CN113620643B - Preparation method of powder falling prevention silicon dioxide aerogel felt - Google Patents
Preparation method of powder falling prevention silicon dioxide aerogel felt Download PDFInfo
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- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
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- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
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- 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
- C04B2111/27—Water resistance, i.e. waterproof or water-repellent materials
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- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
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Abstract
The invention belongs to the field of heat insulation materials, and discloses a preparation method of a powder-dropping-prevention silicon dioxide aerogel felt.
Description
Technical Field
The invention belongs to the field of heat insulation materials, and particularly relates to a preparation method of a powder falling prevention silicon dioxide aerogel felt.
Background
At present, developing new energy, improving the utilization rate of the existing energy and saving energy have attracted great attention from various countries. Therefore, the reasonable utilization of energy and the energy conservation have important significance on the sustainable development of the society in China. The development of environment-friendly heat insulation materials by adopting new technology and new process is one of the most effective and economic measures for saving energy.
SiO 2 The aerogel serving as a novel super heat-insulating material has extremely low heat conductivity coefficient which is far lower than that of static air at normal temperature by 0.25W/mK, has incomparable heat-insulating and heat-preserving effects compared with other materials, and has the advantages of low density, water resistance, flame retardance, environmental protection, corrosion resistance,Is not easy to age and has long service life, and is called super heat-insulating material. At present, the composite material is mainly used for heat preservation and insulation in the fields of industrial pipelines, industrial furnace bodies, escape capsules, transportation, household appliances, glass and the like.
SiO due to the method of its preparation 2 The aerogel felt has the common condition that the aerogel powder falls off from the felt body in the transportation, construction and use processes, the powder falling condition brings inconvenience to the construction, brings threat to the health of constructors, and simultaneously can reduce the performance of the aerogel felt. Therefore, on the premise of ensuring good heat insulation performance of the aerogel felt, the development of the aerogel composite material without powder falling is necessary to ensure the health of production and use personnel and meet various requirements of the market. At present, glass fiber cloth, aluminum foil cloth and the like are usually adhered to the surface of an aerogel fiber felt, the labor cost is high, large-scale production is not facilitated, the condition that aerogel powder falls off from a felt body can exist in the process of cutting the aerogel felt, the flexibility of the material after the front side and the back side are adhered is reduced, curling and bending are not good, and storage, transportation, construction and installation are not convenient enough. Therefore, the preparation of the silica aerogel composite material without powder falling is of great significance.
Disclosure of Invention
The invention aims to provide a preparation method of a powder falling prevention silicon dioxide aerogel felt.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the powder falling prevention silicon dioxide aerogel felt is characterized by comprising the following steps:
(1) Preparing silica sol: uniformly mixing a silicon source, ethanol and water to obtain silicon dioxide sol;
(2) Dipping the fiber felt body with the silica sol catalyzed by the gelling catalyst before gelling to prepare silica wet gel felt or dipping the fiber felt body with the silica sol and then catalyzing gelling by the gelling catalyst to prepare the silica wet gel felt;
(3) And packaging treatment: packaging the surfaces of the silica wet gel felt obtained in the step (2), and reserving one surface for non-packaging;
(4) And (3) drying treatment: drying the silica wet gel felt obtained in the step (3) after packaging treatment to obtain a silica aerogel felt;
(5) And (5) packaging the non-packaged surface of the silica aerogel felt obtained in the step (4) to obtain the powder falling prevention silica aerogel felt.
Preferably, in the step (1), the silica sol is prepared by mixing a silicon source, ethanol, water = 1: 2 to 60: 1 to 30 in a molar ratio; the silicon source is one or more than two of ethyl orthosilicate, methyl orthosilicate, butyl orthosilicate, isopropyl orthosilicate or alkyl alkoxy silane; the alkyl alkoxy silane comprises one or more than two of methyl trimethoxy silane, dimethyl dimethoxy silane, methyl triethoxy silane, dimethyl diethoxy silane, vinyl triethoxy silane, propyl trimethoxy silane or propyl triethoxy silane.
Preferably, the step (1) further comprises adding an acidic catalyst into the silica sol, and adjusting the pH of the solution to 2-6, wherein the acidic catalyst is one or a combination of two or more of sulfuric acid, hydrochloric acid, hydrofluoric acid, oxalic acid, acetic acid or benzenesulfonic acid.
Preferably, in the step (2), the gelling catalyst is one or a combination of two of alkaline catalysts such as sodium hydroxide, potassium hydroxide, ammonia water and ammonium fluoride aqueous solution, and the alkaline gelling catalyst adjusts the pH of the silica sol to 6-8;
preferably, in the step (2), the fiber felt body is one of a glass fiber felt, an aluminum silicate fiber felt, a quartz fiber felt, a high silica fiber felt, a carbon fiber felt, a pre-oxidized fiber felt, a mullite fiber felt, a basalt fiber felt, a silicon carbide fiber felt, an alumina fiber felt, and a boron nitride fiber felt.
Preferably, the step (2) further comprises a gel aging process of the silica wet gel felt, specifically, the silica wet gel felt is aged for 8-24 hours at room temperature or under the condition of heating to 30-60 ℃.
Preferably, the aging treatment process further comprises a hydrophobization treatment process of the silica wet gel felt, specifically, the silica wet gel felt is placed in an anhydrous ethanol solution containing 0.2-10% of hydrophobization agent by volume fraction and is kept standing for 1-24h at room temperature.
Preferably, in the step (3) and the step (5), the specific process of the packaging treatment is as follows: and spraying a water-based adhesive or a water-based elastic coating or a flame-retardant coating on the surface of the silica gel felt, wherein the thickness of the packaging layer is 0.01-3mm.
Preferably, the aqueous adhesive comprises one of epoxy resin adhesive, acrylic acid adhesive, acrylate adhesive, EVA adhesive, polyester adhesive, polyether adhesive, polyurethane adhesive, polyurea adhesive, and the like.
Preferably, the water-based paint is one of water-based ethylene-vinyl acetate elastic paint, water-based organosilicon acrylic elastic paint, water-based acrylic elastic paint and water-based rubber emulsion.
Preferably, the flame retardant coating is any one of commercially available flame retardant coatings.
Preferably, in the step (4), the drying treatment is one of supercritical drying, freeze drying and atmospheric drying.
The powder falling prevention silicon dioxide aerogel felt is obtained by the preparation method.
Has the advantages that:
according to the invention, the surface of the silica wet gel felt is packaged, one of the surfaces is reserved and not packaged, the surface of the aerogel felt is sprayed with a water-based adhesive or a water-based elastic coating or a flame-retardant coating, the bonding force between the aerogel and the fibers on the surface of the fibrofelt body is enhanced before drying, then the drying process is carried out, and finally the surface which is not packaged is packaged, so that the phenomena of larger dust pollution and the like caused by the powder falling condition of the aerogel after drying are avoided to a great extent.
Generally, the powder falling phenomenon of the silicon dioxide aerogel composite material mainly occurs in the transportation, construction and use processes after the aerogel felt body is dried, aerogel particles fall off from a fiber matrix, the existing powder falling prevention scheme is that glass fiber cloth, aluminum foil cloth and the like are pasted on the surface of the aerogel felt, the felt body falling aerogel powder can still exist in the process of cutting the aerogel felt, the scheme is not the best scheme, the packaging treatment is directly carried out before the drying, the aerogel on the surface of the felt body is still in a gel state during packaging, the powder falling phenomenon cannot be generated, and the condition that the aerogel powder falls off on the surface of the felt body in the process of packaging the aerogel felt after the aerogel felt is dried is well avoided.
The selection of the packaging layer can change the hydrophobic property of the felt body to a certain extent, and simultaneously can realize the function of flame retardant property.
Detailed Description
The present invention will be further described with reference to the following specific examples. It should be understood that the following examples are illustrative only and are not intended to limit the scope of the present invention.
Example 1:
the preparation method of the powder falling prevention silicon dioxide aerogel felt is characterized by comprising the following steps:
(1) Preparing silica sol: uniformly mixing a silicon source, ethanol and water to obtain silicon dioxide sol;
(2) Adding a gelling catalyst into the sol obtained in the step (1), uniformly stirring to obtain catalyzed silica sol, and dipping and gelling the glass fiber mat in the catalyzed silica sol to obtain a silica wet gel mat;
(3) And packaging treatment: packaging the surface of the wet silica gel felt obtained in the step (2) by using a water-based adhesive, and reserving the upper surface without packaging, wherein the thickness of a packaging layer is 1mm;
(4) And aging treatment: carrying out aging treatment on the surface-packaged silicon dioxide wet gel felt obtained in the step (3) for 24 hours at room temperature;
(5) And (3) hydrophobization treatment: placing the aged silicon dioxide wet gel felt obtained in the step (4) into an absolute ethyl alcohol solution containing a hydrophobizing agent with the volume fraction of 9%, and standing at room temperature for 5 hours;
(6) And (3) drying treatment: performing supercritical drying treatment on the silica wet gel felt after the solvent replacement obtained in the step (5) to obtain a silica aerogel felt;
(7) And (5) packaging the non-packaged upper surface of the silica aerogel felt obtained in the step (6) to obtain the powder falling prevention silica aerogel felt.
Wherein, in the step (1), the silica sol is obtained by mixing a silicon source, ethanol and water according to a molar ratio of 1: 6: 2; the silicon source is tetraethoxysilane.
In the step (2), the gelling catalyst is ammonium fluoride aqueous solution, and the pH of the solution is adjusted to 7.
In the step (3), the water-based adhesive is a polyester adhesive.
The powder falling prevention silicon dioxide aerogel felt is obtained by the preparation method.
The thermal conductivity of the powder falling prevention silica aerogel felt obtained in the embodiment is 0.02 w/(m.DEG C).
Example 2:
the preparation method of the powder falling prevention silicon dioxide aerogel felt is characterized by comprising the following steps:
(1) Preparing silica sol: uniformly mixing a silicon source, ethanol and water to obtain silicon dioxide sol;
(2) Dipping an aluminum silicate fiber felt in the silica sol obtained in the step (1), and then adding a gelling catalyst to obtain a silica wet gel felt;
(3) And packaging treatment: packaging the surface of the silica wet gel felt obtained in the step (2) by adopting a flame retardant coating, reserving the lower surface without packaging, wherein the thickness of a packaging layer is 1.5mm;
(4) And aging treatment: carrying out aging treatment on the surface-packaged silicon dioxide wet gel felt obtained in the step (3) for 10 hours at the temperature of 40 ℃;
(5) And (3) hydrophobization treatment: placing the aged silicon dioxide wet gel felt obtained in the step (4) into an absolute ethyl alcohol solution containing a hydrophobizing agent with the volume fraction of 1%, and standing at room temperature for 20 hours;
(6) And solvent replacement: placing the silicon dioxide wet gel felt subjected to the hydrophobization treatment in the step (5) into absolute ethyl alcohol for solvent replacement, wherein the number of times of replacement is 4, and the time of replacement is 8h;
(7) And drying treatment: performing supercritical drying treatment on the silica wet gel felt after the solvent replacement obtained in the step (6) to obtain a silica aerogel felt;
(8) And (5) packaging the non-packaged lower surface of the silica aerogel felt obtained in the step (7) to obtain the powder falling prevention silica aerogel felt.
Wherein, in the step (1), the silica sol is obtained by mixing a silicon source, ethanol and water according to a molar ratio of 1: 30: 8; the silicon source is methyl orthosilicate.
In the step (2), the gelling catalyst is an ammonia solution, and the pH of the solution is adjusted to 8.
In the step (3), the flame-retardant coating is a commercially available waterborne polyurethane flame-retardant coating.
The powder falling prevention silicon dioxide aerogel felt is obtained by the preparation method.
The thermal conductivity of the powder dropping prevention silica aerogel felt obtained in the embodiment is 0.022 w/(m.DEG C).
Example 3:
the preparation method of the powder falling prevention silicon dioxide aerogel felt is characterized by comprising the following steps:
(1) And preparing silica sol: uniformly mixing a silicon source, ethanol and water to obtain silicon dioxide sol;
(2) Adding a gelling catalyst into the sol obtained in the step (1), uniformly stirring to obtain catalyzed silica sol, and dipping and gelling the quartz fiber felt in the catalyzed silica sol to obtain a silica wet gel felt;
(3) And packaging treatment: packaging the surface of the wet silica gel felt obtained in the step (2) by using a water-based elastic coating, reserving the upper surface without packaging, wherein the thickness of a packaging layer is 2mm;
(4) And aging treatment: carrying out aging treatment on the surface-packaged silicon dioxide wet gel felt obtained in the step (3) for 18h at room temperature;
(5) And (3) drying treatment: drying the aged silica wet gel felt obtained in the step (4) at normal pressure to obtain a silica aerogel felt;
(6) And (5) packaging the non-packaged upper surface of the silica aerogel felt obtained in the step (5) to obtain the powder falling prevention silica aerogel felt.
Wherein, in the step (1), the silica sol is obtained by mixing a silicon source, ethanol and water according to a molar ratio of 1: 50: 25; the silicon source is tetraethoxysilane and methyltrimethoxysilane.
In the step (2), the gelling catalyst is a mixed solution of ammonia water and ammonium fluoride, and the pH of the silica sol is adjusted to 8.
In the step (3), the water-based elastic coating is a water-based ethylene-vinyl acetate elastic coating.
The powder falling prevention silicon dioxide aerogel felt is obtained by the preparation method.
The thermal conductivity of the powder-dropping prevention silica aerogel felt obtained in the embodiment is 0.021 w/(m.DEG C).
Example 4:
the preparation method of the powder falling prevention silicon dioxide aerogel felt is characterized by comprising the following steps:
(1) Preparing silica sol: uniformly mixing a silicon source, ethanol and water to obtain silicon dioxide sol;
(2) Adding a gelling catalyst into the sol obtained in the step (1), uniformly stirring to obtain catalyzed silica sol, and dipping and gelling the mullite fiber felt in the catalyzed silica sol to obtain a silica wet gel felt;
(3) And packaging treatment: packaging the surface of the wet silica gel felt obtained in the step (2) by using a water-based elastic coating, reserving a side surface without packaging, wherein the thickness of a packaging layer is 0.1mm;
(4) And aging treatment: carrying out aging treatment on the surface-packaged silicon dioxide wet gel felt obtained in the step (3) for 15 hours at the temperature of 30 ℃;
(5) And (3) hydrophobization treatment: placing the aged silicon dioxide wet gel felt obtained in the step (4) into an absolute ethyl alcohol solution containing a hydrophobizing agent with the volume fraction of 5%, and standing at room temperature for 12 hours;
(6) And (3) drying treatment: drying the aged silica wet gel felt obtained in the step (5) under normal pressure to obtain a silica aerogel felt;
(7) And (4) packaging the side surface of the silica aerogel felt obtained in the step (6) which is not packaged to obtain the powder falling prevention silica aerogel felt.
Wherein, in the step (1), the silica sol is obtained by mixing a silicon source, ethanol and water according to a molar ratio of 1: 20: 8; the silicon source is isopropyl n-silicate.
In the step (2), the gelling catalyst is ammonia water, and the pH of the solution is adjusted to 9.
In the step (3), the aqueous elastic coating is an aqueous acrylic elastic coating.
The powder falling prevention silicon dioxide aerogel felt is obtained through the preparation method.
The thermal conductivity of the powder-dropping prevention silica aerogel felt obtained in the embodiment is 0.024 w/(m.DEG C).
Example 5:
the preparation method of the powder falling prevention silicon dioxide aerogel felt is characterized by comprising the following steps:
(1) Preparing silica sol: uniformly mixing a silicon source, ethanol and water to obtain silicon dioxide sol;
(2) Adding a gelling catalyst into the sol obtained in the step (1), uniformly stirring to obtain catalyzed silica sol, and dipping and gelling the silicon carbide fibrofelt in the catalyzed silica sol to obtain a silica wet gel felt;
(3) And packaging treatment: packaging the surface of the wet silica gel felt obtained in the step (2) by using a water-based adhesive, reserving a side surface without packaging, wherein the thickness of a packaging layer is 0.05mm;
(4) And (3) drying treatment: performing supercritical drying treatment on the packaged silica wet gel felt obtained in the step (3) to obtain a silica aerogel felt;
(5) And (5) packaging the side surface of the silica aerogel felt obtained in the step (4) which is not packaged to obtain the powder falling prevention silica aerogel felt.
Wherein, in the step (1), the silica sol is obtained by mixing a silicon source, ethanol and water according to a molar ratio of 1: 40: 15; the silicon source is vinyltriethoxysilane.
In the step (2), the gelling catalyst is a mixed solution of ammonium fluoride and ammonia water, and the pH of the solution is adjusted to 8.
In the step (3), the aqueous adhesive is an acrylic adhesive.
The powder falling prevention silicon dioxide aerogel felt is obtained through the preparation method.
The thermal conductivity of the powder dropping prevention silica aerogel felt obtained in the embodiment is 0.022 w/(m.DEG C).
Claims (10)
1. A preparation method of powder falling prevention silicon dioxide aerogel felt is characterized in that,
the method comprises the following steps:
(1) Preparing silica sol: uniformly mixing a silicon source, ethanol and water to obtain silicon dioxide sol;
(2) And dipping treatment: soaking the fiber felt body with the silica sol catalyzed by the gelling catalyst before gelling to prepare the silica wet gel felt or soaking the fiber felt body with the silica sol and catalyzing gelling by the gelling catalyst to prepare the silica wet gel felt;
(3) And packaging treatment: packaging the surfaces of the silica wet gel felt obtained in the step (2), and reserving one surface without packaging;
(4) And drying treatment: drying the silica wet gel felt obtained in the step (3) after packaging treatment to obtain a silica aerogel felt;
(5) Packaging the non-packaged surface of the silica aerogel felt obtained in the step (4) to obtain the powder falling prevention silica aerogel felt;
in the step (3) and the step (5), the specific process of the packaging treatment is as follows: and (3) spraying a water-based adhesive or a water-based elastic coating or a flame-retardant coating on the surface of the silicon dioxide gel felt, wherein the thickness of the packaging layer is 0.01-3mm.
2. The method of preparing the powder fall prevention silica aerogel blanket of claim 1, wherein:
in the step (1), the silica sol is obtained by mixing a silicon source, ethanol and water according to a molar ratio of 1 to (2 to 60) to (1 to 30); the silicon source is one or more than two of ethyl orthosilicate, methyl orthosilicate, butyl orthosilicate, isopropyl orthosilicate or alkyl alkoxy silane; the alkyl alkoxy silane comprises one or more than two of methyl trimethoxy silane, dimethyl dimethoxy silane, methyl triethoxy silane, dimethyl diethoxy silane, vinyl triethoxy silane, propyl trimethoxy silane or propyl triethoxy silane.
3. The method of preparing a powder fall prevention silica aerogel blanket as claimed in claim 1, wherein:
and (2) adding an acidic catalyst into the silica sol obtained in the step (1), and adjusting the pH of the solution to 2-6, wherein the acidic catalyst is one or a combination of more than two of sulfuric acid, hydrochloric acid, hydrofluoric acid, oxalic acid, acetic acid or benzenesulfonic acid.
4. The method of preparing the powder fall prevention silica aerogel blanket of claim 1, wherein:
in the step (2), the gelling catalyst is one or a combination of two of alkaline catalysts such as sodium hydroxide, potassium hydroxide, ammonia water and ammonium fluoride aqueous solution, and the pH of the silica sol is adjusted to 6-8 by the alkaline gelling catalyst.
5. The method of preparing a powder fall prevention silica aerogel blanket as claimed in claim 1, wherein:
in the step (2), the fiber felt body is one of a glass fiber felt, an aluminum silicate fiber felt, a quartz fiber felt, a high silica fiber felt, a carbon fiber felt, a pre-oxidized fiber felt, a mullite fiber felt, a basalt fiber felt, a silicon carbide fiber felt, an alumina fiber felt and a boron nitride fiber felt.
6. The method of preparing the powder fall prevention silica aerogel blanket of claim 1, wherein:
and (2) further comprising a gel aging process of the silica wet gel felt, specifically, carrying out aging treatment on the silica wet gel felt for 8-24 hours at room temperature or at the temperature of 30-60 ℃.
7. The method of preparing the powder fall prevention silica aerogel blanket as claimed in claim 6, wherein:
and (3) after the aging treatment, the process of hydrophobization treatment of the silica wet gel felt is also included, specifically, the silica wet gel felt is placed in an absolute ethyl alcohol solution containing 0.2-10% of hydrophobization agent by volume fraction, and is kept standing for 1-24h at room temperature.
8. The method of preparing a powder fall prevention silica aerogel blanket as claimed in claim 1, wherein:
the water-based adhesive comprises one of epoxy resin adhesive, acrylic acid adhesive, acrylate adhesive, EVA adhesive, polyester adhesive, polyether adhesive, polyurethane adhesive, polyurea adhesive and the like; the water-based paint is one of water-based ethylene-vinyl acetate elastic paint, water-based organosilicon acrylic elastic paint, water-based acrylic elastic paint and water-based rubber emulsion.
9. The method of preparing the powder fall prevention silica aerogel blanket of claim 1, wherein:
in the step (4), the drying treatment is one of supercritical drying, freeze drying and normal pressure drying.
10. A powder fall-off resistant silica aerogel blanket prepared by the method of any of claims 1 to 9.
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| CN114571815A (en) * | 2022-03-10 | 2022-06-03 | 浙江葆润应用材料有限公司 | Multi-layer fireproof PCM composite material for battery pack |
| CN114806325A (en) * | 2022-03-21 | 2022-07-29 | 河南普力特克新材料有限公司 | Encapsulation flame-retardant coating for aerogel and production process thereof |
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| CN115124319B (en) * | 2022-07-04 | 2023-03-24 | 巩义市泛锐熠辉复合材料有限公司 | High-compression silicon dioxide aerogel, aerogel felt and preparation method thereof |
| CN115043408B (en) * | 2022-07-04 | 2023-11-10 | 巩义市泛锐熠辉复合材料有限公司 | Flexible silica aerogel, aerogel felt and preparation method thereof |
| CN115057683A (en) * | 2022-07-13 | 2022-09-16 | 巩义市泛锐熠辉复合材料有限公司 | Wet-method fiber-reinforced high-temperature-resistant aerogel product and preparation method thereof |
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| CN101948296B (en) * | 2010-09-28 | 2013-08-21 | 航天特种材料及工艺技术研究所 | High-performance thermal insulation material and preparation method thereof |
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| CN111018482B (en) * | 2019-11-22 | 2021-08-24 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of fiber-reinforced flexible silica aerogel |
| CN111016332A (en) * | 2019-12-26 | 2020-04-17 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of heat-insulation vacuum plate |
| CN111851070A (en) * | 2020-07-07 | 2020-10-30 | 巩义市泛锐熠辉复合材料有限公司 | Heat-insulating flame-retardant sheet and preparation method thereof |
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