CN103157466A - Application of titanium oxide-supported noble metal catalyst in decomposition reaction of N2O - Google Patents
Application of titanium oxide-supported noble metal catalyst in decomposition reaction of N2O Download PDFInfo
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- CN103157466A CN103157466A CN2011104135076A CN201110413507A CN103157466A CN 103157466 A CN103157466 A CN 103157466A CN 2011104135076 A CN2011104135076 A CN 2011104135076A CN 201110413507 A CN201110413507 A CN 201110413507A CN 103157466 A CN103157466 A CN 103157466A
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Abstract
The invention relates to an application of a titanium oxide-supported noble metal catalyst in a decomposition reaction of nitrous oxide. In the catalyst, TiO2 comprising various crystal forms and mixed crystal forms thereof is employed as a carrier, and a noble metal in the group VIII is used as an active component. The titanium oxide-supported noble metal catalyst is firstly used for the decomposition reaction of N2O, can greatly reduce an initial reaction temperature and a complete conversion temperature of the decomposition of N2O, meets the requirements for relatively good low temperature activity and high temperature stability required by the decomposition of N2O, and can efficiently catalyze the conversion of nitrous oxide in relatively wide concentrations and space velocity ranges. The catalyst has easily available raw materials, simple process and very good application prospects.
Description
Technical field
The present invention relates to a kind of TiO
2Support the application of noble metal catalyst in the nitrous oxide decomposition reaction, specifically, this catalyst is with TiO
2For carrier (contain the crystal formation of various titaniums and mix crystal formation), noble metal Ir, Pb, Pt, Rh, Ru are active component, can be at the initial decomposing N of lower temperature
2The O reaction also can reduce complete decomposition temperature, is the best catalyst of reporting at present.
Background technology
Nitrous oxide (N
2O) be a kind of important greenhouse gases, its content in atmosphere is 319ppbv, comes the 3rd in greenhouse gases, inferior to CO
2And CH
4, but from greenhouse effects, its greenhouse effects are respectively CO
2And CH
4310 times and 21 times, if increase with present year speedup degree (0.18-0.26%), after 50 years, N
2The greenhouse effects of O will equal CO
2Greenhouse effects.In addition, N
2O is NO in stratosphere
xMain source, radical reaction can occur damage the ozone layer, and ozone layer has the ability of very strong absorption sunshine middle-ultraviolet lamp, can stop ultraviolet ray to the mankind's irradiation, the safety of to protect mankind.Nearest more than ten years, along with the continuous enhancing of people's environmental consciousness, increasing scholar began to seek effectively to control N
2O is to the method for airborne release.Wherein, directly decompose waste gas N from ammonia conversion stove etc. under higher temperature
2O is exactly both economical, an effective removing method, and this method has proposed higher requirement to the activity of catalyst, life-span, high high-temp stability etc.
In recent years, N
2O has been subject to great attention as the novel green propellant at space industry.N
2O is the superior propellant of a kind of uniqueness: at first, and N
2O has higher storage density (745kg/m
3), can be with gas or long-term storage in liquid form; Secondly, has very high saturated vapour pressure (52atm, 20 ℃), liquid state or gaseous state N
2O can rely on the vapour pressure of self to discharge storage system, realizes from supercharging, does not need supercharging equipment and propulsion system is simplified greatly; Again, nontoxic, and good with the universal architecture material compatibility, be convenient to system and development.What is more important, N
2O can realize that various modes advances: rely on self vapour pressure with N
2O gas directly sprays and the cold air propelling (can be used for attitude controls) of generation thrust; N
2O produces high-temperature gas mixture body (63.7%N through catalytic decomposition
2+ 36.3%O
2) monopropellant propulsion (be used for track keep); With N
2The high-temperature oxygen-enriched combustion gas that the O catalytic decomposition produces is oxidant, with the bipropellant propulsion (being used for becoming rail) of fuel regnition burning.N
2The auto-pressurizing multimode of this uniqueness of O advances and has cold air, single constituent element and double-base specific impulse feature concurrently, and thrust range is wide, and simple and flexible is that other propellant technology is incomparable at present.
N
2It is to realize N that O decomposes
2O eliminates and N
2Prerequisite and basis that O advances.N
2O decomposition reaction equation is:
N
2O (g) → N
2(g)+
1/
2O
2(g) (Δ H °
RThe exothermic heat of reaction of=-82.5kJ/mol) is strong, pure N
2The O adiabatic decomposition temperature is up to 1640 ℃; Pyrolysis activation energy is very high, almost can't detect N below 600 ℃
2O decomposes.Adopt catalyst technology, can change response path, make N
2O decomposes, improves reaction speed at lower temperature.Therefore, N
2The O catalytic decomposition is N
2One of the basis that O advances and key technology directly determine the engineering feasibility of this new ideas space flight Push Technology.
In a word, no matter be to use at field of Environment Protection or as missile propellant, good low temperature active and high high-temp stability are all to N
2The basic demand of O decomposition catalyst.
N
2The O decomposition catalyst is studied widely, roughly can divide and make following several classes, that is: (1) one pack system oxide; (2) composite metal oxide; (3) molecular sieve catalyst; (4) loaded noble metal catalyst.Front two class catalyst pay attention to inquiring into catalytic decomposition N
2The mechanism of O, rear two class catalyst are laid particular stress on N
2The O degrading activity.
With regard to carrier itself, crystal formation and preparation method's difference has caused catalytic activity and the anti-sintering property of noble metal-based catalysts.A lot of documents have been reported, as Pd/Al
2O
3-La
2O
3Catalyst (Applied Catalysis B:Environmental, 2005.56 (4): p.279-288) improved the catalytic activity of using hydrogen reducing NO; Rh/K-γ-Al
2O
3System can improve dispersion (Catalysis Today, 2004.90 (1-2): p.15-19 of noble metal Rh; Applied Catalysis B:Environmental, 2008.77 (3-4): p.278-283), and then improve catalytic activity; Pt-Ba-γ-Al
2O
3NOx storage and reducing activity and selective (Applied Catalysis B:Environmental, 2008.80 (3-4): p.214-225.) of obviously improving.Yet TiO
2Catalyst basedly but be rarely used in the research of NOx catalytic decomposition, especially be applied to N
2The O decomposition reaction.(J.Phys.Chem.C 2010,114,14101-14109 for Bokhimi and Okumura et al.; Journal of Catalysis 2,002 208 485-489) has reported TiO
2The impact on CO catalytic oxidation activity of the Ir that supports and Au catalyst, but also be not applied at present N
2The report of O decomposition reaction.
Summary of the invention
The object of the present invention is to provide a kind of TiO
2The application of the noble metal catalyst that supports.
For achieving the above object, the technical solution used in the present invention is:
A kind of titanium oxide supports noble metal catalyst at N
2Application in the O decomposition reaction, this catalyst is made of carrier and active component two parts, with TiO
2Crystal is carrier, and active component is VIII family noble metal.Wherein the quality percentage composition of reactive metal in catalyst is 0.1-20%.
Described active component is one or two or more kinds in iridium, palladium, platinum, rhodium and ruthenium, and wherein the quality percentage composition of reactive metal in catalyst is preferably 0.1-5%.
Described TiO
2Crystal formation is rutile or the mixing crystal formation that comprises rutile.
The preparation of described catalyst:
1. the preparation of carrier:
Described TiO
2Carrier obtains with the precipitation method, hydro-thermal method, sol method or calcination, is specially:
1) with the TiO of anatase, rutile, brockite or P25
2One or more in crystal formation mix through 400-900 ℃ of calcining 2-5h acquisition carrier;
2) adopt inorganic precursor thing or the organic precursor thing process hydrolytic precipitation of Ti, room temperature to 90 ℃ stirring in water bath 3-8h, filtration washing, 80-150 ℃ of drying, then 400-900 ℃ of calcining 2-5h obtains carrier;
3) according to above-mentioned 1) or 2) two kinds of TiO that method obtains
2Perhaps the inorganic precursor thing of Ti mixes with water, urea or other basic anhydride, and 80-200 ℃ of Hydrothermal Synthesis 12-72h obtains carrier in the self-pressure still;
4) adopt the organic precursor thing of Ti to mix with ethanol, P123 or F127, in room temperature to 120 ℃ stirring, 400-900 ℃ of calcining obtains carrier under air, hydrogen, nitrogen or argon atmospher;
The inorganic precursor thing of described Ti is titanium tetrachloride, Titanium Nitrate or titanium trichloride;
The organic precursor thing of described Ti is four n-butyl titaniums, 2-ethyl-1-hexanol titanium or isopropyl titanate.
2. the preparation of supported carrier active component:
1) preparation catalyst
By required load amount, adopt dipping method that the noble metal precursor body is loaded on above-mentioned prepared carrier, room temperature is standing 〉=and 12 hours, 80-120 ℃ of oven drying, then in 400-600 ℃ of calcining 2-5h, obtain catalyst;
Or, 2) the deposition-precipitation method Kaolinite Preparation of Catalyst
By required load amount, adopt deposition-precipitation method that the noble metal precursor body is loaded on above-mentioned prepared carrier, be specially: the noble metal of theoretical content is mixed with the Ti carrier, and room-temperature water bath stirs, and adds precipitating reagent, after be heated to 80-100 ℃ and stir 5-8h, filter washing, 80-120 ℃ of oven dry, 400-600 ℃ of calcining obtains catalyst.
Described noble metal precursor body is one or more in chloro-iridic acid, palladium bichloride, chloroplatinic acid, rhodium chloride, ruthenium trichloride;
Described precipitating reagent is urea, NaOH, one or more in potassium hydroxide.
The application of described catalyst:
Described catalyst is used for the nitrous oxide decomposition reaction, and nitrous oxide can be at the initial decomposing N of the lower temperature of 180-200 ℃ with after catalyst contacts
2The O reaction also can reduce complete decomposition temperature;
The volumetric concentration 0.05-100% of nitrous oxide, the Balance Air of dilution nitrous oxide is inert gas.
Described catalyst can make N
2O efficiently decomposes, and 300 ℃ reach 100% conversion, and initial decomposition temperature is lower than 200 ℃; Inert gas is helium or argon gas.
Described nitrous oxide or the air speed that contains the unstripped gas of nitrous oxide are 1000-50000mlh
-1g
-1 cat
Described catalyst before being used for the nitrous oxide decomposition reaction, 300-500 ℃ of reduction 0.5-2h under nitrogen atmosphere.
Titanium oxide of the present invention supports the noble metal catalyst catalyzing N
2O decomposition reaction activity is high, can greatly reduce N
2The initial decomposition reaction temperature of O and complete conversion temperature.At 200 ℃ of initial N of energy
2O decomposition reaction (the initial decomposition reaction of low temperature preferably is active) reaches 100% conversion ratio at 300 ℃, is the N that reports at present
2The highest active catalyst in the O decomposition catalyst.This catalyst has the characteristics of good stability, under 300 ℃ of reaction temperatures, can keep for a long time N
2The high activity that O decomposes, after operation 1500min, through reduction, catalytic activity not only can be recovered, and even also improves to some extent, then passes through long-play, still keeps N
2The high conversion of O decomposition reaction.This catalyst has applicability preferably, at wider concentration 0.05%-100% and air speed 1000ml h
-1g
-1 cat-50000ml h
-1g
-1 catCan make N in scope
2The O Efficient Conversion.Catalyst raw material of the present invention is easy to get, and technique is simple, has good application prospect.
Description of drawings
Fig. 1 is the XRD figure of the embodiment of the present invention 5 and comparing embodiment 3 Kaolinite Preparation of Catalysts.
Fig. 2 is the temperature programming reaction result of the embodiment of the present invention 5 and comparing embodiment 4 Kaolinite Preparation of Catalysts.
Fig. 3 is the reactivity test result of the embodiment of the present invention 5 different crystal forms titanium oxide catalysts.
Fig. 4 is that the embodiment of the present invention 5 titanium oxide support different noble metal catalyst reaction test results.
Fig. 5 is the reactivity test result that the embodiment of the present invention 5 supports different bullion content catalyst.
Fig. 6 is the reaction stability test result of the embodiment of the present invention 6 catalyst.
Fig. 7 is the embodiment of the present invention 7 different N
2The reactivity test result of O concentration.
Fig. 8 is the reactivity test result of the embodiment of the present invention 8 different air speeds.
The specific embodiment
Titanium oxide supports noble metal catalyst and is used for first N
2The O decomposition reaction can greatly reduce initial reaction temperature and complete conversion temperature that nitrous oxide decomposes, has satisfied N
2O decomposes required low temperature active preferably and the requirement of high temperature stability performance; Can transform by the inferior nitrogen of efficiently catalyzing and oxidizing in wider concentration and air speed scope.Catalyst raw material of the present invention is easy to get, and technique is simple, has good application prospect.
Following instance is used for illustrating in greater detail the present invention, but the present invention is not limited to this.
The preparation of carrier:
The TiO that 1) will directly buy
2Carrier directly at 900 ℃ of calcining 3h, obtains the rutile crystal type titanium oxide.
2) TiCl
4Through hydrolysis, 1molTiCl
4Add 200ml water, after 90 ℃ of stirring in water bath 8h, 120 ℃ of dry 12h, then 900 ℃ of calcining 3h obtain the rutile crystal type carrier.
3) 10mmol isopropyl titanate and 40ml ethanol mix, and add 10g P123 and 5g red fuming nitric acid (RFNA) (concentration 75%), put into 80 ℃ of baking ovens after stirring at room 8h, dry 72h, and rear 900 ℃ of calcining 3h obtain the rutile crystal type carrier.
4) adopt anatase, P25, brockite or embodiment 1,2,3 titanium oxides that obtain and NaOH with 1: 10 mix and blend of mass ratio, put into airtight still, keep 72h at 120 ℃ of baking ovens, take out washing, 80 ℃ of dry 12h, rear 900 ℃ of calcinings obtain the rutile crystal type carrier.
The preparation of catalyst:
1) carrier of dipping embodiment 1 acquisition, preparation catalyst series Ir/TiO
2
Take the chloro-iridic acid aqueous solution 0.8733g that contains iridium 2.3wt% mass fraction of dilution, respectively add respectively the carrier of 1.0g embodiment 1 preparation, the room temperature hold over night, after put into 80 ℃ of baking ovens, after dry 24h, 500 ℃ of calcining 2h, obtain catalyst in Muffle furnace.
2) carrier of even phase deposition sedimentation embodiment 1 acquisition, preparation catalyst series Ir/TiO
2
Take the chloro-iridic acid aqueous solution 0.8733g that contains iridium 2.3wt% mass fraction of dilution, add the dilution of 50ml water, then pour in the 150ml aqueous solution of the carrier that contains 1.0g embodiment 1 preparation, then add precipitating reagent urea 20g, after put into water-bath, be warmed up to 90 ℃ and stir 7h, centrifugal filtration, washing, put into 80 ℃ of baking ovens, after dry 24h, 500 ℃ of calcining 2h, obtain catalyst in Muffle furnace.The Ir/TiO that obtains
2Catalyst XRD result as shown in Figure 1, this series Ir/TiO
2There is no obvious IrO on catalyst
2Diffraction maximum, can infer IrO
2Particle may less than 3nm, have decentralization preferably on this catalyst series.Specific area characterization result such as the table 1 of the catalyst that obtains.
Embodiment 3
Compare with embodiment 2, different is that the noble metal precursor body is palladium bichloride, chloroplatinic acid, rhodium chloride or ruthenium trichloride, and unclassified stores consumption and operating condition are identical with embodiment 2.
Embodiment 4
Compare with embodiment 2, the percentage composition of different is Ir is 0.1-5%, and unclassified stores consumption and operating condition are identical with embodiment 2.
Embodiment 5
The activity rating of the catalyst that embodiment 2,3,4 obtains.
Take the catalyst that 0.1g embodiment 2,3,4 obtains, 400 ℃ of reduction 0.5h after the Ar air-blowing is swept 0.5h and dropped to room temperature again under nitrogen atmosphere, start program test that heats up.Gas volume consists of 30vol.%N
2O+70vol.%Ar, total flow is 50ml/min (STP), air speed is 30000ml h
-1g
-1 catConcrete outcome is as shown in Fig. 2,3,4,5, and this catalyst has higher N in 200 ℃ of-300 ℃ of scopes
2The O transformation efficiency.
Embodiment 6
The estimation of stability of the catalyst that embodiment 2 obtains.
Take the catalyst that 0.08g embodiment 21 obtains, 400 ℃ of reduction 0.5h after the Ar air-blowing is swept 0.5h and dropped to room temperature again, begin to warm to 300 ℃ under nitrogen atmosphere, and along with the time surveys actively, gas composition is 30%N
2O+70%Ar, total flow is 50ml/min (STP).This catalyst has carried out loop test twice, and concrete outcome as shown in Figure 6.
Embodiment 7
Compare with embodiment 5, that different is N
2The concentration of O is 0.05%-100%, and unclassified stores consumption and operating condition are identical with embodiment 5.Concrete outcome as shown in Figure 7.
Embodiment 8
Compare with embodiment 5, that different is N
2The air speed of O is 1000-50000ml h
-1g
-1 cat, unclassified stores consumption and operating condition are identical with embodiment 5.Concrete outcome as shown in Figure 8.
Comparing embodiment 1
Preparation Al
2O
3Carrier.
Aluminum nitrate calcining 3h with 9 crystallizations water obtains Al
2O
3
Comparing embodiment 2
900 ℃ of dinectly bruning 3h of cerous nitrate obtain CeO
2
Comparing embodiment 3
The carrier Kaolinite Preparation of Catalyst Ir/Al that even phase deposition sedimentation comparing embodiment 1,2 obtains
2O
3, Ie/CeO
2
Seven parts of chloro-iridic acid aqueous solution 0.8733g that contains iridium 2.3wt% mass fraction that take dilution add the dilution of 50ml water, pour into again in the 150ml aqueous solution of the carrier that contains 1.0 g comparing embodiment 1 and 2 preparations, dropwise add the chloro-iridic acid dilution in room temperature, then add urea 20g, after put into water-bath, be warmed up to 90 ℃ and stir 7h, centrifugal filtration, washing, put into 80 ℃ of baking ovens, after dry 24h, 500 ℃ of calcining 2h, obtain catalyst in Muffle furnace.The Ir/Al that obtains
2O
3, Ir/CeO
2Catalyst XRD result as shown in Figure 1.
Comparing embodiment 4
The activity rating of the catalyst that comparing embodiment 3 obtains.
Take the catalyst that 0.1g comparing embodiment 3 obtains, 400 ℃ of reduction 0.5h after the Ar air-blowing is swept 0.5h and dropped to room temperature again under nitrogen atmosphere, start program test that heats up.Gas composition is 30%N
2O+70%Ar, total flow is 50ml/min (STP).Concrete outcome as shown in Figure 2, this catalyst has N in 300 ℃ of-450 ℃ of scopes
2The O transformation efficiency.
Comparing embodiment 5
The specific area of the catalyst that comparing embodiment 3 obtains, actual bullion content and decentralization characterization result such as table 1.
Table 1 is the embodiment of the present invention 2 and comparing embodiment 5 catalyst physical property measurement results
Claims (10)
1. a titanium oxide supports noble metal catalyst at N
2Application in the O decomposition reaction is characterized in that: this catalyst is made of carrier and active component two parts, with TiO
2Crystal is carrier, and active component is VIII family noble metal; Wherein the quality percentage composition of reactive metal in catalyst is 0.1-20%.
2. according to application claimed in claim 1, it is characterized in that: wherein the quality percentage composition of reactive metal in catalyst is preferably 0.1-5%.
3. according to application claimed in claim 1, it is characterized in that: described active component is one or two or more kinds in iridium, palladium, platinum, rhodium and ruthenium, described TiO
2Crystal formation is rutile or the mixing crystal formation that comprises rutile.
4. according to the described application of claim 1 or 3, it is characterized in that:
Described TiO
2Carrier can the precipitation method, hydro-thermal method, sol method or calcination obtain, and are specially:
1) with the TiO of anatase, rutile, brockite or P25
2One or more in crystal formation mix through 400-900 ℃ of calcining 2-5h acquisition carrier;
Or, 2) adopt the inorganic precursor thing of Ti or organic precursor thing to pass through hydrolytic precipitation, room temperature to 90 ℃ stirring in water bath 3-8h, filtration washing, 80-150 ℃ of drying, then 400-900 ℃ of calcining 2-5h obtains carrier;
3) according to above-mentioned 1) or 2) two kinds of TiO that method obtains
2Perhaps the inorganic precursor thing of Ti and water or contain a kind of or two kinds of aqueous solution in urea, NaOH, potassium hydroxide, Ti and solution mixed proportion are 1: 10,80-200 ℃ of Hydrothermal Synthesis 12-72h obtains carrier in airtight still;
4) adopt the organic precursor thing of Ti to mix with ethanol, P123 or F127, mixed proportion is the 10mmolTi precursor: 10g ethanol (P123 or F127), in room temperature to 120 ℃ stirring, 400-900 ℃ of calcining obtains carrier under air, hydrogen, nitrogen or argon atmospher;
The inorganic precursor thing of described Ti is titanium tetrachloride, Titanium Nitrate or titanium trichloride;
The organic precursor thing of described Ti is four n-butyl titaniums, 2-ethyl-1-hexanol titanium or isopropyl titanate.
5. according to the described application of claim 1 or 4, it is characterized in that:
1) preparation catalyst
By required load amount, adopt dipping method that the noble metal precursor body is loaded on carrier, in dipping process carrier room temperature in dipping standing 〉=12 hours, 80-120 ℃ of oven drying, then in 400-600 ℃ of calcining 2-5h, obtain catalyst;
Or, 2) the deposition-precipitation method Kaolinite Preparation of Catalyst
By required load amount, adopt deposition-precipitation method that the noble metal precursor body is loaded on carrier, be specially: the noble metal of required theoretical content is mixed with the Ti carrier, and room-temperature water bath stirs, and in Ti: precipitating reagent=ratio added precipitating reagent such as urea, NaOH or potassium hydroxide in 1: 30, after be heated to 80-100 ℃ and stir 5-8h, filter washing, 80-120 ℃ of oven dry, 400-600 ℃ of calcining obtains catalyst.
6. according to application claimed in claim 5, it is characterized in that: described noble metal precursor body is one or more in chloro-iridic acid, palladium bichloride, chloroplatinic acid, rhodium chloride, ruthenium trichloride;
Described precipitating reagent is urea, NaOH, one or more in potassium hydroxide.
7. according to application claimed in claim 1, it is characterized in that: described catalyst is used for the nitrous oxide decomposition reaction, and nitrous oxide can be at the initial decomposing N of the lower temperature of 180-200 ℃ with after catalyst contacts
2The O reaction also can reduce complete decomposition temperature;
The volumetric concentration 0.05-100% of nitrous oxide, the Balance Air of dilution nitrous oxide is inert gas.
8. according to the application of the described catalyst of claim 7, it is characterized in that: described catalyst can make N
2O efficiently decomposes, and 300 ℃ reach 100% conversion, and initial decomposition temperature is lower than 200 ℃; Inert gas is helium or argon gas.
9. according to application claimed in claim 7, it is characterized in that: nitrous oxide or the air speed that contains the unstripped gas of nitrous oxide are 1000-50000ml h
-1g
-1 cat
10. according to the described application of claim 1 or 7, it is characterized in that:
Described catalyst before being used for the nitrous oxide decomposition reaction, 300-500 ℃ of reduction 0.5-2h under nitrogen atmosphere.
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| CN105032409A (en) * | 2015-07-03 | 2015-11-11 | 中国科学院过程工程研究所 | Self-assembled nano ruthenium catalyst used for catalytic oxidation of VOCs, and preparation method and applications thereof |
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