CN101597077B - Method for synthesizing mesoporous alumina - Google Patents
Method for synthesizing mesoporous alumina Download PDFInfo
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- CN101597077B CN101597077B CN2009100696712A CN200910069671A CN101597077B CN 101597077 B CN101597077 B CN 101597077B CN 2009100696712 A CN2009100696712 A CN 2009100696712A CN 200910069671 A CN200910069671 A CN 200910069671A CN 101597077 B CN101597077 B CN 101597077B
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Abstract
The invention provides a preparation method of mesoporous alumina. The preparation method comprises the following steps of: adopting an amino acid type surfactant as a template agent, taking sodium metaaluminate as an aluminum source, using hydrochloric acid to regulate pH, adopting a sol-gel method to synthesize a precursor of the mesoporous alumina and carrying out heat treatment to obtain the mesoporous alumina. The method has simple technology and safe operation. The specific surface area of the prepared mesoporous alumina is 268 to 310m<2>/g, the pore volume is 0.45 to 0.51cm<3>/g, the pore size distribution is narrow, and the invention has important application value in the processes of adsorption and catalysis.
Description
Technical field
The invention relates to a kind of preparation method of meso-porous alumina, more precisely about using amino acid type surfactant to prepare the method for meso-porous alumina.
Background technology
1992, U.S. Mobil company used the self-assembly of nanometer synthetic technology to synthesize novel mesopore molecular sieve MCM-41 first, indicated that the research to porous material has got into new epoch.The study on the synthesis of mesoporous material receives much concern in the world in recent years.Meso-porous alumina is that a kind of specific surface area is big, the aperture between 2-50nm, pore size distribution is narrow and the duct is big or small, the novel nano structured material of shape certain ordered.Meso-porous alumina is as a kind of important mesoporous material; Have good adsorption performance, surface acidity and thermostability; Can be used as sorbent material, catalyzer and carrier and be applied in many chemical processes, its preparation, structure and The Characteristic Study have become international focus.
The method that the borolon mesoporous material is commonly used at present is to be template with the tensio-active agent; Utilize physical and chemical processes such as sol-gel, deposition, emulsification or microemulsified; Generate ordered mesoporous material through the interface interaction self-assembly between organism and the inorganics, employed template has cats product, AS, nonionogenic tenside.
People such as Saul Cabrera have adopted the synthesising mesoporous aluminum oxide of cats product CTAB, and the mole through changing Al/ water/trolamine is adjustment aperture recently, and the synthetic sample has adjustable aperture 3.3-6.1nm and the BET surface-area is approximately 250-350m
2/ g.
People such as Bagshaw SA adopt the synthesising mesoporous method of alumina of a kind of neutrality, and as template, alfol is the aluminium source with electroneutral polyoxy ethane tensio-active agent, and the synthetic mesopore orbit is vermiform, and specific surface area reaches 500m
2/ g, its deficiency is that the alkoxide of aluminium costs an arm and a leg.
The AS that synthesising mesoporous aluminum oxide is commonly used has sodium lauryl sulphate, X 2073 etc.It is the preparation that template is carried out meso-porous alumina that people such as Soraya Handjani have adopted sodium lauryl sulphate, and has studied the influence of the use of different templates agent to the meso-porous alumina pattern, and the meso-porous alumina specific surface area that makes is up to 355m
2/ g, pore volume are 0.33m
3/ g.
The invention provides a kind of new nonionic surfactant sodium lauroyl glutamate and carry out the preparation of meso-porous alumina, sodium lauroyl glutamate is a kind of amino acid type surfactant, and its degraded is safety quick, is a kind of environmentally friendly tensio-active agent.It is the aluminium source that present method adopts inexpensive inorganic salt, and process operation is simple, and the specific surface area of prepared meso-porous alumina is up to 310m
2/ g, pore volume 0.51cm
3/ g, pore size distribution is narrow, in absorption and catalytic process, has significant application value.
Summary of the invention
Deficiency to existing synthesising mesoporous aluminum oxide method the object of the present invention is to provide a kind of amino acid type surfactant to prepare the method for meso-porous alumina.
The present invention is based on nanostructure self-assembly mechanism, adopt sol-gel method to prepare meso-porous alumina.Adopting the amino acid type surfactant sodium lauroyl glutamate is template, is the aluminium source with the sodium metaaluminate.
Preparation process is: take by weighing certain amount of surfactant and inorganic aluminate according to stoichiometric relation, at a certain temperature the surfactant-dispersed that takes by weighing is formed micella in deionized water, slowly add inorganic aluminate, stir half a hour.Dropwise drip the analytical pure hydrochloric acid conditioning solution to certain pH, aging certain hour, crystallization certain hour at a certain temperature, filtration washing, oven dry at a certain temperature, roasting.
It is mesoporous material that maller angle XRD diffraction characterizes proof synthetic aluminum oxide, and the BET specific surface area reaches 268-310m
2/ g, pore volume 0.45-0.51cm
3/ g, pore size distribution is narrow, in absorption and catalytic process, has significant application value.
Description of drawings
Fig. 1 a is the maller angle XRD diffractogram according to the meso-porous alumina sample of embodiment one preparation;
Fig. 1 b is the maller angle XRD diffractogram according to the meso-porous alumina sample of embodiment two preparations;
Fig. 2 a is the N according to the meso-porous alumina sample of embodiment one preparation
2The adsorption-desorption thermo-isopleth;
Fig. 2 b is the N according to the meso-porous alumina sample of embodiment two preparations
2The adsorption-desorption thermo-isopleth;
Fig. 3 a is the pore size distribution curve figure according to the meso-porous alumina sample of embodiment one preparation;
Fig. 3 b is the pore size distribution curve figure according to the meso-porous alumina sample of embodiment two preparations
Embodiment
Embodiment one
At 35 ℃ the 11.64g sodium lauroyl glutamate is scattered in the 120mL deionized water and forms micella, slowly add the 2.8g sodium metaaluminate, stir and make it abundant dissolving, Al in the solution half a hour
3+Volumetric molar concentration be 0.24mol/L.Dropwise drip analytical pure hydrochloric acid conditioning solution pH to 7, under this temperature, wore out 5 hours.Colloidal sol is placed crystallizing kettle crystallization 16 hours under 100 ℃ of temperature.With the product filtering and washing, 120 ℃ of dryings 5 hours.Place retort furnace in 600 ℃ of roasting 3h the pressed powder that obtains.The pore structure of the meso-porous alumina that obtains: specific surface area: 310m
2/ g, pore volume 0.51cm
3/ g, mean pore size 4.8nm.
Embodiment two
Operate identically with embodiment one, that different is Al in the solution
3+Volumetric molar concentration for for 0.43mol/L.
At 35 ℃ the 11.64g sodium lauroyl glutamate is scattered in the 80mL deionized water and forms micella, slowly add the 2.8g sodium metaaluminate, stir and make it abundant dissolving, Al in the solution half a hour
3+Volumetric molar concentration be 0.43mol/L.Dropwise drip analytical pure hydrochloric acid conditioning solution pH to 7, under this temperature, wore out 5 hours.Colloidal sol is placed crystallizing kettle crystallization 16 hours under 100 ℃ of temperature.With the product filtering and washing, 120 ℃ of dryings 5 hours.Place retort furnace in 600 ℃ of roasting 3h the pressed powder that obtains.The pore structure of the meso-porous alumina that obtains: specific surface area: 268m
2/ g, pore volume 0.45cm
3/ g, mean pore size 3.7nm.
Claims (1)
1. the compound method of a meso-porous alumina is characterized in that may further comprise the steps: the tensio-active agent and the inorganic aluminate that take by weighing an amount of mol ratio and be 1: 1; Under 35 ℃, the surfactant-dispersed that takes by weighing is formed micella in deionized water; Slowly add inorganic aluminate afterwards and stir half a hour; Dropwise dripping analytical pure hydrochloric acid conditioning solution pH value then is 7; Aging place crystallizing kettle 100 ℃ of following crystallization 16 hours colloidal sol after 5 hours; Behind the filtration washing 120 ℃ of down oven dry 5 hours, 600 ℃ of roastings 3 hours; Said tensio-active agent is a sodium lauroyl glutamate; Said inorganic aluminate is a sodium metaaluminate; Al in the said solution
3+Volumetric molar concentration be 0.24～0.43mol/L.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817543B (en) * | 2010-03-03 | 2012-06-13 | 上海交通大学 | Mesoporous alumina preparation method based on cross-linking reaction |
| CN101746793B (en) * | 2010-03-03 | 2011-05-04 | 上海交通大学 | Preparation method for mesoporous hollow alumina particle |
| CN101948150A (en) * | 2010-09-10 | 2011-01-19 | 中国科学院化学研究所 | Method for purifying water |
| CN102424411A (en) * | 2011-09-15 | 2012-04-25 | 暨南大学 | Preparation method for ordered mesoporous gamma-Al2O3 |
| CN103771474B (en) * | 2012-10-24 | 2015-08-12 | 中国石油化工股份有限公司 | A kind of preparation method of alumina dry glue |
| CN103112878A (en) * | 2012-12-28 | 2013-05-22 | 中国神华能源股份有限公司 | Method for preparing aluminum oxide with large specific surface area |
| CN108484006A (en) * | 2018-03-09 | 2018-09-04 | 清华大学 | A kind of preparation method of the multi-stage porous Alumina Foam Ceramics to match in excellence or beauty with aeroge |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101024165A (en) * | 2007-03-26 | 2007-08-29 | 四川泸天化股份有限公司 | Novel gamma aluminium oxide catalyst and producing technology |
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| CN101024165A (en) * | 2007-03-26 | 2007-08-29 | 四川泸天化股份有限公司 | Novel gamma aluminium oxide catalyst and producing technology |
Non-Patent Citations (1)
| Title |
|---|
| 徐如人等.仿生合成无机手性材料.《无机合成与制备化学 下册》.高等教育出版社,2009,453. * |
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Application publication date: 20091209 Assignee: Tianjin Kaimei Technology Co., Ltd. Assignor: Nankai University Contract record no.: 2012120000062 Denomination of invention: Method for synthesizing mesoporous alumina Granted publication date: 20120425 License type: Exclusive License Record date: 20120928 |
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