CN107185463B - 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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- CN107185463B CN107185463B CN201710491614.8A CN201710491614A CN107185463B CN 107185463 B CN107185463 B CN 107185463B CN 201710491614 A CN201710491614 A CN 201710491614A CN 107185463 B CN107185463 B CN 107185463B
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
Abstract
A kind of SiO2‑Al2O3The synthetic method of mixed oxide aerogel material, comprising: (a) mixes siliceous precursor raw material with Organic Alcohol A, deionized water is then added, reaction is hydrolyzed, obtain colloidal sol；(b) inorganic salt containing aluminium aqueous solution is mixed with alkaline solution and carries out precipitation reaction, obtain 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 filter cake II is obtained by filtration；(d) filter cake II is dispersed in Organic Alcohol C and forms suspension；(e) according to SiO2/Al2O3Mass ratio is 1~5 to be gradually added drop-wise to colloidal sol in suspension, it is to be mixed uniformly after, alkaline solution is added dropwise and adjusts pH value 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, under the premise of not using supercritical drying having synthesized the SiO with large specific surface area, aperture and Kong Rong2‑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 not using supercritical drying, SiO is synthesized2-Al2O3The preparation method of mixed oxide aerogel material.
(2) background technique
Aeroge is the solid with three-dimensional cross-linked porous spongy structure, which has low-density, macrovoid
The features such as rate, large aperture, bigger serface and excellent thermal stability.Therefore, in space flight, optics, machinery, electronics, petroleum
The every field such as work, environmental protection, which suffer from, to be 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 catalysis reaction or be used to prepare various supported catalysts as carrier
Agent.But conventional synthesis aerogel material needs (to need higher pressure and temperature using supercritical drying drying method to reach super
Critical condition), thus need complicated preparation process (such as: since aqueous solvent has very high critical-temperature and pressure,
Need water used in strict control synthesis process, and by multiple organic solvent displacement step by wet gel reticular structure
In water displacement it is clean), metal organic alkoxide costly (purpose: 1) avoids in synthesis as far as possible as precursor raw material
Other impurities are introduced, otherwise need to be removed with a large amount of water washing；2) metal alkoxide uses the water of metering ratio in hydrolytic process,
So not will form water (mainly avoiding generating or using a large amount of aqueous solvent) and high temperature resistant, height theoretically in the synthesis 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) summary of the invention
The technical problem to be solved in the present invention is to provide it is a kind of it is easy, inexpensive, before without using supercritical drying
Put the SiO that synthesis has large specific surface area, aperture and Kong Rong2-Al2O3The method of aerogel material.
In order to solve the above technical problems, the present invention adopts the following technical scheme:
A kind of SiO2-Al2O3The synthetic method of mixed oxide aerogel material, the SiO2-Al2O3Mixed oxide gas
Gel rubber material, specific surface area are not less than 450m2g-1, aperture is not less than 1.5cm not less than 12nm, Kong Rong3g-1；Including walking as follows
It is rapid:
(a) siliceous precursor raw material is mixed with Organic Alcohol A, deionized water is then added, reaction is hydrolyzed, obtains molten
Glue；The siliceous precursor raw material is organosiloxane TEOS or TMOS；The Organic Alcohol A is selected from methanol or ethyl alcohol；It is described
Deionized water: siliceous precursor raw material: the volume ratio of Organic Alcohol be 1:2.5~12.5:3.5~15.5；
(b) inorganic salt containing aluminium aqueous solution is mixed with alkaline solution and carries out precipitation reaction, obtain filter cake I；Described contains aluminium
Inorganic salts are aluminum nitrate or aluminum sulfate, and the mass percent concentration of inorganic salt containing aluminium is 15-25% in inorganic salt containing aluminium aqueous solution；
The alkaline solution is ammonium carbonate solution, ammonium hydroxide or carbonic acid hydrogen aqueous ammonium, and the mass percent concentration of alkaline solution is
1-5%；And the ratio between mass concentration for making inorganic salt containing aluminium aqueous solution and alkaline solution is 8-8.5:1；(c) filter cake I is spent
Ion water washing, to remove foreign ion；It then proceedes to carry out carrying out washing treatment with Organic Alcohol B and filter cake II is obtained by filtration；It is described
Organic Alcohol B be selected from the combination of following one or any of several: methanol, ethyl alcohol, propyl alcohol, butanol, ethylene glycol, butanediol, the third two
Alcohol, glycerine, polyethylene glycol；
(d) it will be dispersed in Organic Alcohol C by the resulting filter cake II of step (c) and form suspension；The Organic Alcohol C is selected from
The combination of following one or any of several: methanol, ethyl alcohol, propyl alcohol, butanol, ethylene glycol, butanediol, propylene glycol, glycerine, poly- second
Glycol；
(e) according to SiO2/Al2O3Mass ratio will be gradually added drop-wise to by the preparation-obtained colloidal sol of step (a) by step for 1~5
Suddenly in suspension prepared by (d), it is to be mixed uniformly after, be added dropwise alkaline solution adjust pH value 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 as far as possible, the present invention selects organosilicon
Oxygen alkane TEOS or TMOS is as siliceous precursor raw material.Further, the siliceous precursor material is preferably TEOS；It is described to have
Machine alcohol A is preferably ethyl alcohol.The temperature of the hydrolysis is 10-100 DEG C, by hydrolysis under this condition to obtain
Nano sol particle with certain partial size and size distribution.Selective hydrolysis temperature is 60~70 DEG C, and hydrolysis time is 6~8 small
When.It is worth noting that, in the step, deionized water, siliceous precursor raw material, Organic Alcohol three feed ratio for product knot
Structure has great influence.
In the step (b), the preferred aluminum nitrate of the 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 additional amount of alkaline solution can make inorganic salt containing aluminium 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
The hole collapsing phenomenon due to caused by capillary force phenomenon in the process, the Organic Alcohol B preferred alcohol.
In the step (d), the Organic Alcohol C preferred alcohol.
In the step (f), calcining time was at 3~6 hours.Further, maturing temperature is preferably 400 DEG C, calcining 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
It carries out:
(a) organosiloxane TEOS is mixed with ethyl alcohol, deionized water is then added, reaction is hydrolyzed in 10-100 DEG C,
Obtain colloidal sol；The deionized water: TEOS: the volume ratio of ethyl alcohol is 1:2.5~12.5:3.5~15.5；
(b) by mass percent concentration be 18-20% aluminum nitrate aqueous solution and mass percent concentration be 2~4%
Ammonium carbonate solution mixes according to mass concentration ratio 8-8.5:1 and carries out precipitation reaction, obtains filter cake I；
(c) filter cake I is washed with deionized, to remove foreign ion；It then proceedes to carry out carrying out washing treatment simultaneously with ethyl alcohol
Filter cake II is obtained by filtration；
(d) suspension will be formed by the resulting filter cake II dispersion of step (c) in ethanol；
(e) according to SiO2/Al2O3Mass ratio will be gradually added drop-wise to by the preparation-obtained colloidal sol of step (a) by step for 1~5
Suddenly in suspension prepared by (d), it is to be mixed uniformly after, be added dropwise alkaline solution adjust pH value to form spawn；
(f) spawn of formation is roasted 4 hours at 400 DEG C, obtains SiO2-Al2O3Mixed oxide airsetting glue material
Material.
Compared with the prior art, the invention has the following advantages that
(1) new method that the present invention reports advantageously forms while having the SiO of large specific surface area, aperture and Kong Rong2-
Al2O3Mixed oxide aerogel material；
(2) preparation that the present invention reports is not needed using 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 convenient for industrialized production.
(4) specific embodiment
With specific embodiment, technical scheme is described further 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 ethyl alcohol (30.3cm3) mixed solution in be hydrolyzed it is anti-
Answer (T=60 DEG C, react 8 hours) to prepare silica solution.By Al (NO3)3·9H2O aqueous solution (aluminum nitrate mass concentration be~
0.25g·ml-1) be slowly added dropwise into containing (NH4)2CO3Aqueous solution (ammonium carbonate mass concentration be~0.03gml-1) in into
Row reaction, forms precipitating, filter cake is obtained by filtration.Obtained 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 under stirring conditions added step-wise to silica solution in the suspension, it is to be mixed uniformly after, be added dropwise
(NH4)2CO3After solution adjusts pH value to form gel sample, sample is roasted to 4 hours under the conditions of 400 DEG C to obtain
SiO2-Al2O3(mass ratio SiO2/Al2O3=1) mixed oxide material.Pass through N2The specific surface for the material that adsorption method obtains
Product is~536m2·g-1；Bore dia is~16nm；Kong Rongwei 2.1cm3·g-1。
Embodiment (2)
By 2cm3Deionized water is added to TEOS (23.5cm3) and ethyl alcohol (30.3cm3) mixed solution in be hydrolyzed it is anti-
Answer (T=60 DEG C, react 6 hours) to prepare silica solution.By Al (NO3)3·9H2O aqueous solution (aluminum nitrate mass concentration be~
0.25g·ml-1) be slowly added dropwise into containing (NH4)2CO3Aqueous solution (ammonium carbonate mass concentration be~0.03gml-1) in into
Row reaction.Obtained filter cake is washed with deionized repeatedly to remove foreign ion.The filter cake alcohol solvent that will be obtained
It is handled and disperses to form suspension in ethanol.Then according to mass ratio SiO2/Al2O3=5 under stirring conditions by silicon
Colloidal sol is added step-wise in the suspension, it is to be mixed uniformly after, be added dropwise (NH4)2CO3Solution adjusts pH value to form gel
After sample, sample is roasted to 4 hours under the conditions of 400 DEG C to obtain SiO2-Al2O3(SiO2/Al2O3=5) mixed oxide
Material.Pass through N2The specific surface area for the material that adsorption method obtains is~483m2·g-1；Bore dia is~12.8nm；Kong Rongwei
1.5cm3·g-1。
Comparative example (1)
By 1.6cm3Deionized water is added to TEOS (18.8cm3) and ethyl alcohol (24.3cm3) mixed solution in be hydrolyzed
Reaction (T=70 DEG C, react 8 hours) is to prepare silica solution.By Al (NO3)3·9H2O aqueous solution (aluminum nitrate mass concentration be~
0.23g·ml-1) be slowly added dropwise into containing (NH4)2CO3Aqueous solution (ammonium carbonate mass concentration be~0.03gml-1) in into
Row reaction.Obtained filter cake is washed with deionized repeatedly to remove foreign ion.The filter cake alcohol solvent that will be obtained
It is handled and disperses to form suspension in ethanol.Then according to mass ratio SiO2/Al2O3=10 under stirring conditions will
Silica solution is added step-wise in the suspension, it is to be mixed uniformly after, be added dropwise (NH4)2CO3Solution adjusts pH value to form gel
After shape sample, sample is roasted to 4 hours under the conditions of 400 DEG C to obtain SiO2-Al2O3(SiO2/Al2O3=10) oxygen is mixed
Compound material.Pass through N2The specific surface area for the material that adsorption method obtains is~484.8m2·g-1；Bore dia is~10.7nm；
Kong Rongwei 1.3cm3·g-1.By compared with embodiment (1)-(2) it is found that working as SiO2/Al2O3Mass ratio is more than 5, i.e., can not obtain
To the SiO in aperture required by the present invention and Kong Rong2-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 the way that filter cake is obtained by filtration, by 200cm3Deionized water is added in filter cake and carries out
Agitator treating 30 minutes, filter cake is then obtained by filtration.Repeat the above washing 10 times.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 obtains is~282m2·g-1, bore dia
For~8.0nm, Kong Rongwei~0.56m3·g-1.By can clearly be found compared with embodiment (1)-(2), made using tradition
Preparation Method can not obtain the SiO of bigger serface, 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, specific surface area are not less than 450m2g-1, aperture is not less than 1.5cm not less than 12nm, Kong Rong3g-1；Including walking as follows
It is rapid:
(a) siliceous precursor material is mixed with Organic Alcohol A, deionized water is then added, reaction is hydrolyzed, obtains colloidal sol；Institute
The siliceous precursor material stated is organosiloxane TEOS or TMOS；The Organic Alcohol A is selected from methanol or ethyl alcohol；It is described go from
Sub- water: siliceous precursor material: the volume ratio of Organic Alcohol A is 1:2.5~12.5:3.5~15.5；
(b) inorganic salt containing aluminium aqueous solution is mixed with alkaline solution and carries out precipitation reaction, obtain filter cake I；Described is inorganic containing aluminium
Salt is aluminum nitrate or aluminum sulfate, and the mass percent concentration of inorganic salt containing aluminium is 15-25% in inorganic salt containing aluminium aqueous solution；It is described
Alkaline solution be ammonium carbonate solution, ammonium hydroxide or carbonic acid hydrogen aqueous ammonium, the mass percent concentration of alkaline solution is 1-
5%；And the ratio between mass concentration for making inorganic salt containing aluminium aqueous solution and alkaline solution is 8-8.5:1；(c) by filter cake I spend from
Sub- water washing, to remove foreign ion；It then proceedes to carry out carrying out washing treatment with Organic Alcohol B and filter cake II is obtained by filtration；Described
Organic Alcohol B be selected from following one or any of several combination: methanol, ethyl alcohol, propyl alcohol, butanol, ethylene glycol, butanediol, propylene glycol,
Glycerine, polyethylene glycol；
(d) it will be dispersed in Organic Alcohol C by the resulting filter cake II of step (c) and form suspension；The Organic Alcohol C is selected from following
The combination of one or any of several: methanol, ethyl alcohol, propyl alcohol, butanol, ethylene glycol, butanediol, propylene glycol, glycerine, poly- second two
Alcohol；
(e) according to SiO2/Al2O3Mass ratio will be gradually added drop-wise to by the preparation-obtained colloidal sol of step (a) by step for 1~5
(d) in the suspension prepared by, it is to be mixed uniformly after, be added dropwise alkaline solution adjust pH value 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 described in claim 1, it is characterised in that: in step (a), the siliceous precursor material is
TEOS；The Organic Alcohol A is ethyl alcohol.
3. synthetic method as described 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 described in claim 1, it is characterised in that: in step (b), the inorganic salt containing aluminium is nitric acid
Aluminium, the mass percent of inorganic salt containing aluminium is 18-20% in 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 described in claim 1, it is characterised in that: in step (c), Organic Alcohol B is ethyl alcohol.
7. synthetic method as described in claim 1, it is characterised in that: in step (d), the Organic Alcohol C is ethyl alcohol.
8. synthetic method as described in claim 1, it is characterised in that: in step (f), calcining time was at 3~6 hours.
9. synthetic method as described in claim 1, it is characterised in that: in step (f), maturing temperature is 400 DEG C, calcining time
It is 4 hours.
10. synthetic method as described 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 ethyl alcohol, deionized water is then added, reaction is hydrolyzed in 10-100 DEG C, obtains
Colloidal sol；The deionized water: TEOS: the volume ratio of ethyl alcohol is 1:2.5~12.5:3.5~15.5；
(b) carbonic acid for being 2~4% with mass percent concentration by the aluminum nitrate aqueous solution that mass percent concentration is 18-20%
Aqueous ammonium mixes according to mass concentration ratio 8-8.5:1 and carries out precipitation reaction, obtains filter cake I；
(c) filter cake I is washed with deionized, to remove foreign ion；It then proceedes to carry out carrying out washing treatment with ethyl alcohol and filter
Obtain filter cake II；
(d) suspension will be formed by the resulting filter cake II dispersion of step (c) in ethanol；
(e) according to SiO2/Al2O3Mass ratio will be gradually added drop-wise to by the preparation-obtained colloidal sol of step (a) by step for 1~5
(d) in the suspension prepared by, it is to be mixed uniformly after, be added dropwise alkaline solution adjust pH value to form spawn；
(f) spawn of formation is roasted 4 hours at 400 DEG C, obtains SiO2-Al2O3Mixed oxide aerogel material.
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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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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