CN104549213B - A kind of gas-fueled vehicles Catalytic methane oxidation catalyst and preparation method thereof - Google Patents
A kind of gas-fueled vehicles Catalytic methane oxidation catalyst and preparation method thereof Download PDFInfo
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Abstract
A kind of gas-fueled vehicles exhaust aftertreatment Catalytic methane oxidation catalyst and preparation method thereof, is stannum zirconium mixed oxide solid solution catalyst, and wherein stannum/atomic percent zirconium is at least 1.1, and reaction expression is Sn1‑xZrxM0.10O2；Wherein M is at least one in rare earth and transition metal；X is coefficient；Component and its percentage by weight：Tin ash SnO2Presoma 50%～70%；Zirconium dioxide ZrO2Presoma 15%～40%；The presoma surplus of stabilizer oxide.Preparation method has following steps successively：1) prepare salt-mixture；2) add precipitant carbamide；3) carry out homogeneous precipitation reaction：4) roasting finished product.The active component content of catalyst of the present invention is high, can significantly improve catalysis oxidation ability of the stannum zirconium solid solution to methane, propane and carbon monoxide in 500 DEG C or so of temperature by combustion of methane.It is and preparation method is simple, it is easy to operate, with low cost.
Description
Technical field
The present invention relates to catalyst, more particularly to a kind of gas-fueled vehicles exhaust aftertreatment is catalyzed with Catalytic methane oxidation
Agent and preparation method thereof.
Background technology
Existing natural gas increasingly rises as a kind of energy of cleaning, the ratio in energy resource structure.But its main component
The ignition temperature of methane is very high, thus efficiency of combustion is relatively low, and can produce a small amount of nitrogen oxides NO in combustionXWith
Other imperfect combustion products, so as to the environmental pollution for causing.Methane oxygen-enriched combusting under catalyst existence condition more meets
Environmental requirement.
The catalyst of automobile-used Catalytic methane oxidation mainly has platinum Pt, palladium Pd, rhodium Rh even load type noble metal catalysts, calcium titanium
Ore deposit type O composite metallic oxide catalyst and supported transitional metal oxide catalyst.Platinum Pt, palladium Pd, rhodium Rh even load types are expensive
Metallic catalyst has a good low-temperature catalytic activity for methyl hydride combustion, but this kind of catalyst exist it is expensive, hot steady
The problems such as qualitative poor and easy-sintering, its application in gas-fueled vehicles exhaust aftertreatment is limited, and Ca-Ti ore type is compound golden
Category oxide catalyst and supported transitional metal oxide catalyst due to specific surface it is little, bad mechanical strength and it is active it is low because
Element, it is also difficult to which useful industrially, Ca-Ti ore type O composite metallic oxide catalyst in strong exothermal reaction, also has high temperature and easily burns
The problems such as knot and the short period element in B positions are easy to run off.
The content of the invention
A technical problem to be solved by this invention is the defect for making up above-mentioned prior art, there is provided a kind of natural gas vapour
Vehicle exhaust post processing Catalytic methane oxidation catalyst.
Another technical problem to be solved by this invention is the defect for making up above-mentioned prior art, there is provided a kind of natural gas
Automobile exhaust post processing Catalytic methane oxidation method for preparing catalyst.
The gas-fueled vehicles exhaust aftertreatment of the present invention is with Catalytic methane oxidation catalyst technology problem by following technology
Scheme is solved.
This gas-fueled vehicles exhaust aftertreatment Catalytic methane oxidation catalyst, belongs to composite oxide solid solution catalysis
Agent.
The characteristics of this gas-fueled vehicles exhaust aftertreatment Catalytic methane oxidation catalyst is：
The composite oxide solid solution catalyst is stannum zirconium mixed oxide solid solution catalyst, wherein stannum/zirconium (Sn/
Zr) atomic ratio is at least 1.1, and reaction expression is Sn1-xZrxM0.10O2；
In reaction expression：
M is at least one in rare earth and transition metal；
X is coefficient；
Its component and its percentage by weight are as follows：
Tin ash SnO2Presoma 50%～70%；
Zirconium dioxide ZrO2Presoma 15%～40%；
The presoma surplus of stabilizer oxide.
The tin ion Sn on the stannum zirconium mixed oxide solid solution catalyst surface4+, it is the master that redox occurs
Want species, its concentration it is excessive or it is too small be unable to generate enough oxidation intermediates, be unfavorable for CH4Oxidation.Due to stannum from
Sub- Sn4+With zirconium ion Zr4+Radius is close to, it is easy to form stannum-zirconium (Sn-Zr) solid solution, and stabilizer oxide is also with solid solution
Body form is present, and when crystal structure is homogeneous solid solution, active component content is high, is at least in stannum/zirconium (Sn/Zr) atomic ratio
In the case of 1.1, tin ion Sn4+Be conducive to the oxidation reaction of catalyst in the degree of segregation of catalyst surface, and heat stability be high,
Oxygen storage capacity is good, can significantly improve stannum-zirconium (Sn-Zr) solid solution to methane CH4, propane C3H8With the catalysis of carbon monoxide CO
Oxidability.
The present invention gas-fueled vehicles exhaust aftertreatment Catalytic methane oxidation catalyst technology problem by it is following enter one
The technical scheme of step is solved.
M in the reaction expression is cerium Ce and yttrium Y or at least one in transition metal Cu, Co, Fe, Mn.
The presoma of the tin ash is four water butter of tin SnCl4·4H2O。
The presoma of the zirconium dioxide is five water zirconium nitrate Zr (NO3)4·5H2O, eight water oxygen zirconium chloride ZrOCl2·
8H2O, and Carbon Dioxide zirconium Zr3CO3·O5In one kind.
The presoma of the stabilizer oxide is six water cerous nitrate Ce (NO3)2·6H2O, five water Yttrium trinitrate Y (NO3)3·
5H2O, cobalt nitrate hexahydrate Co (NO3)2·6H2O, six water manganese nitrate Mn (NO3)2·6H2O, nitrate trihydrate copper Cu (NO3)2·3H2O,
And nine water ferric nitrate Fe (NO3)3·9H2One kind in O.
Preferably：The presoma of the stabilizer oxide is six water cerous nitrate Ce (NO3)2·6H2O and the acid of five liquid glauber salt
Yttrium Y (NO3)3·5H2One kind in O.
The gas-fueled vehicles exhaust aftertreatment of the present invention preparation method technical problem of Catalytic methane oxidation catalyst is led to
Cross technical scheme below to be solved.
This gas-fueled vehicles exhaust aftertreatment preparation method of Catalytic methane oxidation catalyst, belongs to urea combustion
Composite oxide solid solution catalyst is prepared, using carbamide as precipitant.
The characteristics of preparation method of this gas-fueled vehicles exhaust aftertreatment Catalytic methane oxidation catalyst is：
The composite oxide solid solution catalyst is stannum zirconium mixed oxide solid solution catalyst, wherein stannum/zirconium (Sn/
Zr) atomic ratio is at least 1.1, and reaction expression is Sn1-xZrxM0.10O2；
In reaction expression：
M is at least one in rare earth and transition metal；
X is coefficient；
Its component and its percentage by weight are as follows：
Tin ash SnO2Presoma 50%～70%；
Zirconium dioxide ZrO2Presoma 15%～40%；
The presoma surplus of stabilizer oxide；
There are following steps successively：
1) prepare salt-mixture：
By tin ash SnO2Presoma, zirconium dioxide ZrO2Presoma and the presoma of stabilizer oxide press
During ball mill or mortar are respectively placed according to the percentage by weight, salt-mixture is uniformly mixed into：
2) add precipitant carbamide：
The precipitant carbamide that weight is 0.5 times～5.0 times of its weight, ball milling or grinding 0.2h are added in above-mentioned salt-mixture
～1.2h, is obtained pastel；
3) carry out homogeneous precipitation reaction：
Above-mentioned pastel is placed in baking oven, is at 150 DEG C～200 DEG C, to toast 10h～13h in temperature, is uniformly sunk
Form sediment reaction, and the poisonous substance chloride ion Cl in evaporative removal solid solution-1, semi-finished product catalyst is obtained, and pH value will not have both been produced by little
Become big, and " zirconium tinning " structure for being formed, also will not produce pH value from large to small, and be likely to form " stannum bag zirconium " structure；
4) roasting finished product：
During above-mentioned semi-finished product catalyst is placed in chamber type electric resistance furnace also known as Muffle furnace, it is at 500 DEG C～800 DEG C in temperature
Roasting 3h～6h, finished product solid solution catalyst in air atmosphere.
The gas-fueled vehicles exhaust aftertreatment of the present invention preparation method technical problem of Catalytic methane oxidation catalyst is led to
Cross technical scheme further below to be solved.
The step 1) in the presoma of tin ash be four water butter of tin SnCl4·4H2O；
The step 1) in the presoma of zirconium dioxide be five water zirconium nitrate Zr (NO3)4·5H2O, eight water oxygen zirconium chlorides
ZrOCl2·8H2O, and Carbon Dioxide zirconium Zr3CO3·O5In one kind.
The step 1) in the presoma of stabilizer oxide be six water cerous nitrate Ce (NO3)2·6H2O, the acid of five liquid glauber salt
Yttrium Y (NO3)3·5H2O, cobalt nitrate hexahydrate Co (NO3)2·6H2O, six water manganese nitrate Mn (NO3)2·6H2O, nitrate trihydrate copper Cu
(NO3)2·3H2O, and nine water ferric nitrate Fe (NO3)3·9H2One kind in O.
Preferably：The presoma of the stabilizer oxide is six water cerous nitrate Ce (NO3) 26H2O and the acid of five liquid glauber salt
One kind in yttrium Y (NO3) 35H2O.
The step 2) in salt-mixture add precipitant amount of urea be：Rare earth ion in carbamide and salt-mixture and
The mol ratio of transition metal ionss is 20.
Compared with the prior art, the invention has the advantages that：
The catalyst activity component content of the present invention is high, in the case where stannum/zirconium (Sn/Zr) atomic ratio is at least 1.1, stannum
Ion Sn4+Be conducive to the oxidation reaction of catalyst in the degree of segregation of catalyst surface, and heat stability is high, oxygen storage capacity is good,
In Catalytic methane oxidation course of reaction, oxidant is used air as, initiation temperature and complete ignition temperature are low, can be in temperature
500 DEG C or so, by combustion of methane, can significantly improve stannum-zirconium (Sn-Zr) solid solution to methane CH4, propane C3H8With an oxygen
Change the catalysis oxidation ability of carbon CO.The preparation method of the catalyst of the present invention is simple, it is easy to operate, with low cost.
Specific embodiment
With reference to specific embodiment, the present invention will be described.
Specific embodiment one
A kind of reaction expression is Sn0.50Zr0.40Ce0.10O2Gas-fueled vehicles exhaust aftertreatment urged with Catalytic methane oxidation
Agent, its preparation method have following steps successively：
1) prepare salt-mixture
Weigh the four water butter of tin SnCl of presoma of the tin ash of 12.6g4·4H2Before the zirconium dioxide of O, 12.4g
Drive five water zirconium nitrate Zr (NO of body3)4·5H2O, and the six water cerous nitrate Ce (NO of presoma of the stabilizer cerium oxide of 3.1g3)2·
6H2O, is placed in mortar, is uniformly mixed into salt-mixture；
2) the 40g carbamide that weight is 1.42 times of its weight is added in above-mentioned salt-mixture, grind 0.5h, pasty state is obtained
Thing；
3) above-mentioned pastel is placed in baking oven, be 12h to be toasted at 200 DEG C in temperature, semi-finished product catalyst is obtained；
4), in above-mentioned semi-finished product catalyst being placed in chamber type electric resistance furnace also known as Muffle furnace, it is roasting 3h at 500 DEG C in temperature,
Finished product solid solution catalyst Sn0.50Zr0.40Ce0.10O2。
Solid solution catalyst Sn obtained in this specific embodiment one0.50Zr0.40Ce0.10O2, in air and the volume of methane
Than being 30000m for 49, air velocity3Under conditions of/h, catalyst amount are 0.2g, the methane at a temperature of different stabilizers turns
Rate (%) see the table below 1：
Table 1
| Temperature (DEG C) | 340 | 360 | 380 | 400 | 420 | 440 | 460 | 480 | 520 | 560 |
| Specific embodiment one | 31.99 | 52.92 | 71.31 | 85.60 | 92.68 | 97.18 | -- | -- | -- | -- |
| Specific embodiment two | 38.71 | 58.71 | 75.37 | 86.73 | 93.75 | 97.21 | 98.60 | -- | -- | -- |
| Specific embodiment three | 7.58 | 19.47 | 35.28 | 54.06 | 69.11 | 77.70 | 82.04 | 85.60 | 89.59 | 91.65 |
| Specific embodiment four | 21.46 | 39.39 | 62.00 | 80.86 | 90.91 | 95.39 | 96.39 | -- | -- | -- |
| Specific embodiment five | 16.02 | 36.66 | 57.48 | 74.77 | 85.66 | 90.88 | 94.68 | 96.98 | -- | -- |
Specific embodiment two
A kind of reaction expression is Sn0.50Zr0.40Y0.10O2Gas-fueled vehicles exhaust aftertreatment be catalyzed with Catalytic methane oxidation
Agent, substantially with specific embodiment one, difference is its preparation method：
The presoma butter of tin SnCl of tin ash4·4H2O is 13.2g；
The presoma zirconium nitrate Zr (NO of zirconium dioxide3)4·5H2O is 12.9g；
The five water Yttrium trinitrate Y (NO of presoma of stabilizer3)3·5H2O is 2.9g；
Carbamide is 120g, is 4.13 times of salt-mixture weight.
Solid solution catalyst Sn obtained in specific embodiment two0.50Zr0.40Y0.10O2, in air and the volume ratio of methane
It is 30000m for 49, air velocity3Methane conversion under conditions of/h, catalyst amount are 0.2g, at a temperature of different stabilizers
Rate (%) sees the above table 1.
Specific embodiment three
A kind of reaction expression is Sn0.50Zr0.40Co0.10O2Gas-fueled vehicles exhaust aftertreatment urged with Catalytic methane oxidation
Agent, substantially with specific embodiment one, difference is its preparation method：
The presoma butter of tin SnCl of tin ash4·4H2O is 13.5g；
The presoma zirconium nitrate Zr (NO of zirconium dioxide3)4·5H2O is 13.2g；
The presoma cobalt nitrate hexahydrate Co (NO of stabilizer cobalt dioxide3)2·6H2O is 2.2g；
Carbamide is 60g, is 2 times of salt-mixture weight.
Solid solution catalyst Sn obtained in specific embodiment three0.50Zr0.40Co0.10O2, in air and the volume ratio of methane
It is 30000m for 49, air velocity3Methane conversion under conditions of/h, catalyst amount are 0.2g, at a temperature of different stabilizers
Rate (%) sees the above table 1.
Specific embodiment four
A kind of reaction expression is Sn0.50Zr0.40Mn0.10O2Gas-fueled vehicles exhaust aftertreatment urged with Catalytic methane oxidation
Agent, substantially with specific embodiment one, difference is its preparation method：
The presoma butter of tin SnCl of tin ash4·4H2O is 13.3g；
The presoma zirconium nitrate Zr (NO of zirconium dioxide3)4·5H2O is 14.4g；
The six water manganese nitrate Mn (NO of presoma of stabilizer manganese dioxide3)2·6H2O is 2.6g；
Carbamide is 35g, is 1.13 times of salt-mixture weight.
Solid solution catalyst Sn obtained in specific embodiment four0.50Zr0.40Mn0.10O2, in air and the volume ratio of methane
It is 30000m for 49, air velocity3Methane conversion under conditions of/h, catalyst amount are 0.2g, at a temperature of different stabilizers
Rate (%) sees the above table 1.
Specific embodiment five
A kind of reaction expression is Sn0.50Zr0.40Fe0.10O2Gas-fueled vehicles exhaust aftertreatment urged with Catalytic methane oxidation
Agent, substantially with specific embodiment one, difference is its preparation method：
The presoma butter of tin SnCl of tin ash4·4H2O is 15.2g；
The presoma zirconium nitrate Zr (NO of zirconium dioxide3)4·5H2O is 12.4g；
The nine water ferric nitrate Fe (NO of presoma of stabilizer nitrate3)3·9H2O is 2.1g；
Carbamide is 150g, is 5 times of salt-mixture weight.
Solid solution catalyst Sn obtained in specific embodiment five0.50Zr0.40Fe0.10O2, in air and the volume ratio of methane
It is 30000m for 49, air velocity3Methane conversion under conditions of/h, catalyst amount are 0.2g, at a temperature of different stabilizers
Rate (%) sees the above table 1.
Five specific embodiments of the above show, are at least 1.1 in stannum/zirconium (Sn/Zr) atomic ratio of catalyst surface
In the case of, using different rare earths oxide and transition metal oxide as stabilizer, it is solid to stannum zirconium mixed oxide
The methane conversion of solution catalyst is variant, and wherein specific embodiment one and specific embodiment two are respectively adopted cerium
The oxide of Ce and yttrium Y is modified to methane CH as stabilizer4Activity of conversion preferably, stable solid solution can be formed.
And transition metals cobalt Co, manganese Mn in specific embodiment three, specific embodiment four and specific embodiment five
The stannum zirconium mixed oxide solid solution catalyst being modified as stabilizer with ferrum Fe, has certain resistance to catalyst oxidation susceptibility
Hinder effect, cause catalyst light-off temperature to be urged as the stannum zirconium mixed oxide solid solution that stabilizer is modified higher than cerium Ce and yttrium Y
Agent.
Above content is with reference to specific preferred implementation further description made for the present invention, it is impossible to assert
The present invention be embodied as be confined to these explanations.For general technical staff of the technical field of the invention,
Some equivalent substitutes or obvious modification are made on the premise of without departing from present inventive concept, and performance or purposes are identical, all should
It is considered as belonging to the scope of patent protection that the present invention is determined by the claims submitted to.
Claims (6)
1. preparation method of a kind of gas-fueled vehicles exhaust aftertreatment with Catalytic methane oxidation catalyst, it is characterised in that：
The gas-fueled vehicles exhaust aftertreatment Catalytic methane oxidation catalyst belongs to composite oxide solid solution catalyst, institute
It is stannum zirconium mixed oxide solid solution catalyst to state composite oxide solid solution catalyst, and wherein stannum/atomic percent zirconium is at least
1.1, reaction expression is Sn1-xZrxM0.10O2；
In reaction expression：
M is at least one in rare earth and transition metal；
X is coefficient；
Its component and its percentage by weight are as follows：
Tin ash SnO2Presoma 50%～70%；
Zirconium dioxide ZrO2Presoma 15%～40%；
The presoma surplus of stabilizer oxide；
The preparation method has following steps successively：
1) prepare salt-mixture：
By tin ash SnO2Presoma, zirconium dioxide ZrO2Presoma and stabilizer oxide presoma according to institute
State percentage by weight to be respectively placed in ball mill or mortar, be uniformly mixed into salt-mixture：
2) add precipitant carbamide：
In above-mentioned salt-mixture add weight be 0.5 times～5.0 times of its weight precipitant carbamide, ball milling or grinding 0.2h～
1.2h, is obtained pastel；
3) carry out homogeneous precipitation reaction：
Above-mentioned pastel is placed in baking oven, is at 150 DEG C～200 DEG C, to toast 10h～13h in temperature, is carried out homogeneous precipitation anti-
Should, and the poisonous substance chloride ion Cl in evaporative removal solid solution-1, semi-finished product catalyst is obtained, pH value will not have both been produced and changed from small to big,
And " zirconium tinning " structure for being formed, also will not produce pH value from large to small, and be likely to form " stannum bag zirconium " structure；
4) roasting finished product：
During above-mentioned semi-finished product catalyst is placed in chamber type electric resistance furnace also known as Muffle furnace, it is the air at 500 DEG C～800 DEG C in temperature
Roasting 3h～6h, finished product solid solution catalyst in atmosphere.
2. preparation method of the gas-fueled vehicles exhaust aftertreatment as claimed in claim 1 with Catalytic methane oxidation catalyst, its
It is characterised by：
The step 1) in the presoma of tin ash be four water butter of tin SnCl4·4H2O。
3. preparation method of the gas-fueled vehicles exhaust aftertreatment as claimed in claim 1 with Catalytic methane oxidation catalyst, its
It is characterised by：
The step 1) in the presoma of zirconium dioxide be five water zirconium nitrate Zr (NO3)4·5H2O, eight water oxygen zirconium chlorides
ZrOCl2·8H2O, and Carbon Dioxide zirconium Zr3CO3·O5In one kind.
4. preparation method of the gas-fueled vehicles exhaust aftertreatment as claimed in claim 1 with Catalytic methane oxidation catalyst, its
It is characterised by：
The step 1) in the presoma of stabilizer oxide be six water cerous nitrate Ce (NO3)2·6H2O, five water Yttrium trinitrate Y
(NO3)3·5H2O, cobalt nitrate hexahydrate Co (NO3)2·6H2O, six water manganese nitrate Mn (NO3)2·6H2O, nitrate trihydrate copper Cu
(NO3)2·3H2O, and nine water ferric nitrate Fe (NO3)3·9H2One kind in O.
5. preparation method of the gas-fueled vehicles exhaust aftertreatment as claimed in claim 1 with Catalytic methane oxidation catalyst, its
It is characterised by：
The step 2) in salt-mixture add precipitant amount of urea be：Rare earth ion and transition in carbamide and salt-mixture
The mol ratio of metal ion is 20.
6. preparation method of the gas-fueled vehicles exhaust aftertreatment as claimed in claim 1 with Catalytic methane oxidation catalyst, its
It is characterised by：
M in the reaction expression is at least one in cerium Ce and yttrium Y.
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| CN108607544B (en) * | 2018-05-03 | 2021-01-15 | 青岛大学 | Low-temperature catalytic oxidation catalyst for volatile organic compounds and preparation and application thereof |
| CN112264027B (en) * | 2020-10-27 | 2021-11-02 | 南京工业大学 | Copper-cobalt-cerium composite oxide catalytic combustion catalyst and preparation method and application thereof |
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| CN101992083A (en) * | 2010-10-27 | 2011-03-30 | 重庆海特汽车排气系统有限公司 | Composite cerium-zirconium solid solution with high oxygen storage capability and preparation method thereof |
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| 甲烷氧化催化剂的初步研究;嵇玉书等;《应用化学》;19860228;第3卷(第1期);第19-23页 * |
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Effective date of registration: 20181107 Address after: 518000 9E, 9 Meishan Road, Futian District, Shenzhen, Guangdong 2 Patentee after: Han Shuang Address before: 337000 Shang Bu Industrial Park, Pingxiang, Jiangxi Co-patentee before: Han Shuang Patentee before: JIANGXI BAOAN NEW MATERIAL TECH Co.,Ltd. Effective date of registration: 20181107 Address after: 337000 Shang Bu Industrial Park, Pingxiang, Jiangxi Co-patentee after: Han Shuang Patentee after: JIANGXI BAOAN NEW MATERIAL TECH Co.,Ltd. Address before: 337000 Shang Bu Industrial Park, Pingxiang, Jiangxi Co-patentee before: Han Zhao Patentee before: JIANGXI BAOAN NEW MATERIAL TECH Co.,Ltd. |