CN104451150A - Method for removing lead in metals of waste circuit boards - Google Patents
Method for removing lead in metals of waste circuit boards Download PDFInfo
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- CN104451150A CN104451150A CN201310437131.1A CN201310437131A CN104451150A CN 104451150 A CN104451150 A CN 104451150A CN 201310437131 A CN201310437131 A CN 201310437131A CN 104451150 A CN104451150 A CN 104451150A
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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
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- 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 discloses a method for removing lead in metals of waste circuit boards. The method comprises the following steps: putting mixed metals of the waste circuit boards into a quartz crucible by applying a vacuum distillation technology, and further putting the crucible into a heating chamber of a main evaporation chamber of a vacuum heating furnace; starting a water-cooling system; opening a door before closing of the main evaporation chamber, and starting a vacuum unit to vacuumize the vacuum heating furnace to enable the pressure in a cavity of a furnace body to achieve 0.1Pa-0.5Pa, wherein a first-segment collection chamber and a second-segment collection chamber are not subjected to heating control, and the collection chambers are taken as a whole for working at normal temperature; heating the main evaporation chamber to 900 DEG C, keeping the temperature constant for 0.5h-1.5h, gasifying lead in the mixed metals, and depositing in the collection chambers; cooling the vacuum heating furnace to room temperature after heating is stopped, restoring pressure to normal pressure, taking out the crucible, collecting quartz glass tubes in the collection chambers, and recovering the metals. By adopting the method disclosed by the invention, the problems of consumption of chemical reagents, secondary pollution of residual waste liquid and the like do not exist.
Description
Technical field
The present invention relates to removal plumbous in metal of waste circuit board, particularly use vacuum distillation technique to remove method plumbous in metal of waste circuit board.
Background technology
Along with the high speed development of information industry, industrial scale and the range of application of wiring board constantly expand, and the renewal speed of information equipment is accelerated gradually, creates a large amount of electron wastes, and the quantity of old circuit board also increases year by year.In printed circuit board, metal content is very high, and the mineral reserve metal content existed than nature is much higher, according to the literature, wherein containing copper 20%, and iron 8%, nickel 2%, tin 4%, plumbous 2%, aluminium 2%, zinc 1%, antimony 0.4%, also containing precious metals such as a small amount of gold and silver palladiums.If the metal in old circuit board directly abandons and not only wastes resource, the heavy metals such as lead wherein also can serious environment pollution.Therefore environmental protection, economy, efficient method must be utilized to carry out resource utilization and harm reduction process to the metal in old circuit board.
Current old circuit board resource technology mainly comprises pneumatic separation, the mechanical treatment sorting method such as electrostatic separation, and strong acid or strong oxidizer dissolve, the chemical treatment methods such as pyrolysis and bioremediation.Wherein chemical treatment method and bioremediation are in the laboratory study stage mostly, there is the rate of recovery low, secondary pollution problems, and mechanical treatment sorting method does not produce secondary pollution, and are easy to realize through engineering approaches.Chinese invention patent " process for breaking, separating and recovering of waste printed circuit board and equipment used thereof " (Shen Zhigang etc., the patent No. 99102862.7) wiring board is ground into particle, fine powder is broken further again, simultaneously, selection by winnowing is passed through in Powdered discharging, non-metal powder is separated, metal is realized being separated by air trap with nonmetal powder mix.Chinese invention patent " fragmentation of waste and old printed circuit board and high-pressure electrostatic separation method " (Xu Zhenming etc., the patent No. 200510023785.5) wiring board is first broken, pulverize again, then high pressure static electricity method is adopted, producing electrostatic attraction by stationary electrode to metallic particles makes it fall into metal collection district, electronegative non-metallic particle is subject to electrode repels and finally falls into non-metal collection district, realizes nonmetal and metal separation.
Old circuit board is through pneumatic separation, after the mechanical sorting method process such as electrostatic separation, achieve metal to be separated with nonmetallic, obtain metal mixture, and the target of metals resources is the preparation of pure metal, therefore at metal with on the nonmetal basis be separated, Separation and Recovery to be carried out to metal mixture.For separation and the recovery of metal mixture, there is the technique means such as hydrometallurgy and electrolysis at present.Chinese invention patent " a kind of method of wet separation zinc, copper, cadmium, plumbous metallurgical material and application " (Long Shiming, the patent No. 99115282.4) material is carried out Oxidation Leaching, complexing is replaced, the segregation four procedure process of the separation of copper cadmium and zinc, isolates metallic zinc, copper, cadmium, lead respectively from Non-ferrous Metallurgy material.Chinese invention patent " novel process with waste copper slag remanufacture electrolytic zinc copper " (Pan Tonghua, the patent No. 92104817.3) is starting raw material with brass waste residue, through acid-soluble, deironing press filtration, purification, zinc electrolysis, copper stripping, the steps such as cupric electrolysis, remanufacture electrolytic zinc, copper.Although above method can realize separation and the recovery of metal mixture, a large amount of chemical reagent be consumed, and produce a large amount of waste liquid, cause secondary pollution.In addition, in old circuit board, the resource utilization of copper and precious metal receives very big concern, but the harm reduction with the lead of high saturated vapor pressure fails to cause enough attention.
Summary of the invention
The object of the invention is the deficiency for above-mentioned technique means, provide and use vacuum distillation technique to remove method plumbous in metal of waste circuit board.
The present invention adopts Chinese invention patent " device and method of heating under vacuum separating metal copper-lead mixture " (Ding Hui etc., the patent No. 200910311037.5) heating under vacuum furnace apparatus realize the removal harm reduction of metallic lead, and heated for controlling temperature is not carried out to collecting chamber, make it work at normal temperatures as an entirety.Handling object of the present invention is the hybrid metal of old circuit board gained after the method process such as mechanical sorting.
Use the device of heating under vacuum separating metal copper-lead mixture, remove method plumbous in metal of waste circuit board by the principle of vacuum distilling, comprise the following steps:
I. old circuit board hybrid metal is put in quartz crucible, then crucible is put in the heating chamber of vacuum furnace evaporator main room; Start water-cooling system;
Ii. close evaporator main room button fly front, start vacuum pump set and vacuum furnace is vacuumized, make body of heater chamber inner pressure reach 0.1Pa ~ 0.5Pa by force;
Iii. first paragraph collecting chamber and second segment collecting chamber do not carry out computer heating control, and collecting chamber works at normal temperatures as an entirety;
Iv. evaporator main room is heated to 900 DEG C, steady temperature 0.5h ~ 1.5h, the lead gasification in hybrid metal, and deposits at collecting chamber;
V. after stopping heating, vacuum furnace is cooled to room temperature, and recovers pressure to normal pressure, take out crucible and collecting chamber quartz glass tube, Footwall drift.
The present invention utilizes the method for vacuum distilling, can environmental protection, economical, and realize removal harm reduction plumbous in metal of waste circuit board efficiently, working method is simple and easy to do.Comparing with technique means such as electrolysis with hydrometallurgy, there is not the consumption of chemical reagent and the secondary pollution problems of remaining waste in method of the present invention.
Accompanying drawing explanation
Fig. 1 is the vacuum furnace front view utilized in the present invention.
Fig. 2 is the vacuum furnace left view utilized in the present invention.
The vacuum furnace vertical view utilized in the true the present invention of Fig. 3.
Wherein, 1 is frame, and 2 is vacuum chamber components, and 3 is evaporator main room button fly front, 4 is heater assembly, and 5 is electric furnace I, and 6 is electric furnace II, and 7 is boiler tube, 8 is prolong, and 9 is excessively manage, and 10 is vacuum system, 11 is water cooled electrode assembly, and 12 is hinge component, and 13 is door lock assembly, 14 is back up pad, and 15 is blind plate, and 16 is evaporator main room, 17 is 1000 DEG C ~ 500 DEG C collecting chambers, and 18 is 500 DEG C ~ 300 DEG C collecting chambers, and 19 is 20 DEG C of collecting chambers.
Embodiment
The present invention adopts equipment as shown in Figure 1.Vacuum furnace is positioned in frame 1 under the support of back up pad 14, and evaporator main room button fly front 3 is connected with body of heater with door lock assembly 13 by hinge component 12, and body of heater realizes sealing by vacuum chamber components 2 and blind plate 15.The quartz glass tube of collecting chamber is using boiler tube 7 as stainless steel casing, and 20 DEG C of collecting chambers 19 utilize prolong 8 to realize water-cooled effect, and are connected with vacuum system 10 by excessive pipe 9.
Material is positioned in the heating chamber of vacuum furnace evaporator main room 16, starts vacuum system 10.Electric furnace I 5 and electric furnace II 6 do not work in the present invention.Water cooled electrode assembly 11 is energized, and heater assembly 4 starts to heat evaporator main room 16 and constant temperature, and in this process, metallic lead gasification also deposits in 1000 DEG C ~ 500 DEG C collecting chambers, 17,500 DEG C ~ 300 DEG C collecting chambers 18 and 20 DEG C of collecting chambers 19.
Evaporator main room adopts stainless steel, has button fly front and Double water-cooled structure.The heating member of evaporator main room heating system adopts Graphite Electrodes, and heat shield system adopts five layers of stainless steel, and have certain interval between layers to reduce thermal conduction, thermal insulation material and inboard wall of furnace body are point cantact ceramic insulation.Evaporator main room top temperature 1200 DEG C.
1000 DEG C ~ 500 DEG C collecting chambers and 500 DEG C ~ 300 DEG C collecting chambers adopt quartz glass tube, and the heating member of heating system adopts spirrillum iron-chrome-aluminum resistive heating type chamber type electric resistance furnace, has stainless steel casing, is installed on quartz glass tube outside.Heat shield system adopts asbestos material.1000 DEG C ~ 500 DEG C collecting chamber thermostat temperatures are 1000 DEG C ~ 500 DEG C, and temperature can regulable control.500 DEG C ~ 300 DEG C collecting chamber thermostat temperatures are 500 DEG C ~ 300 DEG C, and temperature can regulable control.
20 DEG C of collecting chambers adopt quartz glass tube, have water-cooling structure.Stainless steel casing is installed on quartz glass tube outside.
The vacuum pump set of vacuum system is by mechanical pump, and diffusion pump and flapper valve composition, measuring system adopts digital display compound vacuum gauge measurement of vacuum.Relatively fixed part adopts metallic seal, and moving part adopts viton sealing.In chamber, ultimate pressure is 8.0 × 10
-4pa(pressure measurement point is positioned at 20 DEG C of collecting chamber ends).
For removal harm reduction plumbous in old circuit board hybrid metal, the present invention adopts vacuum distillation technique, utilizes metal to have different gasification temperatures at the same pressure, heating and gasifying metallic lead, thus reaches the object removing lead.The present invention heats old circuit board hybrid metal under a high vacuum, the corresponding reduction of gasification temperature, reduces energy expenditure.Below by way of specific embodiment, the invention will be further described.
Embodiment 1
Old circuit board hybrid metal (plumbous massfraction is 5%) 20g is put in quartz crucible, then is put into by crucible in the heating chamber of vacuum furnace evaporator main room.Close evaporator main room button fly front, start vacuum system and vacuum furnace is vacuumized, make body of heater chamber inner pressure reach 0.1Pa by force.Evaporator main room is heated to 900 DEG C, constant temperature 0.5h.After stopping heating, vacuum furnace is cooled to room temperature, and recovers pressure to normal pressure.Take out crucible and collecting chamber quartz glass tube, namely the lead of removal be deposited in Glass tubing.Plumbous clearance is 99.67%.
Embodiment 2
Old circuit board hybrid metal (plumbous massfraction is 5%) 20g is put in quartz crucible, then is put into by crucible in the heating chamber of vacuum furnace evaporator main room.Close evaporator main room button fly front, start vacuum system and vacuum furnace is vacuumized, make body of heater chamber inner pressure reach 0.2Pa by force.Evaporator main room is heated to 900 DEG C, constant temperature 0.5h.After stopping heating, vacuum furnace is cooled to room temperature, and recovers pressure to normal pressure.Take out crucible and collecting chamber quartz glass tube, namely the lead of removal be deposited in Glass tubing.Plumbous clearance is 99.83%.
Embodiment 3
Old circuit board hybrid metal (plumbous massfraction is 5%) 20g is put in quartz crucible, then is put into by crucible in the heating chamber of vacuum furnace evaporator main room.Close evaporator main room button fly front, start vacuum system and vacuum furnace is vacuumized, make body of heater chamber inner pressure reach 0.5Pa by force.Evaporator main room is heated to 900 DEG C, constant temperature 1h.After stopping heating, vacuum furnace is cooled to room temperature, and recovers pressure to normal pressure.Take out crucible and collecting chamber quartz glass tube, namely the lead of removal be deposited in Glass tubing.Plumbous clearance is 99.88%.
Embodiment 4
Old circuit board hybrid metal (plumbous massfraction is 5%) 20g is put in quartz crucible, then is put into by crucible in the heating chamber of vacuum furnace evaporator main room.Close evaporator main room button fly front, start vacuum system and vacuum furnace is vacuumized, make body of heater chamber inner pressure reach 0.2Pa by force.Evaporator main room is heated to 900 DEG C, constant temperature 1.5h.After stopping heating, vacuum furnace is cooled to room temperature, and recovers pressure to normal pressure.Take out crucible and collecting chamber quartz glass tube, namely the lead of removal be deposited in Glass tubing.Plumbous clearance is 99.87%.
The utilization vacuum distillation technique that the present invention proposes removes method plumbous in metal of waste circuit board, be described by embodiment, person skilled obviously can not depart from content of the present invention, spirit and scope product as herein described and making method are changed or suitably change with combination, realize technology of the present invention.Special needs to be pointed out is, all similar replacements and change apparent to those skilled in the art, they are all deemed to be included in spirit of the present invention, scope and content.
Claims (1)
1. the plumbous method removed in metal of waste circuit board, is characterized in that, uses the device of heating under vacuum separating metal copper-lead mixture, removes method plumbous in metal of waste circuit board, comprise the following steps by the principle of vacuum distilling:
I. old circuit board hybrid metal is put in quartz crucible, then crucible is put in the heating chamber of vacuum furnace evaporator main room; Start water-cooling system;
Ii. close evaporator main room button fly front, start vacuum pump set and vacuum furnace is vacuumized, make body of heater chamber inner pressure reach 0.1Pa ~ 0.5Pa by force;
Iii. first paragraph collecting chamber and second segment collecting chamber do not carry out computer heating control, and collecting chamber works at normal temperatures as an entirety;
Iv. evaporator main room is heated to 900 DEG C, steady temperature 0.5h ~ 1.5h, the lead gasification in hybrid metal, and deposits at collecting chamber;
V. after stopping heating, vacuum furnace is cooled to room temperature, and recovers pressure to normal pressure, take out crucible and collecting chamber quartz glass tube, Footwall drift.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310437131.1A CN104451150A (en) | 2013-09-22 | 2013-09-22 | Method for removing lead in metals of waste circuit boards |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310437131.1A CN104451150A (en) | 2013-09-22 | 2013-09-22 | Method for removing lead in metals of waste circuit boards |
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| CN104451150A true CN104451150A (en) | 2015-03-25 |
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| CN201310437131.1A Pending CN104451150A (en) | 2013-09-22 | 2013-09-22 | Method for removing lead in metals of waste circuit boards |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1760383A (en) * | 2005-11-03 | 2006-04-19 | 上海交通大学 | Vacuum distillation method for separating aluminium element from mixed metals in worn-out printing circuit board |
| CN101717863A (en) * | 2009-12-08 | 2010-06-02 | 天津大学 | Device and method for separating metallic copper and lead mixture through vacuum heating |
| CN101824547A (en) * | 2010-06-02 | 2010-09-08 | 天津大学 | Method for vacuum liquating, crystallizing, separating and recycling lead and zinc in metal of waste circuit board |
| CN102357504A (en) * | 2011-07-27 | 2012-02-22 | 上海交通大学 | Recovery method of lead in waste circuit board |
-
2013
- 2013-09-22 CN CN201310437131.1A patent/CN104451150A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1760383A (en) * | 2005-11-03 | 2006-04-19 | 上海交通大学 | Vacuum distillation method for separating aluminium element from mixed metals in worn-out printing circuit board |
| CN101717863A (en) * | 2009-12-08 | 2010-06-02 | 天津大学 | Device and method for separating metallic copper and lead mixture through vacuum heating |
| CN101824547A (en) * | 2010-06-02 | 2010-09-08 | 天津大学 | Method for vacuum liquating, crystallizing, separating and recycling lead and zinc in metal of waste circuit board |
| CN102357504A (en) * | 2011-07-27 | 2012-02-22 | 上海交通大学 | Recovery method of lead in waste circuit board |
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Application publication date: 20150325 |