CN111217373A - Silica aerogel with customizable shape and rapid preparation method thereof - Google Patents
Silica aerogel with customizable shape and rapid preparation method thereof Download PDFInfo
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Abstract
The invention provides a silicon dioxide aerogel with a customizable shape and a rapid preparation method thereof, wherein the method comprises the following steps: mixing MTMS, a surfactant and deionized water, and uniformly stirring to obtain a precursor solution; adding an acid catalyst into the precursor solution while stirring, sealing, and hydrolyzing in a water bath; and adding an alkali catalyst into the hydrolyzed precursor solution while stirring, standing for gelation, and drying to obtain the silicon dioxide aerogel. The contact angle of the obtained silicon dioxide aerogel is 133.5-143.4 degrees, and the density is 0.064-0.143g/cm3Can bear high temperature and has excellent performance. The method is simple and safe to operate, has a very short production period, does not need the steps of aging, surface modification, solvent exchange and the like, and can complete the whole production flow within 4 hours; the prepared sample is in a large block body, can be customized in shape, can be machined, is suitable for application scenes with special requirements on the shape, and can be produced in large scale.
Description
Technical Field
The invention relates to the field of silicon dioxide aerogel, in particular to silicon dioxide aerogel with a customizable shape and a rapid preparation method thereof.
Background
The aerogel material is a novel solid material with a nanoscale three-dimensional network structure, can be used as a heat insulation material, a drug carrier, a catalyst carrier, an adsorbent, a capacitor and the like due to the advantages of high specific surface area, high porosity, low density, low thermal conductivity and the like, and has wide application prospects in the fields of buildings, medicine, energy, aviation, high-energy physics and the like.
Water glass, tetraethoxysilane, tetramethoxysilane, MTMS, and mixtures thereof are silicon sources for several common silica aerogels. Since hydrophilic silica aerogels tend to collapse due to moisture absorption during drying and subsequent use, there is a greater need for a hydrophobic silica aerogel during production. In the preparation process of the silica aerogel, a supercritical drying method is often adopted. The drying method has high requirements on equipment, usually involves high temperature and high pressure, is high in manufacturing cost and is not beneficial to mass production. Because MTMS has hydrophobic methyl groups, silica aerogel prepared by using MTMS as a silicon source generally has hydrophobicity. Due to the existence of methyl, the wet gel can avoid surface modification and solvent exchange, avoid the waste of a large amount of organic solvents, simultaneously can adopt a normal pressure drying method, avoid high pressure and high risk operation, and realize convenient, simple, rapid and safe preparation. The invention with publication number CN109052415A discloses a preparation method of super-hydrophobic silica aerogel. The method takes MTMS, inulin dispersion liquid and ionic liquid as co-precursors, adopts the steps of plasma spraying and the like, prepares the silicon dioxide aerogel under normal pressure drying, and the sample has higher hydrophobicity. But the preparation process is complex, the required equipment is expensive, and the cost is high. The invention with publication number CN109437832A discloses a preparation method of a self-hydrophobic silica aerogel composite material. The method takes tetraethyl orthosilicate and MTMS as precursors, and adopts a mixed solvent system and supercritical drying to prepare the self-hydrophobic silica aerogel composite material. But adopts complex operations such as supercritical drying and the like, has high requirements on equipment and is not beneficial to continuous production.
Disclosure of Invention
Aiming at the defects of the prior art, such as the produced aerogel is in a powder shape or a small block shape, a supercritical drying method is adopted in the preparation process, the obtained gel needs a surface modification and solvent exchange process, and the like, the invention provides the silica aerogel with the customizable shape and the rapid preparation method thereof, aiming at reducing the preparation cost and the preparation period and saving organic solvent on the one hand, and obtaining a silica aerogel material which has high temperature resistance, high hydrophobicity, low density, is in a large block shape, can be customized in shape, can be applied to scenes with special requirements on the shape, such as electronic devices, can be machined in the later stage, has good adaptability in the application process and can be continuously produced.
In order to achieve the above object, the present invention provides a silica aerogel with a customizable shape and a rapid preparation method thereof, comprising the following steps:
(1) MTMS, a surfactant and deionized water are mixed according to a molar ratio of 1: (0.00079-0.00237): (32.3-56.5), and uniformly stirring to obtain a precursor solution;
(2) adding an acid catalyst into the precursor solution obtained in the step (2) while stirring, and hydrolyzing in a water bath after sealing;
(3) and adding an alkali catalyst into the hydrolyzed precursor solution while stirring, standing for gelation, and drying to obtain the silicon dioxide aerogel.
Preferably, the surfactant of step (1) comprises cetyltrimethylammonium bromide, cetyltrimethylammonium chloride or dioctadecyldimethylammonium bromide.
Preferably, the acid catalyst in step (2) is hydrochloric acid, and the concentration is 0.05-0.15 mol/L.
Preferably, the mixed solution is sealed before hydrolysis in the step (2), and then the mixed solution is put into a constant-temperature water bath kettle at 40-50 ℃ for hydrolysis, wherein the hydrolysis time is 20-40 min.
Preferably, the alkali catalyst in the step (3) is ammonia water, and the concentration is 0.25-1.25 mol/L.
Preferably, the standing and gelling time in the step (3) is 10-30 min.
Preferably, the gel obtained in the step (3) is placed in a constant-temperature air-blast drying oven for drying, and the drying pressure is normal pressure; the drying temperature is 100-150 ℃; the drying time is 2.5-7.0 h.
The invention also provides the silicon dioxide aerogel with the customizable shape prepared by the method.
Preferably, the antenna of the silica aerogel is 133.5 to 143.4 °.
Preferably, the silica aerogel has a density of 0.064-0.143g/cm3。
The scheme of the invention has the following beneficial effects:
(1) the preparation method provided by the invention is simple to operate, safe and convenient, has extremely short production period, does not need the steps of aging, surface modification, solvent exchange and the like, saves a large amount of organic solvent, and can complete the whole production flow within 4 hours; and the silicon dioxide aerogel is a massive body, can be customized in shape, can be machined, and is suitable for large-scale batch production.
(2) The MTMS used in the method provided by the invention has a methyl group, so that the finally obtained aerogel has hydrophobicity without surface modification; and the surfactant can facilitate the phase separation process, thus avoiding a solvent exchange step. Meanwhile, the micron-sized pore diameter formed in the gelling process and the CTAB capable of reducing the surface tension exist, so that the capillary force is greatly reduced, and the obtained wet gel can be directly dried under normal pressure.
(3) The silicon dioxide aerogel provided by the invention has a contact angle of 133.5-143.4 degrees and a density of 0.064-0.143g/cm3Can bear high temperature of about 450 ℃ and has excellent performance.
Drawings
FIG. 1 is a schematic diagram of silica aerogels of different shapes prepared in example 6;
FIG. 2 is a scanning electron micrograph of a silica aerogel prepared in example 6;
FIG. 3 is a contact angle diagram of a silica aerogel prepared in example 6;
FIG. 4 is a thermogravimetric plot of the silica aerogel prepared in example 6;
FIG. 5 is a flow chart of a silica aerogel prepared in example 7;
FIG. 6 is a graph comparing the cycle time of example 6 preparation with that of other people's work.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
Example 1
The embodiment provides a preparation method of silica aerogel, which comprises the following steps:
(1) preparing a precursor solution: according to molar ratio MTMS: deionized water is 1: 48.5, 5mL of MTMS was added to 30mL of deionized water, and 0.01g of CTAB (cetyltrimethylammonium bromide) was added, and the mixture was stirred uniformly to obtain a precursor solution.
(2) Hydrolysis: and continuously stirring the obtained precursor solution, adding 0.3mL of hydrochloric acid with the concentration of 0.1mol/L while stirring, sealing the mixed solution, and putting the mixed solution into a water bath kettle for hydrolysis for 30 min.
(3) Aging the gel: after the mixed solution reaches the room temperature, placing the mixed solution on a magnetic stirrer, adding 0.6mL of ammonia water with the concentration of 1.0mol/L while stirring, slowly pouring the obtained sol into a mold, slightly shaking, standing for 20min, and then gelling. 10mL of ethanol was added to the wet gel for aging, and the gel was replaced once for 12 hours twice.
(4) Surface modification: preparing surface modification liquid from trimethylchlorosilane and n-heptane according to the proportion that the specific gravity of the trimethylchlorosilane is 12%, adding 10mL of modification liquid into each aged wet gel, and replacing once in 12 hours for two times.
(5) Solvent exchange: 10mL of n-heptane was added to the modified wet gel and replaced once for 12h twice.
(6) And (3) grading and drying: and putting the obtained wet gel into a forced air drier, and drying for 6h, 6h, 4h and 2h at 60 ℃, 80 ℃, 100 ℃ and 120 ℃ respectively to obtain the hydrophobic silicon dioxide aerogel.
The basic properties of the hydrophobic silica aerogel obtained in this example are shown in table 1.
Table 1 properties of the aerogel obtained in example 1
| Density (g/cm)3) | 0.072 |
| Porosity of the material | 96.8％ |
| Hydrophilic and hydrophobic property | Hydrophobic |
Example 2
The embodiment provides a preparation method of silica aerogel, which comprises the following steps:
(1) preparing a precursor solution: according to molar ratio MTMS: deionized water is 1: 48.5, 5mL of MTMS was added to 30mL of deionized water, and 0.01g of CTAB (cetyltrimethylammonium bromide) was added, and the mixture was stirred uniformly to obtain a precursor solution.
(2) Hydrolysis: and continuously stirring the obtained precursor solution, adding 0.3mL of hydrochloric acid with the concentration of 0.1mol/L while stirring, sealing the mixed solution, and putting the mixed solution into a water bath kettle for hydrolysis for 30 min.
(3) Aging the gel: after the mixed solution reaches the room temperature, placing the mixed solution on a magnetic stirrer, adding 0.6mL of ammonia water with the concentration of 1.0mol/L while stirring, standing for 20min, and then gelling. 10mL of ethanol was added to the wet gel for aging, and the gel was replaced once for 12 hours twice.
(4) Solvent exchange: 10mL of n-heptane was added to the aged wet gel and replaced once for 12h twice.
(5) And (3) grading and drying: and putting the obtained wet gel into a forced air drier, and drying for 6h, 6h, 4h and 2h at 60 ℃, 80 ℃, 100 ℃ and 120 ℃ respectively to obtain the hydrophobic silicon dioxide aerogel.
The basic properties of the hydrophobic silica aerogel obtained in this example are shown in table 2.
Table 2 properties of the aerogel obtained in example 2
| Density (g/cm)3) | 0.074 |
| Porosity of the material | 96.7％ |
| Hydrophilic and hydrophobic property | Hydrophobic |
Example 3
The embodiment provides a preparation method of silica aerogel, which comprises the following steps:
(1) preparing a precursor solution: according to molar ratio MTMS: deionized water is 1: 48.5, 5mL of MTMS was added to 30mL of deionized water, and 0.01g of CTAB (cetyltrimethylammonium bromide) was added, and the mixture was stirred uniformly to obtain a precursor solution.
(2) Hydrolysis: and continuously stirring the obtained precursor solution, adding 0.3mL of hydrochloric acid with the concentration of 0.1mol/L while stirring, sealing the mixed solution, and putting the mixed solution into a water bath kettle for hydrolysis for 30 min.
(3) Aging the gel: after the mixed solution reaches the room temperature, placing the mixed solution on a magnetic stirrer, adding 0.6mL of ammonia water with the concentration of 1.0mol/L while stirring, slowly pouring the obtained sol into a mold, slightly shaking, standing for 20min, and then gelling. 10mL of ethanol was added to the wet gel for aging, and the gel was replaced once for 12 hours twice.
(4) Surface modification: preparing surface modification liquid from trimethylchlorosilane and n-heptane according to the proportion that the specific gravity of the trimethylchlorosilane is 12%, adding 10mL of modification liquid into each aged wet gel, and replacing once in 12 hours for two times.
(5) And (3) grading and drying: and putting the obtained wet gel into a forced air drier, and drying for 6h, 6h, 4h and 2h at 60 ℃, 80 ℃, 100 ℃ and 120 ℃ respectively to obtain the hydrophobic silicon dioxide aerogel.
The basic properties of the hydrophobic silica aerogel obtained in this example are shown in table 3.
Table 3 properties of the aerogel obtained in example 3
Example 4
The embodiment provides a preparation method of silica aerogel, which comprises the following steps:
(1) preparing a precursor solution: according to molar ratio MTMS: deionized water is 1: 48.5, 5mL of MTMS was added to 30mL of deionized water, and 0.01g of CTAB (cetyltrimethylammonium bromide) was added, and the mixture was stirred uniformly to obtain a precursor solution.
(2) Hydrolysis: and continuously stirring the obtained precursor solution, adding 0.3mL of hydrochloric acid with the concentration of 0.1mol/L while stirring, sealing the mixed solution, and putting the mixed solution into a water bath kettle for hydrolysis for 30 min.
(3) Aging the gel: after the mixed solution reaches the room temperature, placing the mixed solution on a magnetic stirrer, adding 0.6mL of ammonia water with the concentration of 1.0mol/L while stirring, slowly pouring the obtained sol into a mold, slightly shaking, standing for 20min, and then gelling. 10mL of ethanol was added to the wet gel for aging, and the gel was replaced once for 12 hours twice.
(4) And (3) grading and drying: and putting the obtained wet gel into a forced air drier, and drying for 6h, 6h, 4h and 2h at 60 ℃, 80 ℃, 100 ℃ and 120 ℃ respectively to obtain the hydrophobic silicon dioxide aerogel.
The basic properties of the hydrophobic silica aerogel obtained in this example are shown in table 4.
Table 4 properties of the aerogel obtained in example 4
| Density (g/cm)3) | 0.077 |
| Porosity of the material | 96.6％ |
| Hydrophilic and hydrophobic property | Hydrophobic |
Example 5
The embodiment provides a preparation method of silica aerogel, which comprises the following steps:
(1) preparing a precursor solution: according to molar ratio MTMS: deionized water is 1: 48.5, 5mL of MTMS was added to 30mL of deionized water, and 0.01g of CTAB (cetyltrimethylammonium bromide) was added, and the mixture was stirred uniformly to obtain a precursor solution.
(2) Hydrolysis: and continuously stirring the obtained precursor solution, adding 0.3mL of hydrochloric acid with the concentration of 0.1mol/L while stirring, sealing the mixed solution, and putting the mixed solution into a water bath kettle for hydrolysis for 30 min.
(3) And (3) gel: after the mixed solution reaches the room temperature, placing the mixed solution on a magnetic stirrer, adding 0.6mL of ammonia water with the concentration of 1.0mol/L while stirring, slowly pouring the obtained sol into a mold, slightly shaking, standing for 20min, and then gelling.
(4) And (3) grading and drying: and putting the obtained wet gel into a forced air drier, and drying for 6h, 6h, 4h and 2h at 60 ℃, 80 ℃, 100 ℃ and 120 ℃ respectively to obtain the hydrophobic silicon dioxide aerogel.
The basic properties of the hydrophobic silica aerogel obtained in this example are shown in table 5.
Table 5 properties of the aerogel obtained in example 5
| Density (g/cm)3) | 0.074 |
| Porosity of the material | 96.7％ |
| Hydrophilic and hydrophobic property | Hydrophobic |
Example 6
The embodiment provides a method for quickly preparing silica aerogel with a customizable shape, which comprises the following steps:
(1) preparing a precursor solution: according to molar ratio MTMS: deionized water is 1: 48.5, 5mL of MTMS was added to 30mL of deionized water, and 0.01g of CTAB (cetyltrimethylammonium bromide) was added, and the mixture was stirred uniformly to obtain a precursor solution.
(2) Hydrolysis: and continuously stirring the obtained precursor solution, adding 0.3mL of hydrochloric acid with the concentration of 0.1mol/L while stirring, sealing the mixed solution, and putting the mixed solution into a water bath kettle for hydrolysis for 30 min.
(3) And (3) gel: after the mixed solution reaches the room temperature, placing the mixed solution on a magnetic stirrer, adding 0.6mL of ammonia water with the concentration of 1.0mol/L while stirring, slowly pouring the obtained sol into molds with different shapes (cylindrical, square and round cake shapes), slightly shaking, standing for 20min, and then gelling.
(4) And (3) direct drying: and putting the obtained wet gel into a 150 ℃ air blast dryer, and drying for 2.5 hours to obtain the hydrophobic silicon dioxide aerogel.
The basic properties of the hydrophobic silica aerogel obtained in this example are shown in table 6.
Table 6 properties of the aerogel obtained in example 6
Fig. 1 shows silica aerogels with different shapes prepared by the embodiment, and it can be seen from the figure that the silica aerogel prepared by the embodiment has customizable shapes and can be machined, and can be applied to some use scenes with special requirements on shapes. Fig. 2 is a scanning electron microscope image of the silica aerogel prepared in this embodiment, and it can be seen that the pores of the porous material are large pores, which provides conditions for atmospheric drying. Fig. 3 is a contact angle diagram of the silica aerogel prepared in this example, which does not require surface modification and solvent exchange, and the contact angle reaches 143.4 °, so that the hydrophobicity is good, and the organic solvent is saved. Fig. 4 is a thermogravimetric curve of the silica aerogel prepared in this example, and the sample can be stable and resistant to high temperature at 438 ℃. Fig. 6 is a comparison graph of the preparation cycle of the sample of the embodiment and the work of other people, and it can be found that the preparation cycle of the sample of the embodiment is within 4 hours, compared with the work of other people, the preparation cycle is greatly shortened, and theoretical guidance is provided for rapidly preparing silica aerogel.
Example 7
The embodiment provides a method for quickly preparing silica aerogel, which comprises the following steps:
(1) preparing a precursor solution: according to molar ratio MTMS: deionized water is 1: 48.5, 5mL of MTMS was added to 30mL of deionized water, and 0.025g of CTAB (cetyltrimethylammonium bromide) was added, and the mixture was stirred uniformly to obtain a precursor solution.
(2) Hydrolysis: and continuously stirring the obtained precursor solution, adding 0.3mL of hydrochloric acid with the concentration of 0.1mol/L while stirring, sealing the mixed solution, and putting the mixed solution into a water bath kettle for hydrolysis for 30 min.
(3) And (3) gel: after the mixed solution reaches the room temperature, placing the mixed solution on a magnetic stirrer, adding 0.6mL of ammonia water with the concentration of 1.0mol/L while stirring, slowly pouring the obtained sol into a mold, slightly shaking, standing for 20min, and then gelling.
(4) And (3) direct drying: and putting the obtained wet gel into a forced air drier at 100 ℃, and drying for 7h to obtain the hydrophobic silicon dioxide aerogel.
The basic properties of the hydrophobic silica aerogel obtained in this example are shown in table 7.
Table 7 properties of the aerogel obtained in example 7
FIG. 5 is a flow chart of the silica aerogel prepared in this example, which omits the steps of surface modification and solvent exchange, and saves organic solvent; and the normal pressure drying mode is simple and safe to operate, and the rapid preparation of the silicon dioxide aerogel can be realized.
Example 8
The embodiment provides a method for quickly preparing silica aerogel, which comprises the following steps:
(1) preparing a precursor solution: according to molar ratio MTMS: deionized water is 1: 56.5, 5mL of MTMS is added into 35mL of deionized water, 0.01g of CTAB (cetyl trimethyl ammonium bromide) is added, and the mixture is stirred uniformly to obtain a precursor solution.
(2) Hydrolysis: and continuously stirring the obtained precursor solution, adding 0.3mL of hydrochloric acid with the concentration of 0.1mol/L while stirring, sealing the mixed solution, and putting the mixed solution into a water bath kettle for hydrolysis for 30 min.
(3) And (3) gel: after the mixed solution reaches the room temperature, placing the mixed solution on a magnetic stirrer, adding 0.6mL of ammonia water with the concentration of 1.0mol/L while stirring, slowly pouring the obtained sol into a mold, slightly shaking, standing for 20min, and then gelling.
(4) And (3) direct drying: and putting the obtained wet gel into a forced air drier at 100 ℃, and drying for 7h to obtain the hydrophobic silicon dioxide aerogel.
The basic properties of the hydrophobic silica aerogel obtained in this example are shown in table 8.
Table 8 properties of the aerogel obtained in example 8
| Density (g/cm)3) | 0.064 |
| Porosity of the material | 97.2％ |
| Hydrophilic and hydrophobic property | Hydrophobic, contact angle 133.5 ° |
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A rapid preparation method of silica aerogel with a customizable shape is characterized by comprising the following steps:
(1) MTMS, a surfactant and deionized water are mixed according to a molar ratio of 1: (0.00079-0.00237): (32.3-56.5), and uniformly stirring to obtain a precursor solution;
(2) adding an acid catalyst into the precursor solution obtained in the step (2) while stirring, and hydrolyzing in a water bath after sealing;
(3) and adding an alkali catalyst into the hydrolyzed precursor solution while stirring, standing for gelation, and drying to obtain the silicon dioxide aerogel.
2. The method of claim 1, wherein the surfactant of step (1) comprises cetyltrimethylammonium bromide, cetyltrimethylammonium chloride or dioctadecyldimethylammonium bromide.
3. The process according to claim 1, wherein the acid catalyst in the step (2) is hydrochloric acid and has a concentration of 0.05 to 0.15 mol/L.
4. The method according to claim 1, wherein the hydrolysis time in the step (2) is 20-40min and the hydrolysis temperature is 40-50 ℃.
5. The process according to claim 1, wherein the basic catalyst in the step (3) is ammonia water having a concentration of 0.25 to 1.25 mol/L.
6. The method according to claim 1, wherein the gel time is 10 to 30min for the standing in the step (3).
7. The method according to claim 1, wherein the drying in the step (3) is carried out under normal pressure, and the drying temperature is 100 to 150 ℃; the drying time is 2.5-7.0 h.
8. A silica aerogel of customizable shape, characterized in that it is prepared by the process according to any one of claims 1 to 7.
9. The silica aerogel according to claim 8, wherein the silica aerogel contact angle is 133.5 ° to 143.4 °.
10. Silica aerogel according to claim 8, characterized in that it is produced byThe density is 0.064-0.143g/cm3。
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Application publication date: 20200602 |