CN102029153B - Method for preparing nano Ag-loaded honeycomb-structured SnO2 catalyst - Google Patents
Method for preparing nano Ag-loaded honeycomb-structured SnO2 catalyst Download PDFInfo
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- CN102029153B CN102029153B CN201010594718XA CN201010594718A CN102029153B CN 102029153 B CN102029153 B CN 102029153B CN 201010594718X A CN201010594718X A CN 201010594718XA CN 201010594718 A CN201010594718 A CN 201010594718A CN 102029153 B CN102029153 B CN 102029153B
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- honeycomb
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- catalyst
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- heat
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- 239000003054 catalyst Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims description 24
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title abstract 6
- 239000000956 alloy Substances 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000001301 oxygen Substances 0.000 claims abstract description 22
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 22
- 238000005516 engineering process Methods 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 229910001316 Ag alloy Inorganic materials 0.000 claims abstract description 6
- 230000008018 melting Effects 0.000 claims description 28
- 238000002844 melting Methods 0.000 claims description 28
- 239000002994 raw material Substances 0.000 claims description 25
- 229910045601 alloy Inorganic materials 0.000 claims description 22
- 229910052709 silver Inorganic materials 0.000 claims description 20
- 238000007254 oxidation reaction Methods 0.000 claims description 16
- 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
- 238000013019 agitation Methods 0.000 claims description 11
- 239000000155 melt Substances 0.000 claims description 11
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 10
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 10
- 239000004332 silver Substances 0.000 claims description 10
- 238000003723 Smelting Methods 0.000 claims description 3
- 229910052774 Proactinium Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 19
- 229910000510 noble metal Inorganic materials 0.000 abstract description 18
- 238000006555 catalytic reaction Methods 0.000 abstract description 10
- 229910001092 metal group alloy Inorganic materials 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- 238000003754 machining Methods 0.000 abstract 2
- 238000009827 uniform distribution Methods 0.000 abstract 2
- QCEUXSAXTBNJGO-UHFFFAOYSA-N [Ag].[Sn] Chemical class [Ag].[Sn] QCEUXSAXTBNJGO-UHFFFAOYSA-N 0.000 abstract 1
- 239000002082 metal nanoparticle Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 239000000969 carrier Substances 0.000 description 2
- 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
- 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
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 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
- 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
- 239000007787 solid Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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- Catalysts (AREA)
Abstract
The invention relates to a preparation method of a nano Ag-loaded honeycomb-structured SnO2 catalyst. By using the technology, a novel structured Ag/SnO2 catalyst material which has the advantages of large specific area, uniform distribution of nano noble metal, stable catalysis material structure and obvious catalysis effect can be obtained on the basis of machining a supersaturated tin-silver alloy by combining a heat treatment technology under an oxygen atmosphere condition. By using the invention, a novel structured catalysis material which has the advantages of large specific area, uniform distribution of nano noble metal, stable catalysis material structure and obvious catalysis effect can be obtained. Besides, the preparation technology can be combined with the traditional metal alloy material preparation, machining and heat-treating equipment and has the advantages of low investment, low cost and the like.
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, function solenoid material, absorbing material, sensor components and parts material and nano composite material etc., demonstrate 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 practicing thrift 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.Developed at present Ag, Pt, Au nanocrystal have been distributed to zeolite, TiO
2, Al
2O
3, SiO
2, 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 receive the huge surface of nano particle can influence and reunite, and then the performance of nano material character is brought negative effect.The present invention mainly proposes with the problem that carrier effectively combines for solving nano-noble metal; Present technique has combined the processing characteristics of supersaturation metal alloy and the deposition of noble metal in heat treatment process to separate out the method that forms nanophase and matrix oxidation formation metal oxide preferably; The preparation and the preparing carriers of noble metal nano particles are united two into one, embodied the development trend of material preparation technology " efficient, low-cost, short flow process, environmental friendliness, high-performance ".
Summary of the invention
The object of the invention is to invent a kind of combination over-saturation metal alloy compositions processing and separates out principle mutually with parent metal in-situ oxidation, noble metal second; Earlier the over-saturation metal alloy compositions is processed into honeycomb; Through 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 Ag then
2Catalysis material.
The present invention realizes through following scheme:
The honeycomb SnO of preparation loaded with nano Ag
2The method of catalyst contains following processing step:
1) silver of the metallic tin of purity＞99.95% and purity＞99.95% is respectively 1%, 2% and 3% silver according to weight percent meter, surplus is that tin carries out the raw material configuration;
2) alloy melting:
Contain 1%, 2% or 3% silver and the surplus tin that configure are put into vacuum＜10
-3In the vacuum melting furnace of Pa, be respectively 240 ℃, 230 ℃ or 220 ℃ 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, is processed into honeycomb then,
B) the honeycomb sn-ag alloy that obtains is put into heat-treatment furnace, under 180 ℃, 200 ℃ and 220 ℃ of conditions, heat-treat respectively, and the in-situ oxidation that the oxygen of aerating oxygen flow 5～15L/min carries out alloy in heat treatment process is handled.
Step 2) after treating in that raw material melts fully, pours into ingot blank after 1 minute through electromagnetic agitation.
Said oxygen flow is 10L/min.
Said oxygen flow is 5L/min.
A kind of honeycomb SnO for preparing loaded with nano Ag
2The method of catalyst is characterized in that: will be 1%Ag according to percentage by weight, the raw material of Sn surplus be put into vacuum melting furnace, under 240 ℃ of temperature conditions, carries out melting, treats that raw material melts fully and pours into ingot blank through electromagnetic agitation after 1 minute; Then alloy ingot blank is being rolled under the normal temperature condition＜be processed into honeycomb behind the slab of 1mm; At last this honeycomb is put into heat-treatment furnace, at 180 ℃, 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 Ag
2Catalyst.
A kind of honeycomb SnO for preparing loaded with nano Ag
2The method of catalyst is characterized in that: will be 2%Ag according to percentage by weight, the raw material of Sn surplus be put into vacuum melting furnace, under 230 ℃ of temperature conditions, carries out melting, treats that raw material melts fully and pours into ingot blank through electromagnetic agitation after 1 minute; 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 200 ℃, 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 Ag
2Catalyst.
A kind of honeycomb SnO for preparing loaded with nano Ag
2The method of catalyst is characterized in that: will be 3%Ag according to percentage by weight, the raw material of Sn surplus be put into vacuum melting furnace, under 240 ℃ of temperature conditions, carries out melting, treats that raw material melts fully and pours into ingot blank through electromagnetic agitation after 1 minute; 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 220 ℃, 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 Ag
2Catalyst.
The present invention should technology with the basis that is processed as of supersaturation sn-ag alloy, in conjunction with heat treatment technics under the oxygen atmosphere condition obtain that specific area is big, nano-noble metal is evenly distributed, catalysis material sound construction, the tangible new structure Ag/SnO of catalytic effect
2Catalyst material.
Advantage of the present invention be can obtain that specific area is big, nano-noble metal is evenly distributed, catalysis material sound construction, the tangible new structure catalysis material of catalytic effect; And this technology of preparing can combine existing metal alloy compositions preparation, processing and Equipment for Heating Processing, less investment, low cost and other advantages.
It is one that preparation method of the present invention closes three with the preparation of noble metal nano particles and preparing carriers and structural design, has that the technology of preparing cost is low, a flow process weak point, environmental friendliness, high performance characteristics.
Description of drawings
Further specify flesh and blood of the present invention below in conjunction with accompanying drawing with instance, but content of the present invention is not limited to this.
Fig. 1 is the honeycomb SnO that the present invention prepares loaded with nano Ag
2The process chart of catalyst.
The specific embodiment
The sn-ag alloy that at first contains 1%～3% silver medal (percentage by weight) through the melting preparation; Obtain to have the tin ag material of honeycomb then through plate rolling and honeycomb process technology; At last this material is put into the heat-treatment furnace with certain flow oxygen atmosphere and heat-treat and the in-situ oxidation reaction, finally obtain the honeycomb SnO that load has nanometer Ag
2Catalyst article.
1, raw material and batching:
1) raw material: metallic tin (purity＞99.95%) and silver (purity＞99.95%).
2) batching: be respectively 1%, 2%, 3% silver according to percentage by weight, surplus is that tin carries out the raw material configuration.
2, alloy melting:
Contain 1%, 2%, 3% silver and the surplus tin that configure are put into vacuum melting furnace (vacuum＜10
-3Pa), being respectively 240 ℃, 230 ℃ and 220 ℃ 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, is processed into honeycomb then.
2) the honeycomb sn-ag alloy that obtains is put into heat-treatment furnace, under 180 ℃, 200 ℃ and 220 ℃ of conditions, heat-treat respectively, and the in-situ oxidation that the oxygen of aerating oxygen flow 5～15L/min carries out alloy in heat treatment process is handled.
Embodiment 1 will be 1%Ag according to percentage by weight, and the raw material of Sn surplus is put into vacuum melting furnace, under 240 ℃ of temperature conditions, carries out melting, treat that raw material melts fully and pours into ingot blank through electromagnetic agitation after 1 minute; Then alloy ingot blank is being rolled under the normal temperature condition＜be processed into honeycomb behind the slab of 1mm; At last this honeycomb is put into heat-treatment furnace, at 180 ℃, 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 Ag
2Catalyst.
Embodiment 2 will be 2%Ag according to percentage by weight, and the raw material of Sn surplus is put into vacuum melting furnace, under 230 ℃ of temperature conditions, carries out melting, treat that raw material melts fully and pours into ingot blank through electromagnetic agitation after 1 minute; 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 200 ℃, 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 Ag
2Catalyst.
Embodiment 3 will be 3%Ag according to percentage by weight, and the raw material of Sn surplus is put into vacuum melting furnace, under 240 ℃ of temperature conditions, carries out melting, treat that raw material melts fully and pours into ingot blank through electromagnetic agitation after 1 minute; 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 220 ℃, 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 Ag
2Catalyst.
Claims (7)
1. honeycomb SnO who prepares loaded with nano Ag
2The method of catalyst is characterized in that containing following processing step:
1) silver of the metallic tin of purity＞99.95% and purity＞99.95% is respectively 1%, 2% and 3% silver according to weight percent meter, surplus is that tin carries out the raw material configuration;
2) alloy melting:
Contain 1%, 2% or 3% silver and the surplus tin that configure are put into vacuum＜10
-3In the vacuum melting furnace of Pa, be respectively 240 ℃, 230 ℃ or 220 ℃ 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, is processed into honeycomb then,
B) the honeycomb sn-ag alloy that obtains is put into heat-treatment furnace, under 180 ℃, 200 ℃ and 220 ℃ of conditions, heat-treat respectively, and the in-situ oxidation that the oxygen of aerating oxygen flow 5～15L/min carries out alloy in heat treatment process is handled.
2. the honeycomb SnO of preparation loaded with nano Ag according to claim 1
2The method of catalyst is characterized in that: step 2) in treat that raw material melts fully after, pour into ingot blank through electromagnetic agitation after 1 minute.
3. according to the honeycomb SnO of claim 1 described preparation loaded with nano Ag
2The method of catalyst is characterized in that: said oxygen flow is 10L/min.
4. method according to claim 1 prepares the honeycomb SnO of loaded with nano Ag
2Catalyst is characterized in that: said oxygen flow is 5L/min.
5. honeycomb SnO who prepares loaded with nano Ag
2The method of catalyst is characterized in that: will be 1%Ag according to percentage by weight, the raw material of Sn surplus be put into vacuum melting furnace, under 240 ℃ of temperature conditions, carries out melting, treats that raw material melts fully and pours into ingot blank through electromagnetic agitation after 1 minute; Then alloy ingot blank is being rolled under the normal temperature condition＜be processed into honeycomb behind the slab of 1mm; At last this honeycomb is put into heat-treatment furnace, at 180 ℃, 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 Ag
2Catalyst.
6. honeycomb SnO who prepares loaded with nano Ag
2The method of catalyst is characterized in that: will be 2%Ag according to percentage by weight, the raw material of Sn surplus be put into vacuum melting furnace, under 230 ℃ of temperature conditions, carries out melting, treats that raw material melts fully and pours into ingot blank through electromagnetic agitation after 1 minute; 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 200 ℃, 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 Ag
2Catalyst.
7. honeycomb SnO who prepares loaded with nano Ag
2The method of catalyst is characterized in that: will be 3%Ag according to percentage by weight, the raw material of Sn surplus be put into vacuum melting furnace, under 240 ℃ of temperature conditions, carries out melting, treats that raw material melts fully and pours into ingot blank through electromagnetic agitation after 1 minute; 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 220 ℃, 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 Ag
2Catalyst.
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| CN201010594718XA CN102029153B (en) | 2010-12-20 | 2010-12-20 | Method for preparing nano Ag-loaded honeycomb-structured SnO2 catalyst |
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|---|---|---|---|
| CN201010594718XA CN102029153B (en) | 2010-12-20 | 2010-12-20 | Method for preparing nano Ag-loaded honeycomb-structured SnO2 catalyst |
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| CN102029153B true CN102029153B (en) | 2012-10-31 |
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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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| 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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| JP特开2006-239917A 2006.09.14 |
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