CN113247911A - Modification method of silicon dioxide aerogel - Google Patents
Modification method of silicon dioxide aerogel Download PDFInfo
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- CN113247911A CN113247911A CN202110647314.0A CN202110647314A CN113247911A CN 113247911 A CN113247911 A CN 113247911A CN 202110647314 A CN202110647314 A CN 202110647314A CN 113247911 A CN113247911 A CN 113247911A
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- 239000004964 aerogel Substances 0.000 title claims abstract description 68
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000000377 silicon dioxide Substances 0.000 title abstract description 16
- 235000012239 silicon dioxide Nutrition 0.000 title abstract description 16
- 238000002715 modification method Methods 0.000 title abstract description 6
- 239000003607 modifier Substances 0.000 claims abstract description 54
- 239000011261 inert gas Substances 0.000 claims abstract description 52
- 239000007789 gas Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 239000004965 Silica aerogel Substances 0.000 claims description 23
- 239000012779 reinforcing material Substances 0.000 claims description 19
- 239000000835 fiber Substances 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 9
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 8
- AAPLIUHOKVUFCC-UHFFFAOYSA-N trimethylsilanol Chemical compound C[Si](C)(C)O AAPLIUHOKVUFCC-UHFFFAOYSA-N 0.000 claims description 8
- 238000010926 purge Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 6
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 6
- 239000003365 glass fiber Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000004642 Polyimide Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000007710 freezing Methods 0.000 claims description 3
- 230000008014 freezing Effects 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 229920000728 polyester Polymers 0.000 claims description 3
- 229920001721 polyimide Polymers 0.000 claims description 3
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 3
- 229920006231 aramid fiber Polymers 0.000 claims description 2
- 239000010425 asbestos Substances 0.000 claims description 2
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims description 2
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 2
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 2
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011490 mineral wool Substances 0.000 claims description 2
- 229910052895 riebeckite Inorganic materials 0.000 claims description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 2
- 239000004760 aramid Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 238000007664 blowing Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 description 12
- 238000012986 modification Methods 0.000 description 12
- 238000013329 compounding Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 230000002209 hydrophobic effect Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 239000011810 insulating material Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000003733 fiber-reinforced composite Substances 0.000 description 1
- 238000003958 fumigation Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- QABLOFMHHSOFRJ-UHFFFAOYSA-N methyl 2-chloroacetate Chemical compound COC(=O)CCl QABLOFMHHSOFRJ-UHFFFAOYSA-N 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- -1 siloxanes Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011240 wet gel 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a modification method of silicon dioxide aerogel, which comprises the following steps: putting the dried hydrophilic aerogel into a container A, and vacuumizing the container A; adding a modifier into another container B, heating to a plurality of temperatures, maintaining the temperature, introducing inert gas below the liquid level of the modifier, and forming a mixture of the modifier gas and the inert gas above the liquid level of the container B; opening the switches of the connecting pipelines of the container A and the container B under the condition of continuously introducing the inert gas, and inputting the mixture of the modifier gas and the inert gas into the container A from the container B; maintaining for a certain time to modify; and (4) blowing air or inert gas. The method takes inert gas as driving gas, and mixed gas with a certain proportion is continuously generated in the continuous introducing process, so that the aerogel can be continuously modified; can generate mixed gas of the modifier and the inert gas at a lower temperature, and can also improve the reaction safety.
Description
Technical Field
The invention relates to the technical field of silicon dioxide aerogel, in particular to a modification method of silicon dioxide aerogel.
Background
Aerogel is a solid amorphous material with a nano porous network structure, has the advantages of low density, low heat conductivity coefficient and the like, and is highly concerned by academia and industry as an excellent light heat-insulating material at present; wherein, the common silicon dioxide aerogel and the fiber reinforced composite material thereof have been produced on a large scale at home and abroad. In practical use, since aerogel is an open-cell and porous material, the moisture absorbed and adsorbed in air has a negative effect on thermal conductivity, and even causes performance failure. It is therefore important to have good hydrophobicity. Therefore, in the production of aerogel materials, hydrophobization of aerogels with poor or hydrophilic properties is a very important step.
In the known art, the hydrophobicization treatment consists of a modification before drying and a modification after drying of the aerogel. The former is mainly to add a hydrophobizing agent to a precursor for copolymerization or to soak a wet gel in an organic solvent containing a hydrophobizing modifying agent, thereby reacting hydrophilic groups on the surface of the gel with the hydrophobic groups to obtain hydrophobized groups. Such methods can provide aerogel materials with good hydrophobicity, but also have some disadvantages: on one hand, before the reaction with the hydrophilic groups on the surface of the aerogel, the hydrophobic modification reagent reacts with water and alcohols in the aerogel, so that the utilization rate of the modifier is reduced; in addition, because of the large amount of organic solvent used, the safety in large-scale production is great; meanwhile, the recovery and treatment of the solvent also become a negative factor in production under the increasingly severe environmental protection pressure. In addition to the two types of pre-modification methods described above, in chinese invention patent CN1241952A, it is proposed to fumigate a hydrogel with siloxane vapor in the presence of a catalyst to obtain a hydrophobic aerogel; however, in order to keep the porous structure of the gel from collapsing, the water content is required to be more than 50%, the modification temperature must be strictly controlled below 100 ℃, and similarly to the above-mentioned case, the hydrophobization modifying agent reacts with water, which affects the utilization rate of the modifying agent.
In the art of modifying aerogels after drying, US6005012 first proposed hydrophobization of aerogels with halogen-containing silane gas, and chinese invention patent CN103523790A also proposed hydrophobization of aerogels with methyl chloroacetate. Although the halogen-containing compound has higher reactivity, the residual halogen in the modified aerogel can seriously limit the application range of the aerogel; if the heat-insulating material is used as a coating, the coated metal pipeline can be continuously corroded, and the service life of the heat-insulating material is damaged. The gaseous hydrophobic modification processes based on siloxanes and silazanes are proposed in both chinese patents CN1317188C and CN109607551A, but the former uses low temperature (less than 40 ℃), and the condensation and re-volatilization of the gaseous modifier are easy to occur in the actual production, which has a certain damage to the structure of the aerogel, and may be mixed with oxygen in the air to generate explosive mixture in the actual operation; the latter uses acid catalyzed fumigation of the siloxane, the acid is highly corrosive to equipment and can remain in the product and interfere with use. Chinese patent CN104787772A reports a process of inputting trimethylsilanol, hexamethyldisilazane, and trimethylchlorosilane as gaseous hydrophobic modifiers into hydrophilic aerogel under vacuum state, setting of modification temperature and time is more beneficial to process production, the obtained aerogel also has good hydrophobicity, but preferred trimethylsilanol and hexamethyldisilazane have high gasification temperature, resulting in rapid reaction and large consumption of the modifiers, secondary drying treatment of the residual modifiers and their decomposition products is required after modification is completed, and excessive modification results in reduced combustion performance, and it is difficult to ensure that the product reaches a2 level.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a method for modifying silicon dioxide aerogel.
The technical scheme of the invention is as follows:
a method for modifying silica aerogel, comprising the following steps:
step one, putting the dried hydrophilic aerogel into a container A, and vacuumizing the container A;
step two, adding a modifier into another container B, heating to a plurality of temperatures, maintaining the temperatures, and introducing inert gas until the temperature is below the liquid level of the modifier, wherein a mixture of the modifier gas and the inert gas is formed above the liquid level of the container B;
step three, opening the switch of the connecting pipeline of the container A and the container B under the condition of continuously introducing the inert gas, and inputting the mixture of the modifier gas and the inert gas into the container A from the container B;
step four, maintaining for a certain time to modify;
and step five, purging with air or inert gas.
Preferably, in the step one, the hydrophilic aerogel is silica aerogel and aerogel felt, plate and profile which are compounded with the reinforcing material;
further preferably, the reinforcing material is any one or combination of more of glass fiber, ceramic fiber, asbestos, rock wool, pre-oxidized fiber, polyester fiber, aramid fiber and polyimide fiber; the silica aerogel comprises aerogel dried by normal pressure, supercritical, subcritical and freezing modes.
Preferably, in the second step, the modifier includes one or more of trimethylsilanol, hexamethyldisilazane, trimethylchlorosilane, ethyl orthosilicate, methyltriethoxysilane, dimethyldiethoxysilane, methyltrimethoxysilane, dimethyldimethoxysilane, and hexamethyldisiloxane.
Preferably, in the second step, the temperature is from 30 ℃ below the boiling point temperature of the modifier to 20 ℃ above the boiling point temperature, and if the modifier is a combination of more than one compound, the boiling point is lower.
Preferably, in the second and fifth steps, the inert gas includes any one or a combination of more of nitrogen, argon, helium and carbon dioxide.
Preferably, in the fourth step, the time is 0.5 to 10 hours.
The modification method of the silicon dioxide aerogel has the following advantages:
1. taking inert gas as a driving gas, continuously generating mixed gas in a certain proportion in the continuous introducing process, and continuously modifying the aerogel;
2. the mixed gas of the modifier and the inert gas can be generated at a lower temperature, the concentration of the modifier in the mixed gas is lower, so that the mixed gas has better reaction selectivity and is more uniformly distributed in the container A, the condition that (1) the use amount of the modifier is larger due to nonuniform modification is avoided, and the residual modifier and the decomposition products thereof need to be dried for the second time after the modification is finished; (2) the combustion performance is reduced due to excessive modification;
3. the modifiers are dangerous chemicals, and compared with the modification of pure modifier gas, the proportion of the modified gas is reduced, and the proportion of the inert gas is increased, so that the safety risks of explosion, combustion and the like caused by leakage, static electricity and the like can be reduced.
Detailed Description
Example 1
A method for modifying silica aerogel, comprising the following steps:
step one, putting the dried hydrophilic aerogel into a container A, and vacuumizing the container A;
step two, adding a modifier into another container B, heating to a plurality of temperatures, maintaining the temperatures, and introducing inert gas until the temperature is below the liquid level of the modifier, wherein a mixture of the modifier gas and the inert gas is formed above the liquid level of the container B;
step three, opening the switch of the connecting pipeline of the container A and the container B under the condition of continuously introducing the inert gas, and inputting the mixture of the modifier gas and the inert gas into the container A from the container B;
step four, maintaining for a certain time to modify;
and step five, purging with air or inert gas.
In the first step, the hydrophilic aerogel is an aerogel felt formed by compounding silicon dioxide aerogel and a reinforcing material; the mass fraction of the reinforcing material in the aerogel felt is 55%;
the reinforcing material is glass fiber;
the silicon dioxide aerogel is an aerogel dried under normal pressure.
In the second step, the modifier is a combination of trimethylsilanol and ethyl orthosilicate in a mass ratio of 1: 1.
In the second step, the temperature is 105 ℃.
In the second and fifth steps, the inert gas is nitrogen.
In the fourth step, the time is 8 hours.
Example 2
A method for modifying silica aerogel, comprising the following steps:
step one, putting the dried hydrophilic aerogel into a container A, and vacuumizing the container A;
step two, adding a modifier into another container B, heating to a plurality of temperatures, maintaining the temperatures, and introducing inert gas until the temperature is below the liquid level of the modifier, wherein a mixture of the modifier gas and the inert gas is formed above the liquid level of the container B;
step three, opening the switch of the connecting pipeline of the container A and the container B under the condition of continuously introducing the inert gas, and inputting the mixture of the modifier gas and the inert gas into the container A from the container B;
step four, maintaining for a certain time to modify;
and step five, purging with air or inert gas.
In the first step, the hydrophilic aerogel is an aerogel felt formed by compounding silicon dioxide aerogel and a reinforcing material; the mass fraction of the reinforcing material in the aerogel felt is 62%;
the reinforcing material is a combination of glass fibers and ceramic fibers in a mass ratio of 3: 1; the silicon dioxide aerogel is dried aerogel in a supercritical mode.
In the second step, the modifier is a combination of trimethylsilanol and ethyl orthosilicate in a mass ratio of 1: 5.
In the second step, the temperature is 105 ℃.
In the second and fifth steps, the inert gas is argon.
In the fourth step, the time is 10 hours.
Example 3
A method for modifying silica aerogel, comprising the following steps:
step one, putting the dried hydrophilic aerogel into a container A, and vacuumizing the container A;
step two, adding a modifier into another container B, heating to a plurality of temperatures, maintaining the temperatures, and introducing inert gas until the temperature is below the liquid level of the modifier, wherein a mixture of the modifier gas and the inert gas is formed above the liquid level of the container B;
step three, opening the switch of the connecting pipeline of the container A and the container B under the condition of continuously introducing the inert gas, and inputting the mixture of the modifier gas and the inert gas into the container A from the container B;
step four, maintaining for a certain time to modify;
and step five, purging with air or inert gas.
In the first step, the hydrophilic aerogel is an aerogel plate formed by compounding silicon dioxide aerogel and a reinforcing material; the mass fraction of the reinforcing material in the aerogel felt is 75 percent;
the reinforcing material is a combination of glass fibers, ceramic fibers, polyester fibers and polyimide fibers in a mass ratio of 1:2:4: 3; the silicon dioxide aerogel is the aerogel dried under normal pressure.
In the second step, the modifier is trimethylsilanol.
In the second step, the temperature is 105 ℃.
In the second and fifth steps, the inert gas is helium.
In the fourth step, the time is 0.5 h.
Example 4
A method for modifying silica aerogel, comprising the following steps:
step one, putting the dried hydrophilic aerogel into a container A, and vacuumizing the container A;
step two, adding a modifier into another container B, heating to a plurality of temperatures, maintaining the temperatures, and introducing inert gas until the temperature is below the liquid level of the modifier, wherein a mixture of the modifier gas and the inert gas is formed above the liquid level of the container B;
step three, opening the switch of the connecting pipeline of the container A and the container B under the condition of continuously introducing the inert gas, and inputting the mixture of the modifier gas and the inert gas into the container A from the container B;
step four, maintaining for a certain time to modify;
and step five, purging with air or inert gas.
In the first step, the hydrophilic aerogel is a special-shaped piece formed by compounding silica aerogel and a reinforcing material; the mass fraction of the reinforcing material in the aerogel felt is 57%;
the reinforcing material is glass fiber; the silicon dioxide aerogel is an aerogel dried in a freezing mode.
In the second step, the modifier is tetraethoxysilane.
In the second step, the temperature is 155 ℃.
In the second step and the fifth step, the inert gas is the combination of nitrogen and carbon dioxide with the mass ratio of 5: 1.
In the fourth step, the time is 2 hours.
Example 5
A method for modifying silica aerogel, comprising the following steps:
step one, putting the dried hydrophilic aerogel into a container A, and vacuumizing the container A;
step two, adding a modifier into another container B, heating to a plurality of temperatures, maintaining the temperatures, and introducing inert gas until the temperature is below the liquid level of the modifier, wherein a mixture of the modifier gas and the inert gas is formed above the liquid level of the container B;
step three, opening the switch of the connecting pipeline of the container A and the container B under the condition of continuously introducing the inert gas, and inputting the mixture of the modifier gas and the inert gas into the container A from the container B;
step four, maintaining for a certain time to modify;
and step five, purging with air or inert gas.
In the first step, the hydrophilic aerogel is an aerogel felt formed by compounding silicon dioxide aerogel and a reinforcing material; the mass fraction of the reinforcing material in the aerogel felt is 48%;
the reinforcing material is ceramic fiber; the silica aerogel includes aerogel dried by normal pressure.
In the second step, the modifier is a combination of trimethylsilanol and ethyl orthosilicate in a mass ratio of 3: 1.
In the second step, the temperature is 115 ℃.
In the second and fifth steps, the inert gas is nitrogen.
In the fourth step, the time is 8 hours.
The silica aerogels prepared in examples 1 to 5 were examined as follows, and the following examination results were obtained, and the specific examination results are shown in table 1.
Table 1: physical property test results of the silica aerogels prepared in examples 1 to 5;
from the above test data, it can be seen that the silica aerogel prepared according to the present invention has very good strength and very low thermal conductivity.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. A method for modifying silica aerogel is characterized by comprising the following steps:
step one, putting the dried hydrophilic aerogel into a container A, and vacuumizing the container A;
step two, adding a modifier into another container B, heating to a plurality of temperatures, maintaining the temperatures, and introducing inert gas until the temperature is below the liquid level of the modifier, wherein a mixture of the modifier gas and the inert gas is formed above the liquid level of the container B;
step three, opening the switch of the connecting pipeline of the container A and the container B under the condition of continuously introducing the inert gas, and inputting the mixture of the modifier gas and the inert gas into the container A from the container B;
step four, maintaining for a certain time to modify;
and step five, purging with air or inert gas.
2. The method for modifying silica aerogel according to claim 1, wherein in the first step, the hydrophilic aerogel is silica aerogel and aerogel blanket, plate and profile made by combining silica aerogel with reinforcing material.
3. The method for modifying silica aerogel according to claim 2, wherein the reinforcing material is any one or a combination of more of glass fibers, ceramic fibers, asbestos, rock wool, pre-oxidized fibers, polyester fibers, aramid fibers, and polyimide fibers; the silica aerogel comprises aerogel dried by normal pressure, supercritical, subcritical and freezing modes.
4. The method for modifying silica aerogel according to claim 1, wherein in the second step, the modifying agent comprises any one or more of trimethylsilanol, hexamethyldisilazane, trimethylchlorosilane, tetraethoxysilane, methyltriethoxysilane, dimethyldiethoxysilane, methyltrimethoxysilane, dimethyldimethoxysilane, and hexamethyldisiloxane.
5. The method for modifying silica aerogel according to claim 1, wherein in the second step, the temperature is from 30 ℃ below the boiling point temperature of the modifier to 20 ℃ above the boiling point temperature, and if the modifier is a combination of more than one compound, the boiling point is lower.
6. The method for modifying silica aerogel according to claim 1, wherein said inert gas comprises any one or more of nitrogen, argon, helium, and carbon dioxide in the second and fifth steps.
7. The method for modifying silica aerogel according to claim 1, wherein in the fourth step, the time is 0.5 to 10 hours.
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| CN202110647314.0A CN113247911A (en) | 2021-06-10 | 2021-06-10 | Modification method of silicon dioxide aerogel |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114653529A (en) * | 2022-04-01 | 2022-06-24 | 巩义市泛锐熠辉复合材料有限公司 | Device and method for preparing silica aerogel felt and silica aerogel felt |
| CN114751718A (en) * | 2022-04-01 | 2022-07-15 | 巩义市泛锐熠辉复合材料有限公司 | Method for preparing hydrophobic silica aerogel felt under normal pressure |
| CN114773027A (en) * | 2022-06-16 | 2022-07-22 | 巩义市泛锐熠辉复合材料有限公司 | Aerogel felt prepared at low cost and preparation method thereof |
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