CN107511065A - A kind of catalytic purification method containing carbon monoxide waste gas - Google Patents
A kind of catalytic purification method containing carbon monoxide waste gas Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/864—Removing carbon monoxide or hydrocarbons
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- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
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Abstract
The present invention relates to waste gas processing method technical field, specifically a kind of catalytic purification method containing carbon monoxide waste gas, comprise the following steps：In the presence of a catalyst, the waste gas containing carbon monoxide is passed through, oxygen in waste gas is more than the concentration of carbon monoxide, carries out catalytic oxidation, carbon monoxide in waste gas is transformed into carbon dioxide, reaction temperature is 100~50 DEG C；The catalyst is made up of complex carrier and the active component being carried on the complex carrier, and the complex carrier is the composite of rare earth oxide and titanium dioxide, and the active component is Au；And further provide the preparation method of used catalyst in the catalytic purification method；The present invention compared with the existing technology, has the advantages of catalyzing carbon monoxide oxidation activity is high, service life is long, heat endurance is good, it is difficult the shortcomings that possessing high thermal stability and long service life while possessing high catalytic activity to solve prior art.
Description
[technical field]
The present invention relates to waste gas processing method technical field, specifically a kind of catalysis containing carbon monoxide waste gas is net
Change method.
[background technology]
It is well known that CO is typical flammable, toxic compounds.Combustion of fossil fuel, chemical industry and motor vehicle make
With causing a large amount of CO to discharge, as serious environmental problem, the common concern of people is caused.CO low temperature (<100℃)
Elimination has important use value in many aspects, in CO2The purifying of gas, CO gas detectors material in laser, exhale
Gas cleaning plant is smoked, and closed system is (such as：Aircraft, submarine, spacecraft etc.) in the elimination etc. of trace amounts of CO have
Important application prospect.In addition, in fuel cell studies, it is made by low-carbon alcohols and hydrocarbon moiety oxidation or steam reforming
Hydrogen rich gas often contain about 0.5~3mol CO, its presence can cause fuel cell electrode to be poisoned, so as to cause fuel cell
Efficiency is greatly lowered, it is necessary to which selectivity eliminates CO.Therefore, realize that CO aoxidizes conversion and has become catalysis at a lower temperature to grind
One of hot issue studied carefully.
By years of researches, a variety of catalyst with CO oxidation susceptibilities are had been developed that, catalyst can be according to difference
Species is classified with preparation method.It can be divided into noble metal (Au, Pt, Pd etc.), base metal, molecular sieve and alloy by species to urge
Agent etc..It can be divided into traditional infusion process, complexing infusion process, coprecipitation, deposition-precipitation method, chemical gas by method for preparing catalyst
Phase sedimentation, ion-exchange, sol-gal process, electric arc melting method, plasma sputtering method and solvated metal atom dipping
Method etc..The highest attention of scholar is wherein more caused with its extremely low catalytic temperature with noble metal Au catalyst series.
But the general catalyst with CO oxidation susceptibilities is all difficult to possess higher heat while possessing high catalytic activity
Stability and longer service life.
[content of the invention]
A kind of catalytic purification containing carbon monoxide waste gas is provided present invention aim to solve above-mentioned deficiency
Method, this method have the advantages of catalyzing carbon monoxide oxidation activity is high, service life is long, heat endurance is good, solved existing
Technology is difficult the shortcomings that possessing high thermal stability and long service life while possessing high catalytic activity.
A kind of catalytic purification method containing carbon monoxide waste gas is designed to achieve the above object, is comprised the following steps：
In the presence of catalyst, the waste gas containing carbon monoxide is passed through, oxygen in waste gas is more than the concentration of carbon monoxide, urged
Oxidation, carbon monoxide in waste gas is set to transform into carbon dioxide；The catalyst is by complex carrier and is carried on this
Active component on complex carrier is formed, and the complex carrier is the composite of rare earth oxide and titanium dioxide, the work
Property component is Au.
Further, the reaction pressure of the catalytic oxidation is normal pressure, and reaction temperature is -100~50 DEG C.
Further, the rare earth oxide is lanthana or cerium oxide, and the rare earth oxide content is complex carrier
0.1~5wt.% of gross weight, the Au content are 0.1~2wt.% of total catalyst weight.
Further, the content of the lanthana or cerium oxide is 1~5wt.% of complex carrier gross weight, the Au's
Content is 0.5~2wt.% of total catalyst weight.
Present invention also offers a kind of preparation method of used catalyst in above method, comprise the following steps：1) use
Sol-gel process prepares the TiO of rare earth oxide doping2Carrier：At 40 DEG C, by 40vol%Ti (OR)4Ethanol solution delay
It is slow to instill in water, glacial acetic acid, absolute ethyl alcohol and the mixed liquor of lanthanum nitrate hexahydrate or six nitric hydrate ceriums, and be stirred continuously and to be formed
Colloidal sol, 40-60 DEG C is then heated to, continuing stirring makes solvent slowly volatilize, and forms gel, and the product of gained is placed on 80-120
Dry, be finally calcined obtained xerogel at 120-800 DEG C, 400-600 DEG C of sintering temperature, roasting time in DEG C baking oven
6h, obtain the TiO of rare earth oxide doping2Carrier；2) aqueous solution of chloraurate is prepared：Gold chloride is configured to the aqueous solution, its is dense
Spend for 0.00638mol/L；3) solution obtained by step 2) is taken, adds the TiO of rare earth oxide doping made from step 1)2Carry
Body, 50-100 DEG C is heated with stirring to, is aged 1-4h, in 60-120 DEG C of dry 6-18h, is calcined under 300-800 DEG C of temperature conditionss
1-6h, that is, obtain various carrier loaded Au base catalyst.
Further, the Au-based catalyst adulterated through rare earth oxide is fitted into fixed bed reactors, carries out CO low temperature
Oxidation reaction, reaction condition are：The mol ratio of oxygen and carbon monoxide is 1-10 in reaction gas:1, the volume space velocity of reaction gas is
1000-20000h-1。
Further, the mol ratio of the oxygen and carbon monoxide is 8-10:1, the volume space velocity of reaction gas is 3000-
10000h-1。
Further, catalyst is screened to 60-80 mesh, be fitted into reaction tube, and be passed through reaction gas, reaction gas 1%
CO, 10%O2, 89%N2Gaseous mixture, it is 50ml/min to control its flow velocity, then temperature programming, 3 DEG C/min of programming rate, every
One active site of 5-10 DEG C of measure, until CO is converted completely, wherein CO contents are detected with TCD detectors.
The present invention is compared with the existing technology, there is provided a kind of method of the effectively exhaust-gas treatment containing carbon monoxide, that is, is directed to
Made improvements in some shortcomings of existing method, using the titanium dioxide of rare earth doped oxide as carrier loaded Au catalyst
For being catalyzed the oxidation of CO gases, there is the advantages of catalyzing carbon monoxide oxidation activity is high, service life is long, heat endurance is good, solution
Prior art of having determined is difficult to possess lacking for higher heat endurance and longer service life while possessing high catalytic activity
Point；In addition, using method of the present invention, in the waste gas containing carbon monoxide, from subzero 50 degree to normal temperature, this is wider
In reaction temperature region, in the presence of a catalyst, the carbon monoxide in waste gas can be transformed into dioxy long-term and stably
Change carbon, the activity of catalyst does not reduce；And in catalyst noble metal content it is especially low, eliminate waste gas in especially economic method
Middle carbon monoxide, without the generation of unnecessary accessory substance, secondary pollution is not caused, be the side of the highly effective processing containing carbon monoxide
Method, there is larger environmental protection application prospect, be worthy of popularization.
[brief description of the drawings]
Fig. 1 is Au/La used in the embodiment of the present invention 1,2,32O3-TiO2The catalyzing carbon monoxide oxidation of catalyst is lived
Property figure, wherein, (a) Au/TiO2, (b) Au/1La%-TiO2, (c) Au/3La%-TiO2, (d) Au/5La%-TiO2；
Fig. 2 is Au/CeO used in the embodiment of the present invention 4,5,62-TiO2The catalyzing carbon monoxide oxidation activity of catalyst
Figure, wherein, (a) Au/TiO2, (b) Au/1Ce%-TiO2, (c) Au/3Ce%-TiO2, (d) Au/5Ce%-TiO2；
Fig. 3 is the Au/-TiO of rare earth oxide doping used in the embodiment of the present invention 3,62The carbon monoxide of catalyst
The figure of catalysis oxidation stability.
[embodiment]
The invention provides a kind of catalytic purification method containing carbon monoxide waste gas, comprise the following steps：In catalyst
In the presence of, the waste gas containing carbon monoxide is passed through, oxygen in waste gas is more than the concentration of carbon monoxide, so can just there is foot
Enough oxygen aoxidizes carbon monoxide, to carry out catalytic oxidation, carbon monoxide in waste gas is transformed into carbon dioxide；
Catalyst is made up of complex carrier and the active component being carried on the complex carrier, and complex carrier is using sol-gel
Rare earth oxide and the composite of titanium dioxide prepared by method, active component Au.Wherein, the reaction pressure of catalytic oxidation
Power is normal pressure, and reaction temperature is -100~50 DEG C.Rare earth oxide is lanthana or cerium oxide, and rare earth oxide content is compound
0.1~5wt.% of total weight of carrier, Au content are 0.1~2wt.% of total catalyst weight.Preferably, lanthana or oxygen
The content for changing cerium is 1~5wt.% of complex carrier gross weight, and remaining is titanium dioxide；Au content is total catalyst weight
0.5~2wt.%.When the doping of rare earth oxide reaches 5wt.%, reaction temperature is at -30 DEG C, the conversion ratio of carbon monoxide
It just can reach 100%.
The preparation method of catalyst used by present invention also offers a kind of CO catalytic oxidation under low temperature, its principle are：It is first
Carrier is first prepared using sol-gel process, tetrabutyl titanate solution is instilled in the solution containing lanthanum nitrate or cerous nitrate and carried out
Polymeric gel, dry, roasting, prepare the TiO of rare earth oxide doping2Carrier；Catalyst is prepared using deposition-precipitation again,
Carried noble metal is carried out on carrier, described noble metal is gold；1-6h is finally calcined under 300-800 DEG C of temperature conditionss, most
Various carrier loaded Au base catalyst are obtained eventually.Comprise the following steps that：1) rare earth oxide is prepared using sol-gel process to mix
Miscellaneous TiO2Carrier：At 40 DEG C, by 40vol%Ti (OR)4Ethanol solution be slowly dropped into water, glacial acetic acid, absolute ethyl alcohol and six
In the mixed liquor of nitric hydrate lanthanum (or six nitric hydrate ceriums), and it is stirred continuously and forms colloidal sol, then heats to 40-60 DEG C, after
Continuous stirring makes solvent slowly volatilize, and forms gel, the product of gained is placed in 80-120 DEG C of baking oven and dried, and will finally obtain
Xerogel is calcined at 120-800 DEG C, 400-600 DEG C of sintering temperature, roasting time 6h, obtains the TiO of rare earth oxide doping2
Carrier；2) aqueous solution of chloraurate is prepared：Gold chloride is configured to the aqueous solution, its concentration is 0.00638mol/L；3) 1-100ml is taken
Solution obtained by step 2), add the TiO of rare earth oxide doping made from step 1)2Carrier, 50-100 DEG C is heated with stirring to,
1-4h is aged, in 60-120 DEG C of dry 6-18h, 1-6h is calcined under 300-800 DEG C of temperature conditionss, that is, is obtained various carrier loaded
Au base catalyst.
In the present invention, the Au-based catalyst of rare earth oxide doping is used for the method for CO low-temperature oxidations reaction, including such as
Lower step：First, the Au-based catalyst adulterated through rare earth oxide is fitted into fixed bed reactors；Then, CO low temperature is carried out
Oxidation reaction, reaction condition are：The mol ratio of oxygen and carbon monoxide is 1-10 in reaction gas:1, the volume space velocity of reaction gas is
1000-20000h-1, the mol ratio of oxygen and carbon monoxide is preferably 8-10:1, the volume space velocity of reaction gas is preferably 3000-
10000h-1.In the reaction, catalyst can be screened to 60-80 mesh, be fitted into reaction tube, and be passed through reaction gas, reaction gas is
1%CO, 10%O2, 89%N2Gaseous mixture, it is 50ml/min to control its flow velocity, then temperature programming, 3 DEG C/min of programming rate, often
An active site is determined every 5-10 DEG C, until CO is converted completely, wherein CO contents are detected with TCD detectors.Catalyst
Dosage, it must be enough in the case of making carbon monoxide presence, change into carbon dioxide, generally, carbon monoxide is dense in waste gas
It is 10-30L per hour to spend for 0.05-1vol%, every gram of catalyst treatment exhausted air quantity.
The first purpose of this method is by Au/TiO2Catalyst is improved so that catalyst surface oxidability
Significantly increase.
The second purpose of this method is the doping TiO by rare earth oxide2Surface forms second of active sites, from
And significantly improve CO low-temperature catalytic oxidation activities.
The present invention is made with reference to specific embodiment further explained below, but be not intended to limit the present invention, each embodiment
In used raw material be commercially available, analysis is pure.
Embodiment 1
Catalyst used by a kind of low-temperature catalytic oxidation method, with the TiO of rare earth doped oxide2For carrier, activity
Component is Au, and wherein active component is 0.5~2wt.% relative to the mass percent of carrier.Lanthana or oxygen wherein in carrier
The mass percent for changing cerium is 1~5wt.%, and remaining is titanium dioxide.
Catalyst A preparation method, comprises the following steps used by a kind of above-mentioned low-temperature catalytic oxidation：
(1) TiO of rare earth oxide doping is prepared using sol-gal process2Carrier：At 40 DEG C, by 40vol%Ti
(OR)4Ethanol solution be slowly dropped into 5ml water, 10ml glacial acetic acid, the mixing of 25ml absolute ethyl alcohols and 0.13g lanthanum nitrate hexahydrates
In liquid, and it is stirred continuously and forms colloidal sol, then heat to 60 DEG C, continuing stirring makes solvent slowly volatilize, and forms gel.Gained produces
Thing dries 24h at 80 DEG C.Obtained xerogel is finally calcined 6h in 550 DEG C, obtains 1%La-TiO2Carrier.
(2) aqueous solution of chloraurate is prepared：Gold chloride is configured to the aqueous solution, its concentration is 0.00638mol/L.
(3) 1%La-TiO obtained by 2g steps 1) is added into the solution obtained by step 2)2Carrier, in the situation of stirring
Under be heated to 65 DEG C of ageing 2h, 60 DEG C of drying 24 hours, 350 DEG C are calcined 2h, that is, used by obtaining a kind of low-temperature catalytic oxidation
Catalyst Au/1%La-TiO2, it is named as A.A kind of work of catalyst involved for the reaction of CO low-temperature oxidations of gained
Property figure as shown in Figure 1 b, as can be seen from the figure because lanthana doping, CO catalytic oxidation activities improve.
Embodiment 2
Prepare catalyst Au/3%La-TiO used by a kind of low-temperature catalytic oxidation method2, B is named as, in step (1)
Lanthanum nitrate hexahydrate dosage is 0.39g, and the Oxidation of Carbon Monoxide activity figure of gained catalyst as illustrated in figure 1 c, can from figure
Go out the doping because lanthana, CO catalytic oxidation activities significantly improve.Other are the same as embodiment 1.
Embodiment 3
Prepare catalyst Au/5%La-TiO used by a kind of low-temperature catalytic oxidation method2, C is named as, in step (1)
Lanthanum nitrate hexahydrate dosage is 0.65g, and the Oxidation of Carbon Monoxide activity figure of gained catalyst as shown in Figure 1 d, can from figure
Go out the doping because lanthana, CO catalytic oxidation activities significantly improve, the stability diagram of gained catalyst as shown in fig. 3, it was found that
Catalyst stability significantly improves.Other are the same as embodiment 1.
Embodiment 4
Prepare catalyst Au/1%Ce-TiO used by a kind of low-temperature catalytic oxidation method2, D is named as, in step (1)
Six nitric hydrate cerium dosages are 0.26g, and the Oxidation of Carbon Monoxide activity figure of gained catalyst as shown in Figure 2 b, can from figure
Go out the doping because cerium oxide, CO catalytic oxidation activities significantly improve.Other are the same as embodiment 1.
Embodiment 5
Prepare catalyst Au/3%Ce-TiO used by a kind of low-temperature catalytic oxidation method2, E is named as, in step (1)
Six nitric hydrate cerium dosages are 0.78g, and the Oxidation of Carbon Monoxide activity figure of gained catalyst as shown in Figure 2 c, can from figure
Go out the doping because cerium oxide, CO catalytic oxidation activities significantly improve.Other are the same as embodiment 1.
Embodiment 6
Prepare catalyst Au/5%Ce-TiO used by a kind of low-temperature catalytic oxidation method2, F is named as, in step (1)
Six nitric hydrate cerium dosages are 1.3g, and the CO low temperature oxidation activity figure of gained catalyst as shown in Figure 2 d, can from figure
To find out because the doping of cerium oxide, CO catalytic oxidation activities significantly improve.The stability diagram of gained catalyst as shown in figure 3,
It was found that catalyst stability significantly improves.Other are the same as embodiment 1.
Embodiment 7
The catalyst of the gained of embodiment 1,2,3,4,5,6 is reacted for CO low temperature oxidation, step is as follows：Will
0.2g fresh catalysts are screened to 60-80 mesh, are fitted into 3.5mm reaction tube, and are passed through reaction gas (1%CO, 10%O2、
89%N2Gaseous mixture), it is 50ml/min to control its flow velocity, then temperature programming, 3 DEG C/min of programming rate, is surveyed every 5 to 10 DEG C
A fixed active site, until CO is converted completely.Wherein CO contents are detected with TCD detectors.The conversion of each catalyst carbon monoxide
Rate is shown in Fig. 1 and 2.
By the Au/TiO of the rare earth doped oxide used in this method it can be seen from accompanying drawing 1 and accompanying drawing 22Catalyst is used for
The advantages that CO low temperature oxidation reacts, and has obtained higher CO reactivities, and service life is grown, and heat endurance is good.Gained
Stability as shown in Figure 3, can find out the characteristics of catalyst stability is lasting from figure.
The present invention is simultaneously not limited to the embodiments described above limitation, other any Spirit Essences and principle without departing from the present invention
Lower made change, modification, replacement, combination, simplification, should be equivalent substitute mode, be included in the protection model of the present invention
Within enclosing.
Claims (8)
1. a kind of catalytic purification method containing carbon monoxide waste gas, it is characterised in that comprise the following steps：In depositing for catalyst
Under, the waste gas containing carbon monoxide is passed through, oxygen in waste gas is more than the concentration of carbon monoxide, and it is anti-to carry out catalysis oxidation
Should, carbon monoxide in waste gas is transformed into carbon dioxide；The catalyst is by complex carrier and is carried on the complex carrier
On active component form, the complex carrier is the composite of rare earth oxide and titanium dioxide, and the active component is
Au。
2. the method as described in claim 1, it is characterised in that：The reaction pressure of the catalytic oxidation is normal pressure, reaction
Temperature is -100~50 DEG C.
3. the method as described in claim 1, it is characterised in that：The rare earth oxide is lanthana or cerium oxide, described dilute
Native oxide content is 0.1~5wt.% of complex carrier gross weight, the content of the Au for total catalyst weight 0.1~
2wt.%.
4. the method as described in claim 1, it is characterised in that：The content of the lanthana or cerium oxide is complex carrier gross weight
1~5wt.% of amount, the Au content are 0.5~2wt.% of total catalyst weight.
5. the method as any one of Claims 1-4, it is characterised in that the preparation method of the catalyst, including with
Lower step：
1) TiO of rare earth oxide doping is prepared using sol-gel process2Carrier：At 40 DEG C, by 40vol%Ti (OR)4's
Ethanol solution is slowly dropped into the mixed liquor of water, glacial acetic acid, absolute ethyl alcohol and lanthanum nitrate hexahydrate or six nitric hydrate ceriums, not
Disconnected stirring forms colloidal sol, then heats to 40-60 DEG C, and continuing stirring makes solvent slowly volatilize, and forms gel, and the product of gained is put
Put and dried in 80-120 DEG C of baking oven, is finally calcined obtained xerogel at 120-800 DEG C, 400-600 DEG C of sintering temperature,
Roasting time 6h, obtain the TiO of rare earth oxide doping2Carrier；
2) aqueous solution of chloraurate is prepared：Gold chloride is configured to the aqueous solution, its concentration is 0.00638mol/L；
3) solution obtained by step 2) is taken, adds the TiO of rare earth oxide doping made from step 1)2Carrier, it is heated with stirring to
50-100 DEG C, 1-4h is aged, in 60-120 DEG C of dry 6-18h, 1-6h is calcined under 300-800 DEG C of temperature conditionss, that is, obtained each
The carrier loaded Au base catalyst of kind.
6. method as claimed in claim 5, it is characterised in that：The Au-based catalyst adulterated through rare earth oxide is loaded and fixed
In bed reactor, CO low-temperature oxidation reactions are carried out, reaction condition is：The mol ratio of oxygen and carbon monoxide is 1- in reaction gas
10:1, the volume space velocity of reaction gas is 1000-20000h-1。
7. method as claimed in claim 6, it is characterised in that：The mol ratio of the oxygen and carbon monoxide is 8-10:1, instead
Should the volume space velocity of gas be 3000-10000h-1。
8. method as claimed in claim 7, it is characterised in that：Catalyst is screened to 60-80 mesh, is fitted into reaction tube, and
It is passed through reaction gas, reaction gas 1%CO, 10%O2, 89%N2Gaseous mixture, it is 50ml/min to control its flow velocity, then program liter
Temperature, 3 DEG C/min of programming rate, an active site is determined every 5-10 DEG C, until CO is converted completely, wherein CO contents are examined with TCD
Device is surveyed to be detected.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109731616A (en) * | 2019-02-01 | 2019-05-10 | 上海应用技术大学 | A kind of catalyst of zirconium metal-organic framework materials load and its preparation and application |
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| CN101028601A (en) * | 2007-04-13 | 2007-09-05 | 中国科学院山西煤炭化学研究所 | Hydrogen-enriched CO slective oxidation catalyst, its production and use |
| CN101380575A (en) * | 2008-10-28 | 2009-03-11 | 华东理工大学 | High stability nano gold catalyst for CO normal temperature oxidation and preparation method thereof |
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| CN109731616A (en) * | 2019-02-01 | 2019-05-10 | 上海应用技术大学 | A kind of catalyst of zirconium metal-organic framework materials load and its preparation and application |
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