CN108203115A - A kind of production technology of ultra-pure lead oxide - Google Patents
A kind of production technology of ultra-pure lead oxide Download PDFInfo
- Publication number
- CN108203115A CN108203115A CN201611187437.6A CN201611187437A CN108203115A CN 108203115 A CN108203115 A CN 108203115A CN 201611187437 A CN201611187437 A CN 201611187437A CN 108203115 A CN108203115 A CN 108203115A
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- China
- Prior art keywords
- lead
- electrolyte
- ultra
- electrolytic
- production technology
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910000464 lead oxide Inorganic materials 0.000 title claims abstract description 13
- 238000005516 engineering process Methods 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 title abstract 3
- 239000003792 electrolyte Substances 0.000 claims abstract description 23
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 230000003647 oxidation Effects 0.000 claims abstract description 13
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 13
- 238000005266 casting Methods 0.000 claims abstract description 11
- 239000000654 additive Substances 0.000 claims abstract description 7
- 230000000996 additive effect Effects 0.000 claims abstract description 7
- 229920001732 Lignosulfonate Polymers 0.000 claims abstract description 6
- 150000001491 aromatic compounds Chemical class 0.000 claims abstract description 6
- 238000007664 blowing Methods 0.000 claims abstract description 6
- 239000000498 cooling water Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004094 surface-active agent Substances 0.000 claims abstract description 6
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 238000005868 electrolysis reaction Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 abstract description 6
- 229910052737 gold Inorganic materials 0.000 abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 238000003672 processing method Methods 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 239000011135 tin Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 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]
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/18—Electrolytic production, recovery or refining of metals by electrolysis of solutions of lead
-
- 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)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
A kind of production technology of ultra-pure lead oxide, the peace of current density 100 200/square metre, 0.3 0.5 volts of voltage, the temperature of electrolyte is less than 40 degrees Celsius, and electrolyte internal circulating load is controlled less than 15 liters/min；Purifying again to electrolytic lead under conditions of the additive that addition is made of surfactants such as aromatic compound and ligninsulfonates in electrolyte, to gained lead pig through casting grain, after ball grinds, into electrical heating leady oxide roaster, after the oxidation of 37 hours, with acetic acid examine without after lead metal can blowing, and sent with the conveyer with cooling water jecket in crushing system, can steadily produce Ag, Au and require ultra-pure lead oxide product less than 100ppb, 1ppb respectively.
Description
Technical field
The present invention relates to a kind of preparation process of lead oxide, particularly a kind of production technology of ultra-pure lead oxide.
Background technology
At present, the production of lead oxide both at home and abroad is raw material generally with general electrolytic lead, using " Shimadzu method " or " Ba Dun
Method " is into powder, then roasting oxidation, and purity is low, product can only achieve common commercial use (such as battery, paint, electronics industry)
It is required that.It is higher and higher to the purity requirement of lead oxide based on the Accurate Determining to platinum group metal mineral content and grade and evaluation, oxygen
It is especially low to change trace element requirement in lead, especially Ag, Au require to be less than 100ppb, 1ppb, such ultra high purity nitric oxide respectively
Lead product, existing common process technology are difficult to reach and meet the requirements, it is necessary to have a kind of new advanced technologies to solve.
Invention content
The purpose of the present invention is to provide a kind of production technologies of ultra-pure lead oxide, can be steadily using the production technology
Ag, Au are produced, respectively ultra-pure lead oxide product of the requirement less than 100ppb, 1ppb.
It includes the following steps：
The first step, electrolytic lead purify again：Common electrolytic lead is used as raw material, electrolytic parameter control is：Current density
100-200 peaces/square metre, voltage 0.3-0.5 volts, the temperature of electrolyte is less than 40 degrees Celsius, and electrolyte internal circulating load is controlled small
In 15 liters/min；The additive being made of surfactants such as aromatic compound and ligninsulfonates is added in electrolyte；Electricity
Content is primary every detection in 18-26 hours in Ag+ in solution liquid, will carry out removing Ag processing as content is more than 0.05ppm；Gained
Cathode lead cleans spare by ingot casting；
Second step, oxidation；By lead pig obtained by the first step through casting grain, after ball grinds, roasted into electrical heating leady oxide
Stove, after the oxidation of 3-7 hours, with acetic acid examine without after lead metal can blowing, and with the conveyer with cooling water jecket
It send in crushing system, obtains qualified PbO products.
Since this method is by again purifying, the content of Ag in electrolytic lead is further reduced, the additive in electrolyte used
Can with unwanted metal ion formed conjugate, can effectively remove Fe, Ag, Zn, Ni, Co, Cu, Sn (i.e. iron, silver, zinc, nickel,
Cobalt, copper, tin) etc. impurity, oxidation environment is reasonable, craft science, can steadily produce Ag, Au require respectively less than 100ppb,
The ultra-pure lead oxide product of 1ppb.
Specific embodiment
Embodiment one
The first step, electrolytic lead purify again：Common electrolytic lead is used as raw material, electrolytic parameter control is：Current density
100-200 peaces/square metre, 0.4 volt of voltage, 38 degrees Celsius of the temperature of electrolyte, the control of electrolyte internal circulating load is at 13 liters/min；
The additive being made of surfactants such as aromatic compound and ligninsulfonates is added in electrolyte；In electrolyte in Ag+
Content is primary every detection in 24 hours, will carry out removing Ag processing as content is more than 0.05ppm；Except Ag processing methods are：According to
30% dilute HCL is added dropwise in the concentration of Ag+, and electrolyte is filtered with special ultra micro cycle filter pump, until Ag+ contents are small
Until 0.05ppm.The cathode lead of gained cleans spare by ingot casting；
Second step, oxidation；By lead pig obtained by the first step through casting grain, after ball grinds, roasted into electrical heating leady oxide
Stove, after the oxidation of 6 hours, with acetic acid examine without after lead metal can blowing, and sent with the conveyer with cooling water jecket
In crushing system, qualified PbO products are obtained.
It is molded with dry method extruder grain, then obtains graininess manufactured goods.
Embodiment two
The first step, electrolytic lead purify again：Common electrolytic lead is used as raw material, electrolytic parameter control is：Current density
150 peaces/square metre, 0.35 volt of voltage, 39 degrees Celsius of the temperature of electrolyte, the control of electrolyte internal circulating load is at 15 liters/min；Electrolysis
The additive being made of surfactants such as aromatic compound and ligninsulfonates is added in liquid；Content in Ag+ in electrolyte
It is primary every detection in 23 hours, it will carry out removing Ag processing as content is more than 0.05ppm；Except Ag processing methods are：According to Ag+'s
30% dilute HCL is added dropwise in concentration, and electrolyte is filtered with special ultra micro cycle filter pump, until Ag+ contents are less than
Until 0.05ppm.The cathode lead of gained cleans spare by ingot casting；
Second step, oxidation；By lead pig obtained by the first step through casting grain, after ball grinds, roasted into electrical heating leady oxide
Stove, after the oxidation of 7 hours, with acetic acid examine without after lead metal can blowing, and sent with the conveyer with cooling water jecket
In crushing system, qualified PbO products are obtained.
It is molded with dry method extruder grain, then obtains graininess manufactured goods.
Embodiment three
The first step, electrolytic lead purify again：Common electrolytic lead is used as raw material, electrolytic parameter control is：Current density
170 peaces/square metre, 0.37 volt of voltage, 40 degrees Celsius of the temperature of electrolyte, the control of electrolyte internal circulating load is at 15 liters/min；Electrolysis
The additive being made of surfactants such as aromatic compound and ligninsulfonates is added in liquid；Content in Ag+ in electrolyte
It is primary every detection in 22 hours, it will carry out removing Ag processing as content is more than 0.05ppm；Except Ag processing methods are：According to Ag+'s
30% dilute HCL is added dropwise in concentration, and electrolyte is filtered with special ultra micro cycle filter pump, until Ag+ contents are less than
Until 0.05ppm.The cathode lead of gained cleans spare by ingot casting；
Second step, oxidation；By lead pig obtained by the first step through casting grain, after ball grinds, roasted into electrical heating leady oxide
Stove, after the oxidation of 4.5 hours, with acetic acid examine without after lead metal can blowing, and with the conveyer with cooling water jecket
It send in crushing system, obtains qualified PbO products.
It is molded with dry method extruder grain, then obtains graininess manufactured goods.
Claims (2)
1. a kind of production technology of ultra-pure lead oxide, it is characterised in that it includes the following steps：
The first step, electrolytic lead purify again：Common electrolytic lead is used as raw material, electrolytic parameter control is：Current density 100-
200 peaces/square metre, voltage 0.3-0.5 volts, the temperature of electrolyte is less than 40 degrees Celsius, and electrolyte internal circulating load is controlled less than 15
Liter/min；The additive being made of aromatic compound and ligninsulfonate as surfactant is added in electrolyte；Electrolysis
Ag+ contents are primary every detection in 18-26 hours in liquid, will carry out removing Ag processing as content is more than 0.05ppm；The cathode of gained
Lead cleans spare by ingot casting；
Second step, oxidation：By lead pig obtained by the first step through casting grain, after ball grinds, into electrical heating leady oxide roaster, warp
After crossing the oxidation of 3-7 hours, with acetic acid examine without after lead metal can blowing, and sent with the conveyer with cooling water jecket in powder
Broken system obtains qualified PbO products.
2. the production technology of ultra-pure lead oxide according to claim 1, which is characterized in that with dry method extruder grain into
Type then obtains graininess manufactured goods.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611187437.6A CN108203115A (en) | 2016-12-20 | 2016-12-20 | A kind of production technology of ultra-pure lead oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611187437.6A CN108203115A (en) | 2016-12-20 | 2016-12-20 | A kind of production technology of ultra-pure lead oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108203115A true CN108203115A (en) | 2018-06-26 |
Family
ID=62603642
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611187437.6A Pending CN108203115A (en) | 2016-12-20 | 2016-12-20 | A kind of production technology of ultra-pure lead oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108203115A (en) |
-
2016
- 2016-12-20 CN CN201611187437.6A patent/CN108203115A/en active Pending
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| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180626 |
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| WD01 | Invention patent application deemed withdrawn after publication |