CN102078812B - Method for preparing nanometer Pd loaded honeycomb structure SnO2 catalyst - Google Patents
Method for preparing nanometer Pd loaded honeycomb structure SnO2 catalyst Download PDFInfo
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- CN102078812B CN102078812B CN201010594709.0A CN201010594709A CN102078812B CN 102078812 B CN102078812 B CN 102078812B CN 201010594709 A CN201010594709 A CN 201010594709A CN 102078812 B CN102078812 B CN 102078812B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 27
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title abstract 6
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 57
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000001301 oxygen Substances 0.000 claims abstract description 20
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 230000008018 melting Effects 0.000 claims description 28
- 238000002844 melting Methods 0.000 claims description 28
- 229910045601 alloy Inorganic materials 0.000 claims description 27
- 239000000956 alloy Substances 0.000 claims description 27
- 239000002994 raw material Substances 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 22
- 229910052763 palladium Inorganic materials 0.000 claims description 20
- 238000007254 oxidation reaction Methods 0.000 claims description 16
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 15
- 238000011065 in-situ storage Methods 0.000 claims description 15
- 230000003647 oxidation Effects 0.000 claims description 15
- 238000012545 processing Methods 0.000 claims description 13
- 238000005516 engineering process Methods 0.000 claims description 12
- 238000013019 agitation Methods 0.000 claims description 11
- 239000000155 melt Substances 0.000 claims description 8
- 238000003723 Smelting Methods 0.000 claims description 3
- 229910052774 Proactinium Inorganic materials 0.000 claims description 2
- 229910000510 noble metal Inorganic materials 0.000 abstract description 18
- 239000000463 material Substances 0.000 abstract description 17
- 238000013461 design Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 229910001252 Pd alloy Inorganic materials 0.000 abstract 1
- 239000000969 carrier Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 238000007669 thermal treatment Methods 0.000 abstract 1
- 239000002082 metal nanoparticle Substances 0.000 description 7
- 238000006555 catalytic reaction Methods 0.000 description 5
- 229910001092 metal group alloy Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002539 nanocarrier Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000005025 nuclear technology Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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Abstract
The invention relates to a method for preparing a SnO2 catalyst loading a nanometer Pd and having a honeycomb structure. The method is combined with a thermal treatment technique under the oxygen atmosphere condition on the basis of the treatment of supersaturated tin-palladium alloy so as to obtain a novel structure Pd/SnO2 catalyst material with the advantages of large specific surface area, uniform nanometer noble metal distribution, firm catalyst material structure and remarkable catalyzing effect. The preparation method integrates the preparation of noble metal nanometer particles, the preparation of carriers and the structure design into a whole, and has the characteristics of low cost of preparation technique, short flow, environment-friendliness and high performance.
Description
Technical field
The present invention relates to the catalysis material field, particularly relate to the technology of preparing of nano-noble metal catalyst.
Background technology
Nano-noble metal has unique photoelectron, chemical characteristic because of it, as catalyst, medical material, electromagnetic functional material, absorbing material, sensor components and parts material and nano composite material etc., present extremely important using value in research fields such as metallurgy, chemical industry, light industry, electronics, national defence, nuclear technology, Aero-Space.But we notice such fact in the application of noble metal nano particles, for consumption, the reduction material/product cost of saving noble metal, usually noble metal nano particles is loaded on certain carrier/surface of solids, comprise vacuum moulding machine, inert gas evaporation, DIFFUSION CONTROLLED reunion, chemistry and the electrochemical deposition etc. of metal.Now developed into Ag, Pt, Au nanocrystal have been distributed to zeolite, TiO
2, Al
2O
3, SiO
2, the surface such as graphite, CNT.On this application direction, existing material preparation technology (physics, chemical method etc.) is fixedly remaining in some problems aspect the noble metal nano particles effectively, material is not enough to the physics, the chemical property that keep high in application, this is a huge challenge that faces during noble metal nano particles uses.If noble metal nano particles because and can not form effective metallurgical binding between the carrier, in use might be subjected to the impact of the huge surface energy of nano particle and reunite, and then the performance of nano material character is brought negative effect.The present invention mainly proposes for the problem that solves nano-noble metal and the effective combination of carrier, present technique combines the processing characteristics of supersaturation metal alloy and the method that the Precipitation of noble metal in heat treatment process forms nanophase and matrix oxidation formation metal oxide preferably, preparation and the carrier preparation of noble metal nano particles are united two into one, embodied the development trend of material preparation technology " efficiently, low cost, short flow process, environmental friendliness, high-performance ".
Summary of the invention
The present invention is in conjunction with over-saturation metal alloy compositions processing and parent metal in-situ oxidation, noble metal Second Phase Precipitation principle, first the over-saturation metal alloy compositions is processed into honeycomb, then by under certain oxidizing atmosphere condition, the alloy that is processed into honeycomb being heat-treated and the in-situ oxidation processing, finally prepare the honeycomb SnO that is evenly distributed with nano-noble metal Pd
2Catalysis material.
The present invention realizes by following scheme:
A kind of honeycomb SnO for preparing loaded with nano Pd
2The method of catalyst contains following processing step:
1) palladium of the metallic tin of purity＞99.95% and purity＞99.95% is respectively 0.5%, 1%, 1.5% palladium according to percentage by weight, surplus is that tin carries out the raw material configuration.
2) alloy melting:
Contain 0.5%, 1%, 1.5% palladium and the surplus tin that configure are put into vacuum＜10
-3In the vacuum melting furnace of Pa, be respectively 250 ℃ at smelting temperature and carry out being cast into ingot blank after the melting.
3) alloy ingot blank processing and Technology for Heating Processing:
A) alloy ingot blank is rolled under normal temperature condition＜strip of 1mm, then is processed into honeycomb,
B) the honeycomb tin palldium alloy that obtains is put into heat-treatment furnace, under 150 ℃ of conditions, heat-treat, and the in-situ oxidation that the oxygen that passes into oxygen flow 5～15L/min in heat treatment process carries out alloy is processed.
Step 2) after raw material melts fully, pours into ingot blank by electromagnetic agitation after 1 minute in.
Described step 3) oxygen flow is 10L/min in.
A kind of honeycomb SnO for preparing loaded with nano Pd
2The method of catalyst is characterized in that: will be 0.5%Pd according to percentage by weight, the raw material of Sn surplus be put into vacuum melting furnace, carries out melting under 250 ℃ of temperature conditions, melts fully and pours into ingot blank by electromagnetic agitation after 1 minute until raw material; Then alloy ingot blank is being rolled under the normal temperature condition＜be processed into honeycomb after the strip of 1mm; At last this honeycomb is put into heat-treatment furnace, at 150 ℃, oxygen flow is to heat-treat with in-situ oxidation under the atmospheric condition of 15L/min to react; The final honeycomb SnO that obtains loaded with nano Pd
2Catalyst.
A kind of honeycomb SnO for preparing loaded with nano Pd
2The method of catalyst is characterized in that: will be 1%Pd according to percentage by weight, the raw material of Sn surplus be put into vacuum melting furnace, carries out melting under 250 ℃ of temperature conditions, melts fully and pours into ingot blank by electromagnetic agitation after 1 minute until raw material; Then alloy ingot blank is being rolled under the normal temperature condition＜be processed into honeycomb after the strip of 1mm; At last this honeycomb is put into heat-treatment furnace, at 150 ℃, oxygen flow is to heat-treat with in-situ oxidation under the atmospheric condition of 10L/min to react; The final honeycomb SnO that obtains loaded with nano Pd
2Catalyst.
A kind of honeycomb SnO for preparing loaded with nano Pd
2The method of catalyst is characterized in that: will be 1.5%Pd according to percentage by weight, the raw material of Sn surplus be put into vacuum melting furnace, carries out melting under 250 ℃ of temperature conditions, melts fully and pours into ingot blank by electromagnetic agitation after 1 minute until raw material; Then alloy ingot blank is being rolled under the normal temperature condition＜be processed into honeycomb after the strip of 1mm; At last this honeycomb is put into heat-treatment furnace, at 150 ℃, oxygen flow is to heat-treat with in-situ oxidation under the atmospheric condition of 5L/min to react; The final honeycomb SnO that obtains loaded with nano Pd
2Catalyst.
The technology of the present invention is with the basis that is processed as of supersaturation tin palldium alloy, in conjunction with heat treatment technics under the oxygen atmosphere condition obtain that specific area is large, nano-noble metal is evenly distributed, catalysis material sound construction, the obvious new structure Pd/SnO of catalytic effect
2Catalyst material.
This clam preparation method's advantage be can obtain that specific area is large, nano-noble metal is evenly distributed, catalysis material sound construction, the obvious new structure catalysis material of catalytic effect; And this technology of preparing can be in conjunction with existing metal alloy compositions preparation, processing and Equipment for Heating Processing, less investment, low cost and other advantages.It is one that this technology of preparing closes three with the preparation of noble metal nano particles and carrier preparation and structural design, has that the technology of preparing cost is low, flow process is short, an environmental friendliness, high performance characteristics.
Description of drawings
Further specify flesh and blood of the present invention below in conjunction with accompanying drawing with example, but content of the present invention is not limited to this.
Fig. 1 is the honeycomb SnO of preparation loaded with nano Pd
2The process chart of catalyst.
The specific embodiment
The tin palldium alloy that at first contains 0.5%～1.5% palladium (percentage by weight) by the melting preparation, then obtain to have the tin palladium material of honeycomb by plate rolling and honeycomb process technology, at last this material is put into the heat-treatment furnace with certain flow oxygen atmosphere and heat-treated and the in-situ oxidation reaction, finally obtain the honeycomb SnO that load has nanometer Pd
2Catalyst article.
1, raw material and batching:
1) raw material: metallic tin (purity＞99.95%) and palladium (purity＞99.95%).
2) batching: be respectively 0.5%, 1%, 1.5% palladium according to percentage by weight, surplus is that tin carries out the raw material configuration.
2, alloy melting:
Contain 0.5%, 1%, 1.5% palladium and the surplus tin that configure are put into vacuum melting furnace (vacuum＜10
-3Pa), being respectively 250 ℃ at smelting temperature carries out being cast into ingot blank after the melting.
3, alloy ingot blank processing and Technology for Heating Processing
1) alloy ingot blank is rolled under normal temperature condition＜strip of 1mm, then is processed into honeycomb.
2) the honeycomb tin palldium alloy that obtains is put into heat-treatment furnace, under 150 ℃ of conditions, heat-treat, and the in-situ oxidation that the oxygen that passes into oxygen flow 5～15L/min in heat treatment process carries out alloy is processed.
Embodiment 1 will be 0.5%Pd according to percentage by weight, and the raw material of Sn surplus is put into vacuum melting furnace, carries out melting under 250 ℃ of temperature conditions, melt fully and will pour into ingot blank by electromagnetic agitation after 1 minute until raw material; Then alloy ingot blank is being rolled under the normal temperature condition＜be processed into honeycomb after the strip of 1mm; At last this honeycomb is put into heat-treatment furnace, at 150 ℃, oxygen flow is to heat-treat with in-situ oxidation under the atmospheric condition of 15L/min to react; The final honeycomb SnO that obtains loaded with nano Pd
2Catalyst.
Embodiment 2 will be 1%Pd according to percentage by weight, and the raw material of Sn surplus is put into vacuum melting furnace, carries out melting under 250 ℃ of temperature conditions, melt fully and will pour into ingot blank by electromagnetic agitation after 1 minute until raw material; Then alloy ingot blank is being rolled under the normal temperature condition＜be processed into honeycomb after the strip of 1mm; At last this honeycomb is put into heat-treatment furnace, at 150 ℃, oxygen flow is to heat-treat with in-situ oxidation under the atmospheric condition of 10L/min to react; The final honeycomb SnO that obtains loaded with nano Pd
2Catalyst.
Embodiment 3 will be 1.5%Pd according to percentage by weight, and the raw material of Sn surplus is put into vacuum melting furnace, carries out melting under 250 ℃ of temperature conditions, melt fully and will pour into ingot blank by electromagnetic agitation after 1 minute until raw material; Then alloy ingot blank is being rolled under the normal temperature condition＜be processed into honeycomb after the strip of 1mm; At last this honeycomb is put into heat-treatment furnace, at 150 ℃, oxygen flow is to heat-treat with in-situ oxidation under the atmospheric condition of 5L/min to react; The final honeycomb SnO that obtains loaded with nano Pd
2Catalyst.
Claims (6)
1. honeycomb SnO who prepares loaded with nano Pd
2The method of catalyst is characterized in that containing following processing step:
1) palladium of the metallic tin of purity＞99.95% and purity＞99.95% is respectively 0.5%, 1%, 1.5% palladium according to percentage by weight, surplus is that tin carries out the raw material configuration;
2) alloy melting:
Contain 0.5%, 1%, 1.5% palladium and the surplus tin that configure are put into vacuum＜10
-3In the vacuum melting furnace of Pa, be respectively 250 ℃ at smelting temperature and carry out being cast into ingot blank after the melting;
3) alloy ingot blank processing and Technology for Heating Processing:
A) alloy ingot blank is rolled under normal temperature condition＜strip of 1mm, then is processed into honeycomb,
B) the honeycomb tin palldium alloy that obtains is put into heat-treatment furnace, under 150 ℃ of conditions, heat-treat, and the in-situ oxidation that the oxygen that passes into oxygen flow 5～15L/min in heat treatment process carries out alloy is processed.
2. the honeycomb SnO of preparation loaded with nano Pd according to claim 1
2The method of catalyst is characterized in that: step 2) in after raw material melts fully, pour into ingot blank by electromagnetic agitation after 1 minute.
3. the honeycomb SnO of preparation loaded with nano Pd according to claim 1
2The method of catalyst is characterized in that: oxygen flow is 10L/min described step 3).
4. honeycomb SnO who prepares loaded with nano Pd
2The method of catalyst is characterized in that: will be 0.5%Pd according to percentage by weight, the raw material of Sn surplus be put into vacuum melting furnace, carries out melting under 250 ℃ of temperature conditions, melts fully and pours into ingot blank by electromagnetic agitation after 1 minute until raw material; Then alloy ingot blank is being rolled under the normal temperature condition＜be processed into honeycomb after the strip of 1mm; At last this honeycomb is put into heat-treatment furnace, at 150 ℃, oxygen flow is to heat-treat with in-situ oxidation under the atmospheric condition of 15L/min to react; The final honeycomb SnO that obtains loaded with nano Pd
2Catalyst.
5. honeycomb SnO who prepares loaded with nano Pd
2The method of catalyst is characterized in that: will be 1%Pd according to percentage by weight, the raw material of Sn surplus be put into vacuum melting furnace, carries out melting under 250 ℃ of temperature conditions, melts fully and pours into ingot blank by electromagnetic agitation after 1 minute until raw material; Then alloy ingot blank is being rolled under the normal temperature condition＜be processed into honeycomb after the strip of 1mm; At last this honeycomb is put into heat-treatment furnace, at 150 ℃, oxygen flow is to heat-treat with in-situ oxidation under the atmospheric condition of 10L/min to react; The final honeycomb SnO that obtains loaded with nano Pd
2Catalyst.
6. honeycomb SnO who prepares loaded with nano Pd
2The method of catalyst is characterized in that: will be 1.5%Pd according to percentage by weight, the raw material of Sn surplus be put into vacuum melting furnace, carries out melting under 250 ℃ of temperature conditions, melts fully and pours into ingot blank by electromagnetic agitation after 1 minute until raw material; Then alloy ingot blank is being rolled under the normal temperature condition＜be processed into honeycomb after the strip of 1mm; At last this honeycomb is put into heat-treatment furnace, at 150 ℃, oxygen flow is to heat-treat with in-situ oxidation under the atmospheric condition of 5L/min to react; The final honeycomb SnO that obtains loaded with nano Pd
2Catalyst.
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|---|---|---|---|
| CN201010594709.0A CN102078812B (en) | 2010-12-20 | 2010-12-20 | Method for preparing nanometer Pd loaded honeycomb structure SnO2 catalyst |
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| CN201010594709.0A CN102078812B (en) | 2010-12-20 | 2010-12-20 | Method for preparing nanometer Pd loaded honeycomb structure SnO2 catalyst |
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| CN102078812B true CN102078812B (en) | 2013-01-16 |
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| CN102489337A (en) * | 2011-12-01 | 2012-06-13 | 昆明理工大学 | SnO2 catalytic material loaded with nano precious metals and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1788839A (en) * | 2005-12-20 | 2006-06-21 | 中国科学院合肥物质科学研究院 | Foamed aluminum carried titanium dioxide catalyst, its preparation method and uses |
| CN101733165A (en) * | 2009-12-18 | 2010-06-16 | 广东工业大学 | Preparation method of integral type catalyst with low content of noble metal and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2006239917A (en) * | 2005-03-01 | 2006-09-14 | Matsushita Electric Ind Co Ltd | Honeycomb structure and its manufacturing method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1788839A (en) * | 2005-12-20 | 2006-06-21 | 中国科学院合肥物质科学研究院 | Foamed aluminum carried titanium dioxide catalyst, its preparation method and uses |
| CN101733165A (en) * | 2009-12-18 | 2010-06-16 | 广东工业大学 | Preparation method of integral type catalyst with low content of noble metal and application thereof |
Non-Patent Citations (3)
| Title |
|---|
| JP特开2006-239917A 2006.09.14 |
| N.Tsud et al.XPS, ISS and TPD study of Pd–Sn interactions on Pd–SnOx systems.《Thin Solid Films》.2001,第391卷204-208. * |
| N.Tsudetal.XPS ISS and TPD study of Pd–Sn interactions on Pd–SnOx systems.《Thin Solid Films》.2001 |
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