CN116199522A - PU sponge-based silicon aerogel felt and preparation method thereof - Google Patents
PU sponge-based silicon aerogel felt and preparation method thereof Download PDFInfo
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- CN116199522A CN116199522A CN202310056919.1A CN202310056919A CN116199522A CN 116199522 A CN116199522 A CN 116199522A CN 202310056919 A CN202310056919 A CN 202310056919A CN 116199522 A CN116199522 A CN 116199522A
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 95
- 239000010703 silicon Substances 0.000 title claims abstract description 95
- 239000004964 aerogel Substances 0.000 title claims abstract description 94
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000002131 composite material Substances 0.000 claims abstract description 40
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 17
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 16
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- 238000007598 dipping method Methods 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 230000032683 aging Effects 0.000 claims abstract description 9
- 108010009736 Protein Hydrolysates Proteins 0.000 claims abstract description 8
- 239000000413 hydrolysate Substances 0.000 claims abstract description 8
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 239000004965 Silica aerogel Substances 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 22
- 239000002585 base Substances 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 5
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 4
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims 1
- 238000009413 insulation Methods 0.000 abstract description 14
- 239000012774 insulation material Substances 0.000 abstract description 2
- 239000004814 polyurethane Substances 0.000 description 86
- 239000000835 fiber Substances 0.000 description 18
- 239000000243 solution Substances 0.000 description 17
- 239000000843 powder Substances 0.000 description 15
- 230000002209 hydrophobic effect Effects 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 7
- 239000002245 particle Substances 0.000 description 6
- 238000000352 supercritical drying Methods 0.000 description 6
- 230000006835 compression Effects 0.000 description 5
- 238000007906 compression Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 230000009975 flexible effect Effects 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000002791 soaking Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 125000001165 hydrophobic group Chemical group 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000013305 flexible fiber Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011859 microparticle Substances 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 230000007480 spreading Effects 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 229920003225 polyurethane elastomer Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- -1 siloxanes Chemical class 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000011240 wet gel Substances 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/40—Porous or lightweight materials
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The application relates to the technical field of heat insulation materials, in particular to a PU sponge-based silicon aerogel felt and a preparation method thereof. The preparation method of the PU sponge-based silicon aerogel felt provided by the application comprises the following steps: uniformly mixing siloxane, orthosilicate, water and absolute ethyl alcohol, and then sequentially adding acetic acid and hexadecyl trimethyl ammonium bromide for heating reaction to obtain silicon source hydrolysate; adding an alkali catalyst into the silicon source hydrolysate, and fully and uniformly stirring to obtain a silicon dioxide sol solution; immersing the PU sponge into the silicon dioxide sol solution for gum dipping treatment, and standing and aging under normal temperature conditions to obtain a PU sponge/silicon aerogel composite material; adding the PU sponge/silicon aerogel composite material into absolute ethyl alcohol to perform solvent replacement; and drying the PU sponge/silicon aerogel composite material subjected to solvent replacement to obtain the PU sponge-based silicon aerogel felt. The PU sponge-based silicon aerogel felt prepared by the method has good flexibility, rebound resilience and excellent heat insulation performance.
Description
Technical Field
The application relates to the technical field of heat insulation materials, in particular to a PU sponge-based silicon aerogel felt and a preparation method thereof.
Background
Silica aerogel is a solid material with interconnected nano-porous structure, which is formed by mutually polymerizing nano-scale silica solid particles to form a three-dimensional network skeleton. The average pore size of the silicon aerogel is about 20nm, which is smaller than the average free motion path of air molecules, so that the heat conduction and heat convection are greatly limited, the equivalent heat conduction coefficient is very low, and the silicon aerogel is a solid material with the lowest heat conduction coefficient in the world at present. The silicon aerogel is usually powder, particles or blocks, has low strength, high brittleness and poor toughness, and the powder is extremely easy to escape and float in the air, so that serious pollution is caused, and the operability and application of the silicon aerogel in construction are limited. In order to solve the problems, fiber mats such as ceramic fiber mats, glass fiber mats, pre-oxidized fiber mats and the like are used as substrates for preparing fiber-reinforced silica aerogel mats in the current production. The fiber felt is prepared from short fibers with the diameter of micron through processes such as lapping, needling and the like, has large rigidity and poor flexibility, and is stable in size, but the short fibers are easy to fall off, and the structural difference in the thickness direction and the plane direction is large, so that the anisotropy of the final product in mechanical and thermal properties is caused. In addition, the porous structure formed by the short fiber aggregate has large pore size, poor binding property to aerogel powder and particles and outstanding powder falling problem, thereby affecting the heat insulation performance and application of the felt. In order to solve the problem that the fiber reinforced silica aerogel felt has poor tensile property and rebound resilience in practical application, patent CN111908889A discloses a composite fiber reinforced aerogel felt and a preparation method thereof, and specifically, a flexible fiber net tire and an aluminum silicate fiber net tire are alternately layered and laid on an XY plane, and are connected through Z-direction needling flexible fibers to obtain a composite fiber felt body, and the composite fiber felt body is used as a base material to prepare the fiber reinforced silica aerogel felt, so that the stability of heat insulation performance is improved, and the mechanical flexibility is enhanced. However, the preparation process of the composite fiber felt is complex, takes long time, is not beneficial to industrialized mass production, the felt body is of a porous fiber short fiber aggregate structure, the binding effect on the aerogel is not ideal, and the patent CN111039295B discloses a method for preparing the silica aerogel and the self-hydrophobic silica aerogel heat-insulation felt pad by a one-step method. Patent CN108383129a discloses a preparation method of flexible hydrophobic silica aerogel, specifically discloses a preparation method of flexible hydrophobic silica aerogel by using methyltrialkoxysilane and orthosilicate as silicon sources, and in the preparation process, volatile ammonia water with strong pungent smell is used as a base catalyst, so serious environmental pollution and safety problems are easily caused; the prepared silicon aerogel does not contain a reinforced base material, and after the silicon aerogel is dried, the three-dimensional porous structure of the silicon aerogel is partially collapsed, and the silicon aerogel presents a mixed system of powder, particles and irregular blocks, and cannot be directly applied. Patent CN111848114a discloses a super heat insulation aerogel composite material and a preparation process thereof, and in particular discloses a preparation method of the aerogel composite material by compounding silica aerogel and reinforced foam, wherein the wet gel composite material is immersed into a hydrophobic reagent for hydrophobic modification in the preparation process, and as the PU sponge is not resistant to organic solvent soaking, the PU sponge skeleton is dissolved, and the mechanical property is lost until the structure is completely disintegrated. Based on the analysis, the preparation method for the silicon aerogel felt, which has simple technical process and can obtain the silicon aerogel felt with good flexibility and mechanical property, is very important.
Disclosure of Invention
The embodiment of the application provides a preparation method of a PU sponge-based silicon aerogel felt, which aims to solve the problems of poor flexibility, serious powder falling and complex preparation process of a fiber-based silicon aerogel felt in the prior art. In a first aspect, the present application provides a method for preparing a PU sponge-based silica aerogel blanket, including the steps of: step S101, uniformly mixing siloxane, tetraethoxysilane, water and absolute ethyl alcohol, and then sequentially adding acetic acid and Cetyl Trimethyl Ammonium Bromide (CTAB) for heating reaction to obtain silicon source hydrolysate; step S102, adding an alkali catalyst into the silicon source hydrolysate, and fully and uniformly stirring to obtain a silicon dioxide sol solution; step S103, immersing the PU sponge into a silica sol solution for gum dipping treatment, and then standing and aging for 6-2 hours under normal temperature conditions to obtain a PU sponge/silica aerogel composite material; step S104, adding the PU sponge/silicon aerogel composite material into absolute ethyl alcohol to perform solvent replacement, and removing water in the PU sponge/silicon aerogel composite material; and step S105, drying the PU sponge/silicon aerogel composite material to obtain the PU sponge-based silicon aerogel felt. In some embodiments, the silicone: orthosilicate: absolute ethyl alcohol: the molar ratio of water is (0.4-1): (0-0.04): (3-12): (4-8). In some embodiments, acetic acid: the molar ratio of the siloxane is (0.002-0.01): 1. in some embodiments, the PU sponge has a density of 20 to 60kg/m3 and a thickness of 5 to 20mm. In some embodiments, cetyltrimethylammonium bromide: the molar ratio of the siloxane is (0.002-0.005): 1. cetyl trimethyl ammonium bromide can promote polycondensation reaction, is favorable for further polymerization of the oligomer to form a long-chain silicon dioxide framework structure expanding to a three-dimensional space, and ensures that the condensation reaction is more sufficient. In some embodiments, in step S101, the heating reaction is performed at 50-60℃for 10-16 hours. In some embodiments, the molar ratio of siloxane to base catalyst is 1 (0.005 to 0.015). In some embodiments, in step S102, the stirring speed is 500-1500 rpm and the stirring time is 5-15 min. In some embodiments, in step S103, the dipping time is 1-6 hours. In some embodiments, in step S104, the number of solvent substitutions is 1-3, each for a period of 4-12
h. In some embodiments, in step S105, the drying mode is normal pressure drying or supercritical drying. In some embodiments, the siloxane is any one or a mixture of two of dimethyldiethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane. The dimethyl diethoxy silane, the methyl triethoxy silane and the ethyl trimethoxy silane have hydrophobic groups, so that the composite material subjected to gum dipping treatment does not need to be subjected to hydrophobic modification by using the siloxanes, and the damage to PU sponge is avoided. In some embodiments, the orthosilicate is any one or a mixture of two of methyl orthosilicate and ethyl orthosilicate. In some embodiments, the base catalyst is an aqueous solution of NaOH or KOH. NaOH or KOH is used as a catalyst, so that the catalyst has high safety, no pollution to the environment, convenient operation and low cost. In the second aspect, the application also provides the PU sponge-based silicon aerogel felt prepared by the preparation method, the PU sponge-based silicon aerogel felt is soft in texture, the compression rebound rate in the thickness direction can reach 60-95%, the powder falling is less, the water contact angle is 110-140 degrees, and the heat conductivity coefficient is 0.023-0.012W/m.K. The PU sponge-based silicon aerogel felt prepared by the method can be applied to heat preservation and heat insulation under non-high temperature scenes (lower than 120 ℃), such as buildings, industrial pipelines and the like, and the fields of heat insulation, cold chain transportation, medical cold insulation and the like of refrigerators and vending machines, and can be applied to clothing, outdoor products and the like as an interlayer to play a role in heat insulation or warmth retention. The preparation method provided by the application adopts the PU sponge with a fine and uniform open pore structure as a base material, the PU sponge is provided with a polygonal structure formed by polyurethane elastomer polymers, a three-dimensional network skeleton formed by mutually interweaving and stacking the polyhedrons, and a large number of open-type micro air holes filled with air and communicated with each other, the air holes are fine and uniform, the hole orientation is small, the opening ratio is high, and the polyurethane sponge has good softness, rebound resilience and heat insulation and heat preservation. In the process of preparing the silica sol solution, siloxane with hydrophobic groups is used as a raw material, the subsequent hydrophobic modification of the composite material after the gum dipping treatment is not needed, the damage of a hydrophobic modification reagent to the molecular structure of the PU sponge is avoided, and the characteristics of the PU sponge are fully reserved; naOH or KOH is used as a base catalyst, so that volatile gas is avoided, and the method is safe, environment-friendly, convenient to operate and low in cost; after the PU sponge is subjected to gum dipping treatment by the silica sol liquid, the silica sol liquid is filled in micropores of the PU sponge and forms silica solid microparticles with nano-scale three-dimensional porous structures through polycondensation reaction, the silica solid microparticles are mutually piled to further form three-dimensional porous structures with submicron and micron scales, and thus the mutual embedding of the multi-scale three-dimensional porous structures is realized. After the wet PU sponge/silicon aerogel composite material is subjected to ethanol replacement and drying treatment, the prepared PU sponge-based silicon aerogel felt has good flexibility, rebound resilience and excellent heat insulation performance. The beneficial effects that technical scheme that this application provided brought include: 1. according to the preparation method, PU sponge with good flexibility, rebound resilience and uniform compact air holes is used as a base material, siloxane with one or more flexible groups is used as a silicon source precursor, and after sol, gum dipping, gel, aging, replacement and drying treatment, the integrity of a sponge structure and good mechanical properties are reserved, the flexibility of a silicon aerogel framework is also ensured, and the prepared sponge-based silicon aerogel felt has a good flexible effect; 2. according to the preparation method, the PU sponge with the three-dimensional porous structure and the silicon aerogel with the multi-level three-dimensional porous structure are compounded, the prepared sponge-based silicon aerogel felt has a multi-scale micropore structure, micropores with various sizes and shapes are mutually overlapped and communicated, and the formed pore diameter passage is complex and changeable, so that the movement heat transfer of air molecules is further limited, and therefore, the sponge-based silicon aerogel felt has extremely low heat conductivity and excellent heat insulation performance; 3. the preparation method provided by the application can effectively prevent the solid powder and particles of the silicon aerogel from moving away and escaping, so that the solid powder and the particles are well bound, and the powder falling problem is effectively solved; 4. the surface of the silicon aerogel prepared by the preparation method provided by the application has a large number of hydrophobic groups, the PU sponge-based silicon aerogel felt is endowed with a hydrophobic effect without hydrophobic treatment, the stability of the heat insulation performance of the material in actual use is ensured, and the problem of the reduction of the heat insulation performance of the silicon aerogel felt caused by humidity and water is avoided; meanwhile, the process flow is simplified, and the time and the economic cost are reduced; 5. the PU sponge-based silicon aerogel felt prepared by the preparation method provided by the application has a self-extinguishing effect when meeting open fire, plays a role in flame retardance, and avoids the potential safety problem caused by fire and inflammability in the use process of the conventional PU sponge.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art. Fig. 1 is a schematic flow chart of a preparation method of a PU sponge-based silica aerogel blanket provided in an embodiment of the present application; FIG. 2 is a physical diagram of the PU sponge-based silica aerogel blanket prepared in example 1 of the present application; fig. 3 is a bending diagram of the PU sponge-based aerogel blanket prepared in example 1 of the present application.
Detailed Description
For the purposes of making the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present application based on the embodiments herein. The embodiment of the application provides a preparation method of a PU sponge-based silicon aerogel felt, which can solve the problems of poor flexibility, serious powder falling and complex preparation process of a fiber-based silicon aerogel felt in the prior art. Fig. 1 is a schematic flow chart of a preparation method of a PU sponge-based silica aerogel blanket provided in the present application, and referring to fig. 1, the preparation method provided in the present application includes the following steps: step S101, siloxane, tetrasilicate, water and absolute ethyl alcohol are taken and mixed uniformly, then acetic acid and Cetyl Trimethyl Ammonium Bromide (CTAB) are added in sequence, and the mixture is stirred for 10 to 16 hours under the water bath condition of 50 to 60 ℃ to obtain silicon source hydrolysate; step S102, adding an alkali catalyst into the silicon source hydrolysate, and stirring for 5-15 min at a rotating speed of 500-1500 rpm to obtain a silicon dioxide sol solution; step S103, immersing the PU sponge into the silica sol solution for gum dipping treatment, wherein the gum dipping time is 1-6 hours, and standing and aging for 6-24 hours under the normal temperature condition to obtain the PU sponge/silicon aerogel composite material; step S104, placing the PU sponge/silicon aerogel composite material in absolute ethyl alcohol for 1-3 times of solvent replacement, wherein the time for each replacement is 4-12 hours, and fully removing the moisture in the PU sponge/aerogel composite material; and step S105, performing normal pressure or supercritical drying on the PU sponge/silicon aerogel composite material to obtain the PU sponge-based silicon aerogel felt. The PU sponge-based silica aerogel blanket provided by the application and the preparation method thereof are described in detail below with reference to examples. Example 1: example 1 provides a method for preparing a PU sponge-based silica aerogel blanket, comprising the following steps: (1) Uniformly mixing 10mol of methyltriethoxysilane, 0.4mol of methyl orthosilicate, 80mol of water and 50mol of absolute ethyl alcohol, sequentially adding 0.05mol of acetic acid and 0.02mol of Cetyl Trimethyl Ammonium Bromide (CTAB), and stirring for 15 hours under the water bath condition of 50 ℃ to obtain a silicon source hydrolysate; (2) Adding 0.10mol of sodium hydroxide into the silicon source hydrolysate, and fully stirring for 10min at the rotating speed of 800rpm to obtain silicon dioxide sol solution; (3) Soaking porous PU sponge felt body with density of 50kg/m3 and thickness of 10mm in silica sol solution for 6h, and soaking in the solution at 24
Standing and aging for 12 hours at the temperature to obtain the PU sponge/silicon aerogel composite material; (4) Placing the PU sponge/silicon aerogel composite material in absolute ethyl alcohol for 2 times of solvent replacement, wherein the time for each replacement is 8 hours, and fully removing the water in the PU sponge/silicon aerogel composite material; (5) And carrying out supercritical drying on the PU sponge/silicon aerogel composite material to obtain the PU sponge-based silicon aerogel felt. The physical diagram of the PU sponge-based silica aerogel felt prepared in the example 1 is shown in fig. 2. The PU sponge-based silicon aerogel felt is soft in texture, has a compression rebound rate of 80% in the thickness direction, is less in powder falling, has a water contact angle of 120 degrees and has a heat conduction coefficient of 0.017W/m.K. The PU sponge-based aerogel blanket prepared in example 1 was bent, see fig. 3, and as can be seen from fig. 3, the PU sponge-based aerogel blanket exhibited good flexibility. The self-extinguishing test is carried out on the PU sponge and the PU sponge-based silicon aerogel felt prepared in the embodiment 1, and the specific process is as follows: the PU sponge and the PU sponge-based silicon aerogel felt are respectively ignited by utilizing a lighter, and the PU sponge has the advantages of quick ignition, large flame, quick fire spreading and complete combustion of the whole PU sponge; the PU sponge-based silicon aerogel felt has the advantages of low ignition speed, small flame, extinguishment of open flame after 3-5 seconds, and incapability of spreading fire, so that the PU sponge-based silicon aerogel felt prepared by the method has a good flame-retardant self-extinguishing effect. Example 2: example 2 provides a method for preparing a PU sponge-based silica aerogel blanket, comprising the following steps: (1) Taking 6mol of methyltriethoxysilane, 0.1mol of tetraethoxysilane, 100mol of water and 40mol of absolute ethyl alcohol, uniformly mixing, sequentially adding 0.03mol of acetic acid and 0.03mol of Cetyl Trimethyl Ammonium Bromide (CTAB), and stirring for 12 hours under the water bath condition of 50 ℃ to obtain a silicon source hydrolysate; (2) Adding 0.15mol of sodium hydroxide into the silicon source hydrolysate, and fully stirring for 15min at a rotating speed of 1000rpm to obtain a silicon dioxide sol solution; (3) Soaking a porous PU sponge felt body with the density of 40kg/m3 and the thickness of 10mm in a silica sol solution for 2 hours, and standing and aging for 24 hours at 24 ℃ to obtain a PU sponge/silicon aerogel composite material; (4) Placing the PU sponge/silicon aerogel composite material in absolute ethyl alcohol for 3 times of solvent replacement, wherein the time for each replacement is 12 hours, and fully removing the water in the PU sponge/silicon aerogel composite material; (5) And carrying out supercritical drying on the PU sponge/silicon aerogel composite material to obtain the PU sponge-based silicon aerogel felt. The PU sponge-based silica aerogel felt prepared in example 2 has soft texture, a compression rebound rate in the thickness direction of 85%, less powder falling, a water contact angle of 112 degrees and a heat conduction coefficient of 0.019W/m.K. Example 3: example 3 provides a method for preparing a PU sponge-based silica aerogel blanket, comprising the steps of: (1) Uniformly mixing 15mol of dimethyl diethoxysilane, 0.6mol of methyl orthosilicate, 120mol of water and 100mol of absolute ethyl alcohol, sequentially adding 0.12mol of acetic acid and 0.045mol of Cetyl Trimethyl Ammonium Bromide (CTAB), and stirring for 12 hours under the water bath condition of 55 ℃ to obtain silicon source hydrolysate; (2) Adding 0.15mol of sodium hydroxide into the silicon source hydrolysate, and fully stirring for 10min at a rotating speed of 1000rpm to obtain a silicon dioxide sol solution; (3) Dipping a porous PU sponge felt body with the density of 35kg/m3 and the thickness of 10mm in a silicon dioxide sol solution for 6 hours, and standing and aging for 12 hours at 24 ℃ to obtain a PU sponge/silicon aerogel composite material; (4) Placing the PU sponge/silicon aerogel composite material in absolute ethyl alcohol for 2 times of solvent replacement, wherein the time for each replacement is 10 hours, and fully removing the water in the PU sponge/silicon aerogel composite material; (5) And carrying out supercritical drying on the PU sponge/silicon aerogel composite material to obtain the PU sponge-based silicon aerogel felt. The PU sponge-based silica aerogel felt prepared in example 3 has soft texture, compression rebound rate in the thickness direction of 70%, less powder falling, water contact angle of 132 degrees and heat conductivity coefficient of 0.015W/m.K. Example 4: example 4 provides a method for preparing a PU sponge-based silica aerogel blanket, comprising the following steps: (1) Uniformly mixing 24mol of ethyl trimethoxy silane, 0.6mol of methyl orthosilicate, 270mol of water and 150mol of absolute ethyl alcohol, sequentially adding 0.144mol of acetic acid and 0.072mol of Cetyl Trimethyl Ammonium Bromide (CTAB), and stirring for 12 hours under the water bath condition of 50 ℃ to obtain a silicon source hydrolysate; (2) Adding 0.24mol of sodium hydroxide into the silicon source hydrolysate, and fully stirring for 10min at the rotating speed of 800rpm to obtain silicon dioxide sol solution; (3) Dipping a porous PU sponge felt body with the density of 50kg/m3 and the thickness of 8mm in a silicon dioxide sol solution for 6 hours, and standing and aging for 12 hours at 24 ℃ to obtain a PU sponge/silicon aerogel composite material; (4) Placing the PU sponge/silicon aerogel composite material in absolute ethyl alcohol for 2 times of solvent replacement, wherein the time for each replacement is 8 hours, and fully removing the water in the PU sponge/silicon aerogel composite material; (5) And carrying out supercritical drying on the PU sponge/silicon aerogel composite material to obtain the PU sponge-based silicon aerogel felt. The PU sponge-based silica aerogel felt prepared in example 4 has soft texture, compression rebound rate in the thickness direction of 83%, less powder falling, water contact angle of 135 degrees and heat conductivity coefficient of 0.014W/m.K. In the description of the present specification, reference to the terms "one embodiment/manner," "some embodiments/manner," "example," "a particular example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment/manner or example is included in at least one embodiment/manner or example of the present application. In this specification, the schematic representations of the above terms are not necessarily for the same embodiment/manner or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments/modes or examples. Furthermore, the various embodiments/modes or examples described in this specification and the features of the various embodiments/modes or examples can be combined and combined by persons skilled in the art without contradiction. It should be noted that in this application, relational terms such as "first" and "second" and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element. In the present application, the meaning of "plurality" means at least two, for example, two, three, etc., unless explicitly specified otherwise. The foregoing is merely illustrative of the present application and enables one skilled in the art to understand or practice the present application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. The preparation method of the PU sponge-based silicon aerogel felt is characterized by comprising the following steps of: uniformly mixing siloxane, orthosilicate, water and absolute ethyl alcohol, and then sequentially adding acetic acid and hexadecyl trimethyl ammonium bromide for heating reaction to obtain silicon source hydrolysate; adding an alkali catalyst into the silicon source hydrolysate, and fully and uniformly stirring to obtain a silicon dioxide sol solution; immersing the PU sponge into the silicon dioxide sol solution for gum dipping treatment, and standing and aging under normal temperature conditions to obtain a PU sponge/silicon aerogel composite material; adding the PU sponge/silicon aerogel composite material into absolute ethyl alcohol to perform solvent replacement; and drying the PU sponge/silicon aerogel composite material subjected to solvent replacement to obtain the PU sponge-based silicon aerogel felt.
2. The method for preparing the PU sponge-based aerogel blanket according to claim 1, wherein the siloxane: orthosilicate: absolute ethyl alcohol: the molar ratio of water is 4-1: 0-04:3-12:4-8.
3. The method for preparing the PU sponge-based aerogel blanket according to claim 1, wherein acetic acid: the molar ratio of siloxane is 002-01: 1.
4. the method for preparing the PU sponge-based aerogel blanket according to claim 1, wherein the cetyl trimethylammonium bromide: the molar ratio of the siloxane is (002-005): 1.
5. the method for preparing the PU sponge-based silica aerogel felt according to claim 1, wherein the heating reaction condition is 50-60 ℃, and the reaction time is 10-16 h.
6. The method for preparing the PU sponge-based aerogel blanket according to claim 1, wherein the molar ratio of siloxane to base catalyst is 1:005-015.
7. The method for preparing the PU sponge-based aerogel blanket according to claim 1, wherein the siloxane is any one or a mixture of two of dimethyl diethoxy silane, methyl triethoxy silane and ethyl trimethoxy silane.
8. The method for producing a PU sponge-based aerogel blanket as claimed in claim 1, wherein the orthosilicate is any one or a mixture of two of methyl orthosilicate and ethyl orthosilicate.
9. The method for preparing the PU sponge-based aerogel blanket according to claim 1, wherein the base catalyst is sodium hydroxide or potassium hydroxide.
10. A PU sponge-based aerogel blanket, characterized in that it is produced by the production method of any one of claims 1 to 9.
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| CN117510181A (en) * | 2023-11-07 | 2024-02-06 | 武汉中科先进材料科技有限公司 | Super-hydrophobic and enhanced silicon dioxide aerogel felt and preparation method thereof |
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