CN102489297A - Tio2 catalytic material for loading nano precious metals and preparation method thereof - Google Patents
Tio2 catalytic material for loading nano precious metals and preparation method thereof Download PDFInfo
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- CN102489297A CN102489297A CN2011103923611A CN201110392361A CN102489297A CN 102489297 A CN102489297 A CN 102489297A CN 2011103923611 A CN2011103923611 A CN 2011103923611A CN 201110392361 A CN201110392361 A CN 201110392361A CN 102489297 A CN102489297 A CN 102489297A
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- 239000000463 material Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 230000003197 catalytic effect Effects 0.000 title abstract description 11
- 239000010970 precious metal Substances 0.000 title abstract 4
- 239000000956 alloy Substances 0.000 claims abstract description 30
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000012545 processing Methods 0.000 claims abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000001301 oxygen Substances 0.000 claims abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 4
- 229910000510 noble metal Inorganic materials 0.000 claims description 66
- 238000006555 catalytic reaction Methods 0.000 claims description 34
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 27
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 26
- 239000010936 titanium Substances 0.000 claims description 26
- 229910052719 titanium Inorganic materials 0.000 claims description 26
- 239000002923 metal particle Substances 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000007254 oxidation reaction Methods 0.000 claims description 10
- 229910052737 gold Inorganic materials 0.000 claims description 9
- 238000011065 in-situ storage Methods 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 8
- 238000005096 rolling process Methods 0.000 claims description 8
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 7
- 229910001882 dioxygen Inorganic materials 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 229910052763 palladium Inorganic materials 0.000 claims description 7
- 238000003723 Smelting Methods 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 239000004567 concrete Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 5
- 239000000969 carrier Substances 0.000 abstract description 2
- 238000013461 design Methods 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 150000003608 titanium Chemical class 0.000 abstract 1
- 239000002082 metal nanoparticle Substances 0.000 description 6
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- 238000003825 pressing Methods 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 239000012876 carrier material Substances 0.000 description 2
- 229910001092 metal group alloy Inorganic materials 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
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 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
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 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
- 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
- 238000005025 nuclear technology Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000011160 research 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 Tio2 catalytic material for loading nano precious metals and a preparation method thereof. The technique is based on processing of oversaturated titanium-based alloy, and combined with the heat treatment technique on the condition of an oxygen atmosphere to obtain the Tio2 catalytic material of a multi-layer cylindrical honeycomb structure. The Tio2 catalytic material has a large specific surface area, the nano precious metals are evenly distributed, the structure of the catalytic material is firm, and the catalytic effect is obvious. The preparation technique integrates preparation of precious metal nano particles, preparation of carriers and structural design into one, and has the advantages of being low in cost, short in process, environment-friendly and high in property. Products prepared through the technique can be used in the fields of automobiles, oil, chemical industry and the like.
Description
Technical field:
The present invention relates to a kind of multi-layer cylinder shape honeycomb TiO of loaded with nano noble metal
2Catalysis material and preparation method thereof belongs to the catalysis material technical field.
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., oneself demonstrates 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 catalytic activity of the metal oxide carrier catalysis material of loaded with nano noble metal and the structure of metal oxide carrier have very big relation; Particularly metal oxide carrier material specific area size; Determined the distribution of nano-noble metal, and the quantity of catalytic activity point.Therefore, the present invention passes through carrier TiO
2The structural design of material obtains multi-layer cylinder shape honeycomb TiO
2Carrier to be increasing its specific area, thereby improves the specific area of the nano-noble metal of load, improved the catalytic activity point of catalyst, finally improves the catalytic performance of such catalyst.
Summary of the invention:
The purpose of this invention is to provide TiO2 catalysis material of a kind of loaded with nano noble metal and preparation method thereof, obtain the TiO that the surface is combined with the nano-noble metal particle evenly, securely
2Catalysis material solves nano-noble metal and can not effectively combine with carrier, causes the physics of catalysis material, the problem of unstable chemcial property.
Technical scheme of the present invention is: the TiO of loaded with nano noble metal
2Catalysis material is to be that carrier, top layer are TiO with the titanium
2And load has the multi-layer cylinder shape honeycomb catalysis material of nano-noble metal particle.The nano-noble metal of load is one or more any mixture among Au, Pd, the Pt, and grain graininess is a nanoscale, and its percentage by weight is 1%～3% (accounting for the percentage by weight of whole catalysis material).
The TiO of loaded with nano noble metal of the present invention
2The preparation method of catalysis material is: the titanium-base alloy that at first contains 1%～3% noble metal (percentage by weight) through the melting preparation; Then through plate rolling and honeycomb processing; Acquisition has the titanium-based alloy material of multi-layer cylinder shape honeycomb; 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 multi-layer cylinder shape honeycomb TiO that load has nano-noble metal
2The catalysis material product.Concrete preparation process is following:
(1) earlier by 1%～3% percentage by weight, get one or more any mixture among Au, Pd and the Pt, prepare burden with Titanium, put into smelting furnace then, adjustment vacuum<1 * 10
-3Pa carries out melting under 1150 ℃～1350 ℃ temperature conditions, treat that raw material melted the back electromagnetic agitation 1～3 minute fully, pours into a mould ingot blank and cooling naturally then;
(2) under the normal temperature condition; With common metal board rolling method, < the titanium-base alloy strip of 1mm is processed into honeycomb again being rolled into thickness down with the ingot blank that obtains in the middle of the step (1); And be curled into the multi-layer cylinder shape, finally obtain the titanium-base alloy of multi-layer cylinder shape honeycomb;
(3) the honeycomb titanium-base alloy that obtains is put into heat-treatment furnace; Be heated to 300 ℃～600 ℃; Flow by 5～15L/min feeds high purity oxygen gas then; Alloy is heat-treated and in-situ oxidation was handled 1～4 hour, come out of the stove after the cooling naturally then, obtain the multi-layer cylinder shape honeycomb TiO that the firm load in surface has the nano-noble metal particle
2Catalysis material.
The purity of said noble metal and Titanium is equal>99.95%.
Said high purity oxygen gas is that purity is 99.999% oxygen.
The present invention processes alloy material with noble metal and carrier material earlier; Be reprocessed into multi-layer cylinder shape honeycomb; Under certain oxidizing atmosphere condition, alloy heat-treated with in-situ oxidation then and handle; In conjunction with processing characteristics and the deposition of noble metal in heat treatment process of supersaturation metal alloy separate out and form the method that nanophase and matrix oxidation form metal oxide; The preparation and the preparing carriers of noble metal nano particles are united two into one, finally prepare the cylindric multi-layer honeycomb structure Ti O that is evenly distributed with nano-noble metal
2Catalysis material.
The present invention compared with prior art has the following advantages:
(1) 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;
(2) can combine existing metal alloy compositions preparation, processing and Equipment for Heating Processing, have less investment, low cost and other advantages.
(3) development trend of Composite Preparation technology " efficient, low-cost, short flow process, environmental friendliness, high-performance ".
Description of drawings:
Fig. 1 is a process chart of the present invention;
Fig. 2 is the cylinder-shaped honeycomb structure Ti O that area load of the present invention has the nano-noble metal particle
2The catalysis material sketch map.
Specific embodiments:
Below in conjunction with accompanying drawing and embodiment the present invention is done further elaboration, but protection content of the present invention is not limited to said scope.
Embodiment 1: (like Fig. 1)
(1) 1.5% percentage by weight is pressed by elder generation, gets Chun Du>99.95% Au is with Chun Du>99.95% Titanium is prepared burden, and puts into smelting furnace then, adjustment vacuum 1 * 10
-4Pa carries out melting under 1150 ℃ of temperature conditions, treat that raw material melted the back electromagnetic agitation 1 minute fully, pours into a mould ingot blank and cooling naturally then;
(2) under the normal temperature condition; With common metal board rolling method, the ingot blank that obtains in the middle of the step (1) in the titanium-base alloy strip that is rolled into thickness 0.8mm down, is processed into honeycomb again; And be curled into the multi-layer cylinder shape, finally obtain the titanium-base alloy of multi-layer cylinder shape honeycomb;
(3) the honeycomb titanium-base alloy that obtains is put into heat-treatment furnace; Be heated to 300 ℃; The flow of pressing 5L/min then feeds high purity oxygen gas; Alloy is heat-treated and in-situ oxidation was handled 4 hours, come out of the stove after the cooling naturally then, obtain the multi-layer cylinder shape honeycomb TiO that the firm load in surface has the nano-noble metal particle
2Catalysis material is to be that carrier, top layer are TiO with the titanium
2And load has the multi-layer cylinder shape honeycomb TiO of nano-noble metal particle
2Catalysis material, the granularity of the nano-noble metal on titanium carrier surface be less than 100nm, the purity purity > of noble metal and Titanium; 99.95%, the nano-noble metal of load is Au, and its percentage by weight is 1.5%.(like Fig. 2)
Embodiment 2: (like Fig. 1)
(1) 1% percentage by weight is pressed by elder generation, gets purity purity>99.95%Pd is with purity purity>99.95% Titanium is prepared burden, and puts into smelting furnace then, adjustment vacuum<1 * 10
-5Pa carries out melting under 1250 ℃ of temperature conditions, treat that raw material melted the back electromagnetic agitation 2 minutes fully, pours into a mould ingot blank and cooling naturally then;
(2) under the normal temperature condition; With common metal board rolling method, the ingot blank that obtains in the middle of the step (1) in the titanium-base alloy strip that is rolled into thickness 0.6mm down, is processed into honeycomb again; And be curled into the multi-layer cylinder shape, finally obtain the titanium-base alloy of multi-layer cylinder shape honeycomb;
(3) the honeycomb titanium-base alloy that obtains is put into heat-treatment furnace; Be heated to 400 ℃; The flow of pressing 11L/min then feeds high purity oxygen gas; Alloy is heat-treated and in-situ oxidation was handled 3 hours, come out of the stove after the cooling naturally then, obtain the multi-layer cylinder shape honeycomb TiO that the firm load in surface has the nano-noble metal particle
2Catalysis material is to be that carrier, top layer are TiO with the titanium
2And load has the multi-layer cylinder shape honeycomb TiO of nano-noble metal particle
2Catalysis material, the granularity of the nano-noble metal on titanium carrier surface be less than 100nm, the purity purity > of noble metal and Titanium; 99.95%, the nano-noble metal of load is Pd, and its percentage by weight is 1%.(like Fig. 2)
Embodiment 3: (like Fig. 1)
(1) 2% percentage by weight is pressed by elder generation, gets Chun Du>99.95% Au and Pt are with Chun Du>99.95% Titanium is prepared burden, and puts into smelting furnace then, adjustment vacuum 1 * 10
-5Pa carries out melting under 1350 ℃ of temperature conditions, treat that raw material melted the back electromagnetic agitation 3 minutes fully, pours into a mould ingot blank and cooling naturally then;
(2) under the normal temperature condition; With common metal board rolling method, the ingot blank that obtains in the middle of the step (1) in the titanium-base alloy strip that is rolled into thickness 0.4mm down, is processed into honeycomb again; And be curled into the multi-layer cylinder shape, finally obtain the titanium-base alloy of multi-layer cylinder shape honeycomb;
(3) the honeycomb titanium-base alloy that obtains is put into heat-treatment furnace; Be heated to 600 ℃; The flow of pressing 15L/min then feeds high purity oxygen gas; Alloy is heat-treated and in-situ oxidation was handled 1 hour, come out of the stove after the cooling naturally then, obtain the multi-layer cylinder shape honeycomb TiO that the firm load in surface has the nano-noble metal particle
2Catalysis material is to be that carrier, top layer are TiO with the titanium
2And load has the multi-layer cylinder shape honeycomb TiO of nano-noble metal particle
2Catalysis material, the granularity of the nano-noble metal on titanium carrier surface be less than 100nm, the purity purity > of noble metal and Titanium; 99.95%, the nano-noble metal of load is any mixture among Au and the Pt, and its percentage by weight is 2%.(like Fig. 2)
Embodiment 4: (like Fig. 1)
(1) 3% percentage by weight is pressed by elder generation, and any mixture of getting purity 99.95%Au, Pd and Pt is prepared burden with purity 99.95% Titanium, puts into smelting furnace then, adjustment vacuum 1 * 10
-4Pa carries out melting under 1180 ℃ of temperature conditions, treat that raw material melted the back electromagnetic agitation 3 minutes fully, pours into a mould ingot blank and cooling naturally then;
(2) under the normal temperature condition; With common metal board rolling method, the ingot blank that obtains in the middle of the step (1) in the titanium-base alloy strip that is rolled into thickness 0.9mm down, is processed into honeycomb again; And be curled into the multi-layer cylinder shape, finally obtain the titanium-base alloy of multi-layer cylinder shape honeycomb;
(3) the honeycomb titanium-base alloy that obtains is put into heat-treatment furnace; Be heated to 600 ℃; The flow of pressing 15L/min then feeds high purity oxygen gas; Alloy is heat-treated and in-situ oxidation was handled 2 hours, come out of the stove after the cooling naturally then, obtain the multi-layer cylinder shape honeycomb TiO that the firm load in surface has the nano-noble metal particle
2Catalysis material is to be that carrier, top layer are TiO with the titanium
2And load has the multi-layer cylinder shape honeycomb TiO of nano-noble metal particle
2Catalysis material, the granularity of the nano-noble metal on titanium carrier surface be less than 100nm, the purity purity > of noble metal and Titanium; 99.95%, the nano-noble metal of load is any mixture among Au, Pd and the Pt, and its percentage by weight is 3%.(like Fig. 2).
Claims (7)
1. the TiO of a loaded with nano noble metal
2Catalysis material is characterized in that: be to be that carrier, top layer are TiO with the titanium
2And load has the multi-layer cylinder shape honeycomb TiO of nano-noble metal particle
2Catalysis material.
2. the TiO of loaded with nano noble metal according to claim 1
2Catalysis material is characterized in that: the granularity of the nano-noble metal on titanium carrier surface is less than 100nm, the purity purity > of noble metal and Titanium; 99.95%.
3. the TiO of loaded with nano noble metal according to claim 1 and 2
2Catalysis material is characterized in that: the nano-noble metal of load is one or more any mixture among Au, Pd, the Pt, and its percentage by weight is 1%～3%.
4. the preparation method of the TiO2 catalysis material of a loaded with nano noble metal; It is characterized in that: the titanium-base alloy that at first contains 1%～3% noble metal through the melting preparation; Then through plate rolling and honeycomb processing; Acquisition has the titanium-based alloy material of multi-layer cylinder shape honeycomb, at last this material is put into the heat-treatment furnace with certain flow oxygen atmosphere and heat-treats and the in-situ oxidation reaction, finally obtains the multi-layer cylinder shape honeycomb TiO that load has nano-noble metal
2The catalysis material product.
5. the preparation method of the TiO2 catalysis material of loaded with nano noble metal according to claim 4 is characterized in that: concrete preparation process is following:
(1) 1%～3% percentage by weight is pressed by elder generation, and noble metal and Titanium are prepared burden, and puts into smelting furnace then, adjustment vacuum<1 * 10
-3Pa carries out melting under 1150 ℃～1350 ℃ temperature conditions, treat that raw material melted the back electromagnetic agitation 1～3 minute fully, pours into a mould ingot blank and cooling naturally then;
(2) under the normal temperature condition,, the ingot blank that obtains in the middle of the step (1) is being rolled into thickness < the titanium-base alloy strip of 1mm, and then be processed into multi-layer cylinder shape honeycomb down with common metal board rolling method;
(3) the honeycomb titanium-base alloy that obtains is put into heat-treatment furnace; Be heated to 300 ℃～600 ℃; Flow by 5～15L/min feeds high purity oxygen gas then; Alloy is heat-treated and in-situ oxidation was handled 1～3 hour, come out of the stove after the cooling naturally then, obtain the multi-layer cylinder shape honeycomb TiO that the firm load in surface has the nano-noble metal particle
2Catalysis material.
6. according to the preparation method of the TiO2 catalysis material of claim 4 or 5 described loaded with nano noble metals, it is characterized in that: the granularity of the nano-noble metal on titanium carrier surface is less than 100nm.
7. according to the preparation method of the TiO2 catalysis material of claim 4 or 5 described loaded with nano noble metals, it is characterized in that: noble metal is one or more any mixture among Au, Pd, the Pt.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104258849A (en) * | 2014-08-28 | 2015-01-07 | 绍兴文理学院 | Crystalline mesoporous cerium dioxide palladium-loaded material for catalyzing oxidation, and synthesis method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2855467A1 (en) * | 1978-12-19 | 1980-09-18 | Gock Eberhard | Synthetic titanium di:oxide prodn. from rutile - by direct dissolution with sulphuric acid after activation by milling to alter crystal lattice structure |
| CN102068982A (en) * | 2010-12-20 | 2011-05-25 | 昆明理工大学 | Preparation method of nano Pt-loaded honeycomb Al2O3 catalyst |
| CN102068984A (en) * | 2010-12-20 | 2011-05-25 | 昆明理工大学 | Preparation technique of nano Pd-loaded honeycomb-structured Al2O3 catalyst |
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2011
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2855467A1 (en) * | 1978-12-19 | 1980-09-18 | Gock Eberhard | Synthetic titanium di:oxide prodn. from rutile - by direct dissolution with sulphuric acid after activation by milling to alter crystal lattice structure |
| CN102068982A (en) * | 2010-12-20 | 2011-05-25 | 昆明理工大学 | Preparation method of nano Pt-loaded honeycomb Al2O3 catalyst |
| CN102068984A (en) * | 2010-12-20 | 2011-05-25 | 昆明理工大学 | Preparation technique of nano Pd-loaded honeycomb-structured Al2O3 catalyst |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104258849A (en) * | 2014-08-28 | 2015-01-07 | 绍兴文理学院 | Crystalline mesoporous cerium dioxide palladium-loaded material for catalyzing oxidation, and synthesis method thereof |
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