CN102219243B - Method for preparing mesoporous aluminum oxide - Google Patents
Method for preparing mesoporous aluminum oxide Download PDFInfo
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- CN102219243B CN102219243B CN 201010146880 CN201010146880A CN102219243B CN 102219243 B CN102219243 B CN 102219243B CN 201010146880 CN201010146880 CN 201010146880 CN 201010146880 A CN201010146880 A CN 201010146880A CN 102219243 B CN102219243 B CN 102219243B
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Abstract
The invention relates to a method for preparing mesoporous aluminum oxide, which mainly solves the problems that the preparation cost of mesoporous aluminum oxide is high and the preparation operation is complicated in the prior art. The method adopts the following the technical scheme for better solving the problems: inorganic aluminum salt and glucose are taken as raw materials, inorganic ammonia or inorganic salt is taken as a precipitating agent, and the reaction is conducted under the condition that the pH value is 1-14, and the reacting temperature is 1-100 DEG C so as to obtain the mesoporous aluminum oxide, wherein the mole ratio of the inorganic aluminum salt to the glucose is 0.1-10:1, and the precipitating agent using amount is calculated according to the mole ratio of the inorganic aluminum salt and is 1-50:1 of the mole ratio of the inorganic aluminum salt. The method can be used for the industrial preparation of the mesoporous aluminum oxide.
Description
Technical field
The present invention relates to a kind of preparation method of meso-porous alumina.
Background technology
Aluminum oxide is the most frequently used Industrial Catalysis agent carrier of petrochemical industry, its structural parameter such as specific surface area, pore volume, pore size distribution etc. are closely related with selectivity of catalyst, activity and life-span, the improvement of these physical parameters can improve the active ingredient dispersity, effectively promotes mass transfer process in reaction.And the meso-porous alumina pore size distribution is narrower, and specific surface area is larger, and the different electromotive force in surface makes the easier load of different metal ions.Duct shape and size are adjustable, have improved the quality mass transfer, have overcome diffusional resistance, avoid simultaneously unnecessary hole plug phenomenon to occur.Simultaneously, meso-porous alumina also has fabulous application potential as shape-selective catalyst, molecular sieve and selective adsorption or biochemical technology field aspect molecular recognition.
The present preparation method of meso-porous alumina mainly contains exsiccated ammonium alum method, activated aluminum powder hydrolysis method, organometallic compound hydrolysis method, sol-gel method etc., and these methods respectively have relative merits.The exsiccated ammonium alum method is generally take Tai-Ace S 150 and bicarbonate of ammonia as raw material, and by adding other compounds, such as polyoxyethylene glycol, polysorbate60 etc. obtains the Al in certain specific surface area and aperture
2O
3Material, this process raw materials used more, process is complicated; Activated aluminum powder method and exsiccated ammonium alum method are similar, need more step just can obtain Al
2O
3Material; The raw materials used costliness of organometallic compound hydrolysis method is difficult to large-scale application; The sol-gel fado adopts neutrality, positively charged ion or anion surfactant to do template, just can obtain Al through a series of processes
2O
3Material, although this process required equipment is simple, processing requirement is strict, the experimental result poor repeatability.
Find that through the literature search to prior art a large amount of synthetic Al is arranged at present
2O
3The bibliographical information of material.BenjingXu (Xu Benjing) is at " Microporous and Mesoporous Materials " (micropore and mesoporous material) 2006, 91, " Synthesis of mesoporous alumina with highly thermal stability using glucosetemplate in aqueous system " (the utilizing glucose to do the meso-porous alumina that template prepares high thermal stability in liquid phase) of delivering on 293-295, mention in this article and add appropriate glucose in aluminum isopropylate, make aluminum isopropylate: glucose: the water mol ratio is 1: 1: 75, then dropwise add dilute nitric acid solution to regulate the pH value, the alumina material in preparation certain specific surface area and aperture.Be the aluminium source owing to adopting organic aluminium salt in the document, exist synthetic cost high, in addition the problem of preparation manipulation complexity.
Summary of the invention
Technical problem to be solved by this invention is to have in prior art that synthetic cost is high, the problem of complicated operation, and a kind of new mesoporous alumina preparation method is provided.The method has low, the simple to operate advantage of meso-porous alumina preparation cost.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of preparation method of meso-porous alumina, take inorganic aluminate and glucose as raw material, take inorganic ammonia or inorganic ammonium salt as precipitation agent, be made into mixing solutions, be 1～14 in the pH value, temperature of reaction is to react under 1～100 ℃ of condition, reaction product obtains meso-porous alumina through filtration, drying and 300～700 ℃ of roastings, wherein the mol ratio of inorganic aluminate and glucose is 0.1～10: 1, the precipitation agent consumption take the inorganic aluminate molar ratio computing as the inorganic aluminate mol ratio 1～50: 1.
In technique scheme, the inorganic aluminate preferred version is selected from least a in aluminum nitrate, aluminum chloride or Tai-Ace S 150, the mol ratio preferable range of inorganic aluminate and glucose is 1～5: 1, precipitation agent and inorganic aluminate, take inorganic aluminate molar ratio computing preferable range as 5～20: 1, the pH value of solution preferable range is 5～12, and the temperature of reaction preferable range is 20～50 ℃, and precipitation agent is selected from ammonia soln, volatile salt or ammonium bicarbonate soln.
The present invention in preparation meso-porous alumina process, is raw material owing to adopting inorganic aluminate cheap, that be easy to get, greatly reduces preparation cost, adopts in addition precipitator method technique to prepare meso-porous alumina, makes processing step few, and the reaction times is short, and is simple to operate.Adopting the meso-porous alumina specific surface area that method of the present invention prepares is 150～400 meters
2/ gram, pore volume are 0.1～0.5 centimetre
3/ gram, pore size distribution is 3.5～8 nanometers, has obtained technique effect preferably.
The present invention is further elaborated below by embodiment.
Embodiment
[embodiment 1]
Took 7.5026 gram nine water aluminum nitrates and 3.9634 gram glucose in 1: 1 in molar ratio, pack in 500 ml beakers, then add 100 ml deionized water, stir under 20 ℃ and fully dissolved in 30 minutes, drip 2.5% ammonia soln, regulator solution pH=9 continues to stir after 1 hour, washing, suction filtration.
After draining, take out sample and put into air dry oven, regulating temperature is 100 ℃, is incubated 6 hours, the dry rear dry thing that takes out.Sample after drying is inserted in retort furnace with temperature control 500 ℃ of roastings 4 hours, the alumina material that cooling taking-up obtains preparing.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 264 meters
2/ gram, pore volume are 0.36 centimetre
3/ gram, mean pore size are 5.4 nanometers.
[embodiment 2]
Took 7.5026 gram nine water aluminum nitrates and 1.9817 gram glucose in 2: 1 in molar ratio, pack in 500 ml beakers, then add 100 ml deionized water, stir under 20 ℃ and fully dissolved in 30 minutes, drip 2.5% ammonia soln, regulator solution pH=9 continues to stir after 1 hour, washing, suction filtration.
After draining, take out sample and put into air dry oven, regulating temperature is 100 ℃, is incubated 6 hours, the dry rear dry thing that takes out.Sample after drying is inserted in retort furnace with temperature control 500 ℃ of roastings 4 hours, the alumina material that cooling taking-up obtains preparing.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 246 meters
2/ gram, pore volume are 0.36 centimetre
3/ gram, mean pore size are 5.8 nanometers.
[embodiment 3]
Took 7.5035 gram nine water aluminum nitrates and 0.7927 gram glucose in 5: 1 in molar ratio, pack in 500 ml beakers, then add 100 ml deionized water, stir under 20 ℃ and fully dissolved in 30 minutes, drip 2.5% ammonia soln, regulator solution pH=9 continues to stir after 1 hour, washing, suction filtration.
After draining, take out sample and put into air dry oven, regulating temperature is 100 ℃, is incubated 6 hours, the dry rear dry thing that takes out.Sample after drying is inserted in retort furnace with temperature control 500 ℃ of roastings 4 hours, the alumina material that cooling taking-up obtains preparing.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 223 meters
2/ gram, pore volume are 0.40 centimetre
3/ gram, mean pore size are 7.1 nanometers.
[embodiment 4]
Took 7.5026 gram nine water aluminum nitrates and 1.9817 gram glucose in 2: 1 in molar ratio, pack in 500 ml beakers, then add 100 ml deionized water, stir under 20 ℃ and fully dissolved in 30 minutes, drip 2.5% ammonia soln, regulator solution pH=5 continues to stir after 1 hour, washing, suction filtration.
After draining, take out sample and put into air dry oven, regulating temperature is 100 ℃, is incubated 6 hours, the dry rear dry thing that takes out.Sample after drying is inserted in retort furnace with temperature control 500 ℃ of roastings 4 hours, the alumina material that cooling taking-up obtains preparing.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 177 meters
2/ gram, pore volume are 0.15 centimetre
3/ gram, mean pore size are 3.5 nanometers.
[embodiment 5]
Took 7.5026 gram nine water aluminum nitrates and 1.9817 gram glucose in 2: 1 in molar ratio, pack in 500 ml beakers, then add 100 ml deionized water, stir under 20 ℃ and fully dissolved in 30 minutes, drip 2.5% ammonia soln, regulator solution pH=12 continues to stir after 1 hour, washing, suction filtration.
After draining, take out sample and put into air dry oven, regulating temperature is 100 ℃, is incubated 6 hours, the dry rear dry thing that takes out.Sample after drying is inserted in retort furnace with temperature control 500 ℃ of roastings 4 hours, the alumina material that cooling taking-up obtains preparing.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 267 meters
2/ gram, pore volume are 0.42 centimetre
3/ gram, mean pore size are 6.4 nanometers.
[embodiment 6]
Took 7.5026 gram nine water aluminum nitrates and 1.9817 gram glucose in 2: 1 in molar ratio, pack in 500 ml beakers, then add 100 ml deionized water, stir under 20 ℃ and fully dissolved in 30 minutes, drip 2.5% ammonia soln, regulator solution pH=9 continues to stir after 1 hour, washing, suction filtration.
After draining, take out sample and put into air dry oven, regulating temperature is 100 ℃, is incubated 6 hours, the dry rear dry thing that takes out.Sample after drying is inserted in retort furnace with temperature control 300 ℃ of roastings 4 hours, the alumina material that cooling taking-up obtains preparing.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 262 meters
2/ gram, pore volume are 0.32 centimetre
3/ gram, mean pore size are 3.5 nanometers.
[embodiment 7]
Took 7.5026 gram nine water aluminum nitrates and 1.9817 gram glucose in 2: 1 in molar ratio, pack in 500 ml beakers, then add 100 ml deionized water, stir under 20 ℃ and fully dissolved in 30 minutes, drip 2.5% ammonia soln, regulator solution pH=9 continues to stir after 1 hour, washing, suction filtration.
After draining, take out sample and put into air dry oven, regulating temperature is 100 ℃, is incubated 6 hours, the dry rear dry thing that takes out.Sample after drying is inserted in retort furnace with temperature control 700 ℃ of roastings 4 hours, the alumina material that cooling taking-up obtains preparing.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 171 meters
2/ gram, pore volume are 0.34 centimetre
3/ gram, mean pore size are 7.9 nanometers.
[embodiment 8]
Took 7.5026 gram nine water aluminum nitrates and 1.9817 gram glucose in 2: 1 in molar ratio, pack in 500 ml beakers, then add 100 ml deionized water, stir under 50 ℃ and fully dissolved in 30 minutes, drip 2.5% ammonia soln, regulator solution pH=9 continues to stir after 1 hour, washing, suction filtration.
After draining, take out sample and put into air dry oven, regulating temperature is 100 ℃, is incubated 6 hours, the dry rear dry thing that takes out.Sample after drying is inserted in retort furnace with temperature control 500 ℃ of roastings 4 hours, the alumina material that cooling taking-up obtains preparing.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 271 meters
2/ gram, pore volume are 0.46 centimetre
3/ gram, mean pore size are 5.9 nanometers.
[embodiment 9]
Took 7.5026 gram nine water aluminum nitrates and 1.9817 gram glucose in 2: 1 in molar ratio, pack in 500 ml beakers, then add 100 ml deionized water, stir under 20 ℃ and fully dissolved in 30 minutes, drip 2.5% ammonium bicarbonate soln, regulator solution pH=9 continues to stir after 1 hour, washing, suction filtration.
After draining, take out sample and put into air dry oven, regulating temperature is 100 ℃, is incubated 6 hours, the dry rear dry thing that takes out.Sample after drying is inserted in retort furnace with temperature control 500 ℃ of roastings 4 hours, the alumina material that cooling taking-up obtains preparing.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 268 meters
2/ gram, pore volume are 0.38 centimetre
3/ gram, mean pore size are 6.2 nanometers.
[embodiment 10]
Take 5.22 gram aluminum chloride and 1.9817 gram glucose in 2: 1 in molar ratio, in 500 ml beakers of packing into, then add 100 ml deionized water, stir under 20 ℃ and fully dissolved in 30 minutes, drip 2.5% ammonia soln, regulator solution pH=9, continue to stir after 1 hour washing, suction filtration.
After draining, take out sample and put into air dry oven, regulating temperature is 100 ℃, is incubated 6 hours, the dry rear dry thing that takes out.Sample after drying is inserted in retort furnace with temperature control 500 ℃ of roastings 4 hours, the alumina material that cooling taking-up obtains preparing.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 265 meters
2/ gram, pore volume are 0.41 centimetre
3/ gram, mean pore size are 6.2 nanometers.
[embodiment 11]
Take 6.0 gram Tai-Ace S 150 and 1.9817 gram glucose in 2: 1 in molar ratio, in 500 ml beakers of packing into, then add 100 ml deionized water, stir under 20 ℃ and fully dissolved in 30 minutes, drip 2.5% ammonia soln, regulator solution pH=9, continue to stir after 1 hour washing, suction filtration.
After draining, take out sample and put into air dry oven, regulating temperature is 100 ℃, is incubated 6 hours, the dry rear dry thing that takes out.Sample after drying is inserted in retort furnace with temperature control 500 ℃ of roastings 4 hours, the alumina material that cooling taking-up obtains preparing.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 259 meters
2/ gram, pore volume are 0.33 centimetre
3/ gram, mean pore size are 6.6 nanometers.
Claims (1)
1. the preparation method of a meso-porous alumina, take 6.0 gram Tai-Ace S 150 and 1.9817 gram glucose, pack in 500 ml beakers, then add 100 ml deionized water, stir under 20 ℃ and fully dissolved in 30 minutes, drip 2.5% ammonia soln, regulator solution pH=9, continue to stir after 1 hour washing, suction filtration; After draining, take out sample and put into air dry oven, regulating temperature is 100 ℃, is incubated 6 hours, the dry rear dry thing that takes out; Sample after drying is inserted in retort furnace with temperature control 500 ℃ of roastings 4 hours, the alumina material that cooling taking-up obtains preparing; Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 259 meters
2/ gram, pore volume are 0.33 centimetre
3/ gram, mean pore size are 6.6 nanometers.
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| CN102616820B (en) * | 2012-04-24 | 2013-12-25 | 上海大学 | Method for preparing mesoporous gamma-Al2O3 nano material with high specific surface area at low temperature |
| CN104528646A (en) * | 2014-11-05 | 2015-04-22 | 朱忠良 | Natural gas primary reforming insulation cryogenic reaction process in synthetic ammonia industry |
| CN106186013B (en) * | 2016-07-25 | 2017-07-21 | 福建师范大学泉港石化研究院 | A kind of method that use rheological phase reaction method synthesizes flower ball-shaped meso-porous alumina |
| CN108840718B (en) * | 2018-08-29 | 2020-11-06 | 郑州孚莱孚特性材料有限公司 | Preparation method of alumina foamed ceramic |
| CN112779050A (en) * | 2019-11-11 | 2021-05-11 | 中国石油天然气股份有限公司 | Processing method of poor-quality catalytic diesel oil |
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Non-Patent Citations (2)
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| 杨泠 等.介孔氧化铝的制备及应用.《化学进展》.2010,第22卷(第1期),32-43. * |
| 许本静.糖类模板下介孔氧化铝的合成、表征及其催化应用研究.《中国博士学位论文全文数据库工程科技Ⅰ辑》.2008,(第3期),37、42-45、90-95. * |
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