CN106145168B - Using the method for the synthesising mesoporous aluminum oxide of supermolecular gel ionic liquid common mode plate - Google Patents
Using the method for the synthesising mesoporous aluminum oxide of supermolecular gel ionic liquid common mode plate Download PDFInfo
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Abstract
The invention discloses a kind of method of the synthesising mesoporous aluminum oxide of use supermolecular gel ionic liquid common mode plate, this method includes procedure below：Using organic silicon source or inorganic silicon source as raw material, organogel or hydrogel are used for master module, ionic liquid is auxiliary template, meso-porous alumina with different pore size, pore volume, specific surface area, different mesoporous order degrees and different-shape, the 8nm of gained aluminum oxide mesoporous pore size 2, the 80nm of doughnut caliber 40, the 400m of specific surface area 200 can be obtained by templated synthesis, high-temperature calcination etc.2/ g, mesoporous unordered or high-sequential.
Description
Technical field
The present invention relates to a kind of method of use supermolecular gel template controlledly synthesis meso-porous alumina, belong to material preparation
Technical field.
Background technology
The present invention relates to a kind of method of use supermolecular gel-ionic liquid common mode plate controlledly synthesis meso-porous alumina,
Belong to technical field of material.
Aluminum oxide is a kind of porous, high dispersive, the amphoteric compound of metamorphosis complexity, with a variety of crystalline phases, is adapted to use
Make catalyst, catalyst carrier, adsorbent etc..But the aluminum oxide aperture wider distribution that generally prepares and duct is unordered.In order to
Reaction needs different from what is separated are met, synthesis has high-specific surface area, pore-size distribution and the regulatable mesoporous oxidation of the degree of order
Aluminium is significant.
Preparing the common experimental method of meso-porous alumina has hard template method and soft template method at present.Hard template method is generally with tool
It is template to have the mesoporous carbon of meso-hole structure, mesopore molecular sieve, silicon source presoma is introduced into the duct of template, then remove hard template
So as to obtain the meso-porous alumina to hard template positive or anti-phase duplication, its major defect is that template is difficult to remove, and step is numerous
Trivial, cost is high.Soft template method, as template, unordered vermiform can be obtained by soft template method generally using surfactant
Duct or even ordered mesoporous pore canals, specific surface area are higher, even aperture distribution, but it has the disadvantage that synthesis condition is not easily-controllable, mesoporous
There is certain difficulty in structure.
Supramolecular Functions gel-low molecule organogel or hydrogel, refer to gelator in suitable organic solvent or
Pass through non-covalent bond interaction self assembly shape between intermolecular hydrogen bonding, pi-pi accumulation, hydrophobic effect or Van der Waals force equimolecular in water
Linear, fibrous or banded structure, then forms three-dimensional net structure, prevents the flowing of organic solvent or hydrone, makes whole
Individual system gelation.The self assembled three-dimensional network structure for the nano-scale that supermolecular gel system has can be provided with high ratio
The reaction interface of surface area, its microstructure such as fiber thickness length, the degree of cross linking, duct shape etc. can be subject to by suitable parameter
Regulation and control.The characteristics of based on its microstructure, supermolecular gel can be used as the preferable template of nano material synthesis.Ionic liquid refers to
The liquid being made up of completely ion, now refers to fused salt when less than 100 DEG C in liquid condition, typically by organic cation and nothing more
Machine anion is constituted.Ionic liquid has the advantages that surface tension is low, stability is high, dissolubility good, meanwhile, ionic liquid also by
Referred to as supermolecule solvent, it can form the hydrogen bond of " extension " in the liquid state, and then it is good, long-range order to be self-assembly of tissue
Nanostructure Network, can be used as nanometer and the template of mesoporous synthesis.Study respectively in supermolecular gel or ionic liquid
Synthesising mesoporous material such as TiO2、ZnO、SiO2、Al2O3, but synthesis is generally unordered mesoporous, and lacks and flexibly have to mesoporous
Effect regulation and control.Being used in conjunction with for two kinds of templates, is expected to further enhance its ability of regulation and control to mesoporous synthesis, so far there is not yet adopting
With supermolecular gel-synthesising mesoporous Al of ionic liquid common mode plate2O3Research report.
The content of the invention
Supermolecular gel-mesoporous oxidation of ionic liquid common mode plate controlledly synthesis is used it is an object of the invention to provide one kind
The method of aluminium.This method process is simple, can realize the flexible modulation to aluminum oxide meso-hole structure, pattern.
The present invention provides a kind of method of use supermolecular gel-synthesising mesoporous aluminum oxide of ionic liquid common mode plate, to have
Machine silicon source or inorganic silicon source are raw material, and it is auxiliary mould for master module, ionic liquid to use the organogel factor or hydrogelator
Plate, to be respectively synthesized different target products, i.e., unordered or ordered mesoporous aluminium oxide, doughnut pencil aluminum oxide, its feature
It is,
When target product is unordered or during ordered mesoporous aluminium oxide, comprise the following steps：
(A1) weigh the organogel factor to be added in organic solvent, be heated to 80 DEG C of -140 DEG C of dissolvings and form transparent molten
Liquid；Or weigh hydrogelator and be added to the water, it is heated to 50 DEG C of -100 DEG C of dissolvings and forms clear solution；
(A2) weigh in the clear solution obtained by silicon source, ionic liquid are added separately to step (A1), cooled down after mixing
Plastic 24h-48h；
(A3) ammoniacal liquor is added dropwise into wet gel made from step (A2) than 0.2-1 by silicon source and the amount of the material of ammoniacal liquor, it is quiet
Put 24h-48h；
(A4) by gel obtained by step (A3) in 40 DEG C -80 DEG C dry 12-72h, and 3h-7h is calcined after 400-900 DEG C,
Unordered or ordered mesoporous aluminium oxide is made；
When target product is doughnut pencil aluminum oxide, comprise the following steps：
(B1) weigh the organogel factor to be added in organic solvent, be heated to 80 DEG C of -140 DEG C of dissolvings and form transparent molten
Liquid；
(B2) using organic solvent of the dialysis in gel obtained by water displacement step (B1), then it is freeze-dried 24h-
Corresponding xerogel is made in 48h；
(B3) silicon source and ionic liquid are added in the ethanol solution containing hydrochloric acid, add citric acid, react 3h-
7h, obtains Alumina gel, and xerogel obtained by step (B2) is immersed in into 3-7h in Alumina gel；
(B4) by the gel after being soaked obtained by step (B3) in 40 DEG C -80 DEG C dry 12-72h, and after 400 DEG C -900 DEG C
3-7h is calcined, doughnut pencil aluminum oxide is made.
The method of use supermolecular gel of the present invention-synthesising mesoporous aluminum oxide of ionic liquid common mode plate, wherein, aluminium
Source is preferably aluminium isopropoxide, aluminum sulfate, aluminum nitrate or sodium metaaluminate.
The method of use supermolecular gel of the present invention-synthesising mesoporous aluminum oxide of ionic liquid common mode plate, wherein, it is excellent
It is to weigh the organogel factor according to 2wt%-8wt% to be added in organic solvent in choosing, step (A1), according to 1wt%-
8wt% weighs hydrogelator and is added to the water；It is to weigh the organogel factor according to 2wt%-8wt% to add in step (B1)
Into organic solvent.
The method of use supermolecular gel of the present invention-synthesising mesoporous aluminum oxide of ionic liquid common mode plate, wherein, step
Suddenly the organogel factor described in (A1) be preferably amino acid derivatives (such as N- bay-Pidolidones-di-n-butyl acid amides),
The hydrogelator is preferably agarose；(B1) the organogel factor described in is preferably amino acid derivatives (such as N- months
Osmanthus-Pidolidone-di-n-butyl acid amides).
The method of use supermolecular gel of the present invention-synthesising mesoporous aluminum oxide of ionic liquid common mode plate, wherein, step
Suddenly (A1), organic solvent described in (B1) are preferably ethanol, acetone or propane diols.
The method of use supermolecular gel of the present invention-synthesising mesoporous aluminum oxide of ionic liquid common mode plate, wherein, step
Suddenly (A2), ionic liquid described in (B3) are preferably glyoxaline ion liquid (carbon-based -3- methylimidazolium chlorides of such as 1- 16).
The method of use supermolecular gel of the present invention-synthesising mesoporous aluminum oxide of ionic liquid common mode plate, wherein, it is excellent
By silicon source in choosing, step (A2): the amount ratio of ionic liquid material weighs silicon source, ionic liquid for 0.4-4 and is added separately to
In clear solution obtained by step (1).
The method of use supermolecular gel of the present invention-synthesising mesoporous aluminum oxide of ionic liquid common mode plate, wherein, it is excellent
Silicon source is pressed in choosing, step (B3): the amount ratio of ionic liquid material is 0.4-4, silicon source:Hydrochloric acid: the amount ratio of lemon acid substance
For 1:0.5-6:0.1-1, silicon source and ionic liquid are added in the ethanol solution containing hydrochloric acid, citric acid is added.
Beneficial effects of the present invention：
Gel-ionic liquid common mode plate is prepared and simply and readily removed, and synthetic method is realized to the mesoporous structure of aluminum oxide
Flexible modulation, is resulted in the mesoporous of different pore size, pore volume, specific surface area, different mesoporous order degrees and different-shape
Aluminum oxide, gained aluminum oxide mesoporous pore size 2-8nm, doughnut caliber 40-80nm, specific surface area 200-400m2/ g, mesoporous nothing
Sequence or high-sequential, can meet aluminum oxide as the different application demand of catalyst, catalyst carrier and adsorbent etc..
Brief description of the drawings
Accompanying drawing 1 is the sample transmission electron microscope that example 1 is obtained；
Accompanying drawing 2 is the sample X-ray diffractogram that example 1 is obtained；
Accompanying drawing 3 is the Sample Scan electron microscope that example 1 is obtained；
Accompanying drawing 4 is the sample transmission electron microscope that example 2 is obtained；
Accompanying drawing 5 is the Sample Scan electron microscope that example 3 is obtained.
Embodiment
Embodiments of the invention are elaborated below：The present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and process, but protection scope of the present invention is not limited to following embodiments, following implementation
The experimental method of unreceipted actual conditions in example, generally according to normal condition.
Silicon source：
In the present invention, silicon source is not particularly limited, usual silicon source can be enumerated as aluminium isopropoxide, aluminum sulfate, nitric acid
Aluminium or sodium metaaluminate.
The organogel factor, the addition of hydrogelator in step (A1)：
In the present invention, the organogel factor, the addition of hydrogelator in step (A1) are not particularly limited, led to
It is to weigh the organogel factor according to 2wt%-8wt% to be added in organic solvent in normal step (A1), according to 1wt%-8wt%
Hydrogelator is weighed to be added to the water；
If be added to according to the organogel factor is weighed less than 2wt% in organic solvent, due to the organogel factor
Addition is too small, causes plastic effect bad；And be added to according to the organogel factor is weighed more than 8wt% in organic solvent,
Because the consumption of the organogel factor is excessive, cause to waste, and the gel formed is excessively fine and close, limits its template action
Play, have no other beneficial effects.
If be added to the water according to hydrogelator is weighed less than 1wt%, because the addition of hydrogelator is too small,
Cause plastic effect bad；And be added to the water according to hydrogelator is weighed more than 8wt%, due to the consumption of hydrogelator
It is excessive, cause to waste, and the gel formed is excessively fine and close, limits the performance of its template action, has no other beneficial effects.
The addition of the organogel factor in step (B1)：
In the present invention, the addition to the organogel factor in step (B1) is not particularly limited, usual step (B1)
In be to weigh the organogel factor according to 2wt%-8wt% to be added in organic solvent；
If be added to according to the organogel factor is weighed less than 2wt% in organic solvent, due to the organogel factor
Addition is too small, causes plastic effect bad；And be added to according to the organogel factor is weighed more than 8wt% in organic solvent,
Because the consumption of the organogel factor is excessive, cause to waste, and the gel formed is excessively fine and close, limits its template action
Play, have no other beneficial effects.
The organogel factor, the species of hydrogelator described in step (A1)：
In the present invention, the organogel factor, the species of hydrogelator described in step (A1) are not particularly limited,
The organogel factor described in usual step (A1) can be amino acid derivatives, such as N- bays-Pidolidone-di-n-butyl
Acid amides, the hydrogelator can be agarose.
The species of the organogel factor in step (B1)：
In the present invention, the species to the organogel factor in step (B1) is not particularly limited, described in usual (B1)
The organogel factor is amino acid derivatives, such as N- bay-Pidolidone-di-n-butyl acid amides.
Organic solvent in step (A1), (B1)：
In the present invention, organic solvent described in step (A1), (B1) is not particularly limited, usual step (A1),
(B1) organic solvent described in is ethanol, acetone or propane diols.
Ionic liquid described in step (A2), (B3)：
In the present invention, ionic liquid described in step (A2), (B3) is not particularly limited, usual step (A2),
(B3) ionic liquid described in is glyoxaline ion liquid.
Silicon source, ionic liquid consumption in step (A2)：
In the present invention, silicon source, ionic liquid consumption in step (A2) are not particularly limited, pressed in usual step (A2)
Silicon source: the amount ratio of ionic liquid material be 0.4-4 weigh silicon source, ionic liquid be added separately to it is transparent obtained by step (1)
In solution；
If by silicon source in step (A2): the amount ratio of ionic liquid material weighs silicon source, ionic liquid less than 0.4 and added respectively
Enter into the clear solution obtained by step (1) in step (A2), because silicon source consumption is too small, cause template action not enough；And
By silicon source: the amount ratio of ionic liquid material be more than 4 weigh silicon source, ionic liquid be added separately to it is transparent obtained by step (1)
In solution, because silicon source consumption is excessive, cause to waste, and excessive silicon source is difficult to be evenly dispersed in gel, has no other
Beneficial effect.
Silicon source, ionic liquid consumption in step (B3)：
In the present invention, silicon source, ionic liquid consumption in step (B3) are not particularly limited, pressed in usual step (B3)
Silicon source: the amount ratio of ionic liquid material is 0.4-4；
If by silicon source in step (B3): the amount ratio of ionic liquid material weighs silicon source, ionic liquid less than 0.4, due to
Silicon source consumption is too small, causes template action not enough；And by silicon source: the amount ratio of ionic liquid material weighs silicon source, ionic liquid more than 4
Body, because silicon source consumption is excessive, causes to waste, and excessive silicon source is difficult to be evenly dispersed in gel, has no other beneficial
Effect.
Silicon source, hydrochloric acid, Citric Acid Dosage in step (B3)：
In the present invention, silicon source, hydrochloric acid, Citric Acid Dosage in step (B3) are not particularly limited, usual silicon source:Hydrochloric acid
: the amount ratio of lemon acid substance is 1:0.5-6:0.1-1.
Embodiment 1：
Weigh 0.6g N- bay-Pidolidone-di-n-butyl acid amides (abbreviation GP-1) and be added in 28.4g propane diols and add
Heat forms clear solution to 110 DEG C of dissolvings, then adds 2.0g aluminium isopropoxides, 0.6g 1- decyl -3- methylimidazolium chlorides
([C10Mim] Cl), it is uniformly mixed, gained mixed system is put into refrigerator and cools down plastic 24h；Gel is taken out, slowly
4mL ammoniacal liquor is added dropwise, 36h is stood at room temperature；It is utilized respectively ethanol, propane diols and is centrifuged off GP-1 for solvent, products therefrom is 60
48h is dried at DEG C.Then 400 DEG C of calcining 7h are warming up to 1 DEG C/min.Accompanying drawing 1 is the transmission electron microscope picture of gained sample, accompanying drawing 2
For the X ray diffracting spectrum of sample, accompanying drawing 3 is the scanning electron microscope (SEM) photograph of sample, and its pattern is irregular.Test result shows system
What is obtained is ordered into mesoporous γ-Al2O3, its specific surface area is 384m2It is 2.8nm, pore volume 0.26cm that/g, BJH, which calculate average pore size,3/
g。
Embodiment 2
Weigh 2.4g GP-1 and be added in 27.6g propane diols and be heated to 140 DEG C of dissolvings and form clear solution, then add
Carbon-based -3- the methylimidazolium chlorides ([C of 2.0g aluminium isopropoxides, 5.1g 1- 1616Mim] Cl), it is uniformly mixed, by gained
Mixed system, which is put into refrigerator, cools down plastic 36h；Gel is taken out, 3mL ammoniacal liquor is slowly added dropwise, 48h is stood at room temperature；It is sharp respectively
It is that solvent is centrifuged off GP-1 with ethanol, propane diols, products therefrom dries 12h at 80 DEG C.Then it is warming up to 1 DEG C/min
600 DEG C of calcining 5h.Test result is ordered into mesoporous γ-Al made from showing2O3, its specific surface area is 304m2/ g, BJH calculate flat
Equal aperture is 2.78nm, pore volume 0.48cm3/g。
Embodiment 3
Weigh 1.5g N- bay-Pidolidone-di-n-butyl acid amides (abbreviation GP-1) and be added in 28.5g propane diols and add
Heat forms clear solution to 80 DEG C of dissolvings, then adds 2.0g aluminium isopropoxides, 6.3g [C10Mim] Cl, it is uniformly mixed, by institute
Obtain mixed system and be put into cooling plastic 24h in refrigerator；Gel is taken out, 0.7mL ammoniacal liquor is slowly added dropwise, 24h is stood at room temperature；Point
It is that solvent is centrifuged off GP-1 not using ethanol, propane diols, products therefrom dries 72h at 40 DEG C.Then heated up with 1 DEG C/min
To 900 DEG C of calcining 3h.Test result shows that obtained is unordered mesoporous γ-Al2O3, its specific surface area is 164.0m2/ g, BJH are counted
Calculation average pore size is 2.85nm, pore volume 0.40cm3/g.Embodiment 4：
Embodiment 4
Weigh 1.5g agaroses and be added in 28.5g water and be heated to 90 DEG C of dissolvings and form clear solution, then add 3.0g
Aluminum nitrate, 6.7g [C16Mim] Cl, it is uniformly mixed；；Gained mixed system is put into refrigerator and cools down plastic 48h；By gel
Take out, 6mL ammoniacal liquor is slowly added dropwise, stand at room temperature after 48h, 48h is dried at 60 DEG C.Then 700 DEG C are warming up to 1 DEG C/min
Calcine 5h.Test result shows that obtained is unordered mesoporous γ-Al2O3, its specific surface area is 306m2/ g, BJH calculated hole diameters are
6.2nm, pore volume 0.85cm3/g.Accompanying drawing 4 is the transmission electron microscope picture of gained sample.
Embodiment 5
Weigh 0.3g agaroses and be added in 29.7g water and be heated to 50 DEG C of dissolvings and form clear solution, then add 3.0g
Aluminum nitrate, 12.1g [C10Mim] Cl, it is uniformly mixed；；Gained mixed system is put into refrigerator and cools down plastic 30h；Will be solidifying
Glue is taken out, and 3mL ammoniacal liquor is slowly added dropwise, and stands at room temperature after 36h, and 12h is dried at 80 DEG C.Then 400 are warming up to 1 DEG C/min
DEG C calcining 7h.Test result shows that obtained is unordered mesoporous γ-Al2O3, its specific surface area is 287m2/ g, BJH calculated hole diameters
For 8nm, pore volume 0.56cm3/g。
Embodiment 6
Weigh 2.4g agaroses and be added in 27.6g water and be heated to 100 DEG C of dissolvings and form clear solution, then add 3.0g
Aluminum nitrate, 1.2g [C16Mim] Cl, it is uniformly mixed；；Gained mixed system is put into refrigerator and cools down plastic 24h；By gel
Take out, 1mL ammoniacal liquor is slowly added dropwise, stand at room temperature after 24h, 72h is dried at 40 DEG C.Then 900 DEG C are warming up to 1 DEG C/min
Calcine 3h.Test result shows that obtained is unordered mesoporous γ-Al2O3, its specific surface area is 222.83m2/ g, BJH calculated hole diameters
For 3.0nm, pore volume 0.64cm3/g。
Embodiment 7：
Weigh and cool down plastic after being heated to 100 DEG C of dissolvings in 0.4g GP-1 addition 19.6g propane diols, gained is organic solidifying
Glue is dialysed in pure water, and a water is changed per half an hour, and suction filtration obtains the gel refrigeration drying 24h of gained after dialysing 5 times
To GP-1 xerogel；By 2.0g aluminium isopropoxides, 0.6g [C10Mim] Cl is added to the ethanol solution containing 0.2mL 37wt%HCl
In, 0.2g citric acids are added, 7h is reacted, obtains Alumina gel；Xerogel obtained by step 1 is soaked in the aluminium obtained by step 2
80 DEG C of volatilization 12h after 3h in colloidal sol, are then warming up to 400 DEG C of calcining 7h with 1 DEG C/min.Accompanying drawing 5 is electric for the scanning of gained sample
Mirror figure.From scanning electron microscope (SEM) photograph it can be seen that resulting aluminum oxide is in doughnut pencil, average caliber is 80nm, and nitrogen is inhaled de-
Its specific surface area of attached Experimental Characterization is 227m2/g。
Embodiment 8：
Weigh and cool down plastic after being heated to 120 DEG C of dissolvings in 1.6g GP-1 addition 18.4g propane diols, gained is organic solidifying
Glue is dialysed in pure water, and a water is changed per half an hour, and suction filtration obtains the gel refrigeration drying 48h of gained after dialysing 5 times
To GP-1 xerogel；By 2.0g aluminium isopropoxides, 8.4g [C16Mim] Cl is added in the ethanol solution containing 2mL 37wt%HCl,
2.1g citric acids are added, 3h is reacted, obtains Alumina gel；Xerogel obtained by step 1 is soaked in the Alumina gel obtained by step 2
40 DEG C of volatilization 72h after middle 7h, are then warming up to 900 DEG C of calcining 3h with 1 DEG C/min.During aluminum oxide is in made from scanning electron microscope observation
Hollow fiber pencil, average caliber 50nm, its specific surface area of nitrogen adsorption desorption Experimental Characterization is 320m2/g。
Embodiment 9
Weigh and cool down plastic after being heated to 110 DEG C of dissolvings in 1.0g GP-1 addition 19.0g propane diols, gained is organic solidifying
Glue is dialysed in pure water, and a water is changed per half an hour, and suction filtration obtains the gel refrigeration drying 36h of gained after dialysing 5 times
To GP-1 xerogel；By 2.0g aluminium isopropoxides, 6.0g [C10Mim] Cl is added in the ethanol solution containing 1mL 37wt%HCl,
0.5g citric acids are added, 5h is reacted, obtains Alumina gel；Xerogel obtained by step 1 is soaked in the Alumina gel obtained by step 2
60 DEG C of volatilization 48h after middle 5h, are then warming up to 700 DEG C of calcining 5h with 1 DEG C/min.During aluminum oxide is in made from scanning electron microscope observation
Hollow fiber pencil, average caliber 60nm, its specific surface area of nitrogen adsorption desorption Experimental Characterization is 288m2/g。
Gel-ionic liquid common mode plate is prepared and simply and readily removed, and synthetic method is realized to the mesoporous structure of aluminum oxide
Flexible modulation, is resulted in the mesoporous of different pore size, pore volume, specific surface area, different mesoporous order degrees and different-shape
Aluminum oxide, can meet aluminum oxide as the different application demand of catalyst, catalyst carrier and adsorbent etc..
Claims (8)
1. the method for a kind of use supermolecular gel-synthesising mesoporous aluminum oxide of ionic liquid common mode plate, with organic silicon source or inorganic
Silicon source is raw material, and it is auxiliary template for master module, ionic liquid to use the organogel factor or hydrogelator, to be respectively synthesized
Different target products, i.e., unordered or ordered mesoporous aluminium oxide, doughnut pencil aluminum oxide, it is characterised in that
When target product is unordered or during ordered mesoporous aluminium oxide, comprise the following steps：
(A1) weigh the organogel factor to be added in organic solvent, be heated to 80 DEG C of -140 DEG C of dissolvings and form clear solution；Or
Person weighs hydrogelator and is added to the water, and is heated to 50 DEG C of -100 DEG C of dissolvings and forms clear solution；
(A2) weigh in the clear solution obtained by silicon source, ionic liquid are added separately to step (A1), plastic is cooled down after mixing
24h-48h；
(A3) ammoniacal liquor is added dropwise into wet gel made from step (A2) than 0.2-1 by silicon source and the amount of the material of ammoniacal liquor, stands
24h-48h；
(A4) by gel obtained by step (A3) in 40 DEG C -80 DEG C dry 12-72h, and 3h-7h is calcined after 400-900 DEG C, be made
Unordered or ordered mesoporous aluminium oxide；
When target product is doughnut pencil aluminum oxide, comprise the following steps：
(B1) weigh the organogel factor to be added in organic solvent, be heated to 80 DEG C of -140 DEG C of dissolvings and form clear solution；
(B2) using organic solvent of the dialysis in gel obtained by water displacement step (B1), 24h-48h systems are then freeze-dried
Obtain corresponding xerogel；
(B3) silicon source and ionic liquid are added in the ethanol solution containing hydrochloric acid, add citric acid, reacted 3h-7h, obtain
To Alumina gel, xerogel obtained by step (B2) is immersed in 3-7h in Alumina gel；
(B4) by the gel after being soaked obtained by step (B3) in 40 DEG C -80 DEG C dry 12-72h, and after 400 DEG C of -900 DEG C of roastings
3-7h, is made doughnut pencil aluminum oxide.
2. the method for use supermolecular gel according to claim 1-synthesising mesoporous aluminum oxide of ionic liquid common mode plate, its
It is characterised by, source of aluminium is aluminium isopropoxide, aluminum sulfate, aluminum nitrate or sodium metaaluminate.
3. the method for use supermolecular gel according to claim 2-synthesising mesoporous aluminum oxide of ionic liquid common mode plate, its
It is characterised by, is to weigh the organogel factor according to 2wt%-8wt% to be added in organic solvent in step (A1), according to
1wt%-8wt% weighs hydrogelator and is added to the water；Be in step (B1) according to 2wt%-8wt% weigh organogel because
Son is added in organic solvent.
4. use supermolecular gel-synthesising mesoporous aluminum oxide of ionic liquid common mode plate according to any one of claims 1 to 3
Method, it is characterised in that the organogel factor described in step (A1) is that amino acid derivatives, the hydrogelator are
Agarose；(B1) the organogel factor described in is amino acid derivatives.
5. use supermolecular gel-synthesising mesoporous aluminum oxide of ionic liquid common mode plate according to any one of claims 1 to 3
Method, it is characterised in that organic solvent described in step (A1), (B1) be ethanol, acetone or propane diols.
6. use supermolecular gel-synthesising mesoporous aluminum oxide of ionic liquid common mode plate according to any one of claims 1 to 3
Method, it is characterised in that ionic liquid described in step (A2), (B3) be glyoxaline ion liquid.
7. use supermolecular gel-synthesising mesoporous aluminum oxide of ionic liquid common mode plate according to any one of claims 1 to 3
Method, it is characterised in that by silicon source in step (A2): the amount ratio of ionic liquid material be 0.4-4 weigh silicon source, ionic liquid
It is added separately in the clear solution obtained by step (1).
8. use supermolecular gel-synthesising mesoporous aluminum oxide of ionic liquid common mode plate according to any one of claims 1 to 3
Method, it is characterised in that in step (B3) press silicon source: the amount ratio of ionic liquid material be 0.4-4, silicon source:Hydrochloric acid: citric acid
The amount ratio of material is 1:0.5-6:0.1-1, silicon source and ionic liquid are added in the ethanol solution containing hydrochloric acid, lemon is added
Lemon acid.
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| CN101372342A (en) * | 2008-10-22 | 2009-02-25 | 南京工业大学 | Method for preparing mesoporous aluminum oxide molecular sieve with ion liquid as template |
| CN102167373A (en) * | 2011-03-04 | 2011-08-31 | 南京工业大学 | Method for synthesizing mesoporous aluminum oxide by using dicationic imidazolium ionic liquid |
| CN103241757A (en) * | 2013-05-17 | 2013-08-14 | 南开大学 | Method for preparing gamma-Al2O3 mesoporous nanometer material by one-step process |
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