CN108636417A - A kind of metal oxide catalyst and preparation method thereof of removing NO - Google Patents
A kind of metal oxide catalyst and preparation method thereof of removing NO Download PDFInfo
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- CN108636417A CN108636417A CN201810380789.6A CN201810380789A CN108636417A CN 108636417 A CN108636417 A CN 108636417A CN 201810380789 A CN201810380789 A CN 201810380789A CN 108636417 A CN108636417 A CN 108636417A
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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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
-
- 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
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
-
- 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
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
-
- 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
- B01J23/72—Copper
Abstract
The invention discloses a series of preparation method of copper cerium bimetallic oxide loaded catalysts and its applications in the selective-catalytic-reduction denitrified reactions of low temperature CO.Catalyst uses the materials such as carbon nanotube, activated carbon, aluminium oxide, titanium dioxide as solid carrier, and is prepared by infusion process that is simple and easily repeating.This catalyst have good denitration activity and stability, 140 260 DEG C of lower temperature windows and it is aerobic under conditions of can be achieved NOxEfficient Conversion the features such as long lifespan, there is good commercial application potentiality and with of low cost.
Description
Technical field
The invention belongs to industrial catalyst technology and environmental protection technical fields, and in particular to a kind of metal oxygen of removing NO
Compound catalyst and preparation method thereof, especially a kind of copper/cerium gold for carbon monoxide under low temperature selective reducing nitrogen oxide
Belong to oxide carried type catalyst and preparation method thereof.
Background technology
Air pollution problems inherent becomes to become increasingly conspicuous because of economic fast development and quickly propelling for industrialization.Plant gas
In the nitrogen oxides (NO that gives offx) be one of main source of atmosphere pollution, for nitrogen oxides of exhaust gas removing at
For the vital task of environmental improvement.That be now widely used for environmental improvement is the selective catalytic reduction (NH based on ammonia3-
SCR) technology.Although technique has higher transformation efficiency of the oxides of nitrogen, it is clearly disadvantageous that there is also some, such as safe
Property it is low, of high cost, equipment investment is big and technical sophistication etc..And carbon monoxide selective catalysis reduction (CO-SCR) technology, it can
Carbon monoxide present in flue gas is efficiently used as reducing agent, has cost relatively low, process is simple, the spies such as safety height
Point has prodigious industrial application value.The report that noble metal catalyst is used for CO-SCR technologies existing at present.Chinese patent
CN103949249A reports a kind of Ir/CexZr1-xO2/γ-Al2O3Catalyst has preferable nitrogen oxides reduction activation,
But the activity of this catalyst at low temperature is very low, only has 7% at 250 DEG C.Meanwhile noble metal fancy price makes it in work
Many difficulties are encountered in industry practical application.Non-precious metal catalyst is developed for the practical application of CO-SCR processes with important
Meaning.With carbon nanotube and γ-Al2O3There are document report (Dasireddy et for the copper-iron double metal catalyst of carrier
al.,Chem.Eng.J.,2017,326,886-900).But conversion of nitric oxide gas rate of this catalyst at 250 DEG C is only
75%.In addition, the preparation process of the catalyst is complex, needs to use gel method and chemical vapor deposition, be unfavorable for advising greatly
Mould produces.The more simple preparation method of exploitation becomes the key factor for accelerating Catalyst process.Further, since flue
Contain a certain amount of oxygen in gas, during CO-SCR, oxygen will preferentially be reacted with reducing agent carbon monoxide, lead to one
The conversion ratio of nitrogen oxide declines rapidly.How under aerobic conditions keep catalyst for it is nitric oxide production it is highly selective be also urgently
Problem to be solved.
In conclusion development cost is relatively low, preparation method is simple, can realize one under lower temperature window and aerobic conditions
The catalyst that nitrogen oxide effectively converts has important industrial application value.
Invention content
The present invention is directed to from the actual demand of industry, develop the CO-SCR processes catalysis with good industrial potential
Agent.
This catalyst is characterized in that chief active component is copper and/or cerium metal oxide.It is metal oxide supported in
On the solid materials such as carbon nanotube, activated carbon, aluminium oxide, titanium dioxide, the total content of copper and/or cerium is in the active constituent
5-20%, the preferably molar fraction of copper are 25%~75%.
The carbon nanotube has the following properties that：Specific surface area 100-500m2/ g, average pore size 2-5nm, hole hold 1.5-
2cm3/g。
The absorbent charcoal carrier has the following properties that：Specific surface area 800-2000m2/ g, density 450-550kg/m3, hole
Hold 1.5-2cm3/g。
The alumina support has the following properties that：30-60 microns of grain size, specific surface area 50-90m2/ g, density
3500-4500kg/m3。
The titania support has the following properties that：20-40 microns of grain size, specific surface area 50-90m2/ g, density
4000-4500kg/m3。
The preparation method of above-mentioned catalyst includes the following steps：
1) Vehicle element carries out surface modification and oxidation processes to carrier；The pretreatment includes pickling, is washed and dry
Dry, the acid includes one kind or its mixture arbitrarily combined in the concentrated sulfuric acid, concentrated nitric acid, concentrated hydrochloric acid.
2) active constituent solution is prepared, copper and/or cerium compound are dissolved in water, solution is made；
3) the solution impregnation steps 1 for using step 2) to prepare) resulting vehicle, it dries, roasting；It may also include before drying
Supersound process and agitating procedure.The temperature of the drying is 100-150 DEG C, and the temperature of the roasting is 300-400 DEG C.
The beneficial effects of the present invention are, the catalyst using the oxide of the lower copper of price and/or cerium as urging
The key component of agent is prepared using infusion process that is simple and easily repeating, and the catalyst being prepared is under lower temperature window
With good conversion of nitric oxide gas activity, and exists in oxygen and remain to keep higher nitric oxide selectivity.Together
When, which has the characteristics that excellent in stability, long lifespan, therefore has good commercial application potentiality.
Description of the drawings
Fig. 1 show the conversion of nitric oxide gas rate of the used catalyst of 1-5 of the embodiment of the present invention.
Fig. 2 show in the embodiment of the present invention 5 nitric oxide production conversion ratio under different carbonomonoxide concentrations.
Fig. 3 show in the embodiment of the present invention 5 nitric oxide production conversion ratio under different temperatures.
Fig. 4 show in the embodiment of the present invention 5 nitric oxide production conversion ratio under different oxygen-carbon monoxide mole ratios.
Specific implementation mode
Below by drawings and examples, the present invention is further elaborated, and the purpose is to be conducive to be best understood from the present invention
Hold the protection domain being not intended to limit the present invention.
Embodiment 1
It is that 5 grams of carbon nanotubes are put into 480 milliliters that carbon nanotube, which is carried out surface modification and oxidation processes, concrete mode,
(volume ratio of concentrated nitric acid and the concentrated sulfuric acid is 3 in concentrated nitric acid and concentrated sulfuric acid mixed solution:1) it, is placed at room temperature for 24 hours under stiring.
Later gained mixture is made to be washed with deionized to pH close to neutral (pH=6~7), dry 12 is small in 110 DEG C of baking ovens
When.
It weighs 1.5200 grams of copper nitrates and is dissolved in 20 ml deionized waters, acquired solution is added dropwise 1.6
In the carbon nanotube carrier that gram above-mentioned processing obtains, gained mixture is placed at room temperature under stiring using being ultrasonically treated 3 hours
It is 24 hours, then 12 hours dry in 120 DEG C of baking ovens.Finally roasted 3 hours in 350 DEG C in a nitrogen atmosphere.
The activity rating of catalyst carries out in fixed bed reactors.0.2 gram of catalyst is packed into reactor, and is put into control
Temperature is in 220 DEG C of heating furnace.Reaction gas group becomes：5000ppm carbon monoxide, 250ppm nitric oxides, Balance Air are helium
Gas, reaction gas total flow are 300 ml/mins, and acquired results are referring to Fig. 1.
In embodiment in the present embodiment and later, the amount of nitrogen oxides in product uses nitrogen-oxide analyzer,
(CAL-600-HCLD) it is measured, nitric oxide production conversion ratio is carried out by reacting the numerical value for reaching stable state and after continuing 1 hour
It determines.
Embodiment 2
It prepares with evaluation condition with embodiment 1, difference lies in active components to be changed to 1.2400 grams by 1.5200 grams of copper nitrates
Cerous nitrate, acquired results are referring to Fig. 1.
Embodiment 3
It prepares with evaluation condition with embodiment 1, difference lies in active components to be changed to 0.8800 gram by 1.5200 grams of copper nitrates
Copper nitrate and 0.5200 gram of cerous nitrate, acquired results are referring to Fig. 1.
Embodiment 4
It prepares with evaluation condition with embodiment 1, difference lies in active components to be changed to 0.4800 gram by 1.5200 grams of copper nitrates
Copper nitrate and 0.8600 gram of cerous nitrate, acquired results are shown in Fig. 1.
Embodiment 5
For concrete mode with embodiment 1, preparing for catalyst is as follows.
0.2000 gram of copper nitrate and 1.0800 grams of cerous nitrates are weighed, and is dissolved in 20 ml deionized waters, by institute
Solution is obtained to be added dropwise in the carbon nanotube carrier that 1.6 grams of above-mentioned processing obtain, gained mixture, which uses, to be ultrasonically treated 3 hours,
And be placed at room temperature for 24 hours under stiring, it is then 12 hours dry in 120 DEG C of baking ovens.Finally in a nitrogen atmosphere in 350 DEG C
Roasting 3 hours.
The activity rating of catalyst carries out in fixed bed reactors.0.2 gram of catalyst is packed into reactor, and is put into control
Temperature is in 220 DEG C of heating furnace.Reaction gas group becomes：Carbonomonoxide concentration 5000ppm, 250ppm nitric oxide, Balance Air
For helium, reaction gas total flow is 300 milliliters per minute.Acquired results are included in Fig. 1.
The activity rating of catalyst carries out in fixed bed reactors.0.2 gram of catalyst is packed into reactor, and is put into control
Temperature is in 220 DEG C of heating furnace.Reaction gas group becomes：Carbonomonoxide concentration 1000-5000ppm, 250ppm nitric oxide is put down
Weighing apparatus gas is helium, and reaction gas total flow is 300 milliliters per minute.Acquired results are included in Fig. 2.
The activity rating of catalyst carries out in fixed bed reactors.0.2 gram of catalyst is packed into reactor, and is put into control
Temperature is in 140,160,180,220,240,260 DEG C of heating furnace.Reaction gas group becomes：Carbonomonoxide concentration 5000ppm,
250ppm nitric oxides, Balance Air are helium, and reaction gas total flow is 300 milliliters per minute.Acquired results are included in Fig. 3.
The activity rating of catalyst carries out in fixed bed reactors.0.2 gram of catalyst is packed into reactor, and is put into control
Temperature is in 220 DEG C of heating furnace.Reaction gas group becomes：Carbonomonoxide concentration 5000ppm, 250ppm nitric oxide, 0,0.1,
0.2,0.3,0.4,0.5% oxygen (corresponding oxygen/carbon monoxide ratio is respectively 0,0.2,0.4,0.6,0.8,1).Balance
Gas is helium, and reaction gas total flow is 300 milliliters per minute.Acquired results are included in Fig. 4.
The activity rating of catalyst carries out in fixed bed reactors.0.2 gram of catalyst is packed into reactor, and is put into control
Temperature is in 220 DEG C of heating furnace.Reaction gas group becomes：Carbonomonoxide concentration 1%, 1000ppm nitric oxides, 0,0.5,1%
Oxygen, Balance Air are helium, and reaction gas total flow is 300 milliliters per minute.Acquired results are included in table 1.
Embodiment 6
Activated carbon is to immerse activated carbon in the hydrochloric acid of 6 mol/Ls and impregnate 24 hours by pretreatment, concrete mode, it
After make to be washed with deionized to pH close to 7, dry 24 hours in 100 DEG C of baking ovens.
0.2000 gram of copper nitrate and 1.0800 grams of cerous nitrates are weighed, and is dissolved in 20 ml deionized waters, by institute
Solution is obtained to be added dropwise on the absorbent charcoal carrier that 1.6 grams of above-mentioned processing obtain, gained mixture, which uses, to be ultrasonically treated 3 hours, and
It is placed at room temperature for 24 hours under stiring, it is then 12 hours dry in 120 DEG C of baking ovens.Finally in a nitrogen atmosphere in 350 DEG C of roastings
It burns 3 hours.
The activity rating of catalyst carries out in fixed bed reactors.0.2 gram of catalyst is packed into reactor, and is put into control
Temperature is in 220 DEG C of heating furnace.Reaction gas group becomes：5000ppm carbon monoxide, 250ppm nitric oxides, 0,0.3,2,5%
Oxygen, Balance Air are helium, and reaction gas total flow is 300 milliliters per minute.
Embodiment 7
0.2000 gram of copper nitrate and 1.0800 grams of cerous nitrates are weighed, and is dissolved in 20 ml deionized waters, by institute
It obtains solution to be added dropwise on 1.6 grams of commercialization alumina supports without other processing, gained mixture is small using being ultrasonically treated 3
When, and be placed at room temperature for 24 hours under stiring, it is then 12 hours dry in 120 DEG C of baking ovens.Finally in a nitrogen atmosphere in 350
DEG C roasting 3 hours.
The activity rating of catalyst carries out in fixed bed reactors.0.2 gram of catalyst is packed into reactor, and is put into control
Temperature is in 220 DEG C of heating furnace.Reaction gas group becomes：5000ppm carbon monoxide, 250ppm nitric oxides, 0,0.3,2,5%
Oxygen, Balance Air are helium, and reaction gas total flow is 300 milliliters per minute.
Embodiment 8
0.2000 gram of copper nitrate and 1.0800 grams of cerous nitrates are weighed, and is dissolved in 20 ml deionized waters, by institute
It obtains solution to be added dropwise on 1.6 grams of commercialization titania supports without other processing, gained mixture uses supersound process 3
Hour, and be placed at room temperature for 24 hours under stiring, it is then 12 hours dry in 120 DEG C of baking ovens.Finally in a nitrogen atmosphere in
350 DEG C roast 3 hours.
The activity rating of catalyst carries out in fixed bed reactors.0.2 gram of catalyst is packed into reactor, and is put into control
Temperature is in 220 DEG C of heating furnace.Reaction gas group becomes：5000ppm carbon monoxide, 250ppm nitric oxides, 0,0.3,2,5%
Oxygen, Balance Air are helium, and reaction gas total flow is 300 milliliters per minute.
The reaction condition and conversion of nitric oxide gas rate of catalyst in 1 embodiment 5-8 of table
| Embodiment | Catalyst | Reaction temperature | NO concentration | CO concentration | O2Concentration | NO conversion ratios |
| 5 | Cu1:Ce3/CNT | 220℃ | 1000ppm | 1% | 0 | 98% |
| 5 | Cu1:Ce3/CNT | 220℃ | 1000ppm | 1% | 0.5% | 96.8% |
| 5 | Cu1:Ce3/CNT | 220℃ | 1000ppm | 1% | 1.0% | 7.6% |
| 6 | Cu1:Ce3/AC | 220℃ | 250ppm | 5000ppm | 0 | 42.6% |
| 6 | Cu1:Ce3/AC | 220℃ | 250ppm | 5000ppm | 0.3% | 41.5% |
| 6 | Cu1:Ce3/AC | 220℃ | 250ppm | 5000ppm | 2% | 14.8% |
| 6 | Cu1:Ce3/AC | 220℃ | 250ppm | 5000ppm | 5% | 15.4% |
| 7 | Cu1:Ce3/Al2O3 | 220℃ | 250ppm | 5000ppm | 0 | 43.8% |
| 7 | Cu1:Ce3/Al2O3 | 220℃ | 250ppm | 5000ppm | 0.3% | 42.2% |
| 7 | Cu1:Ce3/Al2O3 | 220℃ | 250ppm | 5000ppm | 2% | 22.3% |
| 7 | Cu1:Ce3/Al2O3 | 220℃ | 250ppm | 5000ppm | 5% | 24.1% |
| 8 | Cu1:Ce3/TiO2 | 220℃ | 250ppm | 5000ppm | 0 | 49.3% |
| 8 | Cu1:Ce3/TiO2 | 220℃ | 250ppm | 5000ppm | 0.3% | 48.0% |
| 8 | Cu1:Ce3/TiO2 | 220℃ | 250ppm | 5000ppm | 2% | 17.9% |
| 8 | Cu1:Ce3/TiO2 | 220℃ | 250ppm | 5000ppm | 5% | 19.8% |
Technical scheme of the present invention is described in detail in above-described embodiment.It is apparent that the present invention is not limited being retouched
The embodiment stated.Based on the embodiments of the present invention, those skilled in the art can also make a variety of variations accordingly, but appoint
What is equal with the present invention or similar variation shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of metal oxide catalyst of removing NO, which is characterized in that including carrier and the activearm being attached on carrier
Part, the carrier is carbon nanotube, activated carbon, aluminium oxide or titanium dioxide, and the active constituent is the oxidation of copper and/or cerium
The content of object, wherein copper and/or cerium is 5-20%.
2. catalyst according to claim 1, which is characterized in that the carbon nanotube has the following properties that：Specific surface
Product 100-500m2/ g, average pore size 2-5nm, hole hold 1.5-2cm3/g。
3. catalyst according to claim 1, which is characterized in that the absorbent charcoal carrier has the following properties that：Compare table
Area 800-1500m2/ g, density 450-550kg/m3, hole holds 1.5-2cm3/g。
4. catalyst according to claim 1, which is characterized in that the alumina support has the following properties that：Grain size
30-60 microns, specific surface area 50-90m2/ g, density 3500-4500kg/m3。
5. catalyst according to claim 1, which is characterized in that the titania support has the following properties that：Grain
20-40 microns of diameter, specific surface area 50-90m2/ g, density 4000-4500kg/m3。
6. catalyst according to claim 1, which is characterized in that in the active constituent molar fraction of copper be 25%~
75%.
7. described in claim 1 remove NO copper/cerium metal oxide catalyst preparation method, which is characterized in that including with
Lower step：
1) Vehicle element carries out surface modification and oxidation processes to carrier；
2) active constituent solution is prepared, copper and/or cerium compound are dissolved in water, solution is made；
3) the solution impregnation steps 1 for using step 2) to prepare) resulting vehicle, it dries, roasting.
8. method according to claim 7, which is characterized in that pretreatment includes pickling described in step 1), washing and drying,
The acid includes one kind or its mixture arbitrarily combined in the concentrated sulfuric acid, concentrated nitric acid, concentrated hydrochloric acid.
9. method according to claim 7, which is characterized in that further include being ultrasonically treated and stirring before drying in step 3)
Process.
10. method according to claim 7, which is characterized in that the temperature dried described in step 3) is 100-150 DEG C, institute
The temperature for stating roasting is 300-400 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109731569A (en) * | 2018-12-27 | 2019-05-10 | 安徽元琛环保科技股份有限公司 | Cellular SCR denitration and preparation method with three-dimensional multistage cellular structure |
| CN109772346A (en) * | 2019-02-28 | 2019-05-21 | 兖矿水煤浆气化及煤化工国家工程研究中心有限公司 | A kind of preparation method and its application of denitrogenation at low temperature of composite catalyst |
| WO2020248723A1 (en) * | 2019-05-31 | 2020-12-17 | 南京杰科丰环保技术装备研究院有限公司 | Filter material integrating dust removal, denitration and mercury removal and preparation method therefor |
| CN115090294A (en) * | 2022-08-09 | 2022-09-23 | 石河子大学 | Nickel-based molded catalyst for CO-SCR flue gas denitration and preparation method thereof |
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| CN103157478A (en) * | 2013-04-02 | 2013-06-19 | 中国科学技术大学 | CuO-CeO2/MWCNT(Multi Walled Carbon Nanotubes) catalyst and preparation method thereof |
| CN103949249A (en) * | 2014-04-11 | 2014-07-30 | 浙江大学 | Catalyst used for gas-fired boiler carbon monoxide selective reduction of nitrogen oxides, and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109731569A (en) * | 2018-12-27 | 2019-05-10 | 安徽元琛环保科技股份有限公司 | Cellular SCR denitration and preparation method with three-dimensional multistage cellular structure |
| CN109731569B (en) * | 2018-12-27 | 2021-12-10 | 安徽元琛环保科技股份有限公司 | Honeycomb type SCR denitration catalyst with three-dimensional multi-stage pore channel structure and preparation method thereof |
| CN109772346A (en) * | 2019-02-28 | 2019-05-21 | 兖矿水煤浆气化及煤化工国家工程研究中心有限公司 | A kind of preparation method and its application of denitrogenation at low temperature of composite catalyst |
| CN109772346B (en) * | 2019-02-28 | 2022-01-25 | 兖矿水煤浆气化及煤化工国家工程研究中心有限公司 | Preparation method of composite material catalyst and application of composite material catalyst in denitrification at low temperature |
| WO2020248723A1 (en) * | 2019-05-31 | 2020-12-17 | 南京杰科丰环保技术装备研究院有限公司 | Filter material integrating dust removal, denitration and mercury removal and preparation method therefor |
| CN115090294A (en) * | 2022-08-09 | 2022-09-23 | 石河子大学 | Nickel-based molded catalyst for CO-SCR flue gas denitration and preparation method thereof |
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Application publication date: 20181012 |