CN100445208C - Preparing process of mesoprous composite Ba-Al oxide with great specific surface area - Google Patents
Preparing process of mesoprous composite Ba-Al oxide with great specific surface area Download PDFInfo
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- CN100445208C CN100445208C CNB2006101305002A CN200610130500A CN100445208C CN 100445208 C CN100445208 C CN 100445208C CN B2006101305002 A CNB2006101305002 A CN B2006101305002A CN 200610130500 A CN200610130500 A CN 200610130500A CN 100445208 C CN100445208 C CN 100445208C
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- oxide
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- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
The present invention discloses preparation process of mesoporous composite Ba-Al oxide with great specific surface area and belongs to the field of mesoporous material preparing technology. The present invention prepares mesoporous composite Ba-Al oxide with triblock copolymer EO20PO70EO20 (P123) as the structural guiding agent, ammonium carbonate as the precipitant and barium nitrate and aluminum isopropoxide as material in the molar ratio of Ba to P123 to Al in (6-17) to 2 to 100, and through hydrolysis at 55-70deg.c to obtain precursor and roasting the precursor at 550-850deg.c to obtain the mesoporous composite Ba-Al oxide. The present invention has relatively cheap aluminum source, and the prepared mesoporous composite Ba-Al oxide has high heat stability, specific surface area 180-240 sq m/g, mesopores of 4-12 nm size in 80 % and NOx storing capacity of 280-320 micromol/g.
Description
Technical field
The present invention relates to a kind of preparation method of even mesoporous Ba-Al oxide of high-specific surface area.The technology of preparing that belongs to mesoporous material.
Background technology
Ba-Al oxide has better heat-resisting stability and alkaline, can be used as the sorbing material of sour gas, in the purifying vehicle exhaust field potential using value is arranged.But during common immersion process for preparing, the precursor compound of barium is to the obstruction in duct, makes that little (specific surface area is lower than 150m after 600 ℃ of roastings for the sample specific surface area of preparation
2/ g), the dispersity of barium compound is not high, and is lower to the absorption storage power of oxynitride, generally is lower than 240 μ mol/g.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of mesoprous composite Ba-Al oxide with great specific surface area, this method adopts cheap relatively aluminum isopropylate as the aluminium source, and the sample specific surface area that makes is bigger, and the aperture is even.
The present invention is realized by following technical proposals, a kind of preparation method of mesoprous composite Ba-Al oxide with great specific surface area, and its feature comprises following process:
1). with aluminum isopropylate (AIP), triblock copolymer polytrimethylene ether-poly-propyl ether-polytrimethylene ether (EO
20PO
70EO
20, P123), nitrate of baryta (Ba (NO
3)
2) be raw material, Ba in molar ratio: P123: Al=(6~17): place deionized water mix raw material at 2: 100, under the violent stirring, in 55~70 ℃ of hydrolysis 6 hours, synthetic presoma;
2). after presoma reduced to 20~25 ℃, drip sal volatile, make to generate BaCO fully
3Till, continue to stir 2 hours;
3). presoma leaves standstill more than 48 hours at 20~25 ℃, after the filtration, in 20~25 ℃ of dryings 2~3 days, in 550~850 ℃ of roasting temperatures 4~6 hours, obtains mesoporous Ba-Al oxide again.
The invention has the advantages that: adopting cheap relatively aluminum isopropylate as the aluminium source, is structure directing agent with triblock copolymer P123, and the mesoporous Ba-Al-O composite oxides heat-resistant stability of preparation is good, and specific surface area is 180~240m
2/ g, 80% mesoporous aperture is 4~12nm, is 280~320 μ mol/g to the storage capacity of nitrogen oxide NOx.
Embodiment
Embodiment one
Add 5.8g P123,10.2g AIP, 1.09g Ba (NO in the there-necked flask
3)
2And 90mL H
2O stirs and is warming up to 60 ℃, continues to stir 6 hours so that the AIP hydrolysis; Slowly drip 2.1mL2M (NH when reducing to 20 ℃
4)
2CO
3Solution, and continue to stir 2 hours; Presoma left standstill 48 hours in 20 ℃, filtered the back in 20 ℃ of dryings 2 days, 600 ℃ of following roastings 4 hours.
The Ba-Al-O composite oxides specific surface area 236.4m that makes
2/ g, 80% pore distribution is in 4.5~9nm scope, and the most probable aperture is 6.2nm.At 400ppm NO, 5%O
2(volume ratio), N
2Under the EQUILIBRIUM CONDITION, be 320 μ mol/g to the storage capacity of NO.
Embodiment two
Add 5.8g P123,10.2g AIP, 0.81g Ba (NO in the there-necked flask
3)
2And 90mL H
2O stirs and is warming up to 65 ℃, continues to stir 6 hours so that the AIP hydrolysis; Slowly drip 1.6mL 2M (NH when reducing to 20 ℃
4)
2CO
3, and continue to stir 2 hours; Presoma left standstill 48 hours in 20 ℃, filtered the back in 20 ℃ of dryings 2 days, 700 ℃ of following roastings 4 hours.
The Ba-Al-O composite oxides specific surface area 203.7m that makes
2/ g, 80% pore distribution is in 4.5~9nm scope, and the most probable aperture is 6.2nm.At 400ppm NO, 5% O
2(volume ratio), N
2Under the EQUILIBRIUM CONDITION, be 301 μ mol/g to the storage capacity of NO.
Embodiment three
Add 5.8g P123,10.2g AIP, 1.635g Ba (NO in the there-necked flask
3)
2And 90mL H
2O stirs and is warming up to 70 ℃, continues to stir 6 hours so that the AIP hydrolysis; Slowly drip 3.15mL 2M (NH when reducing to 20 ℃
4)
2CO
3, and continue to stir 2 hours; Presoma left standstill 48 hours in 20 ℃, filtered the back in 20 ℃ of dryings 2 days, 800 ℃ of following roastings 4 hours.
The Ba-Al-O composite oxides specific surface area 181.7m that makes
2/ g, 80% pore distribution is in 4.4~12nm scope, and the most probable aperture is 7.5nm.At 400ppm NO, 5% O
2(volume ratio), N
2Under the EQUILIBRIUM CONDITION, be 285 μ mol/g to the storage capacity of NO.
Claims (1)
1. the preparation method of a mesoprous composite Ba-Al oxide with great specific surface area, its feature comprises following process:
1). with aluminum isopropylate and nitrate of baryta is raw material, and triblock copolymer polytrimethylene ether-poly-propyl ether-polytrimethylene ether is a structure directing agent, and wherein the monomeric unit number of polytrimethylene ether-poly-propyl ether-polytrimethylene ether is EO
20PO
70EO
20, by the mol ratio (6~17) between barium, triblock copolymer polytrimethylene ether-poly-propyl ether-polytrimethylene ether and the aluminium: prepare burden at 2: 100, in deionized water, raw material mixed, under the violent stirring in 55~70 ℃ of hydrolysis 6 hours, synthetic presoma;
2). after presoma is cooled to 20~25 ℃, drip sal volatile, make to generate BaCO fully
3Till, continue again to stir 2 hours;
3). presoma leaves standstill more than 48 hours at 20~25 ℃, after the filtration, in 20~25 ℃ of dryings 2~3 days, in 550~850 ℃ of roasting temperatures 4~6 hours, obtains mesoporous Ba-Al oxide again.
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CNB2006101305002A CN100445208C (en) | 2006-12-21 | 2006-12-21 | Preparing process of mesoprous composite Ba-Al oxide with great specific surface area |
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CNB2006101305002A CN100445208C (en) | 2006-12-21 | 2006-12-21 | Preparing process of mesoprous composite Ba-Al oxide with great specific surface area |
Publications (2)
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CN1986416A CN1986416A (en) | 2007-06-27 |
CN100445208C true CN100445208C (en) | 2008-12-24 |
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CN106032284B (en) * | 2015-03-09 | 2017-06-30 | 中国科学院大连化学物理研究所 | A kind of preparation method that temperature hexa-aluminate is formed with low phase |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6454967B1 (en) * | 1999-11-04 | 2002-09-24 | Samsung Sdi Co., Ltd. | Green-emitting phosphors for plasma display panel and preparing method thereof |
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6454967B1 (en) * | 1999-11-04 | 2002-09-24 | Samsung Sdi Co., Ltd. | Green-emitting phosphors for plasma display panel and preparing method thereof |
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