CN110127754A - A method of high-purity α-PbO is prepared by β-PbO - Google Patents
A method of high-purity α-PbO is prepared by β-PbO Download PDFInfo
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- CN110127754A CN110127754A CN201910434215.7A CN201910434215A CN110127754A CN 110127754 A CN110127754 A CN 110127754A CN 201910434215 A CN201910434215 A CN 201910434215A CN 110127754 A CN110127754 A CN 110127754A
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- Prior art keywords
- pbo
- vacuum
- ball milling
- vacuum ball
- preparation
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- 229910006529 α-PbO Inorganic materials 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000000498 ball milling Methods 0.000 claims abstract description 50
- 239000000843 powder Substances 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 230000001681 protective effect Effects 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 19
- 238000005406 washing Methods 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 229910000831 Steel Inorganic materials 0.000 claims description 11
- 239000011324 bead Substances 0.000 claims description 11
- 239000010959 steel Substances 0.000 claims description 11
- 239000011261 inert gas Substances 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000000227 grinding Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 description 4
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 description 3
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009466 transformation Effects 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
- 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
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Crushing And Grinding (AREA)
Abstract
The present invention provides a kind of methods for preparing high-purity α-PbO by β-PbO, belong to technical field of material.The following steps are included: β-PbO powder is carried out vacuum ball milling in protective atmosphere, α-PbO is obtained.β-PbO is changed into α-PbO by vacuum ball grinding technique by the present invention, provides the preparation method of new α-PbO a kind of, and method is simple, and operation is simple, high financial profit, high production cost, and α-PbO purity obtained is greater than 99%.
Description
Technical field
The present invention relates to technical field of material more particularly to a kind of methods for preparing high-purity α-PbO by β-PbO.
Background technique
α-the PbO and β-PbO of high-purity have higher economic value and wider purposes, and the α-PbO of low-purity
It then has a greatly reduced quality with β-PbO.α-PbO and β-PbO usually metallic lead aoxidized by Shimadzu ball-milling method and Ba Dun vapour phase oxidation process and
, the lead powder purity of acquisition is lower to contain a large amount of metallic lead and Pb3O4Equal substances, are achieved with but as long as temperature is sufficiently high
β-the PbO of high-purity.But α-the PbO of high-purity is not easy to obtain, if the excessively high α-PbO of heating temperature can become-the PbO containing β and Pb3O4
Mixture, heating temperature it is too low then include metallic lead and Pb3O4Equal substances.β-PbO can be obtained by α-PbO heating phase transformation, but by
It is then much more difficult that β-PbO mutually becomes α-PbO.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of methods for preparing high-purity α-PbO by β-PbO.Benefit of the invention
High-purity α-PbO has been made with vacuum ball grinding technique.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
A method of α-PbO is prepared by β-PbO, comprising the following steps:
β-PbO powder is subjected to vacuum ball milling in protective atmosphere, obtains α-PbO.
Preferably, the time of the vacuum ball milling is 14~20h, and the revolving speed of the vacuum ball milling is 425~500rmp.
Preferably, the vacuum pressure of the vacuum ball milling is 1~100Pa, and the protective atmosphere is argon gas.
Preferably, the ball-milling medium that the vacuum ball milling uses is steel ball milling bead.
Preferably, the mass ratio of the steel ball milling bead and β-PbO powder is 15:1~20:1.
Preferably, the mass ratio of the steel ball milling bead and β-PbO powder is 17:1.
Preferably, the partial size of the β-PbO powder is 100~200nm.
Preferably, the vacuum ball milling carries out in vacuum ball grinder.
Preferably, the vacuum ball grinder, which is put on QM-3SP2 planetary ball mill, carries out ball milling.
Preferably, the vacuum ball milling is then to vacuumize first with inert gas to vacuum ball grinder gas washing 1 time；It uses again
Then inert gas vacuumizes vacuum ball grinder gas washing 1 time again, finally again with inert gas to vacuum ball grinder gas washing 1 time,
Then it vacuumizes again.
The present invention provides a kind of methods for preparing α-PbO by β-PbO, comprising the following steps: is protecting β-PbO powder
Vacuum ball milling is carried out in atmosphere, obtains α-PbO.β-PbO is changed into α-PbO, is provided by the present invention by vacuum ball grinding technique
A kind of preparation method of new α-PbO, method is simple, and operation is simple, high financial profit, high production cost, and α-PbO obtained
Purity is greater than 99%.
Detailed description of the invention
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is the XRD diagram of raw material β-PbO of the present invention；
Fig. 2 is the XRD diagram of the product α-PbO of vacuum ball milling of the present invention.
Specific embodiment
The present invention provides a kind of methods for preparing α-PbO by β-PbO, comprising the following steps:
β-PbO powder is subjected to vacuum ball milling in protective atmosphere, obtains α-PbO.
In the present invention, the time of the vacuum ball milling is preferably 14~20h, more preferably 17h, the vacuum ball milling
Revolving speed is preferably 425~500rmp, more preferably 460rmp.
In the present invention, the vacuum pressure of the vacuum ball milling is preferably 1~100Pa, more preferably 50Pa, the protection
Atmosphere is preferably argon gas.
In the present invention, the ball-milling medium that the vacuum ball milling uses is preferably steel ball milling bead.
In the present invention, the mass ratio of the steel ball milling bead and β-PbO powder is preferably 15:1~20:1, more
17:1。
In the present invention, the partial size of the β-PbO powder is preferably 100~200nm.
In the present invention, the vacuum ball milling preferably carries out in vacuum ball grinder.
In the present invention, the vacuum ball grinder, which is preferably put on QM-3SP2 planetary ball mill, carries out ball milling.
In the present invention, it is preferred to be passed through protective atmosphere gas washing three times to vacuum ball grinder, then vacuum ball grinder is vacuumized
To 1~100Pa.
In the present invention, then the vacuum ball milling is taken out true preferably first with inert gas to vacuum ball grinder gas washing 1 time
It is empty；With inert gas then vacuum ball grinder gas washing 1 time is vacuumized again again, finally again with inert gas to vacuum ball grinder
It gas washing 1 time, then vacuumizes again.
It is detailed to a kind of method progress for preparing high-purity α-PbO by β-PbO provided by the invention below with reference to embodiment
Illustrate, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
(1) β-PbO powder (100~200nm of partial size) is put in vacuum ball grinder, it is then closed, to vacuum ball grinder
It is passed through argon gas gas washing three times, then vacuum ball grinder is evacuated to 100Pa.
(2) the vacuum ball grinder of the step (1) is put on (QM-3SP2) planetary ball mill and carries out ball milling, finally
α-PbO can be obtained；The vacuum Ball-milling Time is 14h；The vacuum rotational speed of ball-mill is 425rmp；It is true in the vacuum ball grinder
Pneumatics power is 100Pa；The mass ratio of the quality of the steel ball milling bead filled in the vacuum ball grinder and the β-PbO being packed into
For 15:1.Through detecting, the purity of α-PbO is 99.2%.
Fig. 1 is the XRD diagram of raw material β-PbO of the present invention；Fig. 2 is the product α-PbO's of vacuum ball milling of the present invention
XRD diagram, according to Fig. 1~2 as can be seen that α-PbO has been prepared by vacuum ball milling in the present invention really.
Embodiment 2
(1) β-PbO powder (100~200nm of partial size) is put in vacuum ball grinder, it is then closed, to vacuum ball grinder
It is passed through argon gas gas washing three times, then vacuum ball grinder is evacuated to 1Pa.
(2) the vacuum ball grinder of the step (1) is put on (QM-3SP2) planetary ball mill and carries out ball milling, finally
α-PbO can be obtained；The vacuum Ball-milling Time is 20h；The vacuum rotational speed of ball-mill is 500rmp；It is true in the vacuum ball grinder
Pneumatics power is 1Pa；The quality of the steel ball milling bead filled in the vacuum ball grinder and the mass ratio for the β-PbO being packed into are
20:1.Through detecting, the purity of α-PbO is 99.5%.
Embodiment 3
(1) β-PbO powder (100~200nm of partial size) is put in vacuum ball grinder, it is then closed, to vacuum ball grinder
It is passed through argon gas gas washing three times, then vacuum ball grinder is evacuated to 50Pa.
(2) the vacuum ball grinder of the step (1) is put on (QM-3SP2) planetary ball mill and carries out ball milling, finally
α-PbO can be obtained；The vacuum Ball-milling Time is 17h；The vacuum rotational speed of ball-mill is 460rmp；It is true in the vacuum ball grinder
Pneumatics power is 50Pa；The mass ratio of the quality of the steel ball milling bead filled in the vacuum ball grinder and the β-PbO being packed into
For 17:1.Through detecting, the purity of α-PbO is 99.8%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of method for preparing α-PbO by β-PbO, which comprises the following steps:
β-PbO powder is subjected to vacuum ball milling in protective atmosphere, obtains α-PbO.
2. preparation method according to claim 1, which is characterized in that the time of the vacuum ball milling is 14~20h, described
The revolving speed of vacuum ball milling is 425~500rmp.
3. preparation method according to claim 1 or 2, which is characterized in that the vacuum pressure of the vacuum ball milling be 1~
100Pa, the protective atmosphere are argon gas.
4. preparation method according to claim 1, which is characterized in that the ball-milling medium that the vacuum ball milling uses is steel
Ball milling bead.
5. the preparation method according to claim 4, which is characterized in that the matter of the steel ball milling bead and β-PbO powder
Amount is than being 15:1~20:1.
6. preparation method according to claim 5, which is characterized in that the matter of the steel ball milling bead and β-PbO powder
Amount is than being 17:1.
7. preparation method according to claim 1, which is characterized in that the partial size of the β-PbO powder is 100~200nm.
8. preparation method according to claim 1, which is characterized in that the vacuum ball milling carries out in vacuum ball grinder.
9. preparation method according to claim 8, which is characterized in that it is planetary that the vacuum ball grinder is put in QM-3SP2
Ball milling is carried out on ball mill.
10. preparation method according to claim 8, which is characterized in that the vacuum ball milling is first with inert gas to true
Empty ball grinder gas washing 1 time, then vacuumizes；With inert gas then vacuum ball grinder gas washing 1 time is vacuumized, finally again again
With inert gas then vacuum ball grinder gas washing 1 time is vacuumized again again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910434215.7A CN110127754A (en) | 2019-05-23 | 2019-05-23 | A method of high-purity α-PbO is prepared by β-PbO |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910434215.7A CN110127754A (en) | 2019-05-23 | 2019-05-23 | A method of high-purity α-PbO is prepared by β-PbO |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110127754A true CN110127754A (en) | 2019-08-16 |
Family
ID=67572758
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910434215.7A Pending CN110127754A (en) | 2019-05-23 | 2019-05-23 | A method of high-purity α-PbO is prepared by β-PbO |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110127754A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104862481A (en) * | 2014-02-21 | 2015-08-26 | 超威电源有限公司 | Recycling method of waste material containing lead oxide |
-
2019
- 2019-05-23 CN CN201910434215.7A patent/CN110127754A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104862481A (en) * | 2014-02-21 | 2015-08-26 | 超威电源有限公司 | Recycling method of waste material containing lead oxide |
Non-Patent Citations (1)
| Title |
|---|
| M. CORTEZ-VALADEZ ET AL.: "Additional active Raman modes in α-PbO nanoplates", 《PHYSICA E》 * |
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| PB01 | Publication | ||
| PB01 | Publication | ||
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Application publication date: 20190816 |