CN103599790A - Cobalt rare earth composite oxide catalyst for efficiently catalyzing complete oxidation of methane at low temperature - Google Patents
Cobalt rare earth composite oxide catalyst for efficiently catalyzing complete oxidation of methane at low temperature Download PDFInfo
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- CN103599790A CN103599790A CN201310544189.6A CN201310544189A CN103599790A CN 103599790 A CN103599790 A CN 103599790A CN 201310544189 A CN201310544189 A CN 201310544189A CN 103599790 A CN103599790 A CN 103599790A
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Abstract
The invention discloses a cobalt rare earth composite oxide catalyst capable of efficiently catalyzing the complete oxidation of methane at low temperature and a catalyst preparation method. A main active component of the catalyst is spinel type Co3O4, a rare earth element Ln, the addition content range of which is that the Ln/(Ln+Co) molar ratio is 0-0.05, is used as an additive, and the Ln is one or more of La, Ce, Y, Pr, Nd and Sm. The methane ignition temperature and complete combustion temperature of the catalyst are relatively low, the activity of the catalyst is higher than that of a 2% Pd/Al2O3 catalyst prepared in laboratories, and the catalyst is little affected by water vapor and has a relatively high practical value.
Description
Technical field
The invention belongs to catalytic field, relate to a kind of can be efficient, the Catalysts and its preparation method of low-temperature catalyzed combustion of methane.
Background technology
CH
4greenhouse effects effect be 20 times of carbon dioxide, its ignition temperature is 1600
oc, so can produce a large amount of NO by traditional flame combustion process
x, CO etc., can cause secondary pollution to atmosphere.Along with the exhaustion of petroleum-based energy and more and more severeer energy crisis, its reserves of natural gas, because are large, price is lower, it is relatively convenient to use, and occupy more and more consequence in energy field.CH
4as the important component part of natural gas, its molecule is containing a carbon atom and four hydrogen atoms, and with respect to other hydrocarbon, it is a kind of energy of high effect cleaning.Therefore catalytic combustion is to eliminate CH
4pollution to atmosphere is again that the controlled natural gas that utilizes is as the energy one of the most effective method.And the key that development catalyst efficient, good stability is methane catalytic combustion.
At present, methyl hydride combustion catalyst mainly contains support type Pt, Pd noble metal catalyst and non-precious metal catalyst at present as Ca-Ti ore type (ABO
3), hexa-aluminate type (MO6Al
2o
3), spinel-type (AB
2o
4) and other simple composite oxide catalyst.Because noble metal is expensive, development containing on a small quantity or not containing the transition metal oxide of noble metal as methyl hydride combustion catalyst, be subject to extensive concern.
Summary of the invention
The object of the present invention is to provide a kind of Catalysts and its preparation method of efficient, low-temperature catalyzed combustion of methane.
A cobalt rare-earth composite oxide catalyst for high-efficiency low-temperature catalysis combustion of methane, catalyst main active component is spinel-type Co
3o
4, rare-earth elements La, Ce, Y, Pr, Nd, one or more mixed rare-earth elements in Sm are as auxiliary agent.
The preparation method of described cobalt rare-earth composite oxide catalyst, is characterized in that adopting the method for co-precipitation, first configures 0.5 mol
/the cobalt salt of L and rare earths salt, make mixed solution in molar ratio, and Ln/(Ln+Co) molar ratio computing Ln addition scope of wherein take is 0-0.05; At room temperature, add precipitating reagent to precipitate in certain pH, aging after, filter, washing, dry, finally in air atmosphere roasting, obtain finished catalyst, specific surface area of catalyst is 51-95m
2/ g.
In order to reach better technique effect:
Described precipitating reagent is the K of 1 mol/L
2cO
3or Na
2cO
3the aqueous solution.
Ln/ (Ln+Co) molar ratio computing Ln addition be 0.05 and Ln be the preparation of Y, Pr equimolar ratio.
Described rare-earth salts is Co salt, La salt, Ce salt, Y salt, Pr salt, Nd salt and Sm salt; Described cobalt salt is Co (NO
3)
26H
2o is dissolved in distilled water and makes; Described rare earth La salt, Ce salt are by La (NO
3)
36H
2o, Ce (NO
3)
36H
2o is dissolved in distilled water and makes; Described Rare Earth Y salt, Pr salt, Nd salt and Sm salt are by Y
2o
3, Pr
2o
3, Nd
2o
3, Sm
2(CO
3)
3after nitric acid dissolve, make.
Described pH scope is 9-10.
Described burin-in process comprises abundant stirring and standing; Described sintering temperature is 500
oc.
The invention still further relates to the application of described cobalt rare-earth composite oxide catalyst in low-temperature catalyzed combustion of methane.
Described application, is characterized in that consisting of 1% CH at normal pressure, reaction gas
4, 4% O
2, 95% N
2, air speed F/W is 18,000 ml/ (g cat h), furnace temperature is 420-480
ounder the reaction condition of C, realize CH
4complete catalysts oxidation; Described F is feed gas volume flow, and W is catalyst quality.
The feature of catalyst of the present invention is: ignition and the completing combustion temperature of (1) catalyst methane are lower, the active 2%Pd/Al preparing higher than laboratory
2o
3catalyst, and be subject to influence of moisture little, there is higher practical value.(2) use mishmetal salt as rare-earth salts raw material, reduce rare earths separation cost, greatly reduce Catalyst Production cost.(3) compare with loaded noble metal catalyst, the simple easy operating of (4) with low cost method for preparing catalyst, is applicable to large-scale production.
The specific embodiment
Embodiment 1 catalyst 1
By 13 g Co (NO
3)
26H
2o is dissolved in 90ml distilled water, forms Co (NO
3)
2clear solution.By 0.74 g La (NO
3)
36H
2o is dissolved in the distilled water of 5ml, forms La (NO
3)
3clear solution.By Co (NO
3)
2and La (NO
3)
3solution is mixed to form mixed solution, at room temperature stirs, and drips the K of 1 mol/L
2cO
3the aqueous solution is as precipitating reagent, and regulating pH is 9.0, continues to stir 1 h, standing 3 h, sediment after suction filtration, washing, 100
odried overnight under C, 500
oc air atmosphere roasting 4 h, make finished catalyst.Recording specific surface area of catalyst is 69 m
2/ g.
Embodiment 2 catalyst 2
By 13 g Co (NO
3)
26H
2o is dissolved in 90 ml distilled water, forms Co (NO
3)
2clear solution.By 0.744 g Ce (NO
3)
36H
2o is dissolved in the distilled water of 5ml, forms Ce (NO
3)
3clear solution.By Co (NO
3)
2and Ce (NO
3)
3solution is mixed to form mixed solution, and the preparation process of other catalyst is with catalyst 1.Recording specific surface area of catalyst is 55 m
2/ g.
Embodiment 3 catalyst 3
By 13g Co (NO
3)
26H
2o is dissolved in 93 ml distilled water, forms Co (NO
3)
2clear solution.By 0.27 gY
2o
3be dissolved in the nitric acid of 3.2ml 10mol/L, form Y (NO
3)
3clear solution.By Co (NO
3)
2and Y (NO
3)
3solution is mixed to form mixed solution, and the preparation process of other catalyst is with catalyst 1.Recording specific surface area of catalyst is 87 m
2/ g.
Embodiment 4 catalyst 4
By 13g Co (NO
3)
26H
2o is dissolved in 90 ml distilled water, forms Co (NO
3)
2clear solution.By 0.27 gY
2o
3be dissolved in the nitric acid of 3.2ml 10mol/L, form Y (NO
3)
3clear solution.By Co (NO
3)
2and Y (NO
3)
3solution is mixed to form mixed solution, and precipitating reagent is Na
2cO
3, the preparation process of other catalyst is with catalyst 1.Recording specific surface area of catalyst is 91m
2/ g.
Embodiment 5 catalyst 5
By 13 g Co (NO
3)
26H
2o is dissolved in 90ml distilled water, forms Co (NO
3)
2clear solution.By 0.39 g Pr
11o
6be dissolved in the nitric acid of 3.7ml 10mol/L, form Pr (NO
3)
3clear solution.By Co (NO
3)
2and Pr (NO
3)
3solution is mixed to form mixed solution, and the preparation process of other catalyst is with catalyst 1.Recording specific surface area of catalyst is 62 m
2/ g.
Embodiment 6 catalyst 6
By 13 g Co (NO
3)
26H
2o is dissolved in 90 ml distilled water, forms Co (NO
3)
2clear solution.By 0.4 gNd
2o
3be dissolved in the nitric acid of 4.5ml 10mol/L, form Nd (NO
3)
3clear solution.By Co (NO
3)
2and Nd (NO
3)
3solution is mixed to form mixed solution, and the preparation process of other catalyst is with catalyst 1.Recording specific surface area of catalyst is 59 m
2/ g.
Embodiment 7 catalyst 7
13.89g Co (NO just
3)
26H
2o is dissolved in 96ml distilled water, forms Co (NO
3)
2clear solution.By 0.47g Sm
2(CO
3)
3be dissolved in 4.7 ml 10 mol
. l
-1in nitric acid, form Sm (NO
3)
3clear solution.By Co (NO
3)
2and Sm (NO
3)
3solution is mixed to form mixed solution, and the preparation process of other catalyst is with catalyst 1.Recording specific surface area of catalyst is 51 m
2/ g.
Embodiment 8 catalyst 8
By 13g Co (NO
3)
26H
2o is dissolved in 90 ml distilled water, forms Co (NO
3)
2clear solution.By 0.56g Sm
2(CO
3)
3be dissolved in 5 ml 10 mol
. l
-1in nitric acid, form Sm (NO
3)
3clear solution.By Co (NO
3)
2and Sm (NO
3)
3solution is mixed to form mixed solution, and the preparation process of other catalyst is with catalyst 1.Recording specific surface area of catalyst is 65 m
2/ g.
Embodiment 9 catalyst 9
By 13g Co (NO
3)
26H
2o is dissolved in 90 ml distilled water, forms Co (NO
3)
2clear solution.By 0.54g La (NO
3)
36H
2o is dissolved in the distilled water of 2.5ml, forms La (NO
3)
3clear solution. by 0.48g Y (NO
3)
36H
2o is dissolved in the distilled water of 2.5ml, forms Y (NO
3)
3clear solution.By Co (NO
3)
2, Y (NO
3)
3and La (NO
3)
3solution is mixed to form mixed solution, and the preparation process of other catalyst is with catalyst 1.Recording specific surface area of catalyst is 95 m
2/ g.
Embodiment 10 catalyst 10
By 13g Co (NO
3)
26H
2o is dissolved in 90 ml distilled water, forms Co (NO
3)
2clear solution.By 0.54g La (NO
3)
36H
2o is dissolved in the distilled water of 2.5ml, forms La (NO
3)
3clear solution. by 0.21g Pr
11o
6be dissolved in 2.0ml 10 mol
. l
-1in nitric acid, form Pr (NO
3)
3clear solution.By Co (NO
3)
2, La (NO
3)
3and Pr (NO
3)
3solution is mixed to form mixed solution, and the preparation process of other catalyst is with catalyst 1.Recording specific surface area of catalyst is 66 m
2/ g.
Embodiment 11 catalyst 11
By 13g Co (NO
3)
26H
2o is dissolved in 90 ml distilled water, forms Co (NO
3)
2clear solution.By 0.21g Pr
11o
6be dissolved in 2.0ml 10 mol
. l
-1in nitric acid, form Pr (NO
3)
3clear solution.By 0.48g Y (NO
3)
36H
2o is dissolved in the distilled water of 2.5ml, forms Y (NO
3)
3clear solution.By Co (NO
3)
2, Y (NO
3)
3and Pr (NO
3)
3solution is mixed to form mixed solution, and the preparation process of other catalyst is with catalyst 1.Recording specific surface area of catalyst is 87m
2/ g.
Embodiment 12 catalytic methane combustion reaction active testings
Get the quartz tube reactor that 100 mg 40-60 order catalyst 1-11 are placed in internal diameter 6 mm, pass into 1% CH
4, 4% O
2, 95% N
2reacting gas, air speed is 18,000 ml/ (g cat h), under normal pressure, by controlling heating furnace temperature programming successive reaction, the results are shown in table 1.
Table 1 differential responses temperature catalyst catalysis CH
4combustion transformation capability
Note: for catalyst 11, Ln/(Ln+Co) molar ratio computing Ln addition be 0.05 and Ln be Y, the preparation of Pr equimolar ratio, this catalyst is 390
oCtime CH
4conversion ratio reaches 93%, has higher CH
4oxidation catalytic activity.
Embodiment 13 and the active contrast test of loaded noble metal catalyst catalytic methane combustion reaction
Catalyst 3 and 2%Pd/Al
2o
3methane oxidization catalyzing reactivity contrasts.By 13.9 g Al (NO
3)
39H
2o is dissolved in 90ml distilled water, forms Al (NO
3)
3clear solution.Drip ammonia spirit as precipitating reagent, regulating pH is 9.0, continues to stir 1 h, standing 3 h, sediment after suction filtration, washing, 100
odried overnight under C, 600
oc air atmosphere roasting 6 h, make finished product Al
2o
3catalyst.Then in the acid of catalyst surface dipping 1.3g chlorine palladium, 100
oc dried overnight, 500
oc air atmosphere roasting 4 h, make finished catalyst.Recording specific surface area of catalyst is 208 m
2/ g.
Get 20 mg 40-60 order catalyst 3 and 2%Pd/Al
2o
3be placed in respectively the quartz tube reactor of internal diameter 6 mm, pass into 1% CH
4, 4% O
2, 95% N
2reacting gas, air speed is 90,000 ml/ (g cat h), under normal pressure, by controlling heating furnace temperature programming successive reaction, the results are shown in table 2.
Table 2 differential responses temperature catalyst catalysis CH
4conversion rate of oxidation
Catalyst stability test under embodiment 14 steam existence conditions
Get the quartz tube reactor that 100 mg 40-60 order catalyst 8 are placed in internal diameter 6 mm, pass into 1% CH
4, 4% O
2, 95% N
2, reacting gas, adopt Bubbling method to introduce 5% steam, air speed is 18,000 ml/ (g cat h), under normal pressure, furnace temperature 450
ounder the reaction condition of C, carry out successive reaction 60 h, CH
4conversion ratio still maintain 95%.
Claims (9)
1. a cobalt rare-earth composite oxide catalyst for high-efficiency low-temperature catalysis combustion of methane, is characterized in that catalyst main active component is spinel-type Co
3o
4, rare-earth elements La, Ce, Y, Pr, Nd, one or more mixed rare-earth elements in Sm are as auxiliary agent.
2. the preparation method of cobalt rare-earth composite oxide catalyst described in claim 1, is characterized in that adopting the method for co-precipitation, first configures 0.5 mol
/the cobalt salt of L and rare earths salt, make mixed solution in molar ratio, and Ln/(Ln+Co) molar ratio computing Ln addition scope of wherein take is 0-0.05; At room temperature, add precipitating reagent to precipitate in certain pH, aging after, filter, washing, dry, finally in air atmosphere roasting, obtain finished catalyst, specific surface area of catalyst is 51-95m
2/ g.
3. preparation method as claimed in claim 2, is characterized in that described precipitating reagent is the K of 1 mol/L
2cO
3or Na
2cO
3the aqueous solution.
4. preparation method as claimed in claim 2, it is characterized in that Ln/ (Ln+Co) molar ratio computing Ln addition be 0.05 and Ln be Y, the preparation of Pr equimolar ratio.
5. preparation method as claimed in claim 2, is characterized in that described rare-earth salts is Co salt, La salt, Ce salt, Y salt, Pr salt, Nd salt and Sm salt; Described cobalt salt is Co (NO
3)
26H
2o is dissolved in distilled water and makes; Described rare earth La salt, Ce salt are by La (NO
3)
36H
2o, Ce (NO
3)
36H
2o is dissolved in distilled water and makes; Described Rare Earth Y salt, Pr salt, Nd salt and Sm salt are by Y
2o
3, Pr
2o
3, Nd
2o
3, Sm
2(CO
3)
3after nitric acid dissolve, make.
6. preparation method as claimed in claim 2, is characterized in that described pH scope is 9-10.
7. preparation method as claimed in claim 2, is characterized in that described burin-in process comprises abundant stirring and standing; Described sintering temperature is 500
oc.
8. the application of claim 1 cobalt rare-earth composite oxide catalyst in low-temperature catalyzed combustion of methane.
9. application as claimed in claim 7, is characterized in that consisting of 1% CH at normal pressure, reaction gas
4, 4% O
2, 95% N
2, air speed F/W is 18,000 ml/ (g cat h), furnace temperature is 420-480
ounder the reaction condition of C, realize CH
4complete catalysts oxidation; Described F is feed gas volume flow, and W is catalyst quality.
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|---|---|---|---|
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|---|---|---|---|
| CN201310544189.6A CN103599790A (en) | 2013-11-06 | 2013-11-06 | Cobalt rare earth composite oxide catalyst for efficiently catalyzing complete oxidation of methane at low temperature |
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|---|---|---|---|
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103990460A (en) * | 2014-05-16 | 2014-08-20 | 上海纳米技术及应用国家工程研究中心有限公司 | Propane complete oxidation catalyst as well as preparation method and application thereof |
| CN103990461A (en) * | 2014-05-16 | 2014-08-20 | 上海纳米技术及应用国家工程研究中心有限公司 | Propane full-catalytic oxidation agent of cobaltosic oxide as well as preparation method and application of oxidation agent |
| CN105327706A (en) * | 2015-09-23 | 2016-02-17 | 上海交通大学 | Catalyst for low temperature catalytic removal of environment pollutants, and preparation method thereof |
| CN107185553A (en) * | 2017-06-20 | 2017-09-22 | 浙江明华空气净化科技有限公司 | A kind of catalysis oxidation at room temperature removes catalyst of formaldehyde and preparation method thereof |
| CN108355666A (en) * | 2018-02-08 | 2018-08-03 | 山西大学 | A kind of O composite metallic oxide catalyst and its preparation method and application |
| CN113856690A (en) * | 2021-09-09 | 2021-12-31 | 福州大学 | Cobalt-based catalyst for catalytic combustion of low-concentration methane |
| CN115069259A (en) * | 2022-07-06 | 2022-09-20 | 四川大学 | Method for improving sintering resistance of cobalt oxide catalyst by doping lanthanum |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103990460A (en) * | 2014-05-16 | 2014-08-20 | 上海纳米技术及应用国家工程研究中心有限公司 | Propane complete oxidation catalyst as well as preparation method and application thereof |
| CN103990461A (en) * | 2014-05-16 | 2014-08-20 | 上海纳米技术及应用国家工程研究中心有限公司 | Propane full-catalytic oxidation agent of cobaltosic oxide as well as preparation method and application of oxidation agent |
| CN103990460B (en) * | 2014-05-16 | 2016-04-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Propane completely oxidizing catalyst and its preparation method and application |
| CN103990461B (en) * | 2014-05-16 | 2016-07-20 | 上海纳米技术及应用国家工程研究中心有限公司 | Propane complete catalysts oxidation agent of Cobalto-cobaltic oxide and its preparation method and application |
| CN105327706A (en) * | 2015-09-23 | 2016-02-17 | 上海交通大学 | Catalyst for low temperature catalytic removal of environment pollutants, and preparation method thereof |
| CN105327706B (en) * | 2015-09-23 | 2018-07-03 | 上海交通大学 | A kind of catalyst of low-temperature catalyzed removal environmental contaminants and preparation method thereof |
| CN107185553A (en) * | 2017-06-20 | 2017-09-22 | 浙江明华空气净化科技有限公司 | A kind of catalysis oxidation at room temperature removes catalyst of formaldehyde and preparation method thereof |
| CN108355666A (en) * | 2018-02-08 | 2018-08-03 | 山西大学 | A kind of O composite metallic oxide catalyst and its preparation method and application |
| CN113856690A (en) * | 2021-09-09 | 2021-12-31 | 福州大学 | Cobalt-based catalyst for catalytic combustion of low-concentration methane |
| CN113856690B (en) * | 2021-09-09 | 2023-08-18 | 福州大学 | Cobalt-based catalyst for low-concentration methane catalytic combustion |
| CN115069259A (en) * | 2022-07-06 | 2022-09-20 | 四川大学 | Method for improving sintering resistance of cobalt oxide catalyst by doping lanthanum |
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Application publication date: 20140226 |