CN106732605B - A kind of non-noble metal oxide catalyst and preparation method with water resistant protective layer - Google Patents
A kind of non-noble metal oxide catalyst and preparation method with water resistant protective layer Download PDFInfo
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- CN106732605B CN106732605B CN201611223208.5A CN201611223208A CN106732605B CN 106732605 B CN106732605 B CN 106732605B CN 201611223208 A CN201611223208 A CN 201611223208A CN 106732605 B CN106732605 B CN 106732605B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
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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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- 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
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/50—Carbon oxides
- B01D2257/502—Carbon monoxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention discloses a kind of non-noble metal oxide catalyst and preparation method with water resistant protective layer.For catalyst of the invention using nano transition metal Fe/Co composite oxides as active component, surface has high-molecular porous film, so that catalyst has excellent water repelling property.The catalyst is prepared using solid phase method, and synthesis process is simple to operation, and not high to equipment requirement, catalyst is low in cost.There is very high activity and stability using the oxidation reaction of catalyst of the invention to CO, while the catalyst can also be used for the oxidation elimination of other harmful poisonous gases, such as formaldehyde, effumability organic pollutant (VOCs).
Description
Technical field
The present invention relates to catalyst preparation technical fields, specifically, a kind of your non-gold with water resistant protective layer are related to
Belong to oxide catalyst and preparation method.
Background technique
It is well known that CO is a kind of toxic and colorless and odorless gas.Due to chemical industry, combustion of fossil fuel and machine
The fast development of motor-car causes a large amount of CO discharge, it has also become serious environmental problem causes the common concern of people.CO
Low temperature (100 DEG C of <) elimination have important application value in many aspects, in vcehicular tunnel and underground parking air
The elimination of CO, CO gas detector material, CO2The purifying of gas in laser, tobacco drop evil, breath for gas purification device with
And the elimination etc. of trace amounts of CO has important application prospect in closed system (such as aircraft, submarine, spacecraft).Therefore exist
Realize that CO oxidation conversion has become one of hot issue of catalyticing research under lower temperature.
The elimination of CO is broadly divided into physics and chemical two kinds of purification methods.Physical method mainly utilizes specific surface biggish such as
The porous materials such as activated carbon realize the physical absorption of CO at normal temperature by weak model ylid bloom action power.But physisorphtion
There are some disadvantages, and such as the CO of low concentration, the efficiency of adsorption cleaning is lower.Chemical method is mainly the effect for utilizing catalyst
CO is oxidized to CO2, achieve the purpose that CO is purified.Wherein the catalyst of CO catalysis oxidation mainly has noble metals and base metal two
Major class, noble metal have excellent activity in terms of CO catalysis oxidation, but since it is expensive, be easy to sulfur poisoning and high temperature is burnt
Knot limits its application.
For non-precious metal catalyst, such as Co3O4、CuO/CeO2、CuO-MnO2Deng wherein Co3O4Since it is to low temperature CO
Oxidation reaction has excellent catalytic properties and is widely noticed, but Co3O4It is extremely sensitive to steam, even if containing micro water
It can also cause its rapid deactivation.The researchs such as Grillo find steam there are carbonate easy to form, to cover Co3O4's
Active site makes catalyst lose activity (F.Grillo, et al., Applied Catalysis B:Environmental
2004,48:267-274).Therefore Co a kind of high performance and with water resistant protective layer is prepared3O4Catalyst causes ours
Concern.
Summary of the invention
For overcome the deficiencies in the prior art, there is water resistant protective layer the purpose of the present invention is to provide a kind of high activity
Non-noble metal oxide catalyst and preparation method.Catalyst CO catalytic oxidation activity with higher and stability, can
The CO catalytic oxidation under low temperature under aqueous conditions, it can also be used to which the oxidation of other toxic and harmful gas is eliminated, such as formaldehyde, effumability
Organic pollutant (VOCs) etc..
The present invention is based on following both sides thinkings to improve Co3O4The performance of catalyst, first is that being carried out with transition metal to it
It is modified；Second is that designing one layer of water resistant protective layer for it.By the above both sides design, so that the catalyst has greater catalytic
While active, it may have higher stability and water repelling property.
Catalyst of the invention, using non-noble metal oxide as the active component of catalyst, such as Fe/Co composite oxides
(FeaCobOx), wherein the molar ratio of iron and cobalt is 1:32-3:8；Catalyst table is made by the solid phase method that oxalic acid ethylene glycol assists
Macromolecule layer (the Fe of face attachment 0.1%-30.0% contentaCobOx@MC), pass through control maturing temperature, calcining time and oxalic acid
The content of catalyst surface macromolecule layer is controlled with ethylene glycol dosage.
Technical solution of the present invention is specifically described as follows.
The present invention provides a kind of non-noble metal oxide catalyst with water resistant protective layer, by non-noble metal oxide
It is constituted with the high-molecular porous film that its surface has；Wherein: the high-molecular porous film is by oxalic acid and ethylene glycol copolyreaction
It obtains.
In the present invention, the non-noble metal oxide is the mixture of cobaltosic oxide and di-iron trioxide.
In the present invention, in catalyst, the mass percent of polymeric membrane is 0.1%-30.0%, and the molar ratio of iron and cobalt is
1:32-3:8.Preferably, the mass percent of polymeric membrane is 1-5%, and the molar ratio of iron and cobalt is 1:16-5:16.
The present invention also provides a kind of preparation method of above-mentioned non-noble metal oxide catalyst with water resistant protective layer, tools
Steps are as follows for body: after ferric nitrate, cobalt nitrate, oxalic acid and ethylene glycol are mixed ultrasound, doing overnight in 105~115 DEG C of drying boxes
It is dry；1-10h is roasted in air at a temperature of 200-600 DEG C again, obtains non-noble metal oxide catalyst.
In the present invention, the molar ratio of ferric nitrate and cobalt nitrate is 3:64~9:16；Mole of oxalic acid, ethylene glycol and cobalt nitrate
Than for (1~2): (1~2): 1.
In the present invention, maturing temperature is 200~400 DEG C.
Compared with prior art, the beneficial effects of the present invention are:
(1) active component is non-noble metal oxide, such as cobaltosic oxide, iron oxide, and surface has macromolecule layer,
And surface macromolecule layer can only penetrate reaction gas molecule, such as CO, O2Deng, but H cannot be penetrated2O；Macromolecule layer is water resistant protective layer.
(2) preparation method is simple for catalyst in the present invention, and not high to equipment requirement, expense is more cheap, repeats
Property is good.
(3) catalyst water-resistance with higher and the stability, (0.6vol.%H under aqueous conditions2O), catalyst can
Keep at least 15 days activity constant at 70 DEG C；And the catalyst inactivated in reaction atmosphere, it can be handled in 200 DEG C of nitrogen atmospheres
Activity can be restored completely after 30min.
(4) oxidation that the catalyst can also be used for other harmful poisonous gases is eliminated, such as formaldehyde, effumability organic contamination
Object (VOCs) etc..
Detailed description of the invention
Fig. 1 is a kind of schematic diagram of non-noble metal oxide catalyst with water resistant protective layer of the invention.
Fig. 2 is Fe prepared by embodiment 13Co16OxThe photo of the transmission electron microscope (TEM) of@MC catalyst.
Fig. 3 is Fe prepared by embodiment 13Co16OxCatalysis of the@MC catalyst in different moisture contents to CO oxidation reaction
Activity curve.
Fig. 4 is Fe prepared by embodiment 23Co16Ox@MC catalyst is in wet environment (0.6vol.%H2O) and at 70 DEG C pair
The catalytic activity curve of CO oxidation reaction.
Fig. 5 is Fe prepared by embodiment 23Co16Ox@MC catalyst is in wet environment (0.6vol.%H2O differential responses in)
At a temperature of to the catalytic activity curve of CO oxidation reaction.
Specific embodiment
The following examples will further be described the present invention, but be not limited to the scope of the present invention.
Fig. 1 is a kind of schematic diagram of non-noble metal oxide catalyst with water resistant protective layer of the invention.A is non-expensive
Metal oxide；B is high-molecular porous film layer.
Embodiment 1
The cobalt nitrate of 9.31g, the ferric nitrate of 2.23g and 4.00g oxalic acid are weighed respectively in agate mortar, are uniformly mixed；
2mL ethylene glycol is added thereto, grinds 30min, moves it into beaker, is put into 110 DEG C of drying box after being ultrasonically treated 1h
Overnight；It is then placed in Muffle furnace and roasts 3h at 250 DEG C, obtain catalyst.Fig. 2 is Fe prepared by embodiment 1aCobOx@MC
The photo of the transmission electron microscope (TEM) of catalyst.
Catalytic performance of the catalyst to CO oxidation reaction is tested in fixed bed reactor system.By 200mg
The catalyst of 40-60 mesh is packed into reactor, and catalyst is pre-processed 30min in 200 DEG C of nitrogen before test；Then pass to containing
0.15%CO, 18.9%O2, remaining be N2The reaction gas of (Balance Air), air speed are 15000mL/ (gh), and control reaction temperature waits for
Reaction measures the conversion ratio of CO after reaching stable.Moisture content is adjusted by controlling bubbler temperature.
Activity evaluation shows the Fe using preparation3Co16Ox@MC catalyst, under normal conditions (3-10ppm H2O)
The temperature that CO is converted completely is about -100 DEG C, in humid conditions (0.6vol.%H2O) the complete conversion temperature of CO is 70 DEG C.
For CO catalysis oxidation, complete conversion temperature is lower, shows that catalyst activity is better.When for different moisture contents, CO turns
Test results are shown in figure 3 for rate, in Fig. 3, a:0.6vol.%H2O；B:1.2vol.%H2O；C:2.3vol.%H2O；d:
3.1vol.%H2O；E:4.2vol.%H2O；F:7.4vol.%H2O；G:20vol.%H2O.As a result it indicates: when steam is lower than
When 3.1vol.%, moisture content influences catalyst activity more significant；When moisture content is more than a certain amount of
(3.1vol.%), with the increase of moisture content, catalyst activity illustrates that catalyst has good water resistant without significant change
Performance.
Embodiment 2
The catalyst prepared using embodiment 1, reducing catalyst maturing temperature is 230 DEG C, and other of catalyst prepare item
The evaluation method of part and catalyst is the same as embodiment 1.
Activity evaluation shows the Fe using preparation3Co16Ox@MC catalyst, in humid conditions (0.6vol.%
H2O) the complete conversion temperature of CO is 60 DEG C；And in wet condition (0.6vol.%H2O) and reaction temperature is at 70 DEG C to catalysis
The stability of agent is tested, and test results are shown in figure 4, and there is no variations for the activity of the operation rear catalyst through 350h.
In order to evaluate catalytic stability when different CO conversion ratios, in wet condition (0.6vol.%H2O it) and at a temperature of differential responses surveys
The stability of catalyst is tried, test results are shown in figure 5, in Fig. 5: the catalyst activity measured at a:40 DEG C；It is surveyed at b:50 DEG C
The catalyst activity obtained；The catalyst activity measured at c:60 DEG C；The catalyst activity measured at d:70 DEG C.As a result it indicates:
It is activity stabilized 24% or so after reaction 96h at 40 DEG C；It is activity stabilized 61% or so after reaction 96h at 50 DEG C；60
DEG C when, react 96h after it is activity stabilized 97% or so；It is activity stabilized~100% after reaction 96h at 70 DEG C, and do not send out
Changing.
Embodiment 3
The catalyst prepared using embodiment 1, improving catalyst maturing temperature is 350 DEG C, and other of catalyst prepare item
The evaluation method of part and catalyst is the same as embodiment 1.
Activity evaluation shows the Fe using preparation3Co16Ox@MC catalyst, under normal conditions (3-10ppm H2O)
The complete conversion temperature of CO is -96 DEG C, in humid conditions (0.6vol.%H2O) the complete conversion temperature of CO is 70 DEG C.
Embodiment 4
The catalyst prepared using embodiment 2, raising catalyst calcining time are 10h, other preparation conditions of catalyst
And the evaluation method of catalyst in humid conditions is the same as embodiment 2.
Activity evaluation shows the Fe using preparation3Co16Ox@MC catalyst, in humid conditions (0.6vol.%
H2O) the complete conversion temperature of CO is 65 DEG C.
Embodiment 5
The catalyst prepared using embodiment 2, it is 4h, other preparation conditions of catalyst that catalyst calcining time is urged in reduction
With embodiment 2.Formaldehyde through catalytic oxidation performance test is carried out to obtained catalyst.
The catalytic performance of catalyst oxidation of formaldehyde reaction is tested in fixed bed reactor system.It will
The catalyst of 200mg40-60 mesh is packed into reactor, and catalyst is pre-processed 30min in 200 DEG C of nitrogen before test；Then lead to
Enter reaction gas (wherein content of formaldehyde is 200mg/L, remaining is air), air speed is 15000mL/ (gh), controls reaction temperature
After reacting and reaching stable, reaction end gas is detected by nickel catalysis transition furnace using FID after carbon molecular sieve chromatography post separation
Device detects formaldehyde, CO and CO2Content, to measure the conversion ratio of formaldehyde.Wherein content of formaldehyde passes through control paraformaldehyde water-bath
Temperature and flow control by paraformaldehyde.
Activity evaluation shows the Fe using preparation3Co16Ox@MC catalyst can make formaldehyde turn completely at 100 DEG C
Change.
Comparative example 1
Ethylene glycol, other preparation conditions of catalyst are not added during preparing catalyst as different from Example 3
And the evaluation method of catalyst is the same as embodiment 3.
Activity evaluation shows the catalyst using preparation, under normal conditions (3-10ppm H2O) CO completely turns
Changing temperature is -81 DEG C, in humid conditions (0.6%H2O) the complete conversion temperature of CO is 110 DEG C.
Comparative example 2
Be not added oxalic acid during preparing catalyst as different from Example 3, other preparation conditions of catalyst and
The evaluation method of catalyst is the same as embodiment 3.
Activity evaluation shows the catalyst using preparation, under normal conditions (3-10ppm H2O) CO completely turns
Changing temperature is -82 DEG C, in humid conditions (0.6%H2O) the complete conversion temperature of CO is 110 DEG C.
Comparative example 3
Ferric nitrate, other preparation conditions of catalyst are not added during preparing catalyst as different from Example 3
And the evaluation method of catalyst is the same as embodiment 3.
Activity evaluation shows the Co using preparation16Ox@MC catalyst, under normal conditions (3-10ppm H2O)CO
Complete conversion temperature be -78 DEG C, (0.6%H in humid conditions2O) the complete conversion temperature of CO is 100 DEG C.
Claims (5)
1. a kind of non-noble metal oxide catalyst with water resistant protective layer, which is characterized in that it is by non-noble metal oxide
It is constituted with the high-molecular porous film that its surface has；Wherein: the high-molecular porous film is obtained by oxalic acid and ethylene glycol copolyreaction
It arrives, the non-noble metal oxide is the mixture of cobaltosic oxide and di-iron trioxide；The preparation method of the catalyst is specific
Steps are as follows: after ferric nitrate, cobalt nitrate, oxalic acid and ethylene glycol are mixed ultrasound, being dried overnight in 105~115 DEG C of drying boxes；
1-10h is roasted in air at a temperature of 200-600 DEG C again, obtains non-noble metal oxide catalyst.
2. non-noble metal oxide catalyst according to claim 1, which is characterized in that high-molecular porous in catalyst
The mass percent of film is 0.1%-30.0%, and the molar ratio of iron and cobalt is 1:32-3:8.
3. non-noble metal oxide catalyst according to claim 1 or 2, which is characterized in that macromolecule in the catalyst
The mass percent of perforated membrane is 1-5%, and the molar ratio of iron and cobalt is 1:16-5:16.
4. non-noble metal oxide catalyst according to claim 1, which is characterized in that mole of ferric nitrate and cobalt nitrate
Than for 3:64~9:16；The molar ratio of oxalic acid, ethylene glycol and cobalt nitrate is (1~2): (1~2): 1.
5. non-noble metal oxide catalyst according to claim 1, which is characterized in that maturing temperature is 200~400
℃。
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| CN109395783B (en) * | 2018-11-13 | 2021-10-22 | 上海师范大学 | Cobaltosic oxide @ polydopamine catalyst and preparation method thereof |
| CN113134357A (en) * | 2020-01-20 | 2021-07-20 | 中大汇智源创(北京)科技有限公司 | Water-resistant carbon monoxide catalyst and preparation method thereof |
| CN113385183B (en) * | 2020-03-13 | 2023-08-18 | 中科汇智(东莞)设备科技有限公司 | Preparation method of foam metal-supported water-resistant carbon monoxide catalyst |
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