CN102489297B - 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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- CN102489297B CN102489297B CN201110392361.1A CN201110392361A CN102489297B CN 102489297 B CN102489297 B CN 102489297B CN 201110392361 A CN201110392361 A CN 201110392361A CN 102489297 B CN102489297 B CN 102489297B
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- 239000000463 material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 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 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000012545 processing Methods 0.000 claims abstract description 7
- 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 63
- 238000006555 catalytic reaction Methods 0.000 claims description 31
- 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
- 238000007254 oxidation reaction Methods 0.000 claims description 10
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 9
- 238000011065 in-situ storage Methods 0.000 claims description 9
- 229910052737 gold Inorganic materials 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 8
- 229910052697 platinum Inorganic materials 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
- 239000000155 melt Substances 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
- 238000013461 design Methods 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 239000000969 carrier Substances 0.000 abstract 1
- 150000003608 titanium Chemical class 0.000 abstract 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 15
- 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
- 239000003054 catalyst Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 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
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram 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
- 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
- 238000005025 nuclear technology Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000001556 precipitation Methods 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 nano-noble-metal-loaded
2catalysis material and preparation method thereof, belongs to catalysis material technical field.
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., oneself presents 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, in order to save consumption, the reduction material/product cost of 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 develop 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.) remains in some problems effectively fixing aspect noble metal nano particles, material is not enough to the physics, the chemical property that keep high in application, and this is the huge challenge facing during noble metal nano particles uses.If noble metal nano particles due to and carrier between can not form effective metallurgical binding, be in use likely subject to the huge surface of nano particle can impact and reunite, and then the performance of nano material character is brought to negative effect.
The catalytic activity of metal oxide carrier catalysis material and the structure of metal oxide carrier of nano-noble-metal-loaded have very large relation, particularly metal oxide carrier material specific area size, determine 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 to increase 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 object of this invention is to provide TiO2 catalysis material of a kind of nano-noble-metal-loaded and preparation method thereof, obtain surface uniform, be combined with securely the TiO of nano-noble metal particle
2catalysis material, solves nano-noble metal and effectively combination of carrier, causes the physics of catalysis material, the problem of unstable chemcial property.
Technical scheme of the present invention is: the TiO of nano-noble-metal-loaded
2catalysis material, be taking titanium as carrier, top layer is TiO
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 in Au, Pd, Pt, and grain graininess is nanoscale, and its percentage by weight is the percentage by weight that 1%～3%(accounts for whole catalysis material).
The TiO of nano-noble-metal-loaded of the present invention
2the preparation method of catalysis material is: first prepare the titanium-base alloy containing 1%～3% noble metal (percentage by weight) by melting, then by plate rolling and honeycomb processing, acquisition has the titanium-based alloy material of multi-layer cylinder shape honeycomb, finally this material is put into the heat-treatment furnace with certain flow oxygen atmosphere is heat-treated and in-situ oxidation reaction, finally obtaining load has the multi-layer cylinder shape honeycomb TiO of nano-noble metal
2catalysis material product.Concrete preparation process is as follows:
(1) first by 1%～3% percentage by weight, get one or more any mixture in Au, Pd and Pt, prepare burden with Titanium, then put into smelting furnace, adjust vacuum <1 × 10
-3pa carries out melting under 1150 DEG C～1350 DEG C temperature conditions, and then electromagnetic agitation 1～3 minute after raw material melts completely pours into a mould ingot blank naturally cooling;
(2) under normal temperature condition, by common metal board rolling method, by the ingot blank obtaining in the middle of step (1) under be rolled into the titanium-base alloy strip of thickness <1mm, be processed into again honeycomb, and be curled into multi-layer cylinder shape, finally obtain the titanium-base alloy of multi-layer cylinder shape honeycomb;
(3) the honeycomb titanium-base alloy of acquisition is put into heat-treatment furnace, be heated to 300 DEG C～600 DEG C, then pass into high purity oxygen gas by the flow of 5～15L/min, alloy is heat-treated with in-situ oxidation and is processed 1～4 hour, then after naturally cooling, come out of the stove, obtain surface firmly load have the multi-layer cylinder shape honeycomb TiO of nano-noble metal particle
2catalysis material.
The equal >99.95% of purity of described noble metal and Titanium.
Described high purity oxygen gas is that purity is 99.999% oxygen.
The present invention first makes alloy material by noble metal and carrier material, be reprocessed into multi-layer cylinder shape honeycomb, then under certain oxidizing atmosphere condition, alloy is heat-treated and in-situ oxidation processing, combine processing characteristics and the Precipitation formation nanophase of noble metal in heat treatment process and the method for matrix oxidation formation metal oxide of supersaturation metal alloy, the preparation of noble metal nano particles and carrier preparation 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 large, nano-noble metal is evenly distributed, catalysis material sound construction, the obvious new structure catalysis material of catalytic effect;
(2) can, in conjunction with existing metal alloy compositions preparation, processing and Equipment for Heating Processing, there is less investment, low cost and other advantages.
(3) development trend of composite technology of preparing " efficiently, low cost, short flow process, environmental friendliness, high-performance ".
brief description of the drawings:
Fig. 1 is process chart of the present invention;
Fig. 2 is the cylinder-shaped honeycomb structure Ti O that area load of the present invention has nano-noble metal particle
2catalysis material schematic diagram.
specific embodiments:
Below in conjunction with drawings and Examples, the present invention is further elaborated, but protection content of the present invention is not limited to described scope.
Embodiment 1:(is as Fig. 1)
(1) first by 1.5% percentage by weight, get the Au of purity >99.95%, prepare burden with the Titanium of purity >99.95%, then put into smelting furnace, adjust vacuum 1 × 10
-4pa carries out melting under 1150 DEG C of temperature conditions, and then electromagnetic agitation 1 minute after raw material melts completely pours into a mould ingot blank naturally cooling;
(2) under normal temperature condition, by common metal board rolling method, by the ingot blank obtaining in the middle of step (1) under be rolled into the titanium-base alloy strip of thickness 0.8mm, then be processed into honeycomb, and be curled into multi-layer cylinder shape, finally obtain the titanium-base alloy of multi-layer cylinder shape honeycomb;
(3) the honeycomb titanium-base alloy of acquisition is put into heat-treatment furnace, be heated to 300 DEG C, then pass into high purity oxygen gas by the flow of 5L/min, alloy is heat-treated with in-situ oxidation and is processed 4 hours, then after naturally cooling, come out of the stove, obtain surface firmly load have the multi-layer cylinder shape honeycomb TiO of nano-noble metal particle
2catalysis material, be taking titanium as carrier, top layer is TiO
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 is less than 100nm, the equal >99.95% of purity of noble metal and Titanium, the nano-noble metal of load is Au, its percentage by weight is 1.5%.(as Fig. 2)
Embodiment 2:(is as Fig. 1)
(1) first by 1% percentage by weight, get the equal >99.95%Pd of purity, prepare burden with the equal >99.95% Titanium of purity, then put into smelting furnace, adjust vacuum <1 × 10
-5pa carries out melting under 1250 DEG C of temperature conditions, and then electromagnetic agitation 2 minutes after raw material melts completely pours into a mould ingot blank naturally cooling;
(2) under normal temperature condition, by common metal board rolling method, by the ingot blank obtaining in the middle of step (1) under be rolled into the titanium-base alloy strip of thickness 0.6mm, then be processed into honeycomb, and be curled into multi-layer cylinder shape, finally obtain the titanium-base alloy of multi-layer cylinder shape honeycomb;
(3) the honeycomb titanium-base alloy of acquisition is put into heat-treatment furnace, be heated to 400 DEG C, then pass into high purity oxygen gas by the flow of 11L/min, alloy is heat-treated with in-situ oxidation and is processed 3 hours, then after naturally cooling, come out of the stove, obtain surface firmly load have the multi-layer cylinder shape honeycomb TiO of nano-noble metal particle
2catalysis material, be taking titanium as carrier, top layer is TiO
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 is less than 100nm, the equal >99.95% of purity of noble metal and Titanium, the nano-noble metal of load is Pd, its percentage by weight is 1%.(as Fig. 2)
Embodiment 3:(is as Fig. 1)
(1) first by 2% percentage by weight, get Au and the Pt of purity >99.95%, prepare burden with purity >99.95% Titanium, then put into smelting furnace, adjust vacuum 1 × 10
-5pa carries out melting under 1350 DEG C of temperature conditions, and then electromagnetic agitation 3 minutes after raw material melts completely pours into a mould ingot blank naturally cooling;
(2) under normal temperature condition, by common metal board rolling method, by the ingot blank obtaining in the middle of step (1) under be rolled into the titanium-base alloy strip of thickness 0.4mm, then be processed into honeycomb, and be curled into multi-layer cylinder shape, finally obtain the titanium-base alloy of multi-layer cylinder shape honeycomb;
(3) the honeycomb titanium-base alloy of acquisition is put into heat-treatment furnace, be heated to 600 DEG C, then pass into high purity oxygen gas by the flow of 15L/min, alloy is heat-treated with in-situ oxidation and is processed 1 hour, then after naturally cooling, come out of the stove, obtain surface firmly load have the multi-layer cylinder shape honeycomb TiO of nano-noble metal particle
2catalysis material, be taking titanium as carrier, top layer is TiO
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 is less than 100nm, the equal >99.95% of purity of noble metal and Titanium, the nano-noble metal of load is any mixture in Au and Pt, its percentage by weight is 2%.(as Fig. 2)
Embodiment 4:(is as Fig. 1)
(1) first by 3% percentage by weight, any mixture of getting purity 99.95%Au, Pd and Pt, prepares burden with purity 99.95% Titanium, then puts into smelting furnace, adjusts vacuum 1 × 10
-4pa carries out melting under 1180 DEG C of temperature conditions, and then electromagnetic agitation 3 minutes after raw material melts completely pours into a mould ingot blank naturally cooling;
(2) under normal temperature condition, by common metal board rolling method, by the ingot blank obtaining in the middle of step (1) under be rolled into the titanium-base alloy strip of thickness 0.9mm, then be processed into honeycomb, and be curled into multi-layer cylinder shape, finally obtain the titanium-base alloy of multi-layer cylinder shape honeycomb;
(3) the honeycomb titanium-base alloy of acquisition is put into heat-treatment furnace, be heated to 600 DEG C, then pass into high purity oxygen gas by the flow of 15L/min, alloy is heat-treated with in-situ oxidation and is processed 2 hours, then after naturally cooling, come out of the stove, obtain surface firmly load have the multi-layer cylinder shape honeycomb TiO of nano-noble metal particle
2catalysis material, be taking titanium as carrier, top layer is TiO
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 is less than 100nm, the equal >99.95% of purity of noble metal and Titanium, the nano-noble metal of load is any mixture in Au, Pd and Pt, its percentage by weight is 3%.(as Fig. 2).
Claims (4)
1. the multi-layer cylinder shape honeycomb TiO of a nano-noble-metal-loaded
2catalysis material, is characterized in that: be taking titanium as carrier, top layer is TiO
2and load has the multi-layer cylinder shape honeycomb TiO of nano-noble metal particle
2catalysis material; The nano-noble metal of load is one or more any mixture in Au, Pd, Pt, and its percentage by weight is 1%～3%; The granularity of the nano-noble metal on titanium carrier surface is less than 100nm, the equal >99.95% of purity of noble metal and Titanium.
2. the TiO of a nano-noble-metal-loaded
2the preparation method of catalysis material, it is characterized in that: first prepare the titanium-base alloy containing 1%～3% noble metal by melting, then by plate rolling and honeycomb processing, acquisition has the titanium-based alloy material of multi-layer cylinder shape honeycomb, finally this material is put into the heat-treatment furnace with certain flow oxygen atmosphere is heat-treated and in-situ oxidation reaction, finally obtaining load has the multi-layer cylinder shape honeycomb TiO of nano-noble metal
2catalysis material product; Noble metal is one or more any mixture in Au, Pd, Pt.
3. the TiO of nano-noble-metal-loaded according to claim 2
2the preparation method of catalysis material, is characterized in that: concrete preparation process is as follows:
(1) first by 1%～3% percentage by weight, noble metal and Titanium are prepared burden, then put into smelting furnace, adjustment vacuum <1 × 10
-3pa carries out melting under 1150 DEG C～1350 DEG C temperature conditions, and then electromagnetic agitation 1～3 minute after raw material melts completely pours into a mould ingot blank naturally cooling;
(2) under normal temperature condition, by common metal board rolling method, by the ingot blank obtaining in the middle of step (1) under be rolled into the titanium-base alloy strip of thickness <1mm, and then be processed into multi-layer cylinder shape honeycomb;
(3) the honeycomb titanium-base alloy of acquisition is put into heat-treatment furnace, be heated to 300 DEG C～600 DEG C, then pass into high purity oxygen gas by the flow of 5～15L/min, alloy is heat-treated with in-situ oxidation and is processed 1～3 hour, then after naturally cooling, come out of the stove, obtain surface firmly load have the multi-layer cylinder shape honeycomb TiO of nano-noble metal particle
2catalysis material.
4. according to the TiO of the nano-noble-metal-loaded described in claim 2 or 3
2the preparation method of catalysis material, is characterized in that: the granularity of the nano-noble metal on titanium carrier surface is less than 100nm.
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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 |
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