CN1202010C - Aluminium oxide maintaining high specific surface area under high temperature and its preparing method - Google Patents
Aluminium oxide maintaining high specific surface area under high temperature and its preparing method Download PDFInfo
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- CN1202010C CN1202010C CN 01128872 CN01128872A CN1202010C CN 1202010 C CN1202010 C CN 1202010C CN 01128872 CN01128872 CN 01128872 CN 01128872 A CN01128872 A CN 01128872A CN 1202010 C CN1202010 C CN 1202010C
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- specific surface
- surface area
- high temperature
- temperature
- additive
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Abstract
The present invention relates to novel Al2O3 material maintaining high specific surface area at high temperature and a preparation method thereof. The Al2O3 material is prepared with a sol-gel method under the existence of at least one kind of additive such as rare earth, metal or non-metal oxide. The present invention has the advantages that the Al2O3 material with high specific surface area can maintain the specific surface area over 100m<2>/g for a long time at the temperature of 1000 to 1200 DEG C.
Description
The present invention relates to aluminum oxide and preparation method thereof, especially can at high temperature keep the Al of high-ratio surface
2O
3Material and preparation method thereof.
In recent years, several key areas keep the material of high-ratio surface to propose requirement down to high temperature.This several fields is: (1) catalyticcombustion, and need be at the material that keeps high-ratio surface more than 1000 ℃; (2) some Industrial Catalysis processes, as Sweet natural gas steam reformation preparing synthetic gas, the support of the catalyst of use is specific surface≤10m
2α-Al of/g
2O
3, if keep the material of high-ratio surface to replace down with high temperature, catalyst performance will greatly take on a new look; (3) purifying vehicle exhaust though cleaning catalyst for tail gases of automobiles comes into operation, in use causes catalyst activity to reduce being still open question because of the specific surface of carrier at high temperature descends.And existing high-ratio surface material is (as γ-Al
2O
3, η-Al
2O
3Deng) can not bear high temperature, and resistant to elevated temperatures material such as α-Al
2O
3Do not have high specific surface again.So keep the material of high-ratio surface to carry out a large amount of research down to high temperature abroad in recent years.Mainly be to utilize additive that high specific surface aluminium is carried out surface modification, improving the ability that it at high temperature keeps high-ratio surface, but still be in conceptual phase.
(J.Catalyst, 114, the 112-120 (1998)) such as F.oudet of France La (NO
3)
3The dipping boehmite after 1150 ℃ the calcining 12 hours, specific surface is 63m
2/ g.
(J.Mater.Sci., 26, the 6479-6486 (1991)) such as I.M.Tijburg of Holland 3.5wt%La (NO
3)
3Dipping boehmite or γ-Al
2O
3After, 1050 ℃ of calcinings 145 hours, specific surface energy kept 80m
2/ g; Use [La (EDTA)] (La content is 0.5%) dipping back instead 1050 ℃ of calcinings after 145 hours, specific surface also has 90m
2/ g.
Japanese Patent (JP03088713) has been introduced alumina surface dipping alkaline earth salt after 1000 ℃ of calcinings, and specific surface keeps 100m
2/ g.
European patent (EP222471) has been introduced alumina surface dipping Ba salt 1450 ℃ of calcinings after 50 hours, and specific surface also has 10m
2/ g.
French Patent (FP2596397) was introduced behind the alumina surface dipping rare earth metal salt 1150 ℃ of calcinings after 12 hours, and specific surface remains on 50 ~ 60m
2/ g.
The invention provides a kind of alumina material that at high temperature keeps high-ratio surface, the present invention also provides the preparation method who keeps the alumina material of high-ratio surface under this high temperature.
The aluminum oxide that at high temperature keeps high-ratio surface provided by the present invention be by aluminum salt solution in the presence of additive and pore-forming material with sol-gel method preparation altogether, technology is as follows:
Mixing → dissolving → precipitation → filtration → washing → drying → calcining → product
With aluminium salt and additive and pore-forming material, be dissolved in water, in 45-60 ℃ and certain pH value (6-9) scope and add the precipitation agent reaction under the vigorous stirring, make gel, subsequently at room temperature with gel-filtration, washing, 130 ℃ of dryings down, roasting at last and getting.Additive is selected from oxide compound a kind of of La, Ce, Sm, Ca, Ba and Si element at least, and consumption is 0.5-10mol%; Pore-forming material is selected from a kind of in polyvinyl alcohol, polyoxyethylene glycol, polyacrylamide and the methylcellulose gum, and its consumption is the 0-40mol% of total amount of material.
Alumina material prepared in accordance with the present invention has advantages such as being convenient to batch process and high-ratio surface.At high temperature, promptly still keep its specific surface at 100m under 1100 ℃ one 1200 ℃
2More than/the g.
Embodiment 1
(1) by lanthanum: aluminium=1: 9 (molar percentage) takes by weighing lanthanum nitrate respectively and aluminum nitrate is soluble in water.Add again after waiting to have dissolved and contain 40% (weight) polyvinyl alcohol solution, mix the back in heating in water bath constant temperature under 55 ℃, react with volume ratio weak ammonia dropping in 2: 1, and high-speed stirring constantly, pH=8.6 to reaction system stops dropping ammonia, and the aluminum ion in the solution generates aluminum hydroxide gel fully at this moment.Filter then, wash, dry xerogel.
(2) xerogel bubbling air in tube furnace is decomposed down at 350 ℃; Under 500 ℃, make Al (OH)
3Decompose.
(3) be placed on the product compressing tablet in the high temperature process furnances and feed N
2(g) or dry air; Get product after 32 hours in calcining under 1100 ℃.
(4) calcining back product is the δ phase through XRD analysis, and recording specific surface through surface analyzer is 102.7m
2/ g
Embodiment 2
(1) by lanthanum: barium: aluminium=1: 2: 97 (molar percentage) takes by weighing lanthanum nitrate, nitrate of baryta, aluminum nitrate respectively and is dissolved in the water that contains polyvinyl alcohol 20% (weight), after waiting to have dissolved, heated constant temperature in water-bath, 55 ℃ of temperature, react with slow dropping of 2: 1 weak ammonia of volume ratio, and with the continuous high-speed stirring of electric mixer, stop when dripping weak ammonia to the pH=8.6 of reaction system, all generate Al (OH) this moment
3Gel.Be transferred in the funnel then and filter, wash, the dry then xerogel that gets.
(2) with embodiment 1 they (2)
(3) with embodiment 1 they (3)
(4) product records thing mutually for the δ phase through XRD.Recording specific surface through surface analyzer is 101.8m
2/ g.
Claims (3)
1, a kind of Al
2O
3Material has the ability that keeps high-ratio surface during high-temperature calcination, it is characterized in that described Al
2O
3When material was calcined in 1100-1200 ℃ temperature range, the specific surface of material remained on 100m
2More than/the g.
2, Al according to claim 1
2O
3Preparation methods, it is characterized in that finishing according to the following steps: with aluminium salt with after additive and pore-forming material mix, be dissolved in water, under 45 ℃ of-60 ℃ of temperature, pH value 6-9 and agitation conditions, add precipitation agent and make gel, at room temperature with gel-filtration, washing, drying, make finished product 500 ℃ of following roastings, wherein additive is selected from a kind of in the oxide compound of La, Ce, Sm, Ca, Ba and Si element at least, and consumption is Al
2O
3The 0.5-10mol% of total amount of material; Pore-forming material is selected from a kind of in polyvinyl alcohol, polyoxyethylene glycol, polyacrylamide and the methylcellulose gum, and consumption is the 0-40mol% of total amount of material.
3, Al according to claim 2
2O
3Preparation methods is characterized in that precipitation agent is a weak ammonia.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01128872 CN1202010C (en) | 2001-09-19 | 2001-09-19 | Aluminium oxide maintaining high specific surface area under high temperature and its preparing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01128872 CN1202010C (en) | 2001-09-19 | 2001-09-19 | Aluminium oxide maintaining high specific surface area under high temperature and its preparing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1408645A CN1408645A (en) | 2003-04-09 |
| CN1202010C true CN1202010C (en) | 2005-05-18 |
Family
ID=4668685
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 01128872 Expired - Fee Related CN1202010C (en) | 2001-09-19 | 2001-09-19 | Aluminium oxide maintaining high specific surface area under high temperature and its preparing method |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103159249A (en) * | 2011-12-08 | 2013-06-19 | 沈阳工业大学 | [La(EDTA)]<->-containing solid synthesis method |
| CN102701246B (en) * | 2012-05-08 | 2016-06-15 | 赣州博晶科技有限公司 | A kind of preparation method of the rare earth modified aluminium oxide of high heat stability |
| CN102964118A (en) * | 2012-11-07 | 2013-03-13 | 浙江通达磁业有限公司 | Manganese and zinc series ferrite high-frequency material and method for producing same |
| CN103803615B (en) * | 2012-11-08 | 2015-09-30 | 中国石油化工股份有限公司 | A kind of preparation method of alumina dry glue |
| CN102923744A (en) * | 2012-11-20 | 2013-02-13 | 中国海洋石油总公司 | Preparation method for aluminum oxide by direct forming method |
| CN103818939B (en) * | 2014-01-14 | 2016-06-08 | 杜云峰 | Hydrogen peroxide fluid bed special aluminium oxide and production technology |
| CN103818938B (en) * | 2014-02-27 | 2016-05-04 | 昆明铂生金属材料加工有限公司 | A kind of preparation method of high thermal stability modified aluminium oxide supports |
| CN107697936B (en) * | 2017-11-06 | 2019-09-27 | 哈尔滨工程大学 | A kind of synthetic method improving γ phase nano aluminium oxide crystalline quality |
| CN116283251B (en) * | 2023-03-23 | 2024-02-09 | 广东省先进陶瓷材料科技有限公司 | Alumina ceramic and preparation method and application thereof |
-
2001
- 2001-09-19 CN CN 01128872 patent/CN1202010C/en not_active Expired - Fee Related
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| CN1408645A (en) | 2003-04-09 |
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Effective date of registration: 20131210 Address after: 1 Building 5, building 12, 610000 West Avenue, Chengdu hi tech Zone (West District, Sichuan) Patentee after: Sichuan Tianjian Catalytic Combustion Co, Ltd. Address before: 610301 Qingbaijiang District, Sichuan, Chengdu Patentee before: Chuanhua Group Co., Ltd. Patentee before: Sichuan University |
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