CN114933307B - 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 60
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000004965 Silica aerogel Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 27
- 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 20
- 238000000034 method Methods 0.000 claims abstract description 20
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000032683 aging Effects 0.000 claims abstract description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 14
- 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
- 239000002245 particle Substances 0.000 claims abstract description 11
- 239000002243 precursor Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 43
- 239000004964 aerogel Substances 0.000 claims description 38
- 239000008367 deionised water Substances 0.000 claims description 32
- 229910021641 deionized water Inorganic materials 0.000 claims description 32
- 238000003756 stirring Methods 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 19
- 239000011240 wet gel Substances 0.000 claims description 17
- 239000000499 gel Substances 0.000 claims description 15
- 230000007062 hydrolysis Effects 0.000 claims description 14
- 238000006460 hydrolysis reaction Methods 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 230000003301 hydrolyzing effect Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000002431 foraging effect Effects 0.000 claims description 2
- 239000002904 solvent Substances 0.000 abstract description 11
- 238000009826 distribution Methods 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 18
- 239000000243 solution Substances 0.000 description 9
- 229910021529 ammonia Inorganic materials 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000009413 insulation Methods 0.000 description 3
- 239000003607 modifier Substances 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 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
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000001276 controlling effect Effects 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
- 238000001879 gelation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000010298 pulverizing process 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
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
-
- 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
Abstract
The invention belongs to the technical field of preparation of silica aerogel, and particularly relates to a preparation method of super-hydrophobic silica aerogel powder, wherein the prepared silica aerogel powder not only maintains the advantage of low heat conductivity, but also has the characteristics of super-hydrophobicity and uniform particle size distribution. The preparation method comprises the steps of taking single methyltriethoxysilane as a silicon source precursor, taking ammonia water as a catalyst to form gel, aging in absolute ethanol solution, and drying under normal pressure in air atmosphere to obtain the super-hydrophobic silica aerogel powder. The method has the advantages of simple process, environment friendliness and low cost, does not need complex solvent replacement and gel modification steps, is simple and safe to dry under normal pressure, and is suitable for further popularization and application.
Description
Technical Field
The invention belongs to the technical field of preparation of silica aerogel, and particularly relates to a preparation method of super-hydrophobic silica aerogel powder.
Background
Aerogel is a unique nano porous light functional material, consists of solid phase particle frameworks and holes, has the characteristics of high specific surface area, high porosity, low density, fractal structure and the like, and has excellent properties of high thermal insulation, low acoustic propagation rate, ultralow dielectric constant, low refractive index and the like.
Silica aerogel bulk materials are extremely limited in their application due to their high brittleness and susceptibility to chipping. Compared with the aerogel in a block form, the powder aerogel has the advantages that the severity of the use condition is reduced, so that the powder aerogel has wider application prospect, such as application to the aspects of building heat insulation coating, 3D printing consumables, aerospace, petrochemical industry and the like. Drying is a key process step for producing aerogel, and compared with the supercritical drying technology used for conventionally preparing aerogel, the preparation of aerogel powder by adopting normal pressure drying can simplify the preparation process condition 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 preparation method comprises the steps of preparing wet gel by adopting a silicon source solution, a solvent, a surface modifier and the like, carrying out complex solvent replacement, surface modification, solvent cleaning and the like, and finally drying to obtain the super-hydrophobic aerogel powder (such as CN 104003406A), wherein the aerogel powder prepared by the method has super-hydrophobic performance and uniform particle size distribution, but the preparation process involves multi-step solvent replacement, so that the process is complex, and the used solvent and modifier have certain toxicity. 2. The super-hydrophobic aerogel powder (such as CN 112125311A) is prepared by adopting methyltrimethoxysilane, water and a surfactant through hydrolysis, gelation, pulverization, cleaning and drying, but the surfactant is added in the preparation process of the method, and the wet gel powder is required to be cleaned. 3. The method also involves solvent replacement, and the aerogel powder can be obtained by block crushing, so that the process is still complex.
Disclosure of Invention
Aiming at the problems, the invention provides a 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 above purpose, the invention is realized by the following technical scheme:
a preparation method of super-hydrophobic silica aerogel powder comprises the following steps: the preparation method comprises the steps of taking single methyltriethoxysilane as a silicon source precursor, carrying out hydrolysis, sol-gel and 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 Methyltriethoxysilane (MTES) with deionized water, and stirring and hydrolyzing;
2) Adding a mixed solution of absolute ethyl alcohol and deionized water, and stirring to uniformly mix the mixed solution;
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 the atmospheric pressure in the air atmosphere to obtain silicon dioxide aerogel powder;
the raw materials are as follows: the volume ratio of methyltriethoxysilane, deionized water and absolute ethyl alcohol is 1: (2-15): (0-10).
Preferably, the volume ratio of methyltriethoxysilane to deionized water in step 1) is 1:2.7, deionized water can be added step by step.
Preferably, the hydrolysis temperature in the step 1) is 25-30 ℃ and the hydrolysis time is 1-2 h.
Preferably, the ammonia water is added in an amount of 0.24 to 0.3ml in step 3).
Preferably, the sol in step 4) is allowed to stand for 30 to 60 minutes.
Preferably, the ageing time in step 5) is 12-24 hours and the temperature is 25-65 ℃.
Preferably, the drying time in step 6) is 12-24 hours and the temperature is 50-80 ℃.
Preferably, the stirring speed in steps 1) to 3) is 300 to 400rpm.
The silicon dioxide 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 grain diameter of 2-12 mu m.
According to the preparation method, single methyltriethoxysilane is used as a silicon source precursor, ammonia water is used as a catalyst to form gel, aging is carried out in an absolute ethyl alcohol solution, and the super-hydrophobic silica aerogel powder is prepared by normal pressure drying under an air atmosphere, so that the prepared product has uniform particle size distribution, good dispersibility and excellent heat insulation and super-hydrophobic properties.
The super-hydrophobic silica aerogel powder prepared by the invention is characterized in that the gel network formed by polycondensation is looser by regulating and controlling the total amount of the solvent until the micron-sized network disappears, so that dispersed micron-sized aerogel particles are formed. Meanwhile, the single silicon source methyltriethoxysilane is used for introducing the superhydrophobic group methyl, so that the dried aerogel powder not only has good superhydrophobicity, but also reduces shrinkage of the aerogel powder when water among gel frames is discharged during drying due to the existence of the methyl, and the particle size distribution is more uniform.
The preparation method of the super-hydrophobic silica aerogel powder under the normal pressure drying condition needs to control the total amount of the proper solvent so as to avoid gel agglomeration, thereby preparing the powder with uniform particle size. Therefore, the control of the proper solution proportion is important to the preparation of the silica aerogel powder by normal pressure drying.
The invention has the following advantages:
1. the preparation method adopts normal pressure drying to prepare the super-hydrophobic silica aerogel powder, avoids adverse effects of high equipment requirements, high-temperature and high-pressure conditions, long period and the like caused by supercritical drying preparation of the silica aerogel powder, simplifies the preparation process, improves the safety and reduces the cost.
2. The invention 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 method has uniform particle size and no obvious agglomeration, ensures the performance of the aerogel powder when the aerogel powder is used as various materials, can be regulated and controlled along with preparation parameters, and can be used for preparing aerogel powder materials with the required particle size according to specific requirements in practical application.
Drawings
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
FIG. 1 is a physical diagram of aerogel powder prepared by the invention.
FIG. 2 is a scanning electron micrograph of an aerogel powder prepared in accordance with example 1 of the present invention.
FIG. 3 shows the 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
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a preparation method of super-hydrophobic silica aerogel powder, which comprises the following steps: the preparation method comprises the steps of taking single methyltriethoxysilane as a silicon source precursor, carrying out hydrolysis, sol-gel and 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 make the volume ratio of methyltriethoxysilane to deionized water be 1:2.7. placing the container in a device capable of preserving heat, and hydrolyzing for 1-2 h at the stirring speed of 25-30 ℃ and 300-400 rpm;
2) Adding the mixed solution of absolute ethyl alcohol and deionized water, and stirring at 300-400 rpm to uniformly mix the mixed solution;
3) Adding ammonia water into the mixed solution obtained in the step 2) and stirring at 300-400 rpm, wherein the addition amount of the ammonia water is 0.24-0.3 ml;
4) After stopping stirring, standing the mixture in a container for 30-60 min to obtain wet gel;
5) Placing the wet gel in an oven, and aging for 12-24 hours at 25-65 ℃;
6) Opening the container, and drying the aged wet gel for 12-24 hours at 50-80 ℃ under normal pressure in an air atmosphere to obtain silicon dioxide aerogel powder; the raw materials are as follows: the volume ratio of methyltriethoxysilane, deionized water and absolute ethyl alcohol is 1: (2-15): (0-10).
Example 1
5.5ml of MTES was mixed with 15ml of deionized water at 26℃and kept at 26℃with continuous stirring for 120min to promote the 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 raw materials was MTES: deionized water: absolute ethyl alcohol: ammonia = 1:4.2:2.2:0.04, after stirring for 5min, standing the mixed solution until the mixed solution is gelled for 35-45 min, and then aging the wet gel sample for 24h at 50 ℃.
And (3) drying: and drying the gel sample at 60 ℃ for 24 hours under normal pressure 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℃and kept at 26℃with continuous stirring for 120min to promote the 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 volume ratio of the raw materials was MTES: deionized water: absolute ethyl alcohol: ammonia = 1:4.5:2.2:0.04, after stirring for 5min, standing the mixed solution until the mixed solution is gelled for 35-45 min, and then aging the wet gel sample for 24h at 50 ℃.
And (3) drying: and drying the gel sample at 70 ℃ for 18 hours under normal pressure 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℃and kept at 26℃with continuous stirring for 120min to promote the 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 raw materials was MTES: deionized water: absolute ethyl alcohol: ammonia = 1:4.5:2.7:0.4, after stirring for 5min, standing the mixed solution until the mixed solution is gelled for 35-45 min, and then aging the wet gel sample for 24h at 50 ℃.
And (3) drying: and drying the gel sample at 50 ℃ for 24 hours under normal pressure 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℃and kept at 26℃with continuous stirring for 120min to promote the hydrolysis of the silicon source, after which 6ml of deionized water, 12ml of absolute ethanol and 0.3ml of aqueous ammonia were added so that the volume ratio of the raw materials was MTES: deionized water: absolute ethyl alcohol: ammonia = 1:3.8:2.2:0.04, after stirring for 5min, standing the mixed solution until the mixed solution is gelled for 35-45 min, and then aging the wet gel sample for 20h at 50 ℃.
And (3) drying: and drying the gel sample at 60 ℃ for 24 hours under normal pressure 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℃and maintained at 26℃with continuous stirring for 120min to promote hydrolysis of the silicon source, after which 6ml of deionized water, 7ml of absolute ethanol and 0.3ml of aqueous ammonia were added so that the volume ratio of raw materials was MTES: deionized water: absolute ethyl alcohol: ammonia = 1:3.8:1.3:0.04, after stirring for 5min, standing the mixed solution until the mixed solution is gelled for 35-45 min, and then aging the wet gel sample for 20h at 50 ℃.
And (3) drying: and drying the gel sample at 75 ℃ for 24 hours under normal pressure 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℃and maintained at 26℃with continuous stirring 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 volume ratio of raw materials was MTES: deionized water: absolute ethyl alcohol: ammonia = 1:3.6:0.9:0.04, after stirring for 5min, standing the mixed solution until the mixed solution is gelled for 35-45 min, and then aging the wet gel sample for 20h at 50 ℃.
And (3) drying: and drying the gel sample at 80 ℃ for 12 hours under normal pressure to obtain the aerogel powder.
The water contact angle of the prepared aerogel powder is 151.2 degrees.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the 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 scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (5)
1. The preparation method of the super-hydrophobic silica aerogel powder is characterized by comprising the following steps: the preparation method comprises the steps of taking single methyltriethoxysilane as a silicon source precursor, carrying out hydrolysis, sol-gel and aging, and drying under normal pressure in an air atmosphere to obtain the super-hydrophobic silica aerogel powder, wherein the method specifically comprises the following steps:
1) Uniformly mixing methyltriethoxysilane and deionized water, and stirring and hydrolyzing; wherein, the volume ratio of methyltriethoxysilane to deionized water is 1:2.7; the hydrolysis temperature is 25-30 ℃, and the hydrolysis time is 1-2 hours;
2) Adding a mixed solution of absolute ethyl alcohol and deionized water, and stirring to uniformly mix the mixed solution;
3) Adding ammonia water and stirring; wherein the addition amount of the ammonia water is 0.24-0.3 ml;
4) Standing the prepared sol to obtain wet gel;
5) Placing the wet gel in an oven for aging treatment; aging for 12-24 hours at 25-65 ℃;
6) Drying the aged wet gel under the atmospheric pressure in the air atmosphere to obtain silicon dioxide aerogel powder;
the raw materials are as follows: the volume ratio of methyltriethoxysilane, deionized water and absolute ethyl alcohol is 1: (2-15): (0-10).
2. The method for preparing the super-hydrophobic silica aerogel powder according to claim 1, wherein the sol standing time in the step 4) is 30-60 min.
3. The method for preparing the super-hydrophobic silica aerogel powder according to claim 1, wherein the drying time in the step 6) is 12-24 hours, and the temperature is 50-80 ℃.
4. The method for preparing the super-hydrophobic silica aerogel powder according to claim 1, wherein the stirring speed in the steps 1) to 3) is 300 rpm to 400rpm.
5. The method for preparing the super-hydrophobic silica aerogel powder according to any one of claims 2 to 4, wherein the thermal conductivity of the prepared silica aerogel powder is 0.06 to 0.08W/(m.k), the water contact angle is 150 to 155 degrees, and the average particle size is 2 to 12 μm.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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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