CN201210344906.6A CN103667704B (en) | 2012-09-17 | 2012-09-17 | The metal of separating waste, worn printed wiring base board and nonmetallic method |
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| CN201210344906.6A CN103667704B (en) | 2012-09-17 | 2012-09-17 | The metal of separating waste, worn printed wiring base board and nonmetallic method |
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| CN103667704B true CN103667704B (en) | 2015-10-28 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN112239807A (en) * | 2020-10-28 | 2021-01-19 | 昆明理工大学 | Method for removing copper by ozone oxidation enhanced by ultrasonic |
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- 2012-09-17 CN CN201210344906.6A patent/CN103667704B/en active Active
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| JPH10183264A (en) * | 1996-12-19 | 1998-07-14 | Matsushita Electric Ind Co Ltd | Method for recovering copper from glass epoxy substrate |
| EP0942070A1 (en) * | 1998-03-13 | 1999-09-15 | Delphi Technologies, Inc. | Recovery of metal values from polyester circuit boards by treatment in alkaline solutions of higher alcohols |
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