CN103614556B - A kind of process of waste mobile phone wiring board and the method for recovery noble metal - Google Patents

A kind of process of waste mobile phone wiring board and the method for recovery noble metal Download PDF

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CN103614556B
CN103614556B CN201310462614.7A CN201310462614A CN103614556B CN 103614556 B CN103614556 B CN 103614556B CN 201310462614 A CN201310462614 A CN 201310462614A CN 103614556 B CN103614556 B CN 103614556B
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residue
mobile phone
wiring board
washing
waste mobile
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CN103614556A (en
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华庆亮
武伟男
高麒麟
刘晶
蔡钊荣
马振彦
肖朋
姚晓琳
刘佳丽
王梦
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DALIAN DONGTAI INDUSTRIAL WASTE TREATMENT Co Ltd
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DALIAN DONGTAI INDUSTRIAL WASTE TREATMENT Co Ltd
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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 process of waste mobile phone wiring board and a method for recovery noble metal, burn after the fragmentation of waste mobile phone wiring board; Washing residue after burning; After washing, residue is immersed in sulfuric acid and stirs, and produces copper sulfate product after filtrate is concentrated; Residual sulfuric acid is removed in filter residue washing; After washing, residue adds nitric acid, filters after stirring; Filtrate and filter residue process respectively, pass into O in filtrate 3filter after carrying out oxidizing reaction, filter residue is palladous oxide product, produces Silver Nitrate product after filtrate is concentrated; Filter residue heating is dissolved in chloroazotic acid reacts; Add sodium hydroxide or potassium hydroxide adjustment pH? 10-12, filter, residue is homogeneous heating 30-40min at 140-150 DEG C; Temperature is adjusted to 250-300 DEG C of homogeneous heating 20-30min again, produces golden product.The present invention by the harmless treatment of waste mobile phone wiring board and by wherein noble metal reclaim, solve the pollution problem of waste mobile phone wiring board, and avoid the waste of valuable resource.

Description

A kind of process of waste mobile phone wiring board and the method for recovery noble metal
Technical field
The invention belongs to Electronic Wastes process field, particularly the treatment process of cell phone lines plate.
Background technology
Treatment process at present about wiring board mainly contains following several:
The physiochemical mutagens technique of metal concentrate in A, waste printed circuit board
Whole flow process all adopts machine to subtract the method with physical separation, and final separation obtains the metal concentrate of Multiple components and nonmetal enrich body, can not collect all kinds of noble metal respectively, directly reach the effect of purification.
B, a kind of method carrying gold from useless circuit card
Secondary pickling is adopted to carry out pre-treatment to useless board metal particle, once leach the base metal based on copper adopting nitric acid-sulfuric acid mixed acid solution to leach trapping gold in useless circuit card, by the secondary stripping of dilute nitric acid solution to base metal, the a small amount of oxynitride produced in reaction adopts water to absorb, use non-cyanogen complexing agent thiocarbamide Selectively leaching gold and silver subsequently, finally utilize the gold and silver in base metal iron replacement leach liquor, realize the resource reclaim of gold and silver.Although the method can collect noble metal gold and silver respectively, in treating processes, can the obnoxious flavoures such as oxynitride be produced, form secondary pollution, really can not reach the object of environmental protection.
C, printed circuit board waste process and resource reusing method
Printed circuit board waste process and resource reusing method, by the rich resin of copper system that PCB scrap stock obtain after pulverizing and being separated, generate cupric oxide by high temperature is scorching hot.This method only can collect metallic copper.
D, electrolysis process is utilized directly to reclaim the method for waste circuit board copper
Anode electrolytic cell and waste and old circuit board can relative movement, when anode is connected with waste and old circuit board, waste and old circuit board and anode connected component are in conduction state, utilize anode with the mutual motion of waste and old circuit board, the Copper Foil of different sites on waste and old circuit board can be connected successively with anode, thus the Copper Foil on whole waste and old circuit board can be conducted electricity, separate out into electrolytic copper by electrolytic reaction from negative electrode.This method not only can not collect multiple noble metal, and needs to consume unnecessary energy consumption.
E, to utilize in old circuit board copper for the method for copper sulfate
Pre-treatment is carried out to old circuit board, makes metal and nonmetally to dissociate, to obtain 30 ~ 60 object metal powders; Then by above-mentioned metal powder with mass volume ratio be 1: 10 ~ 20 ratio and concentration be 0.8 ~ 1.5mol/L dilute sulphuric acid mixes, and add sodium-chlor and copper sulfate, make its mass percent concentration reach 5% ~ 10% and 2% ~ 5% respectively; In above-mentioned reaction solution, blast air, react 6 ~ 12 hours under room temperature; Filter, gained filtrate carries out evaporative crystallization, namely obtains CuSO45H2O.This method only can collect copper metal, and reaction time is short.
To sum up, present stage, waste mobile phone treatment process can only continue to reclaim for one-component wherein, so just causes the waste of other valuable resources, and may to environment.Processing cost is higher.
Summary of the invention
The object of this invention is to provide a kind of process of waste mobile phone wiring board and reclaim the method for noble metal, cell phone lines plate containing heavy metal can be carried out harmless treatment by the method, and the noble metal wherein with recovery value is carried out Resource recovery utilization respectively, treatment process is gentle, non-secondary pollution.
The technical solution adopted for the present invention to solve the technical problems is: a kind of process of waste mobile phone wiring board and the method for recovery noble metal, and concrete steps are:
(1) after waste mobile phone wiring board being carried out fragmentation, at 600 DEG C, burning at least 30min(take 30min as the best), collect residue after burning;
(2) after burning, residue water is washed, and after burning, in residue, light materials (plastics etc.) is washed off, collects residue after washing;
(3) residue after washing is immersed in the H of excessive mass concentration 10-20% 2sO 4in solution, stir after 10-15min, filter, filtrate carry out concentrated after produce CuSO 4product, collects separately;
(4) the filter residue washing after filtering, removes residual H 2sO 4;
After (5) (4) step washings, residue is not less than the HNO of 0.5mol/L 3solution (concentration take 0.5mol/L as the best), after stirring 10-30min, filters, collects filtrate and filter residue respectively;
(6) continue to pass into O in the filtrate of (5) step collection 3carry out oxidizing reaction (O 3reusable edible), reaction 10-30min, rear filtration, filter residue is Pd 2o 3product, collects separately; After filtrate is concentrated, produces Silver Nitrate product, collect separately;
(7) by the filter residue that step (5) is collected, be dipped in chloroazotic acid, be heated to obviously micro-boiling, reaction 30-40min;
(8) in the reacted solution of (7) step, add the NaOH of mass concentration 20-40% or KOH solution (take concentration as 30-40% be the best), adjustment pH is 10-12, produces yellowish brown residue, filters;
(9) by the yellowish brown residue after filtration, homogeneous heating 30-40min at 140-150 DEG C; Temperature is adjusted to 250-300 DEG C of homogeneous heating 20-30min again, produces Au product.
The washing waste water produced in described technological process enters sewage plant and processes, and discarded residue carries out sanitary landfill process.
Present invention process method, carries out harmless treatment by waste mobile phone wiring board and is reclaimed by noble metal wherein, thus solves waste mobile phone wiring board heavy metal pollution problem, and avoids the waste of valuable resource.There is following beneficial effect after testing: one ton of useless mobile phone, after processing is refined, the Pd of about 100g can be produced, the Cu of the Au of 300-400g, about 500g about Ag and 2kg.Still there is the heavy metal of other kinds in another waste mobile phone, if arbitrarily abandon, all can causes no small pollution by our environment of life.So present method, carries out harmless treatment by waste mobile phone wiring board and is reclaimed by noble metal wherein, directly solves waste mobile phone wiring board to the problem such as environment and the wasting of resources, creates considerable environmental benefit and economic benefit.
This method has the quality that other treatment processs do not possess:
(1) treatment effect is good: after this method processes, and the heavy metal in waste mobile phone wiring board is all collected, and carries out safe disposal.As the noble metals such as Cu, Ag, Pd, Au all carry out reclaiming rear recycling.Eliminate the problem such as heavy metal environmental pollution and the wasting of resources in waste mobile phone circuit.
(2) recovery value is high: in treating processes, has reclaimed the noble metal in old circuit board plate, as Cu, Ag, Pd, Au etc., obtains very high value added.
Accompanying drawing explanation
Fig. 1 is waste mobile phone wiring board of the present invention process and the process flow sheet reclaiming noble metal.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in detail.
Embodiment 1
The process of waste mobile phone wiring board and a method for recovery noble metal, its practice is:
(1) after 1kg waste mobile phone wiring board being carried out fragmentation, at 600 DEG C, burn 30min, collect residue after burning;
(2) after burning, residue water is washed, and after burning, in residue, light materials (plastics etc.) is washed off, collects residue after washing;
(3) residue after washing is immersed in the H of excessive mass concentration 20% 2sO 4in solution, stir after 12min, filter, filtrate carry out concentrated after produce CuSO 4product, collects separately;
(4) the filter residue washing after filtering, removes residual H 2sO 4;
(5) residue after (4) step washing is immersed in the HNO of 0.5mol/L 3solution, after stirring 30min, filters, collects filtrate and filter residue respectively;
(6) continue to pass into O in the filtrate of (5) step collection 3carry out oxidizing reaction, reaction 20min, rear filtration, filter residue is Pd 2o 3product, collects separately; After filtrate is concentrated, produces Silver Nitrate product, collect separately;
(7) by the filter residue that step (5) is collected, be dipped in chloroazotic acid, be heated to obviously micro-boiling, reaction 40min;
(8) in the reacted solution of (7) step, add the NaOH solution of mass concentration 30%, regulate pH to be 11, produce yellowish brown residue, filter;
(9) by the yellowish brown residue after filtration, homogeneous heating 30min at 145 DEG C; Temperature is adjusted to 256 DEG C of homogeneous heating 25min again, produces Au product.
(10), after this has tested, Pd0.1g, Au0.3g, Ag0.5g and CuSO is collected altogether 45g.
Embodiment 2
The process of waste mobile phone wiring board and a method for recovery noble metal, its practice is:
(1) after 1kg waste mobile phone wiring board being carried out fragmentation, at 600 DEG C, burn 30min, collect residue after burning;
(2) after burning, residue water is washed, and after burning, in residue, light materials (plastics etc.) is washed off, collects residue after washing;
(3) residue after washing is immersed in the H of excessive mass concentration 10% 2sO 4in solution, stir after 10min, filter, filtrate carry out concentrated after produce CuSO 4product, collects separately;
(4) the filter residue washing after filtering, removes residual H 2sO 4;
(5) residue after (4) step washing is immersed in the HNO of 0.5mol/L 3solution, after stirring 30min, filters, collects filtrate and filter residue respectively;
(6) continue to pass into O in the filtrate of (5) step collection 3carry out oxidizing reaction, reaction 20min, rear filtration, filter residue is Pd 2o 3product, collects separately; After filtrate is concentrated, produces Silver Nitrate product, collect separately;
(7) by the filter residue that step (5) is collected, be dipped in chloroazotic acid, be heated to obviously micro-boiling, reaction 40min;
(8) in the reacted solution of (7) step, add the NaOH solution of mass concentration 40%, regulate pH to be 11, produce yellowish brown residue, filter;
(9) by the yellowish brown residue after filtration, homogeneous heating 30min at 145 DEG C; Temperature is adjusted to 256 DEG C of homogeneous heating 25min again, produces Au product.
(10), after this has tested, Pd0.1g, Au0.29g, Ag0.5g and CuSO is collected altogether 44.5g.
Embodiment 3
The process of waste mobile phone wiring board and a method for recovery noble metal, its practice is:
(1) after 1kg waste mobile phone wiring board being carried out fragmentation, at 600 DEG C, burn 30min, collect residue after burning;
(2) after burning, residue water is washed, and after burning, in residue, light materials (plastics etc.) is washed off, collects residue after washing;
(3) residue after washing is immersed in the H of excessive mass concentration 20% 2sO 4in solution, stir after 10min, filter, filtrate carry out concentrated after produce CuSO 4product, collects separately;
(4) the filter residue washing after filtering, removes residual H 2sO 4;
(5) residue after (4) step washing is immersed in the HNO of 0.5mol/L 3solution, after stirring 30min, filters, collects filtrate and filter residue respectively;
(6) continue to pass into O in the filtrate of (5) step collection 3carry out oxidizing reaction, reaction 20min, rear filtration, filter residue is Pd 2o 3product, collects separately; After filtrate is concentrated, produces Silver Nitrate product, collect separately;
(7) by the filter residue that step (5) is collected, be dipped in chloroazotic acid, be heated to obviously micro-boiling, reaction 40min;
(8) in the reacted solution of (7) step, add the KOH solution of mass concentration 30%, regulate pH to be 11, produce yellowish brown residue, filter;
(9) by the yellowish brown residue after filtration, homogeneous heating 30min at 145 DEG C; Temperature is adjusted to 256 DEG C of homogeneous heating 25min again, produces Au product.
After this has tested, collect Pd0.09g, Au0.31g, Ag0.48g and CuSO altogether 44.8g.

Claims (5)

1. the process of waste mobile phone wiring board and a method for recovery noble metal, is characterized in that: concrete steps are:
(1) after waste mobile phone wiring board being carried out fragmentation, at 600 DEG C, burn at least 30min, collect residue after burning;
(2) after burning, residue water is washed, and light materials in residue after burning is washed off, collects residue after washing;
(3) residue after washing is immersed in the H of excessive mass concentration 10-20% 2sO 4in solution, stir after 10-15min, filter, filtrate carry out concentrated after produce CuSO 4product, collects separately;
(4) the filter residue washing after filtering, removes residual H 2sO 4;
The HNO of 0.5-1.0mol/L is added in residue after (5) (4) step washings 3solution, after stirring 10-30min, filters, collects filtrate and filter residue respectively;
(6) continue to pass into O in the filtrate of (5) step collection 3carry out oxidizing reaction, reaction 10-30min, rear filtration, filter residue is Pd 2o 3product, collects separately; After filtrate is concentrated, produces Silver Nitrate product, collect separately;
(7) by the filter residue that step (5) is collected, be dipped in chloroazotic acid, be heated to obviously micro-boiling, reaction 30-40min;
(8) in the reacted solution of (7) step, add NaOH or the KOH solution of mass concentration 20-40%, adjustment pH is 10-12, produces yellowish brown residue, filters;
(9) by the yellowish brown residue after filtration, homogeneous heating 30-40min at 140-150 DEG C; Temperature is adjusted to 250-300 DEG C of homogeneous heating 20-30min again, produces Au product.
2. the process of a kind of waste mobile phone wiring board according to claim 1 and the method for recovery noble metal, it is characterized in that: the washing waste water produced in described method enters sewage plant and processes, discarded residue carries out sanitary landfill process.
3. the process of a kind of waste mobile phone wiring board according to claim 1 and the method for recovery noble metal, is characterized in that: after waste mobile phone wiring board is carried out fragmentation by described (1), at 600 DEG C, burn 30min.
4. the process of a kind of waste mobile phone wiring board according to claim 1 and the method for recovery noble metal, is characterized in that: described (5): the HNO adding concentration 0.5mol/L after (4) step washing in residue 3solution, consumption did not have residue.
5. the process of a kind of waste mobile phone wiring board according to claim 1 and the method for recovery noble metal, it is characterized in that: described (8): in the reacted solution of (7) step, add mass concentration 30-40% NaOH or KOH solution, adjustment pH is 10-12.
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CN104060094B (en) * 2014-06-10 2016-05-11 福建工程学院 A kind of method that reclaims gold and copper from discarded mobile phone
CN104532005B (en) * 2014-12-23 2016-09-14 清远市东江环保技术有限公司 A kind of method of discarded printed circuit boards comprehensive utilization of resources
CN104624611B (en) * 2015-01-23 2016-06-22 长沙紫宸科技开发有限公司 A kind of discarded appliance circuit plate energy method for innocent treatment
CN105087944B (en) * 2015-09-18 2017-08-25 河南省冶金研究所有限责任公司 A kind of method that valuable metal is reclaimed from electron wastes
CN105483386A (en) * 2015-12-09 2016-04-13 清华大学 Method for leaching copper from single-layer waste circuit board
WO2017120815A1 (en) * 2016-01-14 2017-07-20 Entegris, Inc. Integrated electronic waste recycling and recovery system and process of using same
CN105921496A (en) * 2016-06-13 2016-09-07 王枝宝 Waste circuit board residue treatment method
CN107217148A (en) * 2017-06-08 2017-09-29 合肥峰腾节能科技有限公司 A kind of energy-saving processing method of waste electron wiring board
CN107400780A (en) * 2017-07-18 2017-11-28 四川长虹电器股份有限公司 A kind of method that gold, silver and bronze are extracted in the plate from cell phone lines
CN113403479B (en) * 2021-06-21 2024-01-26 苏州市富荣环保科技有限公司 Recovery process of precious metal of waste circuit board

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