CN103949267A - Iron-base composite oxide denitration catalyst and preparation method and application thereof - Google Patents
Iron-base composite oxide denitration catalyst and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an iron-base composite oxide denitration catalyst which comprises three element components including iron, molybdenum and oxygen, wherein the iron and the molybdenum are highly dispersed in a composite oxide; the mole ratio of the iron to the molybdenum is (14-40):1, and the mole ratio of the oxygen to the iron is (1.0-1.88):1. The invention also discloses a preparation method and application of the iron-base composite oxide denitration catalyst. The iron-base composite oxide denitration catalyst disclosed by the invention is in a flocculent structure, has the advantages of high catalytic activity and selectivity, wide temperature range and good low-temperature activity, can be used for purifying or eliminating the nitrogen oxides contained in stationary source flue gas, diesel car tail gas and lean-burn gasoline engine tail gas and has wide application prospect.
Description
Technical field
The present invention relates to a kind of iron-based composite oxides NH
3-SCR denitrating catalyst and preparation method thereof, also relates to this catalyst for removing the application of the nitrogen oxide of stationary source flue gas, exhaust gas from diesel vehicle and fuel-sean gasoline engine tail gas, belongs to catalytic denitration technical field.
Background technology
Nitrogen oxide (NO
x ) be the major pollutants that cause acid rain and photochemical fog, its discharge main from stationary source if coal-burning boiler, industrial furnace and moving source are as the discharge of motor-vehicle tail-gas.China is obtaining SO
2after the phasic results of controlling, during " 12 " to NO
x realize overall control, 2015 NO
x total emission volumn declined 10% than 2010.Particularly within 2012, implement < < fossil-fuel power plant atmospheric pollutant emission standard > >, in this standard, required NO
x (with NO
2meter) discharge is 100 mg/m
3.
SCR (Selective Catalytic Reduction, SCR) is under the condition existing at oxygen, the NO of reducing agent preferentially and in flue gas
x reaction generates nitrogen (N
2) catalytic process.What in SCR technology, can be used as reducing agent comprises ammonia (NH
3), hydrocarbon (HC) and hydrogen (H
2).Adopt NH
3as the SCR technology of reducing agent to NO
x removal efficiency can reach 80 ~ 90 %, denitration efficiency is the highest, is also simultaneously at present internationally recognized main flow, the most ripe, the commercialization denitration technology that is most widely used.Catalyst is the core of SCR technology, the NH of extensive use at present
3-SCR catalyst is to take the catalytic component based on vanadium (V that titanium oxide is carrier
2o
5-WO
3(MoO
3)/TiO
2).Yet, though business vanadium titanium catalyst has higher denitration activity and good water resistant sulfur resistance, active component V wherein
2o
5there is toxicity, can cause secondary pollution to environment, and the narrower (300-400 of reactivity temperature window
oc), high temperature section N
2selectively poor.Therefore, develop efficient, stable, eco-friendly novel NH
3-SCR catalyst replaces traditional catalytic component based on vanadium to be very necessary and to have bright prospects.
About the research and development of Novel SCR denitrating catalyst, researcher has done a large amount of work to this both at home and abroad.Fe is catalyst based has good redox property, and its wide material sources are nontoxic, cheap, receive domestic and international researcher's concern, are considered to have potential NH
3-SCR catalyst.Fe-ZSM-5(K. Krishna, et al., Catal. Today, 2006,114:23), Fe
2o
3(X. L. Mou, et al., Angew. Chem. Int. Ed. 2012,51:1) and Fe-Ti composite oxides (F. D. Liu, et al., Chem. Commun., 2008:2043) catalyst has all shown good catalytic performance, but the catalyst based common denitration activity temperature drift of Fe, the anti-sulphur of water resistant and poor heat stability, complicated process of preparation, has limited its large-scale industrial application.Mo oxidisability is strong, can improve the low temperature active of catalysis, is often used as denitration catalyst agent aid, at V
2o
5/ TiO
2in catalyst, add Mo, improved denitration activity and the heat endurance of catalyst, and can improve the N of catalyst
2selectively (G Busca, et al, Appl. Catal. B.1998,18(1): 1-36), Mo can also suppress in flue gas As to the poisoning effect of catalyst (L Lietti, et al, J. Catal.1999,187 (2): 419-435).Therefore, in iron oxide, add molybdenum, be expected to obtain having highly active NH
3-SCR denitrating catalyst.
In addition, in patent 201110133318.3, mention, the amorphous composite oxide catalysts of high degree of dispersion has higher specific area, more be conducive to the dispersion of active component, catalytic activity compared with crystallinity catalyst is high, be conducive to long-term use, therefore preparing the catalyst that decentralization is high is also a kind of method that improves catalytic activity.
Summary of the invention
The object of this invention is to provide a kind of iron-based composite oxides, be specially Fe-Mo composite oxides, this composite oxides active component high degree of dispersion, has peculiar cotton-shaped pattern, as NH
3during-SCR denitrating catalyst, catalytic activity is high, and catalytic temperature wide ranges, anti-sulphur water resistant are poisoning, excellent performance.
Another object of the present invention is to provide the preparation method of these iron-based composite oxides, and the method is simple to operate, and cost is low, products obtained therefrom excellent performance.
Another object of the present invention is to provide the application of these iron-based composite oxides, and it can be used as the NH that removes stationary source flue gas, exhaust gas from diesel vehicle and fuel-sean gasoline engine nitrogen oxide in tail gas
3-SCR denitrating catalyst, catalyst reveals higher NH at wider reaction temperature interval table
3-SCR activity and N
2selectively, can be applicable to removing of coal-burning power plant and Industrial Boiler flue gas, diesel exhaust and fuel-sean gasoline engine nitrogen oxide in tail gas.
The present invention selects iron and molybdenum as catalyst activity composition, makes the composite oxides of active component high degree of dispersion by the precipitation method, makes its catalytic activity higher, and temperature applicable range is wider.
The concrete technical scheme of the present invention is as follows:
Iron-based composite oxides, is characterized in that: comprise iron, molybdenum, three kinds of elemental compositions of oxygen, and iron and molybdenum high degree of dispersion in composite oxides, the mol ratio of iron and molybdenum is 14-40:1, the mol ratio of oxygen and iron is 1.0-1.88:1.
In above-mentioned iron-based composite oxides, the mol ratio of iron and molybdenum is preferably 18:1, and the mol ratio of oxygen and iron is preferably 1.21:1.
Iron-based combined oxidation denitrating catalyst of the present invention, the Fe-Mo composite oxides of high degree of dispersion of take are active component, the composition of oxide is Fe, Mo and O, and Fe and Mo exist with the form of oxide, composite oxides or the oxide of high degree of dispersion and the mixture of composite oxides.
Composite oxides high degree of dispersion in metal oxide catalyst of the present invention, can pass through X-ray powder diffraction (XRD) and characterize proof.This catalyst pattern is flocculent structure, and its sheet flocculent structure characterizes proof by ESEM (SEM).In the present invention, the actual content of iron molybdenum is measured by ICP-AES.The flocculent structure that catalyst has, is conducive to the dispersion of active component and the increase of specific area, thereby has improved the catalytic activity of catalyst.
The preparation method of above-mentioned iron-based composite oxides, comprises the following steps:
(1) molybdenum salt water is dissolved, wiring solution-forming, standby; Molysite and ascorbic acid water are dissolved, wiring solution-forming, standby;
(2) get the above-mentioned molybdenum solution that contains, adding ammoniacal liquor to regulate its pH is 9, and then keeping solution temperature is 25-40 ℃, is stirred to and generates MoO
4 2-ion, then iron-containing liquor is under agitation slowly added drop-wise to containing in molybdenum solution, in dropping process, keeping the pH of mixed liquor is 6-9, dropwising rear adjusting pH is 9, continues stirring aging, makes precipitation of iron ions complete;
(3) after precipitating completely, filter, will precipitate washing, alcohol wash, dry, dried precipitation grinds, roasting at 450-550 ℃, obtains iron-based composite oxides.
In above-mentioned steps (1), described molybdenum salt is sodium molybdate or ammonium molybdate, and described molysite is ferrous sulfate or ferric sulfate.
In above-mentioned steps (1), containing in molybdenum solution, the concentration of molybdenum ion is 0.025-0.09 mol/L; In iron-containing liquor, the concentration of iron ion is 0.2-0.27 mol/L, and ascorbic acid consumption is 1 mg/mL.
In above-mentioned steps (2), generate MoO
4 2-during ion, stir 0.5 h.
In above-mentioned steps (2), generate MoO
4 2-during ion, the temperature of holding iron-containing liquor is 35 ℃.
In above-mentioned steps (2), drip after iron-containing liquor, aging 3 hours, whole system is fully reacted.
In above-mentioned steps (3), at 60-100 ℃, dry 10-20 hour.
Sintering temperature is an important step of Kaolinite Preparation of Catalyst, and in above-mentioned steps (3), sintering temperature is 450-550
oc, the time is 3-7 hour, excess Temperature or overlong time can cause specific area and catalytic activity to decline, and also can destroy the flocculent structure of catalyst.Sintering temperature is preferably 500 ℃.
Iron-based composite oxides of the present invention, can be used as the NH that removes nitrogen oxide
3-SCR denitrating catalyst.
Preparation method of the present invention is applicable to Industry Promotion, and the predecessor of employing is the common metal salt such as sulfate and molybdate, and molybdate consumption is less, is conducive to reduce costs.By controlling reaction condition, can make the catalyst activity composition high degree of dispersion that makes, and there is peculiar flocculent structure, the composite oxides of high degree of dispersion have higher specific area, more be conducive to the dispersion of active component, high compared with the catalytic activity of crystallinity catalyst, be conducive to long-term use.
The composite oxides denitrating catalyst catalytic activity with flocculent structure of gained of the present invention is high, can be used for NO in stationary source flue gas, exhaust gas from diesel vehicle and fuel-sean gasoline engine tail gas
x purification and elimination, at 50000 h
-1under air speed condition, there is higher NO within the scope of 250-400 ℃
x clearance and N
2selectively, more than removal efficiency 80 %, and there is good anti-SO
2and H
2o poisoning capability.The catalyst effect that wherein iron molybdenum mol ratio is 18:1 is best, at 50000 h
-1under air speed condition, 250-400
onO within the scope of C
x clearance and N
2more than selectively reaching 90 %, 300
oc, passes into 200 ppm SO
2or 10% H
2o, successive reaction 6 hours, its NO
x removal efficiency still can maintain more than 99%.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of embodiment of the present invention 1-7 gained catalyst.
Fig. 2 is the SEM photo of embodiment 1 gained catalyst.
Fig. 3 is the water resistant sulfur resistance test result figures of embodiment 2 gained catalyst at 300 ℃.
The specific embodiment
Below in conjunction with specific embodiment, the invention will be further described.
1,, in following examples, utilize the denitration performance of simulated flue gas detecting catalyst.Total gas flow rate is 300 mL/min, for guaranteeing NO and NH
3charge ratio be 1, import NO and NH
3concentration is 500 ppm, O
2concentration be 5.3 vol.%, He is Balance Air.Get 0.36 mL catalyst sample, put on fixed bed reactors, making reaction velocity is 50000 h
-1, control reaction temperature by 150 ℃ to 450 ℃.Adopt the NO in nitrogen-oxide analyzer, (Model-42i-HI, U.S. power & light company) detection reaction device exit
xconcentration.
De-efficiency or NO
xconversion ratio calculates:
N
2selective calculation:
2, the anti-sulphur method of testing of catalyst water resistant is: when carrying out out of stock experiment according to the method described above, add a road SO in air inlet
2sO in/He Standard Gases simulated flue gas
2, SO
2concentration is 200 ppm.The method for implanting of steam be by He gas by the Drexel bottle of deionized water is housed, by being heated to uniform temperature, obtain the water vapor concentration needing, H
2the concentration of O is 10%.
embodiment 1
Take 1.7655g (NH
4)
6mo
7o
244H
2o is dissolved in 100 mL deionized waters completely, and regulating ammonium molybdate aqueous solution pH is 9, and this solution is put into water-bath, and to keep temperature be 35 ℃, stirs 0.5 h; Take 5.5604 g FeSO
47H
2o and 100 mg C
6h
8o
6be dissolved in completely in 100 mL deionized waters, ferrous sulfate aqueous solution is dropwise added in the ammonium molybdate aqueous solution of vigorous stirring, and keep the general 6-9 of pH > 6(of mixed solution in titration process), the complete adjusting of titration pH=9, continues to stir aging 3 hours.By deionized water, repeatedly washing precipitation is aobvious neutral to filtrate, and filter cake is put into drying box 70
odry 12 hours of C, in Muffle furnace 500
oc roasting makes iron-based composite oxides in 5 hours, is denoted as catalyst 1.
Because molybdenum ion in building-up process is difficult for being combined and being also difficult for co-precipitation with iron ion, therefore, adopt inductively coupled plasma atomic emission (ICP-AES) to the carrying out of ferro element in catalyst and molybdenum element quantitative analysis, determine the real content of each component in catalyst.Gained catalyst is measured through ICP-AES, and the actual mol ratio of iron molybdenum element is 14:1, and the actual mol ratio of oxygen and iron is 1.88:1, utilizes sem observation sample topography, and sample is flocculent structure, as shown in Figure 2.
Utilize X-ray powder diffraction to characterize the structure of sample, acquired results is as accompanying drawing 1, as can be seen from the figure catalyst only presents the crystalline phase of iron oxide, there is no the crystalline phase of molybdenum oxide or iron molybdenum composite oxides, illustrates that the molybdenum in catalyst exists with high dispersive form.
Take the above-mentioned iron-based composite oxides that make of 400 mg, compacting in flakes, is divided into 40-60 object particle by sample sifter and tests for denitration performance, the results are shown in Table 1.
As can be seen from Table 1: catalyst 1 is 300
oc-350
onO in C temperature range
x removal efficiency is more than 90 %, and catalyst denitration activity is improved little.
embodiment 2
Take 1.0593 g (NH
4)
6mo
7o
244H
2o is dissolved in 100 mL deionized waters completely, and regulating ammonium molybdate aqueous solution pH is 9, and this solution is put into water-bath, and to keep temperature be 25 ℃, stirs 0.5 h; Take 6.6725 g FeSO
47H
2o and 100 mg C
6h
8o
6be dissolved in completely in 100 mL deionized waters, ferrous sulfate aqueous solution is dropwise added in the ammonium molybdate aqueous solution of vigorous stirring, and keep the general 6-9 of pH > 6(of mixed solution in titration process), the complete adjusting of titration pH=9, continues to stir aging 3 hours.By deionized water, repeatedly washing precipitation is aobvious neutral to filtrate, and filter cake is put into drying box 80
odry 18 hours of C, in Muffle furnace 550
oc roasting makes iron-based composite oxides in 4 hours, is denoted as catalyst 2.
Gained catalyst XRD figure as shown in Figure 1, is flocculent structure, through ICP-AES, measures, and in catalyst, actual iron molybdenum mol ratio is 18:1, and the actual mol ratio of oxygen and iron is 1.21:1.Take the above-mentioned iron-based composite oxides that make of 400 mg, compacting in flakes, is divided into 40-60 object particle by sample sifter and tests for denitration performance, and denitration performance test result is in Table 2.
As can be seen from Table 2: catalyst 2 is 250
oc-400
onO in C temperature range
x removal efficiency is more than 90 %, and the catalytic activity of catalyst has obtained larger lifting.
300
oc, passes into 200 ppm SO
2or 10%H
2o, successive reaction is carried out the test of water resistant sulfur poisoning-resistant for 6 hours, the results are shown in Figure 3, as can be seen from the figure: catalyst 2 has good anti-SO
2and anti-H
2o poisoning performance.
embodiment 3
Take 0.7566 g (NH
4)
6mo
7o
244H
2o is dissolved in 100 mL deionized waters completely, and regulating ammonium molybdate aqueous solution pH is 9, and this solution is put into water-bath, and to keep temperature be 40 ℃, stirs 0.5 h; Take 7.1491 g FeSO
47H
2o and 100 mg C
6h
8o
6be dissolved in completely in 100 mL deionized waters, ferrous sulfate aqueous solution is dropwise added in the ammonium molybdate aqueous solution of vigorous stirring, and keep the general 6-9 of pH > 6(of mixed solution in titration process), the complete adjusting of titration pH=9, continues to stir aging 3 hours.By deionized water, repeatedly washing precipitation is aobvious neutral to filtrate, and filter cake is put into drying box 90
odry 15 hours of C, in Muffle furnace 450
oc roasting makes iron-based composite oxides in 7 hours, is denoted as catalyst 3.
Gained catalyst XRD figure as shown in Figure 1, is flocculent structure, through ICP-AES, measures, and in catalyst, actual iron molybdenum mol ratio is 30:1, and the actual mol ratio of oxygen and iron is 1.30:1.
Take the above-mentioned iron-based composite oxides that make of 400 mg, compacting in flakes, is divided into 40-60 object particle by sample sifter and tests for denitration performance, and denitration performance test result is in Table 3.
As can be seen from Table 3: catalyst 3 is 300
oc-400
onO in C temperature range
x removal efficiency is more than 90 %, and the catalytic activity of catalyst obtains certain lifting, but than catalyst 2, catalytic activity declines to some extent
.
embodiment 4
Take 0.5885 g (NH
4)
6mo
7o
244H
2o is dissolved in 100 mL deionized waters completely, and regulating ammonium molybdate aqueous solution pH is 9, and this solution is put into water-bath, and to keep temperature be 35 ℃, stirs 0.5 h; Take 7.4139 g FeSO
47H
2o and 100 mg C
6h
8o
6be dissolved in completely in 100 mL deionized waters, ferrous sulfate aqueous solution dropwise added in the ammonium molybdate aqueous solution of vigorous stirring, and keep the pH > 6 of mixed solution in titration process, the complete adjusting of titration pH=9, continues to stir aging 3 hours.By deionized water, repeatedly washing precipitation is aobvious neutral to filtrate, and filter cake is put into drying box 100
odry 10 hours of C, in Muffle furnace 500
oc roasting makes iron-based composite oxides in 3 hours, is denoted as catalyst 4.
Gained catalyst XRD figure as shown in Figure 1, is flocculent structure, through ICP-AES, measures, and in catalyst, actual iron molybdenum mol ratio is 37:1, and the actual mol ratio of oxygen and iron is 1.28:1.
Take the above-mentioned iron-based composite oxides that make of 400 mg, compacting in flakes, is divided into 40-60 object particle by sample sifter and tests for denitration performance, and denitration performance test result is as follows.
As can be seen from Table 4: 300
oc-400
oin C temperature range, the NO of catalyst 4
x removal efficiency more than 90 %, catalyst activity and catalyst 3 quite.
embodiment 5
Identical with embodiment 1 operation, different is to take (NH
4)
6mo
7o
244H
2o 0.4818 g, Fe
2(SO
4)
310.9112 g, make iron-based composite oxides, are denoted as catalyst 5.
Product characterizes explanation: the actual iron molybdenum mol ratio that gained catalyst is measured through ICP-AES is 40:1, and the actual mol ratio of oxygen and iron is 1.0:1, and sample is flocculent structure.
Take the above-mentioned iron-based composite oxides that make of 400 mg, compacting in flakes, is divided into 40-60 object particle by sample sifter and tests for denitration performance, and denitration performance test result is as follows.
As can be seen from Table 5: temperature range is 300
oc-400
oin C temperature range, the NO of catalyst
x removal efficiency is at 90 %, catalyst activity and catalyst 4 quite.
embodiment 6
Identical with embodiment 2 operations, different is only to take FeSO
47H
2o 8.3406 g, make ferric oxide catalyst, are denoted as catalyst 6.Gained sample is particulate iron oxide, and XRD figure is shown in Fig. 1.
Take the above-mentioned iron oxide making of 400 mg, compacting in flakes, is divided into 40-60 object particle by sample sifter and tests for denitration performance, and denitration performance test result is as follows.
As can be seen from Table 6: 300
oc-400
oin C temperature range, the NO of catalyst 6
x removal efficiency, more than 90 %, but is less than 300
othe catalytic activity of C is far below iron molybdenum composite oxide catalysts.
embodiment 7
Identical with embodiment 2 operations, different is only to take (NH
4)
6mo
7o
244H
2o 5.2965 g, make molybdenum oxide catalyst, are denoted as catalyst 7.Gained sample is graininess molybdenum oxide, and XRD figure is shown in Fig. 1.
Take the above-mentioned molybdenum oxide making of 400 mg, compacting in flakes, is divided into 40-60 object particle by sample sifter and tests for denitration performance, and denitration performance test result is as follows.
As can be seen from Table 7: the denitration rate of catalyst is all lower than 70%, 150
oc-250
oc temperature range is interior lower than 1%, and N
2selective also lower, denitration performance is far below iron molybdenum composite oxide catalysts.
Claims (10)
1. iron-based composite oxides, is characterized in that: comprise iron, molybdenum, three kinds of elemental compositions of oxygen, and iron and molybdenum high degree of dispersion in composite oxides, the mol ratio of iron and molybdenum is 14-40:1, the mol ratio of oxygen and iron is 1.0-1.88:1.
2. iron-based composite oxides according to claim 1, is characterized in that: the mol ratio of iron and molybdenum is 18:1, and the mol ratio of oxygen and iron is 1.21:1.
3. iron-based composite oxides according to claim 1, is characterized in that: Fe and Mo with the oxide of high degree of dispersion or/and the form of composite oxides exist.
4. iron-based composite oxides according to claim 1, is characterized in that: its pattern is cotton-shaped.
5. a preparation method for the iron-based composite oxides described in any one in claim 1-4, is characterized in that comprising the following steps:
(1) molybdenum salt water is dissolved, wiring solution-forming, standby; Molysite and ascorbic acid water are dissolved, wiring solution-forming, standby;
(2) get the above-mentioned molybdenum solution that contains, adding ammoniacal liquor to regulate its pH is 9, and then keeping solution temperature is 25-40 ℃, is stirred to and generates MoO
4 2-ion, then iron-containing liquor is under agitation slowly added drop-wise to containing in molybdenum solution, in dropping process, keeping the pH of mixed liquor is 6-9, dropwising rear adjusting pH is 9, continues stirring aging, makes precipitation of iron ions complete;
(3) after precipitating completely, filter, will precipitate washing, alcohol wash, dry, dried precipitation grinds, roasting at 450-550 ℃, obtains iron-based composite oxides.
6. preparation method according to claim 5, is characterized in that: in step (1), described molybdenum salt is sodium molybdate or ammonium molybdate, and described molysite is ferrous sulfate or ferric sulfate.
7. preparation method according to claim 5, is characterized in that: in step (1), containing in molybdenum solution, the concentration of molybdenum ion is 0.025-0.09 mol/L; In iron-containing liquor, the concentration of iron ion is 0.2-0.27 mol/L, and ascorbic acid consumption is 1 mg/mL.
8. preparation method according to claim 5, is characterized in that: in step (2), generate MoO
4 2-during ion, stir 0.5 h, after dropwising, ageing time is 3 hours; In step (3), at 60-100 ℃, dry 10-20 hour; In step (3), roasting time is 3-7 hour.
9. preparation method according to claim 5, is characterized in that: in step (2), keeping the temperature of iron-containing liquor is 35 ℃; In step (3), sintering temperature is 500 ℃.
10. an application for the iron-based composite oxides described in any one in claim 1-4, is characterized in that: as the NH that removes nitrogen oxide
3-SCR denitrating catalyst.
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| CN110833831A (en) * | 2019-11-07 | 2020-02-25 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of chromium-cobalt-based nitric oxide normal-temperature normal-pressure catalyst, product and application thereof |
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| CN113318749B (en) * | 2021-06-23 | 2023-05-09 | 贵州大学 | High-efficiency medium-low temperature NH for resisting heavy metal poisoning 3 SCR denitration catalyst, and preparation method and application thereof |
| CN113926466A (en) * | 2021-11-23 | 2022-01-14 | 商河县格尔环保科技服务中心 | Denitration catalyst and preparation method thereof |
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