CN107185463A - A kind of SiO2‑Al2O3The synthetic method of mixed oxide aerogel material - Google Patents
A kind of SiO2‑Al2O3The synthetic method of mixed oxide aerogel material Download PDFInfo
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- CN107185463A CN107185463A CN201710491614.8A CN201710491614A CN107185463A CN 107185463 A CN107185463 A CN 107185463A CN 201710491614 A CN201710491614 A CN 201710491614A CN 107185463 A CN107185463 A CN 107185463A
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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Abstract
A kind of SiO2‑Al2O3The synthetic method of mixed oxide aerogel material, including：(a) siliceous precursor raw material is mixed with Organic Alcohol A, then adds deionized water and reaction is hydrolyzed, obtain colloidal sol；(b) the inorganic salt containing aluminium aqueous solution is mixed into progress precipitation reaction with alkaline solution, obtains filter cake I；(c) filter cake I is washed with deionized, then proceedes to carry out carrying out washing treatment with Organic Alcohol B and be filtrated to get filter cake II；(d) filter cake II is dispersed in Organic Alcohol C and forms suspension；(e) according to SiO2/Al2O3Mass ratio is 1~5 to be progressively added drop-wise to colloidal sol in suspension, it is to be mixed it is uniform after, alkaline solution regulation pH value is added dropwise to form spawn；(f) spawn of formation is obtained into SiO by calcination process2‑Al2O3Mixed oxide aerogel material.Advantage of the invention is that easy, low cost, having synthesized the SiO with large specific surface area, aperture and pore volume under the premise of without using supercritical drying2‑Al2O3Aerogel material.
Description
(1) technical field
The present invention relates to a kind of SiO2-Al2O3The synthetic method of mixed oxide aerogel material, more particularly, to one kind
Under the premise of without using supercritical drying, SiO is synthesized2-Al2O3The preparation method of mixed oxide aerogel material.
(2) background technology
Aeroge is the solid with three-dimensional cross-linked porous spongy structure, and the material has low-density, macrovoid
The features such as rate, large aperture, bigger serface and excellent heat endurance.Therefore, in space flight, optics, machinery, electronics, oil
The every field such as work, environmental protection suffer from being widely applied.In heterogeneous catalysis field, aerogel material is due to macropore, big table
The characteristic of area and high thermal stability, therefore can be directly used for catalytic reaction or be used to prepare various supported catalysts as carrier
Agent.But, conventional synthesis aerogel material needs to use supercritical drying drying method (to need higher pressure and temperature super to reach
Critical condition), so needing complicated preparation process (for example：Because aqueous solvent has very high critical-temperature and pressure, therefore
Need the water used in strict control building-up process, and by multiple organic solvent displacement step by wet gel network structure
In water displacement it is clean), metal organic alkoxide costly be used as precursor raw material (purpose：1) try one's best and avoid in synthesis
Other impurities are introduced, otherwise need to be removed with substantial amounts of water washing；2) metal alkoxide uses the water of metering ratio in hydrolytic process,
So water (mainly avoiding producing or using substantial amounts of aqueous solvent) and high temperature resistant, height will not be formed in theory in building-up process
The instrument and equipment of pressure, so, be not easy to industrialize extensive synthesis (N.H ü sing, U.Schubert,
Angew.Chem.Int.Ed.1998,37,22-45)。
(3) content of the invention
The technical problem to be solved in the present invention is to provide it is a kind of it is easy, low cost, before without using supercritical drying
Put SiO of the synthesis with large specific surface area, aperture and pore volume2-Al2O3The method of aerogel material.
In order to solve the above technical problems, the present invention is adopted the following technical scheme that：
A kind of SiO2-Al2O3The synthetic method of mixed oxide aerogel material, the SiO2-Al2O3Mixed oxide gas
Gel rubber material, its specific surface area is not less than 450m2g-1, aperture is not less than 1.5cm not less than 12nm, pore volume3g-1；Including following step
Suddenly：
(a) siliceous precursor raw material is mixed with Organic Alcohol A, then adds deionized water and reaction is hydrolyzed, obtain molten
Glue；Described siliceous precursor raw material is organosiloxane TEOS or TMOS；The Organic Alcohol A is selected from methanol or ethanol；It is described
Deionized water：Siliceous precursor raw material：The volume ratio of Organic Alcohol is 1:2.5~12.5:3.5~15.5；
(b) the inorganic salt containing aluminium aqueous solution is mixed into progress precipitation reaction with alkaline solution, obtains filter cake I；Described contains aluminium
Inorganic salts are that the mass percent concentration of inorganic salt containing aluminium in aluminum nitrate or aluminum sulfate, the inorganic salt containing aluminium aqueous solution is 15-25%；
Described alkaline solution is ammonium carbonate solution, ammoniacal liquor or ammonium bicarbonate aqueous solution, and the mass percent concentration of alkaline solution is
1-5%；And cause the ratio between mass concentration of the inorganic salt containing aluminium aqueous solution and alkaline solution to be 8-8.5:1；(c) filter cake I is spent
Ion water washing, to remove foreign ion；Then proceed to carry out carrying out washing treatment with Organic Alcohol B and be filtrated to get filter cake II；It is described
Organic Alcohol B be selected from following a kind of or any several combination：Methanol, ethanol, propyl alcohol, butanol, ethylene glycol, butanediol, the third two
Alcohol, glycerine, polyethylene glycol；
(d) it will be dispersed in as the filter cake II obtained by step (c) in Organic Alcohol C and form suspension；Described Organic Alcohol C is selected from
Following a kind of or any several combination：Methanol, ethanol, propyl alcohol, butanol, ethylene glycol, butanediol, propane diols, glycerine, poly- second
Glycol；
(e) according to SiO2/Al2O3Mass ratio will be progressively added drop-wise to by step for 1~5 by the preparation-obtained colloidal sol of step (a)
Suddenly in the suspension prepared by (d), it is to be mixed it is uniform after, alkaline solution regulation pH value is added dropwise to form spawn；
(f) spawn of formation is obtained into SiO by 300-600 DEG C of calcination process2-Al2O3Mixed oxide gas
Gel rubber material.
In the step (a), in order to reduce the content of aqueous solvent in gel skeleton structure, present invention selection organosilicon as far as possible
Oxygen alkane TEOS or TMOS is used as siliceous precursor raw material.Further, described siliceous precursor material is preferably TEOS；It is described to have
Machine alcohol A is preferably ethanol.The temperature of the hydrolysis is 10-100 DEG C, by hydrolysis under this condition to be had
There are certain particle diameter and the Nano sol particle of size distribution.Selective hydrolysis temperature is 60~70 DEG C, and hydrolysis time is 6~8 hours.
It is worth noting that, in the step, deionized water, siliceous precursor raw material, the rate of charge of Organic Alcohol three are for product structure
With material impact.
In the step (b), the preferred aluminum nitrate of described inorganic salt containing aluminium, inorganic salt containing aluminium in inorganic salt containing aluminium solution
Mass percent is preferably 18-20%；The alkaline solution is preferably sal volatile, the mass percent concentration of alkaline solution
Preferably 2~4%.The addition of alkaline solution can cause inorganic salt containing aluminium to precipitate completely.
In the step (c), replacement Treatment is carried out to the filter cake obtained by step (b) using Organic Alcohol B, to reduce roasting
During caused by capillary force phenomenon hole cave in phenomenon, the Organic Alcohol B preferred alcohols.
In the step (d), described Organic Alcohol C preferred alcohols.
In the step (f), roasting time was at 3~6 hours.Further, sintering temperature is preferably 400 DEG C, roasting time
It is preferred that 4 hours.
The present invention specifically recommends the SiO2-Al2O3The synthetic method of mixed oxide aerogel material is in accordance with the following steps
Carry out：
(a) organosiloxane TEOS is mixed with ethanol, then adds deionized water and reaction is hydrolyzed in 10-100 DEG C,
Obtain colloidal sol；Described deionized water：TEOS：The volume ratio of ethanol is 1:2.5~12.5:3.5~15.5；
(b) aluminum nitrate aqueous solution and mass percent concentration for being 18-20% by mass percent concentration are 2~4%
Ammonium carbonate solution is according to mass concentration ratio 8-8.5:1 mixing carries out precipitation reaction, obtains filter cake I；
(c) filter cake I is washed with deionized, to remove foreign ion；Then proceed to carry out carrying out washing treatment simultaneously with ethanol
It is filtrated to get filter cake II；
(d) it will be disperseed to form suspension in ethanol as the filter cake II obtained by step (c)；
(e) according to SiO2/Al2O3Mass ratio will be progressively added drop-wise to by step for 1~5 by the preparation-obtained colloidal sol of step (a)
Suddenly in the suspension prepared by (d), it is to be mixed it is uniform after, alkaline solution regulation pH value is added dropwise to form spawn；
(f) spawn of formation is calcined 4 hours at 400 DEG C, obtains SiO2-Al2O3Mixed oxide airsetting glue material
Material.
Compared with the prior art, the present invention has advantages below：
(1) new method that the present invention is reported is advantageously formed while having the SiO of large specific surface area, aperture and pore volume2-
Al2O3Mixed oxide aerogel material；
(2) preparation that the present invention is reported need not use supercritical drying process, therefore preparation process does not need complexity
Equipment, precursor material containing aluminium can be inorganic salt containing aluminium, greatly reduce production cost, be easy to industrialized production.
(4) embodiment
Technical scheme is described further with specific embodiment below, but protection scope of the present invention not by
The limitation of the following example.
Embodiment (1)
By 8cm3Deionized water is added to TEOS (23.5cm3) and ethanol (30.3cm3) mixed solution in be hydrolyzed it is anti-
(T=60 DEG C, react 8 hours) is answered to prepare Ludox.By Al (NO3)3·9H2The O aqueous solution (aluminum nitrate mass concentration for~
0.25g·ml-1) be slowly added dropwise into containing (NH4)2CO3The aqueous solution (ammonium carbonate mass concentration is~0.03gml-1) in enter
Row reaction, forms precipitation, is filtrated to get filter cake.Resulting filter cake is washed with deionized repeatedly to remove foreign ion.
Obtained filter cake is subjected to carrying out washing treatment with alcohol solvent and disperses to form suspension in ethanol.Then according to mass ratio
SiO2/Al2O3=1 is added step-wise to Ludox in the suspension under conditions of stirring, it is to be mixed it is uniform after, be added dropwise
(NH4)2CO3Solution adjusts pH value to be formed after gel sample, and sample is calcined under the conditions of 400 DEG C to 4 hours to obtain
SiO2-Al2O3(mass ratio SiO2/Al2O3=1) mixed oxide material.Pass through N2The ratio surface for the material that adsorption method is obtained
Product is~536m2·g-1；Bore dia is~16nm；Pore volume is 2.1cm3·g-1。
Embodiment (2)
By 2cm3Deionized water is added to TEOS (23.5cm3) and ethanol (30.3cm3) mixed solution in be hydrolyzed it is anti-
(T=60 DEG C, react 6 hours) is answered to prepare Ludox.By Al (NO3)3·9H2The O aqueous solution (aluminum nitrate mass concentration for~
0.25g·ml-1) be slowly added dropwise into containing (NH4)2CO3The aqueous solution (ammonium carbonate mass concentration is~0.03gml-1) in enter
Row reaction.Resulting filter cake is washed with deionized repeatedly to remove foreign ion.By obtained filter cake alcohol solvent
Handled and disperse to form suspension in ethanol.Then according to mass ratio SiO2/Al2O3=5 under conditions of stirring by silicon
Colloidal sol is added step-wise in the suspension, it is to be mixed it is uniform after, (NH is added dropwise4)2CO3Solution adjusts pH value to form gel
After sample, sample is calcined under the conditions of 400 DEG C to 4 hours to obtain SiO2-Al2O3(SiO2/Al2O3=5) mixed oxide
Material.Pass through N2The specific surface area for the material that adsorption method is obtained is~483m2·g-1；Bore dia is~12.8nm；Pore volume is
1.5cm3·g-1。
Comparative example (1)
By 1.6cm3Deionized water is added to TEOS (18.8cm3) and ethanol (24.3cm3) mixed solution in be hydrolyzed
(T=70 DEG C, react 8 hours) is reacted to prepare Ludox.By Al (NO3)3·9H2The O aqueous solution (aluminum nitrate mass concentration for~
0.23g·ml-1) be slowly added dropwise into containing (NH4)2CO3The aqueous solution (ammonium carbonate mass concentration is~0.03gml-1) in enter
Row reaction.Resulting filter cake is washed with deionized repeatedly to remove foreign ion.By obtained filter cake alcohol solvent
Handled and disperse to form suspension in ethanol.Then according to mass ratio SiO2/Al2O3=10 will under conditions of stirring
Ludox is added step-wise in the suspension, it is to be mixed it is uniform after, (NH is added dropwise4)2CO3Solution adjusts pH value to form gel
After shape sample, sample is calcined under the conditions of 400 DEG C to 4 hours to obtain SiO2-Al2O3(SiO2/Al2O3=10) mixed oxidization
Thing material.Pass through N2The specific surface area for the material that adsorption method is obtained is~484.8m2·g-1；Bore dia is~10.7nm；Hole
Hold for 1.3cm3·g-1.By being compared with embodiment (1)-(2), work as SiO2/Al2O3Mass ratio can not obtain more than 5
Required aperture of the invention and the SiO of pore volume2-Al2O3Mixed oxide aerogel material.
Comparative example (2)
By 23.14 grams of K2SiO3It is added to 100cm3Siliceous solution A is formed in deionized water and by stirring.By 7.36
Gram Al (NO3)3·9H2O is added to 10cm3The B solution containing aluminium is formed in deionized water and by stirring.A and B solution are mixed
React 30min.Adjust the pH=7 of suspension.By being filtrated to get filter cake, by 200cm3Deionized water is added in filter cake and carried out
Agitator treating 30 minutes, is then filtrated to get filter cake.Washing 10 times more than repeating.Again by 400 DEG C of roastings 5 in air atmosphere
Hour obtains SiO2-Al2O3Material.Pass through N2The specific surface area for the material that adsorption method is obtained is~282m2·g-1, bore dia
For~8.0nm, pore volume is~0.56m3·g-1.By being compared and can clearly being found with embodiment (1)-(2), using tradition system
Preparation Method can not obtain bigger serface, the SiO of large aperture2-Al2O3Material.
Claims (10)
1. a kind of SiO2-Al2O3The synthetic method of mixed oxide aerogel material, the SiO2-Al2O3Mixed oxide airsetting
Glue material, its specific surface area is not less than 450m2g-1, aperture is not less than 1.5cm not less than 12nm, pore volume3g-1；Including following step
Suddenly：
(a) siliceous precursor raw material is mixed with Organic Alcohol A, then adds deionized water and reaction is hydrolyzed, obtain colloidal sol；Institute
The siliceous precursor raw material stated is organosiloxane TEOS or TMOS；The Organic Alcohol A is selected from methanol or ethanol；It is described go from
Sub- water：Siliceous precursor raw material：The volume ratio of Organic Alcohol is 1:2.5~12.5:3.5~15.5；
(b) the inorganic salt containing aluminium aqueous solution is mixed into progress precipitation reaction with alkaline solution, obtains filter cake I；Described is inorganic containing aluminium
Salt is that the mass percent concentration of inorganic salt containing aluminium in aluminum nitrate or aluminum sulfate, the inorganic salt containing aluminium aqueous solution is 15-25%；It is described
Alkaline solution be ammonium carbonate solution, ammoniacal liquor or ammonium bicarbonate aqueous solution, the mass percent concentration of alkaline solution is 1-
5%；And cause the ratio between mass concentration of the inorganic salt containing aluminium aqueous solution and alkaline solution to be 8-8.5:1；(c) by filter cake I spend from
Sub- water washing, to remove foreign ion；Then proceed to carry out carrying out washing treatment with Organic Alcohol B and be filtrated to get filter cake II；Described
Organic Alcohol B is selected from following a kind of or any several combination：Methanol, ethanol, propyl alcohol, butanol, ethylene glycol, butanediol, propane diols,
Glycerine, polyethylene glycol；
(d) it will be dispersed in as the filter cake II obtained by step (c) in Organic Alcohol C and form suspension；Described Organic Alcohol C is selected from following
A kind of or any several combination：Methanol, ethanol, propyl alcohol, butanol, ethylene glycol, butanediol, propane diols, glycerine, poly- second two
Alcohol；
(e) according to SiO2/Al2O3Mass ratio will be progressively added drop-wise to by step for 1~5 by the preparation-obtained colloidal sol of step (a)
(d) in the suspension prepared by, it is to be mixed it is uniform after, alkaline solution regulation pH value is added dropwise to form spawn；
(f) spawn of formation is obtained into SiO by 300-600 DEG C of calcination process2-Al2O3Mixed oxide aeroge
Material.
2. synthetic method as claimed in claim 1, it is characterised in that：In step (a), described siliceous precursor material is
TEOS；The Organic Alcohol A is ethanol.
3. synthetic method as claimed in claim 1, it is characterised in that：In step (a), the temperature of the hydrolysis is 10-
100℃。
4. synthetic method as claimed in claim 3, it is characterised in that：In step (a), hydrolysis temperature is 60~70 DEG C, hydrolysis
Time is 6~8 hours.
5. synthetic method as claimed in claim 1, it is characterised in that：In step (b), described inorganic salt containing aluminium is nitric acid
The mass percent of inorganic salt containing aluminium is 18-20% in aluminium, inorganic salt containing aluminium solution；The alkaline solution is sal volatile,
The mass percent concentration of alkaline solution is 2~4%.
6. synthetic method as claimed in claim 1, it is characterised in that：In step (c), Organic Alcohol B is ethanol.
7. synthetic method as claimed in claim 1, it is characterised in that：In step (d), described Organic Alcohol C is ethanol.
8. synthetic method as claimed in claim 1, it is characterised in that：In step (f), roasting time was at 3~6 hours.
9. synthetic method as claimed in claim 1, it is characterised in that：In step (f), sintering temperature is 400 DEG C, roasting time
For 4 hours.
10. synthetic method as claimed in claim 1, it is characterised in that：The SiO2-Al2O3Mixed oxide aerogel material
Synthetic method carry out in accordance with the following steps：
(a) organosiloxane TEOS is mixed with ethanol, then adds deionized water and reaction is hydrolyzed in 10-100 DEG C, obtain
Colloidal sol；Described deionized water：TEOS：The volume ratio of ethanol is 1:2.5~12.5:3.5~15.5；
(b) carbonic acid that the aluminum nitrate aqueous solution for being 18-20% by mass percent concentration is 2~4% with mass percent concentration
Aqueous ammonium is according to mass concentration ratio 8-8.5:1 mixing carries out precipitation reaction, obtains filter cake I；
(c) filter cake I is washed with deionized, to remove foreign ion；Then proceed to carry out carrying out washing treatment with ethanol and filter
Obtain filter cake II；
(d) it will be disperseed to form suspension in ethanol as the filter cake II obtained by step (c)；
(e) according to SiO2/Al2O3Mass ratio will be progressively added drop-wise to by step for 1~5 by the preparation-obtained colloidal sol of step (a)
(d) in the suspension prepared by, it is to be mixed it is uniform after, alkaline solution regulation pH value is added dropwise to form spawn；
(f) spawn of formation is calcined 4 hours at 400 DEG C, obtains SiO2-Al2O3Mixed oxide aerogel material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109486448A (en) * | 2018-11-17 | 2019-03-19 | 金丽丹 | A kind of preparation method of modified C5 Petropols enhancing EVA hot-melt adhesive |
| CN112830846A (en) * | 2021-01-25 | 2021-05-25 | 成都子之源绿能科技有限公司 | Silicon dioxide aerogel slow release fertilizer and preparation method thereof |
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| CN103877928A (en) * | 2014-02-14 | 2014-06-25 | 浙江工业大学 | Method for synthesizing SiO2-Al2O3 material with macropores and large specific area |
| CN104591193A (en) * | 2014-12-29 | 2015-05-06 | 中国神华能源股份有限公司 | Method for preparing Al2O3-SiO2 aerogel |
| CA2974446A1 (en) * | 2015-01-23 | 2016-07-28 | Wuhan Kaidi Engineering Technology Research Institute Co., Ltd. | Cobalt-based fischer-tropsch synthesis catalyst and preparation method and use thereof |
| CN106630931A (en) * | 2016-10-10 | 2017-05-10 | 南京工业大学 | Preparation method of fiber-reinforced Al2O3-SiO2 aerogel material with wave transmission and heat insulation integrated function |
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| CN103877928A (en) * | 2014-02-14 | 2014-06-25 | 浙江工业大学 | Method for synthesizing SiO2-Al2O3 material with macropores and large specific area |
| CN104591193A (en) * | 2014-12-29 | 2015-05-06 | 中国神华能源股份有限公司 | Method for preparing Al2O3-SiO2 aerogel |
| CA2974446A1 (en) * | 2015-01-23 | 2016-07-28 | Wuhan Kaidi Engineering Technology Research Institute Co., Ltd. | Cobalt-based fischer-tropsch synthesis catalyst and preparation method and use thereof |
| CN106630931A (en) * | 2016-10-10 | 2017-05-10 | 南京工业大学 | Preparation method of fiber-reinforced Al2O3-SiO2 aerogel material with wave transmission and heat insulation integrated function |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109486448A (en) * | 2018-11-17 | 2019-03-19 | 金丽丹 | A kind of preparation method of modified C5 Petropols enhancing EVA hot-melt adhesive |
| CN112830846A (en) * | 2021-01-25 | 2021-05-25 | 成都子之源绿能科技有限公司 | Silicon dioxide aerogel slow release fertilizer and preparation method thereof |
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