CN114162827A - High-temperature-resistant hydrophobic SiO2Preparation method of aerogel heat insulation composite material - Google Patents
High-temperature-resistant hydrophobic SiO2Preparation method of aerogel heat insulation composite material Download PDFInfo
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Abstract
Provides a high-temperature resistant hydrophobic SiO2The preparation method of the aerogel heat insulation composite material comprises the following steps: step one, pretreatment: mixing SiO2Putting the aerogel heat-insulation composite material into a muffle furnace for pretreatment; step two, hydrophobic modification: the pretreated SiO2Placing the aerogel heat-insulation composite material and the hydrophobic modifier in a sealed bottle together, sealing the bottle opening, and then placing the bottle opening in a constant-temperature oven for heat preservation for a period of time; step three, drying: SiO treated by the second step2Taking the aerogel heat-insulation composite material out of the sealed bottle, putting the aerogel heat-insulation composite material into a muffle furnace, heating the aerogel heat-insulation composite material to a certain temperature range, and then preserving heat to remove hydrophobic reagents and reaction byproducts on the surface and inside of the aerogel heat-insulation composite material so as to obtain the high-temperature-resistant hydrophobic SiO2Aerogel heat insulation composite materialThe material has good hydrophobicity which is consistent in performance below 500 ℃, reduces the thermal conductivity of the material on the basis of not changing the structure of the nano-pores, and effectively improves the thermal insulation performance of the material.
Description
Technical Field
The invention relates to the technical field of nano porous materials, in particular to high-temperature-resistant hydrophobic SiO2A preparation method of an aerogel heat insulation composite material.
Background
SiO2The aerogel heat-insulation composite material is used as a high-efficiency heat-insulation and heat-preservation material and is widely applied to the fields of aerospace, petrochemical industry and the like. However, the material has hydrophilicity due to the porous characteristic and a large amount of hydroxyl (-OH) on the surface, and is easy to adsorb moisture in a humid environment, so that the thermal conductivity is increased, and the thermal insulation performance is reduced. Therefore, the application range of the hydrophobic modified polyurethane can be greatly expanded by carrying out hydrophobic modification on the hydrophobic modified polyurethane.
Preparation of hydrophobic SiO2Methods for aerogel materials are largely divided into in situ methods and surface post-treatment methods. The in-situ method is that hydrophobic modifier containing hydrophobic groups and siloxane solution are mixed and then are subjected to sol-gel to directly form hydrophobic SiO2Gelling and drying to obtain hydrophobic SiO2An aerogel. For example, chinese patent CN112320808A discloses a method for preparing transparent hydrophobic aerogel, which comprises using methyl orthosilicate as a silicon source, adding methyltrimethoxysilane, performing acid-base two-step catalysis to form hydrogel, performing ethanol displacement to obtain alcogel, and performing supercritical drying to obtain transparent hydrophobic aerogel. Flexible bulk hydrophobic SiO of Huyin, et al (Huyin, Zhang Ping, Huangdongmei, et al)2Preparation and characterization of aerogels [ J]The silicate bulletin, 2013,000(008): 1037-.]Mixing methyltrimethoxysilane and ethanol, preparing wet gel by an acid-base two-step method, adding a mixed solution of ethanol/ethyl orthosilicate, and preparing the flexible hydrophobic aerogel with the contact angle of 127 DEG after gelling, aging and drying, wherein the hydrophobic SiO prepared by the method2The aerogel heat insulation composite material can only meet the use requirement of a high-temperature environment below 250 ℃. Rao et al [ Rao A V, Kim S Y, Yoo K P.Low-dense, hydrobic aerogels [ J ]].Journal of Non-Crystalline Solids,1995,186:18-22.]Using Tetraethoxysilane (TEOS) as silicon source and phenyl triethoxy siliconHydrophobic SiO which can resist the high temperature of 520 ℃ is prepared by taking alkane (PTES) as a co-precursor through sol-gel2Aerogel, but the preparation process of the aerogel takes 27 days of gelation process at the longest and the process period is longer.
The surface post-treatment method is to use SiO2For example, chinese patent CN110157034A proposes mixing and emulsifying a water dispersion of nanocellulose and a polymer solution to obtain a Pickering emulsion gel, freeze-drying to obtain a nanocellulose/polymer composite aerogel, impregnating the aerogel with a mixed solution of glacial acetic acid, deionized water, absolute ethyl alcohol and methyl hydrogen siloxane, adjusting to a suitable pH value with ammonia water, and finally freeze-drying to obtain a hydrophobic aerogel porous material. The hydrophobic modification process used by the method is complex, and the reagents are various in types. Hydrophobic modification and normal pressure drying of Wangfei silicon dioxide aerogel]Beijing, university of chemical industry.]The hydrophobic SiO is prepared by using tetraethoxysilane as a silicon source and a mixed solution of trimethylchlorosilane and n-heptane as a modifier through solvent replacement, aging, hydrophobic modification and drying2Aerogel and mullite fiber as reinforcement to prepare hydrophobic SiO2The contact angle of the aerogel heat insulation composite material can reach 145 degrees, and the hydrophobic composite material can meet the application requirement under the high-temperature environment of 269 ℃. Research on Chenyimin [ Chenyimin. Metal/silica composite aerogel and Low-cost hydrophobic silica aerogel [ D]Changsha, national defense science and technology university.]Taking polydiethoxysiloxane as a silicon source, performing sol-gel, solution replacement and aging to obtain alcogel, then taking hexamethyldisilazane, hexamethyldisiloxane or trimethylchlorosilane as a hydrophobic modifier to perform hydrophobic modification on the alcogel, repeatedly performing solvent replacement by using ethanol and n-hexane for multiple times to take out the hydrophobic modifier in the alcogel, wherein 24 hours are needed for each replacement, and then drying under normal pressure to prepare the hydrophobic aerogel with a contact angle of more than 120 degrees, wherein the temperature resistance is about 280 ℃. However, this method requires a more complex and time-consuming solvent replacement process, increases the cost of aerogel production, and uses thisThe thermal stability of the hydrophobic aerogel prepared by the method still needs to be improved.
In summary, how to prepare the high temperature resistant hydrophobic SiO by a simple and low cost process2Aerogel insulation composites are a key issue that currently needs to be addressed. The invention provides a gas phase modification method for SiO finished products2The aerogel heat-insulating composite material is subjected to hydrophobic modification, so that hydrophobic SiO is simplified2The production process of the aerogel improves the high-temperature resistance, the hydrophobic property and the heat insulation performance to a certain extent.
Disclosure of Invention
The invention aims to provide high-temperature-resistant hydrophobic SiO2The preparation method of the aerogel heat-insulation composite material has simple preparation process, and the obtained hydrophobic SiO2The aerogel heat insulation composite material can keep good hydrophobic property below 500 ℃, and can reduce the heat conductivity thereof and improve the heat insulation property of the material on the basis of not changing the nano network structure thereof.
The invention uses hydrophobic modifiers such as phenyltriethoxysilane, phenyltrimethoxysilane, methylphenyldimethoxysilane and the like to react SiO2The aerogel heat insulation composite material is subjected to hydrophobic modification, so that-Si-OH on the surface of the aerogel heat insulation composite material is converted into a low-surface-functional group with hydrophobicity, and the aerogel heat insulation composite material has hydrophobic performance in a high-temperature environment resistant to 500 ℃. The method has simple process and low cost, and the obtained hydrophobic SiO2The aerogel heat-insulating composite material has good high-temperature-resistant hydrophobic property and heat-insulating property, and the application scene of the aerogel heat-insulating composite material is greatly expanded.
The technical scheme of the invention is that the invention relates to a high temperature resistant hydrophobic SiO2The preparation method of the aerogel heat insulation composite material comprises the following steps:
step one, pretreatment:
mixing SiO2Pretreating the aerogel heat-insulation composite material in a muffle furnace, heating to 200-400 ℃ at the speed of 1-5 ℃/min, and preserving heat for 1-3 h to ensure that organic groups such as ester groups, methyl groups and the like on the surface and in holes of the composite material are all converted into-OH, so as to complete surface hydroxylation and serve as hydrophobic groupsThe clusters provide reaction sites.
Step two, hydrophobic modification:
the pretreated SiO2Putting the aerogel heat-insulation composite material and the hydrophobic modifier into a sealed bottle according to the mass ratio of 1: 0.1-3, then putting the sealed bottle into a constant-temperature oven at 70-200 ℃, preserving heat for 1-3 days to enable the liquid hydrophobic modifier to slowly evaporate into a gas phase, and reacting with SiO2the-OH reaction on the aerogel heat insulation composite material is converted into a low surface energy functional group with hydrophobic property, so that the aerogel heat insulation composite material has hydrophobic property.
The hydrophobic modifier used in the experiment is any one or a combination of several of phenyl triethoxysilane, phenyl trimethoxysilane, methyl phenyl dimethoxysilane and the like.
Step three, drying:
SiO subjected to gas phase modification2Taking the aerogel heat-insulation composite material out of the sealed bottle, putting the aerogel heat-insulation composite material into a muffle furnace, raising the temperature to 170-280 ℃ at the speed of 1-5 ℃/min, preserving the heat for 1-3 h, removing hydrophobic reagents and reaction byproducts physically adsorbed on the surface and inside of the material, and obtaining the high-temperature-resistant hydrophobic SiO2Aerogel thermal insulation composite.
The invention has the following beneficial effects:
(1) hydrophobic SiO prepared by the invention2The aerogel heat insulation composite material has good hydrophobic property and thermal stability. After the pretreatment meeting certain conditions, the-OH on the surface of the hydrophilic aerogel can perform substitution reaction with hydrophobic groups in a hydrophobic modifier, and after the hydrophobic modification is finished, when the substitution number of the-OH by the hydrophobic groups reaches a certain scale, the contact angle between the composite material and water can reach about 140 degrees, the hydrophobic property can be maintained and not be attenuated after the composite material is respectively subjected to heat treatment for 1800s at 300 ℃, 400 ℃ and 500 ℃ in a muffle furnace air atmosphere, and the contact angle can still be kept about 140 degrees.
(2) The invention is on SiO2The aerogel heat-insulating composite material does not change the internal nano-network structure after finishing hydrophobic modification, and can reduce the heat conductivity of the material to a certain degree, thereby improving the heat-insulating property.
(3) The preparation process is simpleThe cost is low, and batch preparation and production can be realized. The invention takes phenyltriethoxysilane, phenyltrimethoxysilane, methylphenyldimethoxysilane and the like as hydrophobic modifiers, and can be used for preparing SiO finished products2And carrying out hydrophobic modification on the aerogel heat insulation composite material. The invention greatly simplifies the traditional SiO2The hydrophobic modification process of the aerogel heat insulation composite material, the equipment used in the method is simple, the process cost is low, and the method is suitable for industrial production.
Drawings
These and/or other aspects and advantages of the present invention will become more apparent and more readily appreciated from the following detailed description of the embodiments of the invention, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a process for preparing high temperature-resistant hydrophobic SiO in the examples of the present invention2A flow diagram of an aerogel thermal insulation composite;
FIG. 2 shows the high temperature resistant hydrophobic SiO obtained in example 2 of the present invention2Photo of aerogel thermal insulation composite material and contact angle test photo thereof, wherein (a) is the obtained high temperature resistant hydrophobic SiO2The aerogel heat insulation composite material is characterized in that the upper surface of the aerogel heat insulation composite material is provided with water beads in a round ball shape; (b) contact angle test for the water bead in graph (a);
FIG. 3 shows the high temperature resistant hydrophobic SiO obtained in example 2 of the present invention2The contact angles of the aerogel heat insulation composite material after heat treatment for 1800s at 300 ℃, 400 ℃ and 500 ℃ respectively, wherein (a) is the contact angle after heat treatment for 1800s at 300 ℃; (b) contact angle after heat treatment at 400 ℃ for 1800 s; (c) the contact angle is after heat treatment at 500 ℃ for 1800 s.
FIG. 4 is a hydrophobic SiO solid in example 2 of the invention2Aerogel and hydrophilic SiO2Microstructure of aerogel and its N2Adsorption-desorption profiles, wherein (a) is a microscopic structure diagram of the hydrophobic aerogel and (b) is an enlarged view of the portion identified in (a); (c) is a microscopic structure diagram of the hydrophilic aerogel, (d) is an enlarged view of the part identified in (c); (e) n as two aerogels2Adsorption-desorption curve chart.
FIG. 5 is a high temperature resistant hydrophobic SiO solid in example 2 of the present invention2Thermal conductivity of aerogel thermal insulation composite material and non-hydrophobically modified SiO2Thermal conductivity of aerogel insulation composite is plotted against thermal conductivity.
Detailed Description
In order that those skilled in the art will better understand the present invention, the following detailed description of the invention is provided in conjunction with the accompanying drawings and the detailed description of the invention.
Example 1
High-temperature-resistant hydrophobic SiO2The preparation method of the aerogel heat insulation composite material has the process flow as shown in figure 1, and comprises the following steps:
the first step is as follows: mixing SiO2Putting the aerogel heat-insulation composite material into a muffle furnace for pretreatment, heating to 200 ℃ at the speed of 1 ℃/min, and preserving heat for 2 h;
the second step is that: the pretreated SiO2The aerogel heat-insulation composite material and phenyl triethoxysilane are placed into a sealed bottle according to the mass ratio of 1:0.1, the bottle opening is sealed, and then the sealed bottle is placed into a constant-temperature oven at 70 ℃ for heat preservation and reaction for 2 days.
The third step: the hydrophobically modified SiO2Taking the aerogel heat-insulation composite material out of the sealed bottle, putting the aerogel heat-insulation composite material into a muffle furnace, raising the temperature to 170 ℃ at the speed of 1 ℃/min, and preserving the temperature for 1h to obtain hydrophobic SiO2Aerogel thermal insulation composite.
Hydrophobic SiO prepared in example 12The aerogel thermal insulation composite material, the weight gain ratio and the contact angle data after the thermal treatment at different temperatures are shown in table 1.
Example 2
The first step is as follows: mixing SiO2The aerogel heat insulation composite material is put into a muffle furnace for pretreatment, and is heated to 260 ℃ at the speed of 3 ℃/min and is kept warm for 1 h.
The second step is that: the pretreated SiO2The aerogel heat-insulation composite material and phenyl triethoxysilane are placed into a sealed bottle according to the mass ratio of 1:0.5, the bottle opening is sealed, and then the sealed bottle is placed into a constant-temperature oven at 100 ℃ for heat preservation and reaction for 1 day.
The third step: the hydrophobically modified SiO2Taking the aerogel heat-insulating composite material out of the sealed bottle, putting the aerogel heat-insulating composite material into a muffle furnace, raising the temperature to 190 ℃ at the speed of 2 ℃/min, and preserving the temperature for 2h to obtain the high-temperature-resistant hydrophobic SiO2Air condensationGlue a thermal insulation composite.
Example 2 preparation of high temperature resistant hydrophobic SiO2The aerogel thermal insulation composite material, the weight gain ratio and the contact angle data after the thermal treatment at different temperatures are shown in table 1.
FIG. 2 shows the high temperature resistant hydrophobic SiO obtained in this example2The photo of the aerogel heat-insulating composite material and the contact angle test photo thereof can show that the SiO prepared by the invention2The aerogel composite material has excellent hydrophobic property, and the contact angle between the aerogel composite material and water can reach more than 140 degrees;
FIG. 3 shows the high temperature resistant hydrophobic SiO obtained in this example2The contact angles of the aerogel heat insulation composite material after heat treatment for 1800s at 300 ℃, 400 ℃ and 500 ℃ respectively, wherein (a) is the contact angle after heat treatment for 1800s at 300 ℃; (b) contact angle after heat treatment at 400 ℃ for 1800 s; (c) the contact angle of the hydrophobic SiO prepared by the invention is the contact angle after heat treatment for 1800s at 500 DEG, and can be seen from the figure2The aerogel composite material can still keep the hydrophobic property unchanged after being subjected to high-temperature heat treatment at 500 ℃, and has excellent high-temperature-resistant hydrophobic property; FIG. 4 shows the hydrophobic SiO obtained in this example2Aerogel and hydrophilic SiO2Microstructure of aerogel and its N2Adsorption-desorption profiles, wherein (a) is a microscopic structure diagram of the hydrophobic aerogel and (b) is an enlarged view of the portion identified in (a); (c) is a microscopic structure diagram of the hydrophilic aerogel, (d) is an enlarged view of the part identified in (c); (e) n as two aerogels2The adsorption-desorption curve shows that the hydrophilic SiO is treated by using the invention2After the aerogel composite material is subjected to hydrophobic modification, the microstructure of the aerogel composite material cannot be adversely affected; FIG. 5 shows the high temperature resistant hydrophobic SiO obtained in this example2Aerogel heat insulation composite material thermal conductivity and non-hydrophobic modified SiO2Thermal conductivity of aerogel thermal insulation composite material is compared with a graph, and SiO subjected to hydrophobic modification by using the method can be seen from the graph2The heat insulation performance of the aerogel composite material is improved to a certain degree, and the thermal conductivity is reduced by about 0.01 W.m-1·K-1。
Example 3
The first step is as follows: mixing SiO2The aerogel heat insulation composite material is put into a muffle furnace for pretreatment, heated to 300 ℃ at the speed of 4 ℃/min and kept for 3 h.
The second step is that: the pretreated SiO2Putting the aerogel heat-insulation composite material and phenyl trimethoxy silane into a sealed bottle according to the mass ratio of 1:2, sealing the bottle mouth, then putting the bottle mouth into a constant-temperature oven at 200 ℃, and carrying out heat preservation reaction for 1 day.
The third step: the hydrophobically modified SiO2Taking the aerogel heat-insulating composite material out of the sealed bottle, putting the aerogel heat-insulating composite material into a muffle furnace, raising the temperature to 280 ℃ at the speed of 5 ℃/min, and preserving the temperature for 1h to obtain the high-temperature-resistant hydrophobic SiO2Aerogel thermal insulation composite.
Example 3 preparation of high temperature resistant hydrophobic SiO2The aerogel thermal insulation composite material, the weight gain ratio and the contact angle data after the thermal treatment at different temperatures are shown in table 1.
Example 4
The first step is as follows: mixing SiO2The aerogel heat insulation composite material is put into a muffle furnace for pretreatment, and is heated to 360 ℃ at the speed of 5 ℃/min for heat preservation for 2 h.
The second step is that: the pretreated SiO2The aerogel heat-insulation composite material and the methyl phenyl dimethoxy silane are placed into a sealed bottle according to the mass ratio of 1:3, the bottle opening is sealed, and then the sealed bottle is placed into a constant-temperature oven at 200 ℃ for heat preservation reaction for 3 days.
The third step: the hydrophobically modified SiO2Taking the aerogel heat-insulating composite material out of the sealed bottle, putting the aerogel heat-insulating composite material into a muffle furnace, raising the temperature to 170 ℃ at the speed of 3 ℃/min, and preserving the temperature for 1h to obtain the high-temperature-resistant hydrophobic SiO2Aerogel thermal insulation composite.
Example 4 preparation of high temperature resistant hydrophobic SiO2The aerogel thermal insulation composite material, the weight gain ratio and the contact angle data after the thermal treatment at different temperatures are shown in table 1.
Example 5
The first step is as follows: mixing SiO2The aerogel heat insulation composite material is put into a muffle furnace for pretreatment, and is heated to 200 ℃ at the speed of 1 ℃/min and is kept warm for 1 h.
The second step is that: the pretreated SiO2Aerogel heat insulation composite material and phenyl trisPutting the ethoxysilane and the methyltrimethoxysilane into a sealed bottle according to the mass ratio of 1:1:1, sealing the bottle mouth, then putting the bottle into a constant-temperature oven at 150 ℃, and carrying out heat preservation reaction for 3 days.
The third step: the hydrophobically modified SiO2Taking the aerogel heat-insulating composite material out of the sealed bottle, putting the aerogel heat-insulating composite material into a muffle furnace, raising the temperature to 240 ℃ at the speed of 3 ℃/min, and preserving the temperature for 3h to obtain the high-temperature-resistant hydrophobic SiO2Aerogel thermal insulation composite.
High temperature resistant hydrophobic SiO prepared in example 52The aerogel thermal insulation composite material, the weight gain ratio and the contact angle data after the thermal treatment at different temperatures are shown in table 1.
Example 6
The first step is as follows: mixing SiO2The aerogel heat insulation composite material is put into a muffle furnace for pretreatment, and is heated to 400 ℃ at the speed of 1 ℃/min for heat preservation for 3 h.
The second step is that: the pretreated SiO2The aerogel heat-insulation composite material, the phenyltriethoxysilane and the methylphenyldimethoxysilane are placed into a sealed bottle according to the mass ratio of 1:1:0.5, the bottle mouth is sealed, and then the sealed bottle is placed into a constant-temperature oven at 170 ℃ for heat preservation and reaction for 1 day.
The third step: the hydrophobically modified SiO2Taking the aerogel heat-insulation composite material out of the sealed bottle, putting the aerogel heat-insulation composite material into a muffle furnace, raising the temperature to 270 ℃ at the speed of 1 ℃/min, and preserving the temperature for 2h to obtain the high-temperature-resistant hydrophobic SiO2Aerogel thermal insulation composite.
Example 6 preparation of high temperature resistant hydrophobic SiO2The aerogel thermal insulation composite material, the weight gain ratio and the contact angle data after the thermal treatment at different temperatures are shown in table 1.
Example 7
The first step is as follows: mixing SiO2The aerogel heat insulation composite material is put into a muffle furnace for pretreatment, heated to 200 ℃ at the speed of 3 ℃/min and kept for 2 h.
The second step is that: the pretreated SiO2The aerogel heat-insulation composite material, the methyltrimethoxysilane and the methylphenyl dimethoxysilane are placed into a sealed bottle according to the mass ratio of 1:1, the bottle opening is sealed, and then the sealed bottle is placed into a constant-temperature oven at 180 ℃ for heat preservation and reaction for 2 days.
The third step: the hydrophobically modified SiO2Taking the aerogel heat-insulation composite material out of the sealed bottle, putting the aerogel heat-insulation composite material into a muffle furnace, raising the temperature to 200 ℃ at the speed of 1 ℃/min, and preserving the heat for 1h to obtain the high-temperature-resistant hydrophobic SiO2Aerogel thermal insulation composite.
High temperature resistant hydrophobic SiO prepared in example 72The aerogel thermal insulation composite material, the weight gain ratio and the contact angle data after the thermal treatment at different temperatures are shown in table 1.
TABLE 1 sample weighting and contact angles for the different examples
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (6)
1. High-temperature-resistant hydrophobic SiO2The preparation method of the aerogel heat insulation composite material is characterized by comprising the following steps:
step one, pretreatment:
mixing SiO2The aerogel heat-insulating composite material is put into a muffle furnace for pretreatment to promote SiO2The surface hydroxylation of the surface and the internal pore surface of the aerogel heat-insulation composite material is completed, and reaction sites are provided for hydrophobic groups;
step two, hydrophobic modification:
the pretreated SiO2Placing the aerogel heat-insulating composite material and the hydrophobic modifier in a sealed bottle together, and then placing the sealed bottle in a constant-temperature oven to ensure that the gas-phase hydrophobic modifier and SiO2Carrying out substitution reaction on the aerogel heat insulation composite material;
step three, drying:
SiO treated by the second step2Taking the aerogel heat-insulation composite material out of the sealed bottle, putting the aerogel heat-insulation composite material into a muffle furnace, heating to a certain temperature, preserving the temperature for a period of time, removing redundant hydrophobic reagents and reaction byproducts on the surface and inside the material, and obtaining the high-temperature-resistant hydrophobic SiO2Aerogel thermal insulation composite.
2. The high temperature resistant hydrophobic SiO of claim 12The preparation method of the aerogel heat insulation composite material is characterized in that,
the hydrophobic modifier in the second step is one or the combination of several of phenyl triethoxysilane, phenyl trimethoxysilane and methyl phenyl dimethoxysilane.
3. The high temperature resistant hydrophobic SiO of claim 12The preparation method of the aerogel heat insulation composite material is characterized in that,
in the second step, the pretreated SiO2The mass ratio of the aerogel heat-insulating composite material to the hydrophobic modifier is 1 (0.1-3).
4. The high temperature resistant hydrophobic SiO of claim 12The preparation method of the aerogel heat insulation composite material is characterized in that,
in the first step, SiO2The method for pretreating the aerogel heat-insulation composite material in the muffle furnace comprises the following steps: and (3) raising the temperature in the muffle furnace to 200-400 ℃ at a temperature raising rate of 1-5 ℃/min, and then preserving the heat for 1-3 h.
5. The high temperature resistant hydrophobic SiO of claim 12The preparation method of the aerogel heat-insulation composite material is characterized in that in the second step, the temperature of a constant-temperature oven is set to be 70-200 ℃, and the heat preservation time is 1-3 days.
6. The high temperature resistant hydrophobic SiO of claim 12The preparation method of the aerogel heat insulation composite material is characterized in that in the third step,SiO treated by the second step2After the aerogel heat-insulation composite material is placed into a muffle furnace, the temperature in the muffle furnace is increased to 170-280 ℃ at the heating rate of 1-5 ℃/min, and then the heat is preserved for 1-3 h.
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| CN115490484A (en) * | 2022-10-26 | 2022-12-20 | 郑州大学 | Foam concrete of cement fly ash system and preparation method thereof |
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| US20200255295A1 (en) * | 2018-02-14 | 2020-08-13 | Lg Chem, Ltd. | Method for producing hydrophobic silica aerogel granules |
| CN113372754A (en) * | 2021-07-09 | 2021-09-10 | 福建蓝烟新材料有限公司 | Preparation and application of water-based silicon dioxide slurry |
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| CN106007652A (en) * | 2016-05-17 | 2016-10-12 | 南京工业大学 | Preparation method of high-temperature-resistant and hydrophobic SiO2 aerogel felt |
| US20200255295A1 (en) * | 2018-02-14 | 2020-08-13 | Lg Chem, Ltd. | Method for producing hydrophobic silica aerogel granules |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115490484A (en) * | 2022-10-26 | 2022-12-20 | 郑州大学 | Foam concrete of cement fly ash system and preparation method thereof |
| CN115490484B (en) * | 2022-10-26 | 2023-09-22 | 郑州大学 | Foam concrete of cement fly ash system and preparation method thereof |
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| CN114162827B (en) | 2023-10-03 |
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