CN111171489A - Aerogel and temperature-sensitive hydrogel composite heat-insulation and heat-preservation glass - Google Patents
Aerogel and temperature-sensitive hydrogel composite heat-insulation and heat-preservation glass Download PDFInfo
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 115
- 239000011521 glass Substances 0.000 title claims abstract description 80
- 238000009413 insulation Methods 0.000 title claims abstract description 53
- 238000004321 preservation Methods 0.000 title claims abstract description 19
- 239000002131 composite material Substances 0.000 title claims description 17
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- 229910052681 coesite Inorganic materials 0.000 claims abstract description 61
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 61
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 61
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 61
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 61
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- 239000004593 Epoxy Substances 0.000 claims abstract description 4
- 229920001577 copolymer Polymers 0.000 claims abstract description 4
- 239000011148 porous material Substances 0.000 claims description 26
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 24
- 230000002209 hydrophobic effect Effects 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 17
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 12
- 239000001569 carbon dioxide Substances 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 10
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- 239000002562 thickening agent Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 238000012986 modification Methods 0.000 claims description 7
- 230000032683 aging Effects 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 229920001817 Agar Polymers 0.000 claims description 3
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 3
- 108010010803 Gelatin Proteins 0.000 claims description 3
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 3
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 3
- 239000008272 agar Substances 0.000 claims description 3
- 235000010419 agar Nutrition 0.000 claims description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 3
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 3
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- 235000011852 gelatine desserts Nutrition 0.000 claims description 3
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- 229940071826 hydroxyethyl cellulose Drugs 0.000 claims description 3
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 2
- 229940023476 agar Drugs 0.000 claims description 2
- 229940105329 carboxymethylcellulose Drugs 0.000 claims description 2
- 235000010418 carrageenan Nutrition 0.000 claims description 2
- 239000000679 carrageenan Substances 0.000 claims description 2
- 229920001525 carrageenan Polymers 0.000 claims description 2
- 229940113118 carrageenan Drugs 0.000 claims description 2
- 229940014259 gelatin Drugs 0.000 claims description 2
- 235000010413 sodium alginate Nutrition 0.000 claims description 2
- 239000000661 sodium alginate Substances 0.000 claims description 2
- 229940005550 sodium alginate Drugs 0.000 claims description 2
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 claims description 2
- 230000007774 longterm Effects 0.000 abstract description 4
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 238000011068 loading method Methods 0.000 description 5
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 4
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000000499 gel Substances 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
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- 230000008901 benefit Effects 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000007405 data analysis Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000005051 trimethylchlorosilane Substances 0.000 description 2
- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical compound [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 238000005859 coupling reaction Methods 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
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- 230000007246 mechanism Effects 0.000 description 1
- XZWYZXLIPXDOLR-UHFFFAOYSA-N metformin Chemical compound CN(C)C(=N)NC(N)=N XZWYZXLIPXDOLR-UHFFFAOYSA-N 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/24—Homopolymers or copolymers of amides or imides
- C08L33/26—Homopolymers or copolymers of acrylamide or methacrylamide
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- Silicon Compounds (AREA)
Abstract
The invention discloses aerogel and temperature-sensitive hydrogel compounded heat-insulation and heat-preservation glass, which structurally comprises a cavity formed by glass, wherein the cavity is filled with temperature-sensitive hydrogel, and the aerogel is dispersed in the temperature-sensitive hydrogel, wherein the aerogel is hydrophobically modified porous SiO2The aerogel and the temperature-sensitive hydrogel are polyacrylamide temperature-sensitive hydrogels or epoxy copolymer temperature-sensitive hydrogels. Condensing the gasAfter the glue and the temperature-sensitive hydrogel are compounded, the deformation influence on the aerogel framework caused by long-term soaking of liquid can be resisted, so that the heat insulation and heat preservation characteristics of the heat insulation and heat preservation glass are obviously enhanced, and the service life of the heat insulation and heat preservation glass is prolonged.
Description
Technical Field
The invention belongs to the field of personal care, and particularly relates to aerogel and temperature-sensitive hydrogel compounded heat-insulation and heat-preservation glass and a preparation method thereof.
Background
Aerogel is a highly porous material formed by removing the liquid solvent from the gel while maintaining the three-dimensional network structure of the gel. In the 30 s of the 20 th century, Kistler successfully prepared aerogels; since the 70 s in the 20 th century, the sol-gel technology is rapidly developed, and the related performances of the aerogel, such as ultrahigh porosity (80-99.8%), high specific surface area (100-1600 square meters/g) and ultralow density (0.004-0.500 g/cm)3) Is of equal nature toThe method has wide application prospect in the fields of optics, electricity, acoustics, thermology, catalysis and the like.
The aerogel has remarkable superiority in the aspect of serving as a high-temperature heat insulation product. The main principle of the method is that (1) convection: when the diameter of the pores in the aerogel is less than 70nm, the air molecules in the pores lose the energy of free movement and are relatively attached to the walls of the pores, and then the product is in a near vacuum condition; (2) radiation: because the pores in the aerogel are all nano-scale pores and the volume density of the product is extremely low, the number of the pore walls in the product tends to be 'excessive', each pore wall has the effect of a heat shield, and therefore the effect close to the 'excessive heat shield' occurs, and the radiation heat transfer is reduced to be nearly the lowest limit; (3) heat conduction: because of the large number of nanopores, heat flow can only be transmitted along the pore walls in the solid, and the nearly infinite number of pore walls constitute a nearly "infinite path" effect, so that the heat conduction of the solid can be reduced to nearly the lowest limit.
The heat insulation and preservation glass is a high molecular material with responsiveness to temperature, and is substantially a heat insulation temperature-sensitive hydrogel. The main principle is as follows: the solubility of the polymer material in a solution can also undergo significant reversible change along with the change of the external temperature, so that the solution is driven to undergo phase change: when the outside temperature is lower than the designated temperature, the temperature-sensitive hydrogel is transparent, and sunlight can irradiate, so that the temperature of the system can be raised by absorbing heat; when the temperature is higher than the specified temperature, the temperature-sensitive hydrogel turns into milk white, so that the transmission of sunlight is shielded, the transmittance of near infrared radiation is obviously reduced, and the process of absorbing heat by a system is hindered. According to the process, the heat insulation effect is realized.
At present, in the prior art, products prepared by compounding aerogel and temperature-sensitive hydrogel are available, and the products are mainly prepared by dispersing aerogel in the temperature-sensitive hydrogel, so that the products have the characteristics of high heat insulation and heat preservation and heat insulation. However, there are some disadvantages to mixing aerogel and temperature-sensitive hydrogel, such as one of the most obvious disadvantages is that the long-term soaking of the temperature-sensitive hydrogel may cause the possibility of collapse of the aerogel skeleton, and once the aerogel skeleton structure collapses, most of the nanopores are lost, so that the original heat preservation function of the product is lost. This is why most products made by compounding aerogel and temperature-sensitive hydrogel, such as the most representative product, i.e. heat-insulating glass, have a gradually deteriorated heat-insulating and heat-preserving effect with the increase of the usage time.
Therefore, a scheme for finding out the thermal insulation glass compounded by aerogel and temperature-sensitive hydrogel, which can effectively prevent the disadvantages and prolong the service life of the thermal insulation glass, is urgently needed.
Disclosure of Invention
The invention discloses aerogel and temperature-sensitive hydrogel compounded heat-insulation and heat-preservation glass, wherein aerogel is hydrophobically modified porous SiO2An aerogel. After the aerogel and the temperature-sensitive hydrogel are compounded, the deformation influence on an aerogel framework caused by long-term soaking of liquid can be resisted, so that the heat insulation and heat preservation characteristics of the heat insulation and heat preservation glass are obviously enhanced, and the service life of the heat insulation and heat preservation glass is prolonged.
The invention aims to disclose thermal insulation glass compounded by aerogel and temperature-sensitive hydrogel, the thermal insulation glass compounded by aerogel and temperature-sensitive hydrogel structurally comprises a cavity formed by glass, the cavity is filled with the temperature-sensitive hydrogel, the aerogel is dispersed in the temperature-sensitive hydrogel,
wherein the temperature-sensitive hydrogel is polyacrylamide temperature-sensitive hydrogel or epoxy copolymer temperature-sensitive hydrogel;
the aerogel is porous SiO subjected to hydrophobic modification2The preparation method of the aerogel comprises the following steps:
s1, preparing porous SiO2Soaking for 24-48h to obtain aged porous SiO2；
S2, ageing the porous SiO2Mixing with trialkyl coupling agent in ethanol solution, and heating to 60-80 deg.C;
s3, drying the product to obtain the product subjected to hydrophobic modificationPorous SiO of2An aerogel.
Further, the porous SiO2The specific surface area is 200-500 square meters per gram.
Further, the porous SiO2The pore volume of (A) is 0.8-1.5 ml/g.
Further, the temperature-sensitive hydrogel also comprises a thickening agent.
Further, the thickening agent is selected from one or more of gelatin, agar, carboxymethyl cellulose, sodium alginate, carrageenan or hydroxyethyl cellulose.
Further, the aged porous SiO2The amount of the material to the trialkyl coupling agent is 1:1 to 1: 1.5.
Further, the drying is supercritical drying, and the steps are as follows:
adding liquid carbon dioxide into a high-pressure reaction kettle, soaking the product in S3, sealing, introducing nitrogen, and then heating, wherein the pressure is increased along with the heating; after the carbon dioxide in the reaction kettle is converted into a supercritical fluid state, preserving the heat for 3-5h, then cooling to normal temperature and normal pressure, and naturally cooling.
Further, in the high-pressure reaction kettle, the temperature is finally increased to 40-60 ℃, and the pressure is finally increased to 7.2-9.0 MPa.
The invention also aims to disclose a preparation method of the aerogel and temperature-sensitive hydrogel compounded heat-insulation glass.
A preparation method of aerogel and temperature-sensitive hydrogel compounded heat-insulation glass comprises the following steps:
(1) filling temperature-sensitive hydrogel into the glass cavity;
(2) adding aerogel particles into the temperature-sensitive hydrogel;
(3) and sealing the glass.
Further, before sealing the glass, vacuumizing treatment is carried out.
The invention has the following beneficial effects:
the glass adopted by the invention is a product comprising aerogel and temperature-sensitive hydrogel components, so that the glass has the advantages ofHas heat insulating and heat preserving effects, and the effect is obviously superior to the similar products in the prior art. The aerogel adopted by the invention is hydrophobic modified SiO2Aerogel, which has the following advantages:
(1) general SiO2The aerogel has a three-dimensional network structure, but the terminal groups of the three-dimensional network structure are all hydroxyl groups. Thus, SiO2The molecular structure of the aerogel contains a large number of hydroxyl groups, and the aerogel has a strong hydrophilic effect. Thus, SiO in general2After the aerogel is soaked in water, a large amount of water molecules are adsorbed on SiO2The surface of the aerogel is easy to cause the aerogel to absorb a large amount of water molecules to collapse and deform. The invention discloses SiO2Aerogel which is subjected to coupling reaction with trialkyl coupling agent, wherein the trialkyl coupling agent and hydroxyl can be subjected to displacement reaction, and SiO2The hydroxyl end groups of the aerogel are replaced by hydrophobic alkyl groups, thereby completing the synthesis of SiO2And (4) performing hydrophobic modification on the aerogel. Hydrophobically modified SiO2On the one hand, the surface of the aerogel is covered with hydrophobic alkyl chains which are easy to form a film, so that the aerogel is equivalent to SiO2A film is formed between the aerogel and the water phase, and SiO is partially or completely shielded2The aerogel is contacted with the water phase, so that a barrier effect is realized; on the other hand, the surface formed by hydrophobic alkyl chains is not easily wetted and attached by moisture. In both aspects, the water is made to adhere to the hydrophobically modified SiO2Greatly reduces the probability and degree of aerogel, thereby lightening SiO2Loading of aerogel;
(2) SiO of the invention2The aerogel is SiO with a porous structure2The aerogel has the specific surface area of 200-500 square meters per gram and the pore volume of 0.8-1.5 ml/g. This surface area is sufficiently large, on the one hand, to be able to sufficiently spread out the water relative to the SiO in the case of a long-term immersion2The pressure of the aerogel is reduced, so that the pressure of water relative to SiO is relieved to a certain extent2The effect of compression set of the aerogel; sufficient pore volume can effectively release the water phase to be loaded on the SiO for a long time2The stress accumulated during the aerogel production is SiO2The micro deformation of the aerogel provides space, and Si is not caused by the micro deformationO2The aerogel is not easy to deform and collapse, and can maintain the porous aerogel structural form for a long time; on the other hand, the reason is that the temperature sensitive hydrogel is mixed with SiO2The porous structure of the aerogel acts together, which is beneficial to reducing porous SiO2The aerogel loading mechanism is as follows: the polyacrylamide temperature-sensitive hydrogel or the epoxy copolymer temperature-sensitive hydrogel in the water phase can be embedded into SiO together with the water phase2In the porous structure of the aerogel, external energy is irradiated in a water phase containing temperature-sensitive hydrogel in the porous structure, and since hydrogel substances are temperature-sensitive, the hydrogel substances are obviously different from the heat absorption coefficient of the water phase, the temperature-sensitive hydrogel absorbing the external energy is firstly heated, so that the temperature-sensitive hydrogel is equivalent to SiO with the porous structure2Countless local hot spots are generated in the aerogel, and the water phase in the porous structure is heated unevenly, so that the water phase containing the temperature-sensitive hydrogel component is heated in the porous SiO2In the porous structure of the aerogel, the water phase with lower temperature around the hot spot has a tendency to move towards the hot spot with higher temperature, thereby being beneficial to dispersing and reducing the water relative to the porous SiO2Aerogel loading and static pressure.
Thus, for the reasons of the above two aspects, porous SiO2The three-dimensional network structure formed by the aerogel is not easy to collapse and deform, and the porous SiO is ensured2The nano-pores of the aerogel are not damaged, and the porous SiO of the aerogel can be maintained for a long time2The aerogel three-dimensional network structure form. Due to the complex and tortuous surface inside each pore, the energy entering the system is greatly lost in the pores, so that the energy really absorbed by the system is greatly reduced. In other words, the presence of a large number of nanopores ensures that the majority of the energy entering the system on a macroscopic scale is depleted by the nanopores, and the energy absorbed by the system is limited, thus achieving the function of thermal insulation.
In view of the above two reasons, the hydrophobic modified porous SiO2Aerogel becomes an ideal material for heat insulation glass.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention in any way. Porous SiO of the invention2Prepared according to the method with the patent number of CN 101885488A; the temperature-sensitive hydrogel is 85% of polyacrylamide temperature-sensitive hydrogel, and is purchased from Wuhan Gudesh chemical Co. The other materials and methods described in the examples of the present invention are, unless otherwise specified, conventional materials and methods used in the art.
Example 1
The hydrophobic modified porous SiO is used for preparing the aerogel and temperature-sensitive hydrogel composite heat-insulating glass2The structure of the aerogel and temperature-sensitive hydrogel compounded heat-insulation glass comprises a cavity formed by glass; the cavity is filled with polyacrylamide temperature-sensitive hydrogel, wherein the temperature-sensitive hydrogel also comprises 0.1 wt% of gelatin as a thickening agent; the aerogel is dispersed in the temperature-sensitive hydrogel.
Wherein the porous SiO is hydrophobically modified2The total mass of the aerogel is 5g, the total mass of the temperature-sensitive hydrogel is 5000g, the glass cavity is a cuboid, and the volume is about 5L.
The hydrophobically modified porous SiO2An aerogel prepared by the steps of:
s1, 20 parts by mass of porous SiO2Soaking in ethanol for 24h to obtain aged porous SiO2；
S2, ageing the porous SiO2Mixing with trimethylchlorosilane (1:1, n/n) in 100 parts by mass of ethanol solution, and heating to 60 ℃;
s3, performing supercritical drying on the product to obtain hydrophobic modified porous SiO2An aerogel. The supercritical drying method comprises the following steps: adding liquid carbon dioxide into a high-pressure reaction kettle, and adding the hydrophobically modified aged porous SiO formed in S22Soaking in the solution, sealing, introducing nitrogen, slowly heating to 40 deg.C, and increasing pressure during heating; after the carbon dioxide in the reaction kettle is converted into a supercritical fluid state, the pressure is increasedKeeping the temperature at 7.2Mpa for 3 h; then reducing the temperature to normal temperature and normal pressure, and obtaining solid powder hydrophobic modified porous SiO after the high-pressure reaction kettle is naturally cooled2An aerogel.
Wherein, porous SiO2The specific surface area is 200 square meters per gram; the pore volume was 0.8 ml/g.
Finally, the preparation method of the aerogel and temperature-sensitive hydrogel compounded heat-insulation glass comprises the following steps:
(1) filling the glass cavity with temperature-sensitive hydrogel;
(2) adding aerogel particles into the temperature-sensitive hydrogel;
(3) and (3) vacuumizing the system, and then sealing the glass to obtain the aerogel and temperature-sensitive hydrogel compounded heat-insulation glass.
Example 2
The hydrophobic modified porous SiO is used for preparing the aerogel and temperature-sensitive hydrogel composite heat-insulating glass2The structure of the aerogel and temperature-sensitive hydrogel compounded heat-insulation glass comprises a cavity formed by glass; the cavity is filled with polyacrylamide temperature-sensitive hydrogel, wherein the temperature-sensitive hydrogel also comprises 0.2 wt% of agar as a thickening agent; the aerogel is dispersed in the temperature-sensitive hydrogel.
Wherein the porous SiO is hydrophobically modified2The total mass of the aerogel is 5g, the total mass of the temperature-sensitive hydrogel is 5000g, the glass cavity is a cuboid, and the volume is about 5L.
The hydrophobically modified porous SiO2An aerogel prepared by the steps of:
s1, 30 parts by mass of porous SiO2Soaking in ethanol for 48h to obtain aged porous SiO2；
S2, ageing the porous SiO2Mixing with trimethylchlorosilane (1:1.5, n/n) in 200 parts by mass of ethanol solution, and heating to 80 ℃;
s3, performing supercritical drying on the product to obtain hydrophobic modified porous SiO2An aerogel. The supercritical drying method comprises the following steps: reaction under high pressureAdding liquid carbon dioxide into the kettle, and adding the hydrophobically modified aged porous SiO formed in S22Soaking in the solution, sealing, introducing nitrogen, slowly heating to 60 deg.C, and increasing pressure during heating; after the carbon dioxide in the reaction kettle is converted into a supercritical fluid state, the pressure is 9.0Mpa, and the temperature and the pressure are kept for 5 hours; then reducing the temperature to normal temperature and normal pressure, and obtaining solid powder hydrophobic modified porous SiO after the high-pressure reaction kettle is naturally cooled2An aerogel.
Wherein, porous SiO2The specific surface area is 500 square meters per gram; the pore volume was 1.5 ml/g.
Finally, the preparation method of the aerogel and temperature-sensitive hydrogel compounded heat-insulation glass comprises the following steps:
(1) filling the glass cavity with temperature-sensitive hydrogel;
(2) adding aerogel particles into the temperature-sensitive hydrogel;
(3) and (3) vacuumizing the system, and then sealing the glass to obtain the aerogel and temperature-sensitive hydrogel compounded heat-insulation glass.
Example 3
The hydrophobic modified porous SiO is used for preparing the aerogel and temperature-sensitive hydrogel composite heat-insulating glass2The structure of the aerogel and temperature-sensitive hydrogel compounded heat-insulation glass comprises a cavity formed by glass; the cavity is filled with polyacrylamide temperature-sensitive hydrogel, wherein the temperature-sensitive hydrogel also contains 0.3 wt% of carboxymethyl cellulose as a thickening agent; the aerogel is dispersed in the temperature-sensitive hydrogel.
Wherein the porous SiO is hydrophobically modified2The total mass of the aerogel is 5g, the total mass of the temperature-sensitive hydrogel is 5000g, the glass cavity is a cuboid, and the volume is about 5L.
The hydrophobically modified porous SiO2An aerogel prepared by the steps of:
s1, 25 parts by mass of porous SiO2Soaking in ethanol for 36h to obtain aged porous SiO2；
S2, aging the porousSiO2Mixing with hexamethyldisilazane (1:1.2, n/n) in 400 parts by mass of ethanol solution, and heating to 70 ℃;
s3, performing supercritical drying on the product to obtain hydrophobic modified porous SiO2An aerogel. The supercritical drying method comprises the following steps: adding liquid carbon dioxide into a high-pressure reaction kettle, and adding the hydrophobically modified aged porous SiO formed in S22Soaking in the solution, sealing, introducing nitrogen, slowly heating to 50 deg.C, and increasing pressure during heating; after the carbon dioxide in the reaction kettle is converted into a supercritical fluid state, the pressure is 8.2Mpa, and the temperature and the pressure are kept for 4 hours; then reducing the temperature to normal temperature and normal pressure, and obtaining solid powder hydrophobic modified porous SiO after the high-pressure reaction kettle is naturally cooled2An aerogel.
Wherein, porous SiO2The specific surface area is 300 square meters per gram; the pore volume was 1.2 ml/g.
Finally, the preparation method of the aerogel and temperature-sensitive hydrogel compounded heat-insulation glass comprises the following steps:
(1) filling the glass cavity with temperature-sensitive hydrogel;
(2) adding aerogel particles into the temperature-sensitive hydrogel;
(3) and (3) vacuumizing the system, and then sealing the glass to obtain the aerogel and temperature-sensitive hydrogel compounded heat-insulation glass.
Example 4
The hydrophobic modified porous SiO is used for preparing the aerogel and temperature-sensitive hydrogel composite heat-insulating glass2The structure of the aerogel and temperature-sensitive hydrogel compounded heat-insulation glass comprises a cavity formed by glass; the cavity is filled with polyacrylamide temperature-sensitive hydrogel, wherein the temperature-sensitive hydrogel also comprises 0.3 wt% of hydroxyethyl cellulose as a thickening agent; the aerogel is dispersed in the temperature-sensitive hydrogel.
Wherein the porous SiO is hydrophobically modified2The total mass of the aerogel is 5g, the total mass of the temperature-sensitive hydrogel is 5000g, the glass cavity is a cuboid, and the volume is about 5L.
The hydrophobically modified porous SiO2An aerogel prepared by the steps of:
s1, 30 parts by mass of porous SiO2Soaking in ethanol for 40h to obtain aged porous SiO2；
S2, ageing the porous SiO2Mixing with hexamethyldisilazane (1:1.1, n/n) in 300 parts by mass of ethanol solution, and heating to 75 ℃;
s3, performing supercritical drying on the product to obtain hydrophobic modified porous SiO2An aerogel. The supercritical drying method comprises the following steps: adding liquid carbon dioxide into a high-pressure reaction kettle, and adding the hydrophobically modified aged porous SiO formed in S22Soaking in the solution, sealing, introducing nitrogen, slowly heating to 55 deg.C, and increasing pressure during heating; after the carbon dioxide in the reaction kettle is converted into a supercritical fluid state, the pressure is 8.6Mpa, and the temperature and the pressure are kept for 3.5 hours; then reducing the temperature to normal temperature and normal pressure, and obtaining solid powder hydrophobic modified porous SiO after the high-pressure reaction kettle is naturally cooled2An aerogel.
Wherein, porous SiO2The specific surface area is 400 square meters per gram; the pore volume was 1.4 ml/g.
Finally, the preparation method of the aerogel and temperature-sensitive hydrogel compounded heat-insulation glass comprises the following steps:
(1) filling the glass cavity with temperature-sensitive hydrogel;
(2) adding aerogel particles into the temperature-sensitive hydrogel;
(3) and (3) vacuumizing the system, and then sealing the glass to obtain the aerogel and temperature-sensitive hydrogel compounded heat-insulation glass.
Comparative example 1
All technical schemes of the thermal insulation glass compounded with the aerogel and the temperature-sensitive hydrogel described in the embodiment 1 are the same, and the only difference is that the porous SiO of the comparative example 12The specific surface area is 100 square meters per gram.
Comparative example 2
As described in example 1All technical schemes of the aerogel and temperature-sensitive hydrogel composite heat-insulation and heat-preservation glass are the same, and the only difference is that the porous SiO of the comparative example 22The pore volume of (A) was 0.5 ml/g.
Comparative example 3
All technical schemes of the thermal insulation glass compounded with the aerogel and the temperature-sensitive hydrogel described in the embodiment 1 are the same, and the only difference is that the porous SiO of the comparative example 32The specific surface area is 150 square meters per gram and the pore volume is 0.6 ml/g.
Comparative example 4
All technical schemes of the thermal insulation glass compounded with the aerogel and the temperature-sensitive hydrogel described in the embodiment 1 are the same, and the only difference is that the aerogel of the comparative example 4 is porous SiO which is not subjected to hydrophobic modification2An aerogel.
Comparative example 5
All technical schemes of the thermal insulation glass compounded with the aerogel and the temperature-sensitive hydrogel described in the embodiment 1 are the same, and the only difference is that the aged porous SiO in the comparative example 52The mass ratio to trialkyl coupling agent was 1: 0.7.
Comparative example 6
All technical schemes of the thermal insulation glass compounded with the aerogel and the temperature-sensitive hydrogel described in the embodiment 1 are the same, and the only difference is that the system of the comparative example 6 does not contain the temperature-sensitive hydrogel.
Example 5
The aerogel and temperature-sensitive hydrogel composite heat-insulating glass of the above examples 1 to 4 and comparative examples 1 to 6 was subjected to a heat-insulating test. The method comprises the following steps: in a constant temperature and humidity laboratory at 25.9 ℃, a thermometer is inserted into a thermometer socket above the aerogel and temperature-sensitive hydrogel composite heat-insulation and heat-preservation glass of examples 1-4 and comparative examples 1-6 respectively, the thermometer and the socket are sealed by using silicone, the system is ensured to be closed, and the readings of all thermometers are calibrated to be 25.6 ℃; then, the 10 products were arranged in a row, 10 products were irradiated with 850W infrared lamps for 1 hour, and then the values of the 10 sample thermometers were read, and the lot was P1.
Then after 1 month interval, the above operation was repeated, batch P2.
Then after 3 months, the above operation was repeated for batch P3.
The above data are shown in table 1.
TABLE 1 results of temperature measurement of examples 1 to 4 and comparative examples 1 to 6
As can be seen from the above table, the disclosed embodiments of the present invention have a longer service life in terms of thermal insulation performance. Specifically, compared with the corresponding products of comparative examples 1 to 6, from the data analysis of batch P1, the temperature differences of example 4 and comparative examples 1 to 5 are small and are about 27 to 28 ℃, which shows that all the products have ideal heat insulation and preservation effects for the external intense heat irradiation after being newly prepared and the system temperature is only 1 to 2 ℃; however, after one and three month storage, the examples and comparative examples showed more pronounced differentiation from the data analysis of batches P2 and P3: comparative examples 1 to 3 were not made of porous SiO2The aerogel has small specific surface area or pore volume and relatively poor heat insulation effect, which indicates that the porous SiO has poor heat insulation effect2The aerogel structure is obviously collapsed and deformed in the period of time, so that a large number of nano-scale pores disappear, and the heat insulation effect is reduced most obviously; while comparative example 4 is due to porous SiO2The aerogel is not further hydrophobically modified, resulting in relatively easy attachment of water molecules in the aqueous phase to the porous SiO2Aerogel, thereby increasing the porous SiO2Loading of the aerogel, resulting in porous SiO2The aerogel partially deforms, so that partial nanometer pores disappear, and the heat insulation effect is different from that of the embodiment 1; while the aged porous SiO used in comparative example 52The amount of the substance to the trialkyl coupling agent is1:0.7, resulting in a part of hydroxyl groups remaining in the porous SiO without reacting with the trialkyl coupling agent2In the structure of (1), the hydrophobic modification of comparative example 5 is not completely achieved, and thus water molecules are added to the porous SiO of example 52The adsorption of aerogel is stronger, thereby increasing the porous SiO2The aerogel loading results in a slight reduction in service life. In the comparative example 6, the initial heat preservation effect is poor due to the fact that the temperature-sensitive hydrogel is not contained; and because the phenomenon of local hot spots formed by temperature-sensitive hydrogel does not exist, the water phase is easier to be compared with the porous SiO2The aerogel generates a static pressure, thereby creating porous SiO2Aerogels are more susceptible to deformation and collapse due to static pressure, resulting in reduced service life.
The above data, fully show the advancement of examples 1-4 over comparative examples 1-6.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The thermal insulation glass compounded by aerogel and temperature-sensitive hydrogel is characterized in that the thermal insulation glass compounded by aerogel and temperature-sensitive hydrogel structurally comprises a cavity formed by glass, the cavity is filled with the temperature-sensitive hydrogel, the aerogel is dispersed in the temperature-sensitive hydrogel,
wherein the temperature-sensitive hydrogel is polyacrylamide temperature-sensitive hydrogel or epoxy copolymer temperature-sensitive hydrogel;
the aerogel is porous SiO subjected to hydrophobic modification2The preparation method of the aerogel comprises the following steps:
s1, preparing porous SiO2Soaking for 24-48h to obtain aged porous SiO2；
S2, ageing the porous SiO2Mixing with trialkyl coupling agent in ethanol solution, and heating to 60-80 deg.C;
s3, drying the product to obtain the hydrophobic modified porous SiO2An aerogel.
2. The aerogel and temperature-sensitive hydrogel composite heat-insulating glass as claimed in claim 1, wherein the porous SiO is porous2The specific surface area is 200-500 square meters per gram.
3. The aerogel and temperature-sensitive hydrogel composite heat-insulating glass as claimed in claim 1, wherein the porous SiO is porous2The pore volume of (A) is 0.8-1.5 ml/g.
4. The aerogel and temperature-sensitive hydrogel composite heat-insulating and heat-preserving glass as claimed in claim 1, wherein the temperature-sensitive hydrogel further comprises a thickening agent.
5. The aerogel and temperature-sensitive hydrogel compounded heat-insulation and heat-preservation glass as claimed in claim 4, wherein the thickening agent is selected from one or more of gelatin, agar, carboxymethyl cellulose, sodium alginate, carrageenan or hydroxyethyl cellulose.
6. The aerogel and temperature-sensitive hydrogel composite heat-insulating glass according to claim 1, wherein the aged porous SiO is2The amount of the material to the trialkyl coupling agent is 1:1 to 1: 1.5.
7. The aerogel and temperature-sensitive hydrogel composite heat-insulating and heat-preserving glass as claimed in claim 1, wherein the drying is supercritical drying, and comprises the following steps:
adding liquid carbon dioxide into a high-pressure reaction kettle, soaking the product in S3, sealing, introducing nitrogen, and then heating, wherein the pressure is increased along with the heating; after the carbon dioxide in the reaction kettle is converted into a supercritical fluid state, preserving the heat for 3-5h, then cooling to normal temperature and normal pressure, and naturally cooling.
8. The aerogel and temperature-sensitive hydrogel composite heat-insulating glass as claimed in claim 7, wherein the temperature in the autoclave is finally raised to 40-60 ℃ and the pressure is finally raised to 7.2-9.0 MPa.
9. The aerogel and temperature-sensitive hydrogel composite heat-insulating glass according to claim 1, wherein the preparation method comprises the following steps:
(1) filling temperature-sensitive hydrogel into the glass cavity;
(2) adding aerogel particles into the temperature-sensitive hydrogel;
(3) and sealing the glass.
10. The aerogel and temperature-sensitive hydrogel composite heat-insulating glass according to claim 9, wherein before sealing, the glass is vacuumized.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111635243A (en) * | 2020-06-09 | 2020-09-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Renewable silica aerogel composite material, its preparation method, regeneration method and application |
| CN113978046A (en) * | 2021-11-09 | 2022-01-28 | 厦门大学 | Thermal protection structure and preparation method thereof |
| CN114953667A (en) * | 2022-04-24 | 2022-08-30 | 山西阳中新材有限责任公司 | Aerogel-containing temperature-sensitive heat-insulating film and preparation method thereof |
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2020
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111635243A (en) * | 2020-06-09 | 2020-09-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Renewable silica aerogel composite material, its preparation method, regeneration method and application |
| CN111635243B (en) * | 2020-06-09 | 2022-07-22 | 中国科学院苏州纳米技术与纳米仿生研究所 | Renewable silica aerogel composite material, preparation method, regeneration method and application thereof |
| CN113978046A (en) * | 2021-11-09 | 2022-01-28 | 厦门大学 | Thermal protection structure and preparation method thereof |
| CN114953667A (en) * | 2022-04-24 | 2022-08-30 | 山西阳中新材有限责任公司 | Aerogel-containing temperature-sensitive heat-insulating film and preparation method thereof |
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