CN114933307A - Preparation method of super-hydrophobic silica aerogel powder - Google Patents
Preparation method of super-hydrophobic silica aerogel powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 62
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000004965 Silica aerogel Substances 0.000 title claims description 27
- 239000004964 aerogel Substances 0.000 claims abstract description 42
- 238000001035 drying Methods 0.000 claims abstract description 31
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 19
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 13
- 239000010703 silicon Substances 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 9
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 44
- 239000008367 deionised water Substances 0.000 claims description 33
- 229910021641 deionized water Inorganic materials 0.000 claims description 33
- 239000000499 gel Substances 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 18
- 239000011240 wet gel Substances 0.000 claims description 18
- 230000032683 aging Effects 0.000 claims description 12
- 230000007062 hydrolysis Effects 0.000 claims description 10
- 238000006460 hydrolysis reaction Methods 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 230000003301 hydrolyzing effect Effects 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 3
- 230000002431 foraging effect Effects 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 239000002904 solvent Substances 0.000 abstract description 9
- 238000012986 modification Methods 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 5
- 239000007858 starting material Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000000352 supercritical drying Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 238000012643 polycondensation polymerization Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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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
- C01P2006/32—Thermal properties
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention belongs to the technical field of preparation of silicon dioxide aerogel, and particularly relates to a preparation method of super-hydrophobic silicon dioxide aerogel powder. The method takes single methyltriethoxysilane as a silicon source precursor and ammonia water as a catalyst to form gel, and the gel is aged in an absolute ethyl alcohol solution and dried under normal pressure in an air atmosphere to prepare the super-hydrophobic silicon dioxide aerogel powder. The method has the advantages of simple process, environmental protection and low cost, does not need complicated solvent replacement and gel modification steps, is simple and safe in normal-pressure drying, and is suitable for further popularization and application.
Description
Technical Field
The invention belongs to the technical field of preparation of silicon dioxide aerogel, and particularly relates to a preparation method of super-hydrophobic silicon dioxide aerogel powder.
Background
The aerogel is a unique nano-porous light functional material, consists of a solid phase particle framework and holes, has the characteristics of high specific surface area, high porosity, low density, fractal structure and the like, and has excellent performances of high thermal insulation, low sound transmission rate, ultralow dielectric constant, low refractive index and the like.
Silica aerogel bulk materials have greatly limited their use due to their great brittleness and susceptibility to cracking. Compared with the aerogel in a block form, the harsh degree of the using conditions of the powder aerogel is reduced, so that the powder aerogel has a wider application prospect, such as application to building heat-insulating coatings, 3D printing consumables, aerospace, petrochemical industry and other aspects. The drying is a key process step for producing the aerogel, and compared with the conventional supercritical drying technology for preparing the aerogel, the normal-pressure drying for preparing the aerogel powder can simplify the preparation process conditions and reduce the production cost.
The preparation method of the super-hydrophobic aerogel powder reported in the current patent mainly comprises the following steps: 1. the method comprises the steps of preparing wet gel by using a silicon source solution, a solvent, a surface modifier and the like, then performing complex solvent replacement, surface modification, solvent cleaning and the like, and finally drying to obtain the super-hydrophobic aerogel powder (such as CN 104003406A). 2. The preparation method comprises the steps of hydrolyzing, gelling, powdering, cleaning and drying methyltrimethoxysilane, water and a surfactant to obtain the super-hydrophobic aerogel powder (such as CN112125311A), wherein the surfactant is required to be added in the preparation process of the method, and the wet aerogel powder is required to be cleaned. 3. Methyl silicate is used as a precursor, acid-base catalyst and low surface tension solvent are added to prepare wet gel, and the wet gel is dried and crushed to prepare aerogel powder (such as CN 104445224B).
Disclosure of Invention
Aiming at the problems, the invention provides the normal-pressure drying preparation method of the super-hydrophobic silica aerogel powder material, which is simple in process, low in cost and environment-friendly.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation method of super-hydrophobic silica aerogel powder comprises the following steps: the method comprises the steps of taking single methyltriethoxysilane as a silicon source precursor, hydrolyzing, sol-gel, aging, and drying under normal pressure in an air atmosphere to obtain the super-hydrophobic silica aerogel powder.
The method specifically comprises the following steps:
1) uniformly mixing Methyl Triethoxysilane (MTES) and deionized water, stirring, and hydrolyzing;
2) adding a mixed solution of absolute ethyl alcohol and deionized water, and stirring to uniformly mix;
3) adding ammonia water and stirring;
4) standing the prepared sol to obtain wet gel;
5) placing the wet gel in an oven for aging treatment;
6) drying the aged wet gel under normal pressure in an air atmosphere to prepare silicon dioxide aerogel powder;
the raw materials are as follows: the volume ratio of the methyltriethoxysilane to the deionized water to the absolute ethyl alcohol is 1: (2-15): (0-10).
Preferably, the volume ratio of the methyltriethoxysilane to the deionized water in the step 1) is 1: 2.7, deionized water can be added step by step.
Preferably, in the step 1), the hydrolysis temperature is 25-30 ℃, and the hydrolysis time is 1-2 h.
Preferably, the adding amount of the ammonia water in the step 3) is 0.24-0.3 ml.
Preferably, the standing time of the sol in the step 4) is 30-60 min.
Preferably, the aging time in the step 5) is 12-24 hours, and the temperature is 25-65 ℃.
Preferably, the drying time in the step 6) is 12-24 hours, and the temperature is 50-80 ℃.
Preferably, the stirring speed in the steps 1) to 3) is 300 to 400 rpm.
The silica aerogel powder prepared by the method has the heat conductivity coefficient of 0.06-0.08W/(m.K), the water contact angle of 150-155 degrees and the average particle size of 2-12 mu m.
According to the invention, single methyltriethoxysilane is used as a silicon source precursor, ammonia water is used as a catalyst to form gel, the gel is aged in an absolute ethanol solution, and the super-hydrophobic silica aerogel powder is prepared by drying under normal pressure in an air atmosphere.
The super-hydrophobic silica aerogel powder prepared by the invention has the advantages that the gel network formed by condensation polymerization is looser by regulating and controlling the total amount of the solvent until the micron-sized network disappears to form dispersed micron-sized aerogel particles. Meanwhile, a single silicon source of methyltriethoxysilane is used to introduce a super-hydrophobic group methyl, so that the dried aerogel powder has good super-hydrophobicity, the contraction of the aerogel powder generated when water among gel frameworks is discharged during drying is reduced due to the existence of the methyl, and the particle size distribution is more uniform.
According to the invention, the total amount of the proper solvent is required to be controlled in the preparation of the super-hydrophobic silica aerogel powder under the normal pressure drying condition so as to avoid gel blocking, thereby preparing the powder with uniform particle size. Therefore, it is important to control the proper solution formulation rather than to prepare silica aerogel powder by atmospheric drying.
The invention has the following advantages:
1. according to the invention, the super-hydrophobic silica aerogel powder is prepared by normal pressure drying, so that adverse effects of high equipment requirement, high-temperature and high-pressure requirement, long period and the like caused by supercritical drying for preparing the silica aerogel powder are avoided, the preparation process is simplified, the safety is improved, and the cost is reduced.
2. The method does not need solvent replacement and gel surface modification in the normal-pressure preparation process, does not consume solvent and modifier, avoids the generation of a large amount of waste liquid in the gel surface modification process, is safe and environment-friendly, greatly reduces the synthesis process, and reduces the cost.
3. The super-hydrophobic silica aerogel powder prepared by the invention has uniform particle size and no obvious agglomeration, ensures the performance of the aerogel powder when being used as various materials, can be regulated and controlled along with preparation parameters, and can be prepared into aerogel powder materials with required particle size according to specific requirements in practical application.
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In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
FIG. 1 is a diagram of an aerogel powder prepared according to the present invention.
FIG. 2 is a scanning electron micrograph of the aerogel powder prepared in example 1 of the present invention.
Fig. 3 is a water contact angle of the aerogel powder prepared in example 1 of the present invention.
FIG. 4 shows the particle size distribution of the aerogel powder prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of super-hydrophobic silicon dioxide aerogel powder, which comprises the following steps: the method comprises the steps of taking single methyltriethoxysilane as a silicon source precursor, hydrolyzing, sol-gel, aging, and drying under normal pressure in an air atmosphere to obtain the super-hydrophobic silica aerogel powder. The method specifically comprises the following steps:
1) adding methyltriethoxysilane and deionized water into a container, uniformly mixing, and adding deionized water to ensure that the volume ratio of the methyltriethoxysilane to the deionized water is 1: 2.7. placing the container in a heat-insulating device, and hydrolyzing for 1-2 h at the temperature of 25-30 ℃ and the stirring speed of 300-400 rpm;
2) adding a mixed solution of absolute ethyl alcohol and deionized water, and stirring at 300-400 rpm to uniformly mix the absolute ethyl alcohol and the deionized water;
3) adding ammonia water into the mixed solution obtained in the step 2) and stirring at 300-400 rpm, wherein the adding amount of the ammonia water is 0.24-0.3 ml;
4) after stirring is stopped, standing the mixture in the container for 30-60 min to obtain wet gel;
5) placing the wet gel in an oven, and aging for 12-24 h at 25-65 ℃;
6) opening the container, and drying the aged wet gel at 50-80 ℃ for 12-24 h under normal pressure in an air atmosphere to obtain silicon dioxide aerogel powder; the raw materials are as follows: the volume ratio of the methyltriethoxysilane to the deionized water to the absolute ethyl alcohol is 1: (2-15): (0-10).
Example 1
5.5ml of MTES was mixed with 15ml of deionized water at 26 ℃, kept at 26 ℃ and stirred for 120min to promote hydrolysis of the silicon source, after which 8ml of deionized water, 12ml of absolute ethanol and 0.24ml of aqueous ammonia were added so that the volume ratio of the starting materials was MTES: deionized water: anhydrous ethanol: ammonia water 1: 4.2: 2.2: 0.04, continuously stirring for 5min, standing the mixed solution for 35-45 min to gel, and aging the wet gel sample for 24h at 50 ℃.
And (3) a drying process: and drying the gel sample at the normal pressure and the temperature of 60 ℃ for 24 hours to obtain the aerogel powder.
The water contact angle of the prepared aerogel powder is 151.6 degrees.
Example 2
5.5ml of MTES was mixed with 15ml of deionized water at 26 ℃, kept at 26 ℃ and stirred continuously for 120min to promote hydrolysis of the silicon source, after which 10ml of deionized water, 12ml of absolute ethanol and 0.24ml of aqueous ammonia were added so that the raw material volume ratio was MTES: deionized water: anhydrous ethanol: ammonia water 1: 4.5: 2.2: 0.04, continuously stirring for 5min, standing the mixed solution for 35-45 min to gel, and aging the wet gel sample for 24h at 50 ℃.
And (3) a drying process: and drying the gel sample at the normal pressure and the temperature of 70 ℃ for 18h to obtain the aerogel powder.
The water contact angle of the prepared aerogel powder is 154.9 degrees.
Example 3
5.5ml of MTES was mixed with 15ml of deionized water at 26 ℃, kept at 26 ℃ and stirred for 120min to promote hydrolysis of the silicon source, after which 10ml of deionized water, 15ml of absolute ethanol and 0.24ml of aqueous ammonia were added so that the volume ratio of the starting materials was MTES: deionized water: anhydrous ethanol: ammonia water 1: 4.5: 2.7: 0.4, continuously stirring for 5min, standing the mixed solution for 35-45 min to gel, and then carrying out aging treatment on the wet gel sample for 24h at the temperature of 50 ℃.
And (3) a drying process: and drying the gel sample at the normal pressure and the temperature of 50 ℃ for 24h to obtain the aerogel powder.
The water contact angle of the prepared aerogel powder is 152.7 degrees.
Example 4
5.5ml of MTES was mixed with 15ml of deionized water at 26 ℃, kept at 26 ℃ and stirred for 120min to promote hydrolysis of the silicon source, after which 6ml of deionized water, 12ml of absolute ethanol and 0.3ml of ammonia water were added so that the volume ratio of the starting materials was MTES: deionized water: anhydrous ethanol: ammonia water 1: 3.8: 2.2: 0.04, continuously stirring for 5min, standing the mixed solution for 35-45 min to gel, and aging the wet gel sample for 20h at 50 ℃.
And (3) a drying process: and drying the gel sample at the normal pressure and the temperature of 60 ℃ for 24 hours to obtain the aerogel powder.
The water contact angle of the prepared aerogel powder is 150.3 degrees.
Example 5
5.5ml of MTES was mixed with 15ml of deionized water at 26 ℃, kept at 26 ℃ and stirred for 120min to promote hydrolysis of the silicon source, after which 6ml of deionized water, 7ml of absolute ethanol and 0.3ml of ammonia water were added so that the volume ratio of the starting materials was MTES: deionized water: anhydrous ethanol: ammonia water 1: 3.8: 1.3: 0.04, continuously stirring for 5min, standing the mixed solution for 35-45 min to gel, and aging the wet gel sample for 20h at 50 ℃.
And (3) a drying process: and drying the gel sample at the normal pressure and the temperature of 75 ℃ for 24h to obtain the aerogel powder.
The water contact angle of the prepared aerogel powder is 153.6 degrees.
Example 6
5.5ml of MTES was mixed with 15ml of deionized water at 26 ℃, kept at 26 ℃ and stirred continuously for 120min to promote hydrolysis of the silicon source, after which 5ml of deionized water, 5ml of absolute ethanol and 0.3ml of aqueous ammonia were added so that the raw material volume ratio was MTES: deionized water: anhydrous ethanol: ammonia water 1: 3.6: 0.9: 0.04, continuously stirring for 5min, standing the mixed solution for 35-45 min to gel, and aging the wet gel sample for 20h at 50 ℃.
And (3) a drying process: and drying the gel sample at the normal pressure and the temperature of 80 ℃ for 12h to obtain the aerogel powder.
The water contact angle of the prepared aerogel powder is 151.2 degrees.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of super-hydrophobic silica aerogel powder is characterized by comprising the following steps: the method comprises the steps of taking single methyltriethoxysilane as a silicon source precursor, hydrolyzing, sol-gel, aging, and drying under normal pressure in an air atmosphere to obtain the super-hydrophobic silica aerogel powder.
2. The preparation method of the superhydrophobic silica aerogel powder according to claim 1, comprising the following steps:
1) uniformly mixing methyltriethoxysilane and deionized water, stirring and hydrolyzing;
2) adding a mixed solution of absolute ethyl alcohol and deionized water, and stirring to uniformly mix;
3) adding ammonia water and stirring;
4) standing the prepared sol to obtain wet gel;
5) placing the wet gel in an oven for aging treatment;
6) drying the aged wet gel under normal pressure in an air atmosphere to prepare silicon dioxide aerogel powder;
the raw materials are as follows: the volume ratio of the methyltriethoxysilane to the deionized water to the absolute ethyl alcohol is 1: (2-15): (0-10).
3. The method for preparing the superhydrophobic silica aerogel powder according to claim 2, wherein the volume ratio of the methyltriethoxysilane to the deionized water in the step 1) is 1: 2.7.
4. the preparation method of the super-hydrophobic silica aerogel powder according to claim 2, wherein the hydrolysis temperature in the step 1) is 25-30 ℃ and the hydrolysis time is 1-2 h.
5. The preparation method of the super-hydrophobic silica aerogel powder according to claim 2, wherein the amount of ammonia added in step 3) is 0.24-0.3 ml.
6. The preparation method of the superhydrophobic silica aerogel powder according to claim 2, wherein the standing time of the sol in the step 4) is 30-60 min.
7. The preparation method of the super-hydrophobic silica aerogel powder according to claim 2, wherein the aging time in the step 5) is 12-24 hours, and the temperature is 25-65 ℃.
8. The preparation method of the superhydrophobic silica aerogel powder according to claim 2, wherein the drying time in the step 6) is 12-24 hours, and the temperature is 50-80 ℃.
9. The preparation method of the super-hydrophobic silica aerogel powder according to claim 2, wherein the stirring speed in the steps 1) to 3) is 300-400 rpm.
10. The preparation method of the superhydrophobic silica aerogel powder according to any one of claims 2 to 9, wherein the prepared silica aerogel powder has a thermal conductivity of 0.06 to 0.08W/(m-K), a water contact angle of 150 to 155 °, and an average particle size of 2 to 12 μm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115849391A (en) * | 2022-12-20 | 2023-03-28 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of hydrophobic silica aerogel material |
| CN116924413A (en) * | 2023-07-14 | 2023-10-24 | 中国民用航空飞行学院 | Preparation method and application of super-hydrophobic nano powder material |
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| CN103708476A (en) * | 2014-01-07 | 2014-04-09 | 厦门大学 | Preparation method of flexible silica aerogel |
| CN111101819A (en) * | 2019-12-11 | 2020-05-05 | 石家庄铁道大学 | Preparation method of hydrophobic silica aerogel heat-insulation glass |
| US20200172696A1 (en) * | 2018-11-30 | 2020-06-04 | National Cheng Kung University | Aerogel particles and method of making the same |
| CN113264532A (en) * | 2021-05-08 | 2021-08-17 | 南京工业大学 | Super-hydrophobic light transparent high-strength SiO2Method for producing aerogels |
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| CN103708476A (en) * | 2014-01-07 | 2014-04-09 | 厦门大学 | Preparation method of flexible silica aerogel |
| US20200172696A1 (en) * | 2018-11-30 | 2020-06-04 | National Cheng Kung University | Aerogel particles and method of making the same |
| CN111101819A (en) * | 2019-12-11 | 2020-05-05 | 石家庄铁道大学 | Preparation method of hydrophobic silica aerogel heat-insulation glass |
| CN113264532A (en) * | 2021-05-08 | 2021-08-17 | 南京工业大学 | Super-hydrophobic light transparent high-strength SiO2Method for producing aerogels |
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| CN115849391A (en) * | 2022-12-20 | 2023-03-28 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of hydrophobic silica aerogel material |
| CN116924413A (en) * | 2023-07-14 | 2023-10-24 | 中国民用航空飞行学院 | Preparation method and application of super-hydrophobic nano powder material |
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