CN114644503B - Mesoporous silica aerogel/fibrofelt composite heat insulation material and preparation method thereof - Google Patents
Mesoporous silica aerogel/fibrofelt composite heat insulation material and preparation method thereof Download PDFInfo
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- CN114644503B CN114644503B CN202210258873.7A CN202210258873A CN114644503B CN 114644503 B CN114644503 B CN 114644503B CN 202210258873 A CN202210258873 A CN 202210258873A CN 114644503 B CN114644503 B CN 114644503B
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- 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
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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- C04B2111/40—Porous or lightweight materials
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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Abstract
The invention relates to a mesoporous silica aerogel/fibrofelt composite heat-insulating material and a preparation method thereof. The invention provides a method for efficiently preparing a mesoporous silica aerogel/fibrofelt composite heat-insulating material, which can enable mesoporous silica aerogel balls to directly grow on fibrofelt in situ, avoids the use of a binder, and has stable structure and no shedding of aerogel powder; meanwhile, the method avoids the use of a large amount of organic solvents in the traditional aerogel felt preparation process, so that the preparation process becomes more green, and the preparation cost is reduced. In addition, the preparation method avoids the solvent exchange process of the silica gel, the whole preparation process is about 2 to 3 days, and the preparation time of the composite heat insulation felt is obviously shortened. Meanwhile, the preparation method has the advantages of simple process, strong operability, low cost, easy control of process conditions and wide scale application prospect.
Description
Technical Field
The invention belongs to the field of heat insulation materials, and particularly relates to a mesoporous silica aerogel/fibrofelt composite heat insulation material and a preparation method thereof.
Background
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
Currently, the mesoporous silica aerogel/fibrofelt composite heat-insulating material is prepared by directly growing the silica aerogel in situ in the gaps of the fibrofelt. The preparation method avoids the increase of the heat conductivity coefficient caused by using the binder, and the prepared silica aerogel/fibrofelt composite heat-insulating material has good flexibility and does not have the phenomena of brittle fracture, falling off and the like. However, the above sol-gel in-situ growth method still has the following problems in practical application: the use of a large amount of organic solvent is easy to cause adverse effect on the surrounding environment, and the green degree of the preparation process is low; the preparation process is complex in procedure, long in time consumption and high in cost, and the factors cause that the method is not beneficial to large-scale application and popularization.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a mesoporous silica aerogel/fibrofelt composite heat-insulating material and a preparation method thereof. The method is based on in-situ microemulsion hydrothermal growth, and solves the technical problems of how to improve the greenness of the preparation process, simplify the preparation process, reduce the preparation cost and improve the economy of the preparation process in the preparation process of the mesoporous silica aerogel/fibrofelt composite heat-insulating material.
In order to achieve the above technical effects, the present application provides the following technical solutions:
a preparation method of a mesoporous silica aerogel/fibrofelt composite heat insulation material comprises the following steps:
dissolving a triblock copolymer in a dilute hydrochloric acid solution, increasing the temperature, adding mesitylene into the solution, stirring to form a microemulsion, adding tetraethoxysilane, uniformly stirring, pouring the formed mixed sol on a fibrofelt, sealing the fibrofelt by using tinfoil paper or a PTFE film, standing for a period of time in a sealed state, carrying out hydrothermal reaction, then carrying out extraction treatment in absolute ethyl alcohol, and removing the triblock copolymer to obtain the mesoporous silica aerogel/fibrofelt composite heat-insulating material.
Further, after the temperature is raised to 30-45 ℃, adding the mesitylene into the solution and stirring to form the microemulsion.
Further, the triblock copolymer is polyoxyether P123 or F127.
Further, the fiber felt is a quartz fiber felt, an aramid fiber felt or an aluminum silicate fiber felt.
Further, the mass concentration of the dilute hydrochloric acid solution is 3wt% -6wt%.
Further, the mass and dosage ratio of the triblock copolymer, the dilute hydrochloric acid solution, the mesitylene and the ethyl orthosilicate is as follows: 5-10:100-200:5-10:15-25.
Further, after the fiber felt is sealed, the standing temperature is 30-45 ℃; the standing time is 15-24 hours.
Further, the hydrothermal time is 15-48 hours; the hydrothermal temperature is 80-100 ℃.
Further, the temperature of the extraction treatment in the absolute ethyl alcohol is 60-85 ℃.
Further, the time of the extraction treatment in the absolute ethyl alcohol is 15-48 hours.
The invention has the beneficial effects that:
the invention provides a method for efficiently preparing a mesoporous silica aerogel/fibrofelt composite heat-insulating material. The preparation process of the composite aerogel is simplified: a microemulsion drop formed by triblock copolymer and mesitylene in an aqueous solution is used as a template, ethyl orthosilicate is prehydrolyzed in an acidic solution and assembled around the microemulsion globule, when a fibrofelt is added into the precursor solution, the solution is absorbed into the fibrofelt, the fibrofelt is kept stand at a certain temperature and then subjected to hydro-thermal treatment, silicon oxide globules with a mesoscopic structure are formed in situ in gaps of the fibrofelt, and then the template agent is removed by ethanol extraction, so that the mesoporous silicon oxide aerogel/fibrofelt composite heat-insulating material is obtained. The preparation method can enable the mesoporous silica aerogel globules to directly grow on the fibrofelt in situ, avoids the use of a binder, has stable structure of the heat insulation material, and does not cause the shedding of aerogel powder; meanwhile, the method avoids the use of a large amount of organic solvents in the traditional aerogel felt preparation process, so that the preparation process becomes more green, and the preparation cost is reduced.
In addition, the preparation method avoids the solvent exchange process of the silica gel, the whole preparation process is about 2 to 3 days, and the preparation time of the composite heat insulation felt is obviously shortened. Meanwhile, the preparation method has the advantages of simple process, strong operability, low cost, easy control of process conditions and wide scale application prospect.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As an alternative embodiment, the invention provides a method for efficiently preparing a mesoporous silica aerogel/fibrofelt composite thermal insulation material. The preparation method comprises the following steps of firstly dissolving commercial triblock copolymers such as P123, F127 and the like in dilute hydrochloric acid solution with the weight percent of 3-6%, heating to 30-45 ℃, adding a certain amount of mesitylene into the solution, stirring to form microemulsion, and then adding tetraethoxysilane, wherein the mass and dosage ratio of the triblock copolymers/dilute hydrochloric acid solution/mesitylene/tetraethoxysilane is as follows: 5-10, pouring the formed mixed sol on a fibrofelt after uniformly stirring to enable the fibrofelt to be saturated by adsorption, sealing the fibrofelt by using tinfoil paper or a high-temperature-resistant PTFE film to prevent the solution from volatilizing, sealing and standing for 15-24 hours at 30-45 ℃, sealing and hydrothermal for 15-48 hours at 80-100 ℃, extracting at 60-85 ℃ in absolute ethyl alcohol, and removing triblock copolymer to obtain the mesoporous silica aerogel/fibrofelt composite heat-insulating material.
The method adopts a microemulsion hydrothermal in-situ growth method, a triblock copolymer (P123 or F127) surfactant with one hydrophilic end and one hydrophobic end is dissolved in water, mesitylene is dispersed in an aqueous solution to form microemulsion droplets, the hydrophobic end of the triblock copolymer acts around the mesitylene microemulsion droplets, the hydrophilic end faces the solution, and after tetraethoxysilane is added and prehydrolyzed, prehydrolyzed tetraethoxysilane is assembled at the hydrophilic end of the triblock copolymer to form the silicon oxide/triblock copolymer composite sol. When the fiber mat is put into the formed composite sol, the composite sol is adsorbed on the surface of the fiber by physical action. During the sealing and standing process at 30-45 ℃, the liquid drops with the silicon oxide are further assembled together to form silicon oxide spheres with mesostructure, and the crosslinking degree of the silicon oxide spheres is further enhanced and the framework becomes stronger in the further hydrothermal process. Since F127 or P123 and mesitylene have high solubility in ethanol, the template can be removed by an ethanol extraction method to obtain the mesoporous silica aerogel/fibrofelt composite heat-insulating material. Meanwhile, the method has the advantages of simple process, strong operability, easily controlled process conditions and wide scale application prospect.
The present invention is further described in detail below by way of specific examples, which will enable those skilled in the art to more fully understand the present invention, but which are not intended to limit the invention in any way.
Example 1
A method for preparing a heat insulation material by compounding mesoporous silica aerogel and a fiber felt comprises the following steps:
5g of polyoxyether P123 is dissolved in 100g of dilute 3wt% hydrochloric acid solution, 5g of trimesoyl benzene is added into the solution after the temperature is raised to 30 ℃ and stirred to form microemulsion, then 15g of tetraethoxysilane is added, the formed mixed sol is poured on a quartz fibrofelt after being stirred uniformly, then the fibrofelt is sealed by tin foil paper to prevent the solution from volatilizing, then the fibrofelt is sealed and kept stand for 24 hours at 30 ℃, then the fibrofelt is sealed and hydrothermal at 80 ℃ for 48 hours, then extraction treatment is carried out in absolute ethyl alcohol, the extraction temperature is 60 ℃, the extraction treatment time is 48 hours, triblock copolymer is removed, and the mesoporous silica aerogel/fibrofelt composite heat-insulating material is obtained. The thermal conductivity test shows that the thermal conductivity of the quartz fibrofelt is 0.075 w/(m.k), and the thermal conductivity of the obtained composite thermal insulation material is reduced to 0.031 w/(m.k) after the mesoporous oxide silica aerogel is compounded with the quartz fibrofelt.
Example 2
A method for preparing a heat insulation material by compounding mesoporous silica aerogel and a fiber felt comprises the following steps:
dissolving 10g of polyoxyether F127 in 200g of dilute 3wt% hydrochloric acid solution, adding 10g of trimesoyl benzene into the solution after the temperature is raised to 45 ℃, stirring to form a microemulsion, then adding 25g of tetraethoxysilane, pouring the formed mixed sol on an aramid fiber felt after uniform stirring, sealing the aramid fiber felt with tin foil paper to prevent the solution from volatilizing, sealing and standing at 45 ℃ for 15 hours, sealing and hydrothermal at 100 ℃ for 15 hours, then performing extraction treatment in absolute ethyl alcohol, wherein the extraction temperature is 85 ℃, the extraction treatment time is 15 hours, removing a triblock copolymer, and obtaining the mesoporous silica aerogel/fiber felt composite heat-insulating material. The thermal conductivity test shows that the thermal conductivity of the aramid fiber felt is 0.034 w/(m.k), and after the mesoporous oxide silica aerogel is compounded with the aramid fiber felt, the thermal conductivity of the obtained composite heat-insulating material is reduced to 0.028 w/(m.k).
Example 3
Dissolving 8g of polyoxyether F127 in 150g of dilute 3wt% hydrochloric acid solution, heating to 40 ℃, adding 8g of trimesoxazine into the solution, stirring to form a microemulsion, then adding 20g of tetraethoxysilane, pouring the formed mixed sol onto an aramid fiber felt after uniform stirring, sealing the fiber felt with tin foil paper to prevent the solution from volatilizing, sealing and standing at 40 ℃ for 20 hours, then sealing and hydrothermal at 90 ℃ for 30 hours, then performing extraction treatment in absolute ethyl alcohol, wherein the extraction temperature is 80 ℃, the extraction treatment time is 30 hours, removing the triblock copolymer, and obtaining the mesoporous silica aerogel/fiber felt composite heat-insulating material. The thermal conductivity test shows that the thermal conductivity of the aramid fiber felt is 0.034 w/(m.k), and after the mesoporous oxide silica aerogel is compounded with the aramid fiber felt, the thermal conductivity of the obtained composite heat-insulating material is reduced to 0.029 w/(m.k).
Example 4
Dissolving 8g of polyoxyether F127 in 150g of 6wt% dilute hydrochloric acid solution, heating to 40 ℃, adding 8g of trimesoxazine into the solution, stirring to form a microemulsion, then adding 20g of tetraethoxysilane, pouring the formed mixed sol on an aluminum silicate fiber felt after uniform stirring, sealing the fiber felt by using tin foil paper to prevent the solution from volatilizing, sealing and standing at 40 ℃ for 20 hours, then sealing and hydrothermal at 90 ℃ for 30 hours, then performing extraction treatment in absolute ethyl alcohol, wherein the extraction temperature is 80 ℃, the extraction treatment time is 30 hours, removing triblock copolymer, and obtaining the mesoporous silica aerogel/fiber felt composite heat-insulating material. The heat conductivity coefficient test shows that the heat conductivity coefficient of the aluminum silicate fiber felt is 0.094 w/(m.k), and after the mesoporous oxide silica aerogel is compounded with the aluminum silicate fiber felt, the heat conductivity coefficient of the obtained composite heat insulation material is reduced to 0.034 w/(m.k).
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (6)
1. The preparation method of the mesoporous silica aerogel/fibrofelt composite heat-insulating material is characterized by comprising the following steps of:
dissolving a triblock copolymer in a dilute hydrochloric acid solution, increasing the temperature, adding mesitylene into the solution, stirring to form a microemulsion, adding tetraethoxysilane, uniformly stirring, pouring the formed mixed sol on a fibrofelt, sealing the fibrofelt by using a tinfoil paper or a PTFE (polytetrafluoroethylene) film, standing for a period of time in a sealed state, performing hydrothermal reaction, then performing extraction treatment in absolute ethyl alcohol, and removing the triblock copolymer to obtain a mesoporous silica aerogel/fibrofelt composite heat-insulating material;
adding mesitylene into the solution after the temperature is raised to 30-45 ℃ and stirring to form microemulsion;
standing at 30-45 deg.C; standing for 15-24 hours;
the hydrothermal time is 15-48 hours; the hydrothermal temperature is 80-100 ℃;
the temperature of the extraction treatment is 60-85 ℃; the time of extraction treatment is 15-48 hours.
2. The process according to claim 1, wherein the triblock copolymer is a polyoxyether P123 or F127.
3. The production method according to claim 1, wherein the fiber mat is a quartz fiber mat, an aramid fiber mat, or an aluminum silicate fiber mat.
4. The preparation method according to claim 1, characterized in that the mass concentration of the dilute hydrochloric acid solution is 3wt% to 6wt%.
5. The preparation method according to claim 1, wherein the mass ratio of the triblock copolymer, the dilute hydrochloric acid solution, the mesitylene and the ethyl orthosilicate is as follows: 5-10:100-200:5-10:15-25.
6. The mesoporous silica aerogel/fibrofelt composite thermal insulation material prepared by the preparation method according to any one of the preceding claims.
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| CN202210258873.7A CN114644503B (en) | 2022-03-16 | 2022-03-16 | Mesoporous silica aerogel/fibrofelt composite heat insulation material and preparation method thereof |
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| CN202210258873.7A CN114644503B (en) | 2022-03-16 | 2022-03-16 | Mesoporous silica aerogel/fibrofelt composite heat insulation material and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6068882A (en) * | 1995-11-09 | 2000-05-30 | Aspen Systems, Inc. | Flexible aerogel superinsulation and its manufacture |
| CN107827116A (en) * | 2017-12-15 | 2018-03-23 | 江苏泛亚微透科技股份有限公司 | A kind of preparation method of porous silica silicon bulk aeroge |
| CN111253144A (en) * | 2020-02-18 | 2020-06-09 | 江苏泛亚微透科技股份有限公司 | Preparation method of titanium-doped silicon dioxide aerogel/fiber composite material |
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- 2022-03-16 CN CN202210258873.7A patent/CN114644503B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6068882A (en) * | 1995-11-09 | 2000-05-30 | Aspen Systems, Inc. | Flexible aerogel superinsulation and its manufacture |
| CN107827116A (en) * | 2017-12-15 | 2018-03-23 | 江苏泛亚微透科技股份有限公司 | A kind of preparation method of porous silica silicon bulk aeroge |
| CN111253144A (en) * | 2020-02-18 | 2020-06-09 | 江苏泛亚微透科技股份有限公司 | Preparation method of titanium-doped silicon dioxide aerogel/fiber composite material |
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