CN107758674B - Aerogel particle preparation method - Google Patents
Aerogel particle preparation method Download PDFInfo
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- CN107758674B CN107758674B CN201610689630.3A CN201610689630A CN107758674B CN 107758674 B CN107758674 B CN 107758674B CN 201610689630 A CN201610689630 A CN 201610689630A CN 107758674 B CN107758674 B CN 107758674B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/16—Preparation of silica xerogels
- C01B33/163—Preparation of silica xerogels by hydrolysis of organosilicon compounds, e.g. ethyl orthosilicate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
Abstract
The invention discloses a preparation method of aerogel particles, which comprises the following steps: mixing: mixing a siloxane compound with an organic solvent to form a mixed solution; a hydrolysis step: adding an acid catalyst into the mixed solution to perform hydrolysis reaction; condensation step: adding an alkali catalyst into the mixed solution to perform condensation reaction, adding a hydrophobic dispersion solvent during the condensation reaction, and stirring to gelatinize the mixed solution during stirring to produce multiple aerogel particles with uniform structures.
Description
Technical Field
The invention relates to a preparation method of aerogel particles.
Background
Aerogel is a porous material with a three-dimensional net structure, has very low thermal conductivity, and is mainly applied to thermal insulation materials at present.
The preparation method of the aerogel is a sol-gel synthesis method, and mainly comprises the steps of mixing precursors such as silicon alkoxides (alkoxy silanes) or methyl orthosilicate and the like with an organic solvent, and adding an acid catalyst to perform hydrolysis reaction (hydrosis). After the hydrolysis reaction is carried out for a certain period of time, an alkali catalyst is added to carry out condensation reaction (condensation), and sol is gradually formed in the condensation reaction process. Molecules in the sol are continuously subjected to condensation reaction bonding to gradually form semi-solid polymer gel, and the sol is cured for a period of time to form a stable three-dimensional network structure. And finally, extracting and drying the solvents such as water, methanol and the like in the aerogel system by using a supercritical drying technology to obtain the porous dry blocky aerogel.
Because the drying technology adopted by the preparation method of the aerogel is the supercritical drying technology, the aerogel can be prevented from being broken due to the influence of the surface tension of water in the normal pressure drying process. However, since the supercritical drying technique is performed under high pressure, it is only suitable for drying a very small amount of aerogel, and it is not easy to mass-produce and reduce the production cost of aerogel.
On the other hand, the dry block aerogel is usually crushed in the above-mentioned aerogel, but the crushing method is prone to cause the uneven structure and the broken appearance of the aerogel (please refer to fig. 9 to 12), so that it is difficult to obtain the excellent heat insulation property.
In other related prior art, such as taiwan patent application publication No. 200835648, the porous material and the preparation method thereof are mainly prepared by synthesizing a mixture of silicon alkoxide or silicate compound and an organic solvent by a sol-gel method and modifying the mixture with a modifier, so as to replace the hydrophilic functional groups on the surface of the porous material with hydrophobic functional groups, thereby preventing the aerogel from being broken due to the influence of surface tension of moisture, and thus, the aerogel can be dried at room temperature and normal pressure.
The prior art uses the normal temperature and pressure multi-gradient solvent replacement technology for the hydrophobic modification of the aerogel, but the hydrophobic modification process needs to be carried out for more than 24 hours under the normal temperature and pressure condition, the time required by the process is too long, and the process is not cost-effective.
Furthermore, the prior art aerogel still needs to be crushed into dry block-shaped aerogel before use, so the aerogel also has the problems of uneven structure and broken appearance.
Disclosure of Invention
The invention aims to provide a preparation method of aerogel particles with uniform production structure and better heat insulation effect.
In order to achieve the purpose, the invention adopts the following technical scheme.
A method of preparing aerogel particles, comprising the steps of:
mixing: mixing a siloxane compound with an organic solvent to form a mixed solution;
a hydrolysis step: adding an acid catalyst into the mixed solution to perform hydrolysis reaction;
condensation step: adding an alkali catalyst into the mixed solution to perform a condensation reaction, adding a hydrophobic dispersion solvent during the condensation reaction, and stirring to gelatinize the mixed solution during the stirring process to generate a plurality of aerogel particles, wherein the mixed solution is stirred at a speed of 1200rpm to 2000rpm during the condensation reaction.
Further, the hydrophobic dispersion vehicle is one or more selected from the group consisting of: ketones, ethers, esters, aromatics, alkanes.
Further, a post-treatment step is included after the condensation step: filtering out the aerogel particles by a filter, cleaning the aerogel particles by a mixed solution of ethanol and water, and vacuum-drying the aerogel particles at a temperature of 100 ℃ to 115 ℃.
Further, the condensation step is followed by a hydrophobic modification step: heating the mixed solution to vaporize the organic solvent, adding a chloridized organic molecule to react with a hydroxyl group of the aerogel particles to generate hydrophobicity of the aerogel particles, and preventing the aerogel particles from being broken by the hydrophobic dispersion solvent.
Further, the chlorinated organic molecule is one or more selected from the group consisting of: chlorinated siloxanes, chloralkanes, chloranilides.
Further, the organic solvent comprises ethanol, water, mixed with each other; in the hydrophobicity modification step, the temperature of the mixed solution is changed into a first temperature condition, a second temperature condition and a third temperature condition in sequence, wherein the first temperature condition is 78 ℃ to 82 ℃, the second temperature condition is 100 ℃ to 115 ℃, the third temperature condition is 40 ℃ to 45 ℃, and the chloro-acylated organic molecule is added in the third temperature condition.
Further, the method also comprises a post-treatment step after the hydrophobic modification step: filtering out the aerogel particles by a filter, cleaning the aerogel particles by a toluene solvent, and drying the aerogel particles in vacuum.
Aerogel particles made by the steps of:
mixing: mixing a siloxane compound with an organic solvent to form a mixed solution;
a hydrolysis step: adding an acid catalyst into the mixed solution to perform hydrolysis reaction;
condensation step: adding an alkali catalyst into the mixed solution to perform a condensation reaction, adding a hydrophobic dispersion solvent during the condensation reaction, and stirring to gelatinize the mixed solution during the stirring process to generate a plurality of aerogel particles, wherein the particle size of the aerogel particles is 600nm +/-300 nm, and the mixed solution is stirred at a speed of 1200rpm to 2000rpm during the condensation reaction.
Preferably, the hydrophobic dispersion vehicle is one or more selected from the group consisting of: ketones, ethers, esters, aromatics, alkanes.
The aerogel particle preparation method of the present invention has the following effects by the above operations.
1. According to the preparation method, a large amount of incompatible solvents are used for stirring in the condensation step process, so that spherical granular aerogel particles with uniform structures can be produced, aerogel particles with better heat insulation effect can be obtained, and the practicability of the product is improved.
2. The porosity and the size of the pores of the aerogel particles prepared by the preparation method can be regulated and controlled according to preparation conditions (solvent content, solvent viscosity, acid catalyst content and alkali catalyst content).
3. The preparation method can control the preparation time of the aerogel particles by regulating the content of the alkali catalyst.
4. The preparation method can effectively control the size of the micro aerogel particles by controlling the content of the incompatible solvent and the stirring speed, and when the content of the incompatible solvent is higher and the stirring speed is higher, the aerogel particles are smaller; in contrast, the smaller the viscosity of the non-compatible solvent and the slower the stirring speed, the larger the aerogel particles.
5. The invention can shorten the time required by the replacement technology by controlling the temperature condition in the modification step, and can continuously complete the preparation of hydrophilic or hydrophobic aerogel particles within 4 to 5 hours at the fastest speed, thereby improving the production efficiency of the aerogel.
Therefore, the preparation method of the aerogel particles improves the problems that the traditional aerogel has uneven structure and broken appearance, and the heat insulation property is difficult to improve.
Drawings
FIG. 1 is a flow chart illustrating steps of an embodiment of the present invention.
FIG. 2 is a schematic flow chart of the upgrading step according to the embodiment of the present invention.
FIG. 3 is a scanning electron micrograph of aerogel particles prepared according to the present invention under stirring conditions at 1200 rpm.
FIG. 4 is a scanning electron micrograph of aerogel particles made according to the present invention under agitation conditions at 1800 rpm.
FIG. 5 is a transmission electron micrograph of aerogel particles according to the present invention.
FIG. 6 is a transmission electron micrograph of aerogel particles according to the present invention.
FIG. 7 is a graph showing the adsorption and desorption of aerogel particles without a hydrophobic modification step in nitrogen.
FIG. 8 is a hole pattern of the aerogel particles converted according to FIG. 7 according to the present invention.
Fig. 9 is a scanning electron micrograph of currently available aerogel powder at 500 magnifications.
Fig. 10 is a scanning electron micrograph of currently available aerogel powder at 1000 magnifications.
Fig. 11 is a scanning electron micrograph of currently commercially available aerogel powder at 5,000 magnification.
Fig. 12 is a scanning electron micrograph of currently commercially available aerogel powder at 10,000 magnification.
[ notation ] to show
(S1) mixing step (S2) hydrolysis step
(S3) condensation step (S4) (S40) post-treatment step
(S5) a hydrophobic modification step.
Detailed Description
In view of the above technical features, the main effects of the aerogel particle preparation method according to the embodiments of the present invention will be clearly demonstrated in the following embodiments.
Referring to fig. 1, a method for preparing aerogel particles according to an embodiment of the present invention is disclosed, which includes the following steps: a mixing step (S1), a hydrolysis step (S2), a condensation step (S3), and a post-treatment step (S4), wherein:
the mixing step (S1): a siloxane compound is mixed with an organic solvent to form a mixed solution. The siloxane compound (alkoxysilane) is a precursor such as Tetramethylsiloxane (TMOS) or Tetraethylsiloxane (TEOS), or methyl orthosilicate, and the content of the precursor such as siloxane compound or methyl orthosilicate is between 2.1 mol% and 12.5 mol%. The organic solvent is present in an amount between 97.9 mole percent and 87.5 mole percent.
The hydrolysis step (S2): adding an acid catalyst to the mixed solution to perform hydrolysis reaction (hydrolysis). Wherein the content ratio of the siloxane compound to the acid catalyst is 1: 0.3-1: 0.001, carrying out hydrolysis reaction.
And the content ratio of the siloxane compound to the acid catalyst is 1: 0.001 to 1: 0.3. when the content ratio of the siloxane compound to the acid catalyst is 1: 0.001, the time of the hydrolysis reaction is 300 minutes, and when the content ratio of the siloxane compound to the acid catalyst is 1: the hydrolysis time of 0.3 hour is 10 min. It is understood that the time required for the hydrolysis reaction decreases as the content of the acid catalyst increases.
The condensation step (S3): adding an alkali catalyst into the mixed solution to perform condensation reaction (condensation). The molar ratio of the acid catalyst and the ethanol mixed solution to the alkali catalyst and the ethanol mixed solution is, for example, 10: 10 to 10: 40. the molar ratio of the alkali catalyst to the acid catalyst is, for example, 1.0:1.0 to 3.0: 1.0.
In the mixed solution of the alkali catalyst and ethanol, the increase of the content of the alkali catalyst will significantly shorten the condensation reaction time (i.e. the gelation time of the aerogel). (the gelation time is about 1600 minutes when the ratio of the alkali catalyst to the acid catalyst is 1.0: 1.0; the gelation time is reduced to about 5 minutes when the ratio of the alkali catalyst to the acid catalyst is 3.0: 1.0; therefore, the ratio of the alkali catalyst content to the acid catalyst content can be adjusted to adjust the time required for the process.
When the condensation reaction in the condensation step (S3) is nearly completed, the mixed solution may first form a sol (sol). Adding a large amount of hydrophobic dispersion solvent of a non-compatible system into the mixed solution under the sol condition, and rapidly stirring at 1200rpm to 2000rpm, so that the mixed solution is influenced by the repulsion of the hydrophobic dispersion solvent under the rapid stirring condition to be gelatinized into pearl-shaped or spherical aerogel particles, wherein the particle diameter of the aerogel particles is about 600nm +/-300 nm.
The hydrophobic dispersion medium may be C6-C16 ketones, C6-C16 ethers, C6-C16 esters, C7-C16 aromatics, C8-C20 alkanes, halogenated ethers, halogenated esters, halogenated aromatics, halogenated alkanes, or the like. Specifically, examples thereof include toluene, kerosene, and degreasing oil.
The post-processing step (S4): filtering out the aerogel particles by a filter, cleaning the aerogel particles by a mixed solution of ethanol and water for 3 to 4 times, and then vacuumizing and drying the aerogel particles at the temperature of 100 to 115 ℃ to obtain spherical aerogel particles.
Referring to fig. 2, preferably, the aerogel particles may be further hydrophobically modified, and the condensation step may further include a hydrophobic modification step (S5): the temperature of the mixed solution is changed to a first temperature condition, a second temperature condition and a third temperature condition in sequence, wherein the first temperature condition is 78 ℃ to 82 ℃, ethanol of the mixed solution is vaporized (the boiling point of the ethanol is 78 ℃), the second temperature condition is 100 ℃ to 115 ℃ (the boiling point of the water is 100 ℃), water of the mixed solution is vaporized, and the third temperature condition is 40 ℃ to 45 ℃.
Adding a chloroacylated organic molecule at the third temperature condition, the chloroacylated organic molecule being one or more selected from the group consisting of: chlorinated siloxanes, chloralkanes, chloranilides.
Therefore, the chloridized organic molecules and one hydroxyl of the aerogel particles are mutually reacted, so that the aerogel particles generate hydrophobicity, and the aerogel particles are prevented from being broken by virtue of repulsive force between the hydrophobic dispersion solvent and the aerogel particles. If the aerogel particles are subjected to the hydrophobic modification step (S5), the post-treatment step (S40) is to wash the aerogel particles with a toluene solvent to remove the chlorinated organic molecules, and then to vacuum-dry the aerogel particles.
Borrow this, can prepare the porous aerogel granule of the submicron that sphere shape, size homogeneity are high, can improve the homogeneity of appearance, structure of aerogel granule on the one hand, improve the application. In addition, by heating and vaporizing and adding the chloridized organic molecules, the technology of preparing hydrophobic modified aerogel in large quantity can be rapidly realized, so that the aerogel is easier to be produced in quantity and the industrial application scale can be enlarged.
Referring to table one below, a table showing comparison of parameters before and after modification by a specific surface area analyzer (BET) analysis of aerogel particles prepared in the present example is shown:
in table SBETSpecific surface area as measured by BET; vporePore volume measured for BET; dpPore diameter measured for BET; smicroIs the specific surface area of the micropores; vmicroIs the micropore volume.
The data in the table are that under the condition of room temperature, the aerogel particles are desorbed and removed by using a specific surface area analyzer before and after unit weight modification under the condition of vacuumizing to P/Po being 0, nitrogen (N2) is introduced into the aerogel particles to enable the aerogel particles to adsorb nitrogen (N2) until the pressure reaches the saturation condition (P/Po being 1), then the aerogel particles are desorbed by vacuumizing again, and the aerogel particles adsorbing saturated nitrogen are desorbed by nitrogen, and when the pressure of the aerogel particles desorbing to nitrogen (N2) reaches the condition of P/Po being 0. In the adsorption and desorption process, the adsorption and desorption curves of the aerogel particles are measured and analyzed, and the related data of the specific surface area can be obtained.
Referring to fig. 3 and 4, Scanning Electron Microscopes (SEM) are used to capture photomicrographs of the distribution and the apparent size of the aerogel particles at different microscopic scales, which shows that the prepared aerogel particles have a uniform and highly uniform spherical appearance.
Referring to fig. 5 and 6, the internal structure and the hole distribution of the aerogel particles at different microscopic scales are extracted by a Scanning Electron Microscope (SEM). Showing that the aerogel molecules aggregate with each other to form a nano-sized aerogel structure.
Referring to fig. 7, an absorption and desorption curve of the aerogel particles without the hydrophobic modification step under nitrogen gas in the embodiment of the present invention is shown; FIG. 8 shows the conversion of the adsorption and desorption curves of the aerogel particles without the hydrophobic modification step into a pore distribution map.
The operation, use and efficacy of the present invention will be fully understood from the foregoing description of the preferred embodiments, which are given by way of illustration only, and the appended claims are not to be construed as limiting the scope of the invention, which is defined by the appended claims and their equivalents.
Claims (7)
1. A method for preparing aerogel particles, comprising the steps of: mixing: mixing a siloxane compound with an organic solvent to form a mixed solution, wherein the siloxane compound is contained in an amount of between 2.1 and 12.5 mol percent, and the organic solvent is contained in an amount of between 97.9 and 87.5 mol percent; a hydrolysis step: adding an acid catalyst into the mixed solution to perform hydrolysis reaction; condensation step: adding an alkali catalyst into the mixed solution to perform condensation reaction, and in the condensation reaction process, controlling the mixed solution under the sol condition, adding a hydrophobic dispersion solvent, and stirring to enable the mixed solution to be gelatinized in the stirring process to generate a plurality of aerogel particles, wherein in the condensation reaction process, the mixed solution is stirred at the speed of 1200rpm to 2000rpm, and the molar ratio of the acid catalyst to the mixed solution to the alkali catalyst to the mixed solution is 10: 10 to 10: 40, the molar ratio of the base catalyst to the acid catalyst is 1.0:1.0 to 3.0: 1.0.
2. The method of preparing aerogel particles of claim 1, wherein: the hydrophobic dispersion solvent is one or more solvents selected from the group consisting of: ketones, ethers, esters, aromatics, alkanes.
3. The method of preparing aerogel particles of claim 2, wherein: a post-treatment step is also included after the condensation step: filtering out the aerogel particles by a filter, cleaning the aerogel particles by a mixed solution of ethanol and water, and vacuum-drying the aerogel particles at a temperature of 100 ℃ to 115 ℃.
4. The method of preparing aerogel particles of claim 2, wherein: the condensation step is followed by a hydrophobic modification step: heating the mixed solution to vaporize the organic solvent, adding a chloridized organic molecule to react with a hydroxyl group of the aerogel particles to generate hydrophobicity of the aerogel particles, and preventing the aerogel particles from being broken by the hydrophobic dispersion solvent.
5. The method of preparing aerogel particles of claim 4, wherein: the chlorinated organic molecule is one or more selected from the group consisting of: chlorinated siloxanes, chloralkanes, chloranilides.
6. The method of preparing aerogel particles of claim 4, wherein: the organic solvent comprises ethanol and water which are mixed with each other; in the hydrophobicity modification step, the temperature of the mixed solution is changed into a first temperature condition, a second temperature condition and a third temperature condition in sequence, wherein the first temperature condition is 78 ℃ to 82 ℃, the second temperature condition is 100 ℃ to 115 ℃, the third temperature condition is 40 ℃ to 45 ℃, and the chloro-acylated organic molecule is added in the third temperature condition.
7. The method of preparing aerogel particles of claim 4, wherein: the method also comprises a post-treatment step after the hydrophobicity modification step: filtering out the aerogel particles by a filter, cleaning the aerogel particles by a toluene solvent, and drying the aerogel particles in vacuum.
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| CN111218024B (en) * | 2018-11-27 | 2022-05-13 | 台湾气凝胶科技材料开发股份有限公司 | Method for continuously preparing core-shell hydrophilic-hydrophobic bipolar composite aerogel powder |
| CN110898689B (en) * | 2019-09-26 | 2021-11-16 | 上海稀点新材料科技有限公司 | Flat membrane with nano porous structure and preparation method thereof |
| CN113563012B (en) * | 2020-04-29 | 2022-11-04 | 台湾气凝胶科技材料开发股份有限公司 | Preparation method of cold-resisting and heat-insulating hydrophobic aerogel composite jelly and related product thereof |
| CN113563046B (en) * | 2020-04-29 | 2023-03-14 | 台湾气凝胶科技材料开发股份有限公司 | Preparation method of high-temperature-resistant, heat-insulating and fireproof aerogel/inorganic fiber composite adhesive material and application of product thereof |
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| "Monodisperse, nonporous, spherical silica particles";J.D. Wells et al;《Colloids and Surfaces A: Physicochemical and Engineering Aspects 》;20000615;第171-176页 * |
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