CN106587140B - A kind of method for preparing nano oxidized lead powder using waste and old leaded scolding tin - Google Patents
A kind of method for preparing nano oxidized lead powder using waste and old leaded scolding tin Download PDFInfo
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- CN106587140B CN106587140B CN201610954560.XA CN201610954560A CN106587140B CN 106587140 B CN106587140 B CN 106587140B CN 201610954560 A CN201610954560 A CN 201610954560A CN 106587140 B CN106587140 B CN 106587140B
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000002699 waste material Substances 0.000 title claims abstract description 26
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910000464 lead oxide Inorganic materials 0.000 claims abstract description 41
- 238000009833 condensation Methods 0.000 claims abstract description 39
- 230000005494 condensation Effects 0.000 claims abstract description 39
- 238000010438 heat treatment Methods 0.000 claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 23
- 238000001291 vacuum drying Methods 0.000 claims abstract description 8
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 7
- 239000006227 byproduct Substances 0.000 claims abstract description 6
- 230000003647 oxidation Effects 0.000 claims abstract description 5
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical group [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims abstract 10
- 239000010453 quartz Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 12
- 239000000047 product Substances 0.000 abstract description 9
- 229910000679 solder Inorganic materials 0.000 abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 7
- 239000001301 oxygen Substances 0.000 abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 4
- 239000004020 conductor Substances 0.000 abstract description 3
- 239000004973 liquid crystal related substance Substances 0.000 abstract description 3
- 239000011858 nanopowder Substances 0.000 abstract description 3
- 239000000049 pigment Substances 0.000 abstract description 3
- 238000009835 boiling Methods 0.000 abstract description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- 239000005355 lead glass Substances 0.000 abstract description 2
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 31
- 239000003570 air Substances 0.000 description 21
- 238000011084 recovery Methods 0.000 description 9
- 241000500881 Lepisma Species 0.000 description 6
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910001385 heavy metal Inorganic materials 0.000 description 4
- 229910001887 tin oxide Inorganic materials 0.000 description 4
- 239000002893 slag Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000010431 corundum Substances 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 230000000750 progressive effect Effects 0.000 description 2
- 238000009853 pyrometallurgy Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000010793 electronic waste Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 210000004709 eyebrow Anatomy 0.000 description 1
- 210000000720 eyelash Anatomy 0.000 description 1
- 239000005308 flint glass Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- LQBJWKCYZGMFEV-UHFFFAOYSA-N lead tin Chemical compound [Sn].[Pb] LQBJWKCYZGMFEV-UHFFFAOYSA-N 0.000 description 1
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910006529 α-PbO Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/02—Oxides
- C01G21/06—Lead monoxide [PbO]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/02—Oxides
- C01G21/10—Red lead [Pb3O4]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/22—Particle morphology extending in two dimensions, e.g. plate-like with a polygonal circumferential shape
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a kind of method for preparing nano oxidized lead powder using waste and old leaded scolding tin, waste and old leaded scolding tin separating obtained on waste printed circuit board is put into vacuum drying oven by this method, using vacuum control oxygen method, it is lead oxide and tin ash that air is passed through into vacuum drying oven by waste and old solder oxidation.Meanwhile heating, vacuum stove, lead oxide is evaporated using the difference of lead oxide and tin ash boiling point, bringing condensation chamber into by unreacted nitrogen is condensed into nano powder.The nano oxidized lead powder of two kinds of forms is prepared by control system pressure, heating and condensation temperature, condensation distance.Meanwhile the residue in crucible is tin ash powder.Nanometer sized lead oxide product obtained by the present invention has wide application prospect in lead glass manufacture, ceramic material, pigment, light emitting diode, lead-acid accumulator field；Obtained byproduct tin ash is a kind of transparent conductive material, is widely used in fields such as electrode preparation, sensor, battery, liquid crystal displays.
Description
Technical field
The invention belongs to the high-valued recovery of the Disposal of Electronic Wastes in solid wastes recycling field, it is related in electron wastes
Heavy metal lead and the high-valued recovery of tin and the preparation of nano-powder.More particularly to one kind piece is prepared using waste and old leaded scolding tin
The method of shape and shaft-like nano oxidized lead powder.
Background technology
Connecting material of the scolding tin as electronic component in electronic equipment and circuit board, it is in household appliances manufacturing, electronics work
It is widely used in industry, auto manufacturing, maintenance and daily life, dosage is huge.Slicker solder SnPb63 is because its fusing point is low, upper tin
The features such as ability is good, diffusivity is good, there is the irreplaceable advantage of other Pb-free solders.However, in slicker solder scolding tin lead content
Very big, for the content of lead up to 37%, tin accounts for 63% in common SnPb63.According to statistics, between 1994 to 2003 years, the whole world is big
It there are about 500,000,000 computers to go out of use, and contain about 718000 t lead here.Lead is primarily present circuit in electron wastes
In the parts such as plate, diode cone glass and lead-acid accumulator.If these lead are discharged into ring because of irrational removal process
Border, it will cause very big environmental pollution to neighbouring air, soil and water body, or even brought to the health of local resident potential
Harm.Disassemble ground it is reported that being concentrated in the electron wastes such as Guangdong Gui Yu and Taizhou of Zhejiang, local soil, water body etc. all by
Serious heavy metal pollution has been arrived, and researcher also indicates that its blood lead content greatly exceed state to the blood lead analysis of local children
The 10ug/L of family's limit value.In addition, while environment and health are on the hazard, this is also the significant wastage to metals resources.
Mainly there are pyrometallurgy and hydrometallurgy for the recovery process of leaded scolding tin or other slicker solder slags at present.But
The fine lead powder of gasification is included in flying dust caused by pyrometallurgy, secondary pollution may be caused through exhaust emissions to air.It is wet
The metals such as lead, tin and silver in the metallurgical recovery scolding tin using flows such as acidleach, electrolysis of method.Need consumption a large amount of in technical process
Chemical reagent, caused waste liquid have extremely strong corrosivity, it is also possible to cause secondary pollution.In addition, the production of these processes recovery
Product are thick scolding tin, lead bullion and thick tin etc., and economic value is not high, and general enterprises are difficult to obtain higher economy time from removal process
Report.Therefore, develop it is a kind of can the high-valued friendly process process for reclaiming waste and old scolding tin and other slicker solder slags just compel in eyebrow
Eyelash.
Lead oxide powder has extensively in fields such as pigment, flint glass, insecticide, ceramic raw material and lead-acid accumulator manufactures
General application.When its size reaches nanometer dimension, due to the small-size effect, quantum size effect, maroscopic quantity of nano material
Sub- tunnel-effect and show effect etc., it may show special optics, electric property.In addition, tin oxide is also a kind of
The semi-conducting material of wide bandgap.And stannic oxide powder has been widely used in electricity as a kind of outstanding transparent conductive material
The fields such as pole preparation, sensor, liquid crystal display, solar cell, chemical industry catalysis, coating, pressure sensitive preparation.
The content of the invention
The purpose of the present invention be for current heavy metal pollution phenomenon it is universal, it is existing recovery soldering tin technique fall behind, technology is not
The low present situation of foot, recovery added value of product, and a kind of simple and effective leaded scolding tin of recovery is provided and prepares Nanometer sized lead oxide simultaneously
The method of powder, using vacuum control oxygen method, high-purity polymolecularity as raw material, is prepared using waste and old leaded scolding tin in electron wastes
Sheet and shaft-like nano oxidized lead powder, realized while heavy metal lead pollution environment is avoided slicker solder high added value return
Receive.The method that the present invention is established is carried out in closed system, and free from admixture introduces, and obtained product purity is high；Contamination-free is arranged
Put, environmental pollution will not be caused.
The waste and old waste and old leaded scolding tin obtained by physical separation is put into vacuum drying oven heating chamber by the present invention, using vacuum
Oxygen method is controlled, a certain amount of air is passed through into vacuum system, while discharge air using mechanical pump so that kept in system
100-10000Pa dynamic pressure.Then heating, vacuum stove is to certain temperature, using the oxygen in air by the lead in scolding tin and
Tin is aoxidized, and then lead oxide is evaporated using the difference of lead oxide and tin oxide boiling point, using unreacted nitrogen by oxygen
Change lead steam, which is brought into condensation chamber body, is condensed into nano powder.The residue not being evaporated in heating chamber is then byproduct tin oxide
Powder.By controlling the conditions such as heating-up temperature, dynamic air pressure, condensation temperature, the nano oxidized of different shape is prepared
Lead powder.The present invention directly uses air as oxidant and carrier gas, and cost is cheap, and technical process is simple, is easy to industrialize.
In the present invention, the heating-up temperature is 800-1000 DEG C, is heated with 10-20 DEG C/min of heating rate；The dynamic
Atmospheric pressure is 100-10000Pa；The condensation temperature is 100-500 DEG C.
In the present invention, the Nanometer sized lead oxide powder is directly condensate on the quartzy tube wall of condensation chamber, or quartzy tube wall
Silicon chip on.Cyclonic separation method can also be used to collect gained zinc powder.
Nano oxidized lead powder made from the inventive method is sheet or shaft-like, the pattern when condensation temperature is 300-500 DEG C
For sheet, when condensation temperature is 100-200 DEG C, pattern is shaft-like.Described flake nano lead oxide product length and width dimensions are general
For 50-300nm, thickness 10-20nm.Described shaft-like Nanometer sized lead oxide product length is about 50nm, and diameter is about
10-15nm。
In the inventive method, resulting residue is the higher canescence tin ash powder of purity.
The present invention includes step in detail below：
（1）Waste and old leaded scolding tin is contained in alumina crucible, alumina crucible is positioned over adding for tube type vacuum stove
Hot intracavitary；Meanwhile Nanometer sized lead oxide collection device is placed in tube type vacuum stove condensation chamber；Wherein：
The tube type vacuum stove is divided into two sections of heating chamber and condensation chamber, and heating chamber front end sets an air intake valve and thermal insulation
Pipe plug, separated between heating chamber and condensation chamber with adiabatic pipe plug, there is aperture at pipe plug center, and pipe plug is oxidation aluminium material, pipe
Stifled thickness is 3-7cm, a diameter of 0.5-2cm of pipe plug central small hole；
The Nanometer sized lead oxide collection device is 30-90cm away from heating chamber distance；Nanometer sized lead oxide collection device is oxidation
Aluminium flake, quartz plate connect cyclone separator in vacuum drying oven rear end；
（2）All valves of airtight tube type vacuum drying oven, start vavuum pump and extract vacuum furnace air；Before adjusting heating chamber simultaneously
Air intake valve is held, is slowly introducing air, makes the dynamic pressure that 100-10000Pa is kept in tube type vacuum stove；
（3）Start tube type vacuum stove, heating chamber temperature is heated to 800-1000 with 10-20 DEG C/min heating rate
DEG C, and 60-120min is kept, then tube type vacuum stove is naturally cooling to room temperature；Wherein：
In heating process, it is 100-10000Pa to keep dynamic pressure value in tube type vacuum stove；
The temperature of condensation chamber is 50-600 DEG C；
In heating process, high-temperature oxydation, the air of the passive state of nano oxidized lead powder of evaporation carry, are scattered, through adding
Pipe plug aperture between hot chamber and condensation chamber, because thermograde higher between heating chamber and condensation chamber, Nanometer sized lead oxide are cold
It is solidifying to be deposited on the Nanometer sized lead oxide collection device in condensation chamber, the powder on collection device is scraped, that is, obtains the nanometer
Lead oxide powder.
The present invention directly uses air as oxidant and carrier gas, and cost is cheap, and technical process is simple, is easy to industrialize；
The present invention is directed to the obvious processing effect of waste and old leaded scolding tin, can promote the use of the money of the solid waste such as other slicker solder slags
The high-valued recovery of sourceization.Nanometer sized lead oxide product obtained by the present invention is in lead glass manufacture, ceramic material, pigment, luminous two
Pole pipe, lead-acid accumulator field have wide application prospect；Obtained byproduct tin oxide is a kind of transparent conductive material,
The fields such as electrode preparation, sensor, battery, liquid crystal display are widely used.
Brief description of the drawings
Fig. 1 is the electron scanning micrograph figure of sheet lead oxide powder produced by the present invention；
Fig. 2 is the x-ray diffraction pattern of sheet lead oxide powder produced by the present invention；
Fig. 3 is the transmission electron microscope photo figure of shaft-like lead oxide powder produced by the present invention；
Fig. 4 is the x-ray diffraction pattern of shaft-like lead oxide powder produced by the present invention；
Fig. 5 is byproduct tin ash powder photo figure produced by the present invention；
Fig. 6 is the x-ray diffraction pattern of byproduct tin ash powder produced by the present invention.
Embodiment
With reference to specific examples below and accompanying drawing, the present invention is described in further detail.The protection content of the present invention
It is not limited to following examples.Under the spirit and scope without departing substantially from inventive concept, those skilled in the art it is conceivable that change
Change and advantage is all included in the present invention, and using appended claims as protection domain.The process of the implementation present invention,
Condition, reagent, experimental method etc., it is the universal knowledege and common knowledge of this area in addition to the following content specially referred to,
Content is not particularly limited in the present invention.
Embodiment 1
A kind of method for preparing nano oxidized lead powder using waste and old leaded scolding tin, comprises the following steps：
Waste and old leaded scolding tin isolated on 20g waste printed circuit boards is weighed in corundum crucible, is then put into crucible
Tube type vacuum stove heat intracavitary.Quartz plate is put at condensation chamber middle-range heating chamber 60cm as condensation substrate；Heating chamber with it is cold
Separated among solidifying chamber with adiabatic pipe plug, there is hole among pipe plug, can passed through so that air carries lead oxide steam；After closed system
System pressure is evacuated to 1Pa by mechanical pump, intake valve is then adjusted and is passed through air so that 1000Pa dynamics are kept in vacuum drying oven
Pressure.60min to 1000 DEG C and is kept with 10 DEG C/min heating rate heating evaporation chamber；Condensation chamber temperature is constant is for regulation
300 DEG C and keep.Due to thering is air to be passed through in heating process, the scolding tin top layer in crucible can gradually aoxidize to be formed diaphragm with
Lower floor's scolding tin is avoided to be oxidized.With the rise of temperature, oxide layer progressive additive；When temperature is increased to certain value, lead oxide
Not oxidized lead can be evaporated with bottom, lead steam and the oxygen reaction generation lead oxide steam in air, Ran Houhe
The nitrogen that the lead oxide steam being directly evaporated is had neither part nor lot in reaction together is carried in condensation chamber.It is scattered cold due to nitrogen
But thermograde huge between effect and evaporation cavity and condensation chamber, the lead oxide steam into condensation chamber are finally condensate in silicon
On piece.After system is cooled to room temperature, the yellow powder on quartz plate is scraped into collection and obtains Nanometer sized lead oxide powder.Fig. 1 is
The stereoscan photograph for the nano oxidized lead powder sample being collected into.It can be seen that prepared nano oxidized lead powder is from photo
Regular hexagon sheet, for length and width between 50-300 nanometers, thickness is 10-20 nanometers.Fig. 2 x-ray diffraction pattern
Show that prepared product is pure zirconia lead, including α-PbO and β-PbO, wherein β-PbO are principal phase.
Embodiment 2
A kind of method for preparing nano oxidized lead powder using waste and old leaded scolding tin, comprises the following steps：
Waste and old leaded scolding tin isolated on 20g waste printed circuit boards is weighed in corundum crucible, is then put into crucible
Tube type vacuum stove heat intracavitary.Quartz plate is put at 60cm in condensation chamber as condensation substrate.Among heating chamber and condensation chamber
Separated with adiabatic pipe plug, there is hole among pipe plug, can passed through so that air carries lead oxide steam.By mechanical pump after closed system
System pressure is evacuated to 1Pa, intake valve is then adjusted and is passed through air so that 1000Pa dynamic pressures are kept in vacuum drying oven.With 10
DEG C/min heating rate heating evaporation chamber to 1000 DEG C and keeps 100min.Regulation condensation chamber temperature is 100 DEG C and kept.By
In having air to be passed through in heating process, the scolding tin top layer in crucible can gradually aoxidize to form diaphragm to avoid lower floor's scolding tin quilt
Oxidation.With the rise of temperature, oxide layer progressive additive.When temperature is increased to certain value, lead oxide and bottom are not oxidized
Lead can be evaporated, the oxygen reaction generation lead oxide steam in lead steam and air, then and be directly evaporated
The nitrogen that lead oxide steam is had neither part nor lot in reaction together is carried in condensation chamber.Due to the scattered cooling effect and evaporation of nitrogen
Huge thermograde between chamber and condensation chamber, the lead oxide steam into condensation chamber are finally condensate on quartz plate.Treat system
After being cooled to room temperature, the yellow powder on quartz plate is scraped into collection and obtains Nanometer sized lead oxide powder.Fig. 3 is the nanometer being collected into
The transmission electron microscope photo of lead oxide powder sample.It is long it can be seen that prepared nano oxidized lead powder is shaft-like for rule from photo
Degree is about 50nm or so, and diameter is between 10-15nm.Fig. 4 x-ray diffraction pattern shows prepared production under the conditions of this
Product are pure zirconia lead, including β-PbO and α-Pb3O4, wherein β-PbO are principal phase.Fig. 5 is residue tin ash powder, Fig. 6 X-
Other impurity peaks are not found in x ray diffration pattern x, it is pure tin ash to show the residue.
Claims (3)
- A kind of 1. method for preparing nano oxidized lead powder using waste and old leaded scolding tin, it is characterised in that this method includes following step Suddenly：（1）Waste and old leaded scolding tin is contained in alumina crucible, alumina crucible is positioned over to the heating chamber of tube type vacuum stove It is interior；Meanwhile Nanometer sized lead oxide collection device is placed in tube type vacuum stove condensation chamber；Wherein：The tube type vacuum stove is divided into two sections of heating chamber and condensation chamber, and heating chamber front end sets an air intake valve and heat-insulated pipe It is stifled, separated between heating chamber and condensation chamber with adiabatic pipe plug, there is an aperture at pipe plug center, and pipe plug is oxidation aluminium material, pipe plug Thickness is 3-7cm, a diameter of 0.5-2cm of pipe plug central small hole；The Nanometer sized lead oxide collection device is 30-90cm away from heating chamber distance；Nanometer sized lead oxide collection device be alumina wafer, Quartz plate or silicon chip；（2）All valves of airtight tube type vacuum drying oven, start vavuum pump and extract vacuum furnace air；Simultaneously heating chamber front end is adjusted to enter Air valve, air is slowly introducing, makes the dynamic pressure that 100-10000Pa is kept in tube type vacuum stove；（3）Start tube type vacuum stove, heating chamber temperature is heated to 800-1000 DEG C with 10-20 DEG C/min heating rate, and 60-120min is kept, then tube type vacuum stove is naturally cooling to room temperature；Wherein：In heating process, it is 100-10000Pa to keep dynamic pressure value in tube type vacuum stove；The temperature of condensation chamber is 50-600 ℃；In heating process, high-temperature oxydation, the air for the passive state of nano oxidized lead powder evaporated carry, are scattered, through heating chamber Pipe plug aperture between condensation chamber, due to thermograde higher between heating chamber and condensation chamber, Nanometer sized lead oxide condensation is heavy Powder on collection device is scraped on the Nanometer sized lead oxide collection device in condensation chamber, that is, obtained described nano oxidized by product Lead powder.
- 2. according to the method for claim 1, it is characterised in that described obtained nano oxidized lead powder its pattern be sheet or It is shaft-like；When condensation temperature is 300-500 DEG C, pattern is sheet, and when condensation temperature is 100-200 DEG C, pattern is shaft-like；It is described Flake nano lead oxide color is buff, and length and width is respectively 50-300 nanometers, and thickness is 10-20 nanometers；The bar Shape nanometer lead powder color is light yellow, a diameter of 10-15 nanometers, and length is 50 nanometers.
- 3. according to the method for claim 1, it is characterised in that remaining residue is tin ash in the alumina crucible Powder.
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| CN113321236A (en) * | 2020-07-31 | 2021-08-31 | 上海交通大学 | Method for preparing zinc sulfide ultrafine powder by using zinc skins of waste zinc-manganese battery |
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| CN102747227A (en) * | 2012-06-18 | 2012-10-24 | 东南大学 | Method for preparing superfine lead oxide by using electrode active materials of wasted lead acid batteries |
| CN104393364A (en) * | 2014-11-13 | 2015-03-04 | 张家港智电芳华蓄电研究所有限公司 | Method for preparing PbO from waste lead-acid battery by using direct wet method |
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| CN102747227A (en) * | 2012-06-18 | 2012-10-24 | 东南大学 | Method for preparing superfine lead oxide by using electrode active materials of wasted lead acid batteries |
| CN104520240A (en) * | 2014-02-21 | 2015-04-15 | 超威电源有限公司 | Method for recycling lead oxide used for cathode of lead-acid cell directly from waste lead plaster |
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