CN112125311A - Hydrophobic aerogel powder and rapid preparation method thereof - Google Patents
Hydrophobic aerogel powder and rapid preparation method thereof Download PDFInfo
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
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- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
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Abstract
The invention provides hydrophobic aerogel powder and a rapid preparation method thereof, belonging to the technical field of nano porous materials. According to the invention, the aerogel is rapidly prepared by enhancing the gel framework strength, modifying the surface of the nano particles in situ and the like, and then is directly dried under normal pressure by pulverization to rapidly obtain aerogel powder, so that the preparation period is short, and the application of the aerogel in the fields of heat insulation, heat preservation, adsorption separation and the like is facilitated.
Description
Technical Field
The invention relates to hydrophobic aerogel powder and a rapid preparation method thereof, belonging to the technical field of nano porous materials.
Background
Aerogel is a typical nano porous material, and has attracted attention in the fields of heat insulation, gas adsorption, oil-water separation and the like due to the unique nano network structure, low specific surface area, low thermal conductivity, high adsorbability and the like. However, because the drying of the aerogel mostly adopts supercritical drying or normal pressure drying with complicated and lengthy flow, the preparation efficiency of the aerogel is low, which severely limits the popularization in the practical application.
The organic-inorganic hybrid silica aerogel is prepared by taking methyltrimethoxysilane as a single precursor and using a surfactant-water system by professor Kanamori of kyoto university in japan and the like. However, the drying needs to be replaced by ethanol through a solvent and then supercritical drying is carried out, so that the preparation period is long and the equipment dependence is large. The aerogel prepared by using methyltrimethoxysilane as a precursor and alcohol as a solvent has the advantages of large pore structure size, limited nano-pore structure and low specific surface area due to micro-phase separation, and a solvent replacement step is still required before normal-pressure drying, so that the preparation period is influenced. Therefore, a rapid preparation method of aerogel powder is needed to meet the application requirements in practical engineering.
Disclosure of Invention
The invention aims to provide hydrophobic aerogel powder and a rapid preparation method thereof, so that the defects in the prior art are overcome.
The invention provides a quick preparation method of hydrophobic aerogel powder, which comprises the following steps:
weighing 80-110 parts by weight of a precursor methyltrimethoxysilane, 100-140 parts by weight of water and 1.5-2.5 parts by weight of a surfactant, uniformly mixing, and hydrolyzing under the condition of 0-0.2 part by weight of an acid catalyst;
uniformly mixing the hydrolyzed sol system with 0.001-0.004 parts of alkaline catalyst ammonium fluoride, and performing catalytic polymerization to form wet gel;
carrying out pulverization treatment on the obtained wet gel to obtain wet gel powder;
washing the wet gel powder in clear water to wash out residual organic reagent and adsorbed surfactant;
and directly drying the wet gel powder after washing under normal pressure to obtain the final hydrophobic aerogel powder.
Further, the preferred part of methyltrimethoxysilane is 90-100 parts; the preferable amount of water is 110-130 parts; the preferable part of the surfactant is 1.8-2.2 parts; the optimal proportion of the acidic catalyst is 0.05-0.15; the preferred ammonium fluoride is 0.002-0.003 part.
Further, the surfactant includes an ionic surfactant including cetyltrimethylammonium chloride or cetyltrimethylammonium bromide or a block copolymer type surfactant including a polyoxyethylene-polyoxypropylene ether block copolymer.
Further, the acidic catalyst comprises an inorganic acid comprising hydrochloric acid, sulfuric acid, phosphoric acid or nitric acid or an organic acid comprising acetic acid, oxalic acid or citric acid.
Further, the hydrolysis temperature is 10-60 ℃, and preferably 20-40 ℃;
further, the hydrolysis time is 10-30 min, preferably 15-25 min;
further, the temperature is regulated to be 20-60 ℃ after the ammonium fluoride is mixed, and preferably 40-50 ℃.
Furthermore, the pulverization treatment temperature is 10-50 ℃, and preferably 20-30 ℃.
Further, the water washing temperature is 20-70 ℃, and preferably 30-50 ℃;
further, the washing time is 10-30 min.
Further, the drying temperature under normal pressure is 40-100 ℃, and preferably 60-80 ℃.
The invention also provides hydrophobic aerogel powder prepared by the method.
Compared with the prior art, the method of the invention has the following beneficial effects: compared with the aerogel prepared by the traditional method without a typical nano network structure, the method adopts water as a solvent, a surfactant for controlling a pore structure and a catalyst ammonium fluoride for enhancing a gel framework, and directly dries, so that the use of an organic solvent is avoided, and the prepared aerogel powder keeps the pore size distribution of a nano scale, has a higher specific surface area and a smaller pore size and has the typical aerogel nano network structure. Compared with the traditional method for preparing aerogel powder, which needs a long solvent replacement process, the preparation period is more than 2 days, the method provided by the invention can shorten the shortest period for preparing aerogel powder to 2 hours, and the preparation period is greatly reduced.
Drawings
FIG. 1 is an appearance diagram of the hydrophobic aerogel powder prepared in example 1 of the present invention.
FIG. 2 is a scanning electron micrograph of the hydrophobic aerogel prepared in example 1 of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, the present invention shall be described in further detail with reference to the following detailed description and accompanying drawings.
Example 1
Weighing 120 parts by mass of solvent water, adding 0.1 part by mass of acetic acid, adding 2.0 parts by mass of surfactant cetyl trimethyl ammonium chloride, uniformly stirring, adding 100 parts by mass of precursor methyltrimethoxysilane, and stirring for hydrolysis.
The hydrolysis temperature is 25 deg.C, and the hydrolysis time is 20 min.
After hydrolysis, 0.003 part by mass of ammonium fluoride was added and stirred at 20 ℃ until polymerization.
The wet gel obtained by polymerization was subjected to pulverization treatment at 25 ℃.
And (3) washing the wet gel powder with water at 50 ℃ for 20 min.
And directly drying the wet gel powder after washing at normal pressure, wherein the drying temperature is 40 ℃, and obtaining the hydrophobic aerogel powder.
The obtained aerogel powder is shown in figure 1 in appearance picture and in figure 2 in scanning electron microscope picture.
Example 2
Weighing 100 parts by mass of solvent water, adding 0 part by mass of acetic acid, adding 1.5 parts by mass of surfactant cetyl trimethyl ammonium chloride, uniformly stirring, adding 80 parts by mass of precursor methyltrimethoxysilane, and stirring for hydrolysis.
The hydrolysis temperature is 10 deg.C, and the hydrolysis time is 10 min.
After hydrolysis, 0.001 part by mass of ammonium fluoride was added and stirred at 40 ℃ until it was polymerized.
The wet gel obtained by polymerization was subjected to pulverization treatment at a temperature of 10 ℃.
And (3) washing the wet gel powder with water at 20 ℃ for 30 min.
And directly drying the wet gel powder after washing at the normal pressure, wherein the drying temperature is 80 ℃, and obtaining the hydrophobic aerogel powder.
Example 3
Weighing 140 parts by mass of solvent water, adding 0.2 part by mass of acetic acid, adding 2.5 parts by mass of surfactant cetyl trimethyl ammonium chloride, uniformly stirring, adding 110 parts by mass of precursor methyltrimethoxysilane, and stirring for hydrolysis.
The hydrolysis temperature is 60 deg.C, and the hydrolysis time is 30 min.
After hydrolysis, 0.004 weight portion of ammonium fluoride is added and stirred, the temperature is 60 ℃, and the mixture is polymerized.
The wet gel obtained by polymerization was subjected to pulverization treatment at 50 ℃.
And (3) washing the wet gel powder for 10min at 70 ℃.
And directly drying the wet gel powder after washing at normal pressure, wherein the drying temperature is 100 ℃, and obtaining the hydrophobic aerogel powder.
Example 4
Weighing 100 parts by mass of solvent water, adding 0.2 part by mass of acetic acid, adding 2.5 parts by mass of surfactant cetyl trimethyl ammonium chloride, uniformly stirring, adding 110 parts by mass of precursor methyltrimethoxysilane, and stirring for hydrolysis.
The hydrolysis temperature is 25 deg.C, and the hydrolysis time is 15 min.
After hydrolysis, 0.001 part by mass of ammonium fluoride was added and stirred at 25 ℃ until polymerization.
The wet gel obtained by polymerization was subjected to pulverization treatment at 25 ℃.
And (3) washing the wet gel powder with water at 50 ℃ for 15 min.
And directly drying the wet gel powder after washing at the normal pressure, wherein the drying temperature is 80 ℃, and obtaining the hydrophobic aerogel powder.
Example 5
Weighing 140 parts by mass of solvent water, adding 0 part by mass of acetic acid, adding 1.5 parts by mass of surfactant cetyl trimethyl ammonium chloride, uniformly stirring, adding 80 parts by mass of precursor methyltrimethoxysilane, and stirring for hydrolysis.
The hydrolysis temperature is 60 deg.C, and the hydrolysis time is 30 min.
After hydrolysis, 0.004 weight part of ammonium fluoride is added and stirred at 25 ℃ until the mixture is polymerized.
The wet gel obtained by polymerization was subjected to pulverization treatment at 25 ℃.
And (3) washing the wet gel powder with water at 50 ℃ for 25 min.
And directly drying the wet gel powder after washing at normal pressure, wherein the drying temperature is 100 ℃, and obtaining the hydrophobic aerogel powder.
Comparative example
The preparation method is carried out by adopting a traditional method and comprises the following steps:
weighing 120 parts by mass of solvent ethanol, adding 0.1 part by mass of acetic acid, uniformly stirring, adding 100 parts by mass of precursor methyltrimethoxysilane, and stirring for hydrolysis.
The hydrolysis temperature is 25 deg.C, and the hydrolysis time is 20 min.
After hydrolysis, 0.003 part by mass of ammonium fluoride was added and stirred at 20 ℃ until polymerization.
The wet gel obtained by polymerization was subjected to pulverization treatment at 25 ℃.
And (3) washing the wet gel powder with water at 50 ℃ for 20 min.
And directly drying the wet gel powder after washing at normal pressure, wherein the drying temperature is 40 ℃, and obtaining the hydrophobic aerogel powder.
Aerogel structure parameters are shown in table 1.
Table 1 structural characterization results of aerogel samples prepared in different examples
| Examples | Pore size distribution (nm) | Specific surface area (m)2/g) | Pore volume (cm)3/g) |
| Example 1 | 40-60 | 316.1 | 1.25 |
| Example 2 | 30-50 | 296.2 | 1.34 |
| Example 3 | 30-60 | 287.3 | 1.22 |
| Example 4 | 30-50 | 305.5 | 1.43 |
| Example 5 | 30-60 | 298.1 | 1.37 |
| Comparative example | ＞100 | 30.2 | 0.89 |
As can be seen from table 1, the aerogel powder prepared by the method of the present invention maintains the pore size distribution in the nanometer scale, and has a higher specific surface area, which indicates that the pore size is smaller and is a typical aerogel structure, whereas the aerogel powder prepared by the conventional method, as in the comparative example, is actually a porous foam material and does not have a typical nano network structure of aerogel.
The above-described embodiments are merely preferred embodiments of the present invention, and should not be construed as limiting the scope of the present invention, it should be noted that those skilled in the art can make various modifications and decorations without departing from the principle of the present invention, and these modifications and decorations should also be regarded as being within the scope of the present invention.
Claims (10)
1. A quick preparation method of hydrophobic aerogel powder is characterized by comprising the following steps:
weighing 80-110 parts by weight of a precursor methyltrimethoxysilane, 100-140 parts by weight of water and 1.5-2.5 parts by weight of a surfactant, uniformly mixing, and hydrolyzing under the condition of 0-0.2 part by weight of an acid catalyst;
uniformly mixing the hydrolyzed sol system with 0.001-0.004 parts of alkaline catalyst ammonium fluoride, and performing catalytic polymerization to form wet gel;
carrying out pulverization treatment on the obtained wet gel to obtain wet gel powder;
washing the wet gel powder in clear water to wash out residual organic reagent and adsorbed surfactant;
and directly drying the wet gel powder after washing under normal pressure to obtain the final hydrophobic aerogel powder.
2. The method of claim 1, wherein methyltrimethoxysilane is preferably 90 to 100 parts; the preferable amount of water is 110-130 parts; the preferable part of the surfactant is 1.8-2.2 parts; the optimal proportion of the acidic catalyst is 0.05-0.15; the preferred ammonium fluoride is 0.002-0.003 part.
3. The method of claim 1, wherein the surfactant comprises an ionic surfactant comprising cetyltrimethylammonium chloride or cetyltrimethylammonium bromide or a block copolymer type surfactant comprising a polyoxyethylene-polyoxypropylene ether block copolymer.
4. The method of claim 1, wherein the acidic catalyst comprises an inorganic acid comprising hydrochloric acid, sulfuric acid, phosphoric acid, or nitric acid, or an organic acid comprising acetic acid, oxalic acid, or citric acid.
5. The method of claim 1, wherein the hydrolysis temperature is 10 to 60 ℃ and the hydrolysis time is 10 to 30 min.
6. The method according to claim 1, wherein the temperature is controlled to be 20 to 60 ℃ after mixing with ammonium fluoride.
7. The method of claim 1, wherein the pulverization treatment temperature is 10 to 50 ℃.
8. The method according to claim 1, wherein the water washing temperature is 20 to 70 ℃ and the water washing time is 10 to 30 min.
9. The method of claim 1, wherein the atmospheric drying temperature is 40 to 100 ℃.
10. A hydrophobic aerogel powder, characterized by being prepared by the method of claim 1.
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Cited By (4)
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| CN114261986A (en) * | 2022-01-18 | 2022-04-01 | 中国科学技术大学先进技术研究院 | Preparation method of aerogel material and application of aerogel material |
| CN114655960A (en) * | 2022-04-08 | 2022-06-24 | 纳诚(邢台)新材料科技有限公司 | Preparation method of aerogel |
| CN115093241A (en) * | 2022-06-07 | 2022-09-23 | 航天特种材料及工艺技术研究所 | Hydrophobic high-temperature-resistant aerogel material and preparation method thereof |
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| CN115093241A (en) * | 2022-06-07 | 2022-09-23 | 航天特种材料及工艺技术研究所 | Hydrophobic high-temperature-resistant aerogel material and preparation method thereof |
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Application publication date: 20201225 |