CN108996985B - Preparation method of aerogel felt heat insulation material - Google Patents
Preparation method of aerogel felt heat insulation material Download PDFInfo
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- CN108996985B CN108996985B CN201810889041.9A CN201810889041A CN108996985B CN 108996985 B CN108996985 B CN 108996985B CN 201810889041 A CN201810889041 A CN 201810889041A CN 108996985 B CN108996985 B CN 108996985B
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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
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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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
- 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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- 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
- 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 belongs to heat insulationThe field of heat-insulating materials and discloses a preparation method of an aerogel felt heat-insulating material. Mixing orthosilicate ester, ethanol and water uniformly, and adding NH in sequence4Uniformly stirring the solution F and ammonia water to obtain silica sol A; stirring and mixing the resin, the initiator, the coupling agent and the hollow glass beads uniformly in a sealable container to obtain slurry B; soaking the fibrofelt in the silica sol A, taking out the fibrofelt, then soaking the fibrofelt in the freshly prepared slurry B, repeating the operation for 3-4 times, wherein the silica sol A is always in a stirring state when the fibrofelt is soaked in the slurry B, and then taking out the fibrofelt and placing the fibrofelt under a vacuum condition for sealing and standing; and (3) aging and modifying the obtained fibrofelt, then replacing the solvent by absolute ethyl alcohol, and then drying and thermally treating to obtain the aerogel felt heat insulation material. The invention overcomes the problem that the powder falls off and falls off in the traditional silica aerogel felt on the premise of not influencing the heat insulation and preservation effects of the felt body.
Description
Technical Field
The invention belongs to the field of heat insulation materials, and particularly relates to a preparation method of an aerogel felt heat insulation material.
Background
The aerogel is a nano porous material with the porosity of 80-99.8%, and the specific surface area of the aerogel can reach 200-1000 m2The aerogel has extremely low density, is the lightest solid in the world at present, and also has low thermal conductivity (as low as 0.01W/m.K), high porosity (as high as 99%), high light transmittance (as high as 99%), low dielectric constant (as low as 1.0-2.0), low refractive index (as low as 1.05) and the like.
SiO2Compared with other traditional heat insulation materials, the aerogel felt has unparalleled superiority, is a solid material with the best performance of the current heat insulation materials, and is a preferred material for saving energy and reducing consumption. But also because of the structural characteristics of the aerogel, the aerogel has the defects of large brittleness, poor flexibility and the like, and simultaneously, because of the preparation method, SiO2The aerogel felt generally has the condition that the felt body drops aerogel powder in the transportation, construction and use processes, the powder dropping condition not only brings inconvenience to the construction, but also brings threat to the health of constructors, and simultaneously, the performance of the aerogel felt can be reduced, and the application range of the aerogel felt is greatly limited. 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, reduce the dust pollution problem of the aerogel felt in storage, transportation, installation and use and meet the requirements of various fields in the market.
Disclosure of Invention
The invention aims to provide a preparation method of an aerogel felt heat insulation material, which can ensure that the prepared aerogel felt heat insulation material does not fall off powder and reduce the problem of dust pollution of aerogel in storage, transportation, installation and use on the premise of not influencing the heat insulation performance of the aerogel felt heat insulation material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of aerogel felt heat insulation material comprises the following steps:
(1) mixing orthosilicate ester, ethanol and water uniformly, and then adding NH in sequence4Uniformly stirring the solution F and ammonia water to obtain silica sol A;
(2) according to parts by weight, stirring and mixing 2-20 parts of resin, 0.02-0.05 part of initiator, 0.5-5 parts of coupling agent and 100 parts of hollow glass beads uniformly in a sealable container to obtain slurry B;
(3) soaking a fibrofelt in the silica sol A obtained in the step (1), taking out the fibrofelt, and soaking the fibrofelt in a freshly prepared slurry B;
(4) repeating the process of the step (3) for 3-4 times, wherein the silica sol A is always in a stirring state when the fibrofelt is soaked in the slurry B, and then taking out the fibrofelt and placing the fibrofelt under a vacuum condition for sealing and standing for 1-3 hours;
(5) aging the fiber felt obtained in the step (4), soaking the aged fiber felt in a modification solution for 12-24 hours, performing solvent replacement by using absolute ethyl alcohol, and drying to obtain an aerogel heat insulation felt;
(6) carrying out heat treatment on the aerogel heat insulation felt obtained in the step (5) to obtain an aerogel felt heat insulation material;
wherein, in the step (1): in a molar ratio, orthosilicate ester, ethanol and water = 1: 4-12: 2-4; NH (NH)4The amount of the F solution added is such that the molar ratio of NH is4F, orthosilicate ester = (0.002-0.01): 1; the addition of ammonia water ensures that NH is calculated by molar ratio3Orthosilicate = (0.005-0.015) 1; in the step (4), the modifying solution is a mixed solution prepared by mixing hexamethyldisiloxane and absolute ethyl alcohol according to the molar ratio of 1: 2-5.
Preferably, in the step (1), the orthosilicate is tetraethoxysilane or methyl orthosilicate.
Preferably, in step (2), the resin is an epoxy resin or an unsaturated resin, and the unsaturated resin is one or a mixture of more than two of unsaturated polyester resin 191#, unsaturated polyester resin 197#, vinyl resin MFE-2 and vinyl resin VER-2.
Preferably, in the step (2), the initiator is one or a mixture of more than two of methyl ethyl ketone peroxide, cobalt naphthenate, BPO and AIBN.
Preferably, in the step (2), the coupling agent is a silane coupling agent, and the density of the hollow ceramic microspheres is 0.15-0.60 g/cm3。
Preferably, in the step (3), the dipping time of the fiber felt in the silica sol A is 4-6 hours each time, and the dipping time in the slurry B is 2-3 hours each time.
Preferably, in the step (5), the aging is carried out under a heating condition, wherein the heating temperature of the aging is 30-60 ℃, and the aging time is 8-24 hours.
Preferably, in the step (5), the aged fiber mat is immersed in the modifying solution for 12-24 hours.
Preferably, in the step (5), the number of times of solvent replacement is 2-3, and the time of each replacement is 12-36 h.
Preferably, in the step (6), the temperature of the heat treatment is 600-650 ℃ and the time is 0.5-2 h.
In the present invention, the ethanol is preferably of an analytically pure grade or a chemically pure grade.
According to the invention, the fiber felt is alternately impregnated with the silica sol A and the slurry B, the slurry B covers the surface of the fiber felt after the final impregnation is finished, the fiber felt can fix silica aerogel particles layer by layer after being cured, the powder falling condition of the later aerogel particles is reduced, and meanwhile, the uniformity of the distribution of the aerogel particles can be ensured through stepwise impregnation, so that the pore structure distribution is more orderly and complete. Secondly, the slurry B is cured and molded, then the hollow glass beads and the silicon dioxide aerogel particles are closely combined, finally the unsaturated resin is removed through the heat treatment effect, the rest hollow glass beads and the silicon dioxide aerogel particles are distributed in a three-dimensional space framework in the fiber felt, the fiber felt can be ensured to have good heat insulation performance, meanwhile, the powder falling phenomenon of the traditional silicon dioxide aerogel felt is avoided to a certain extent, and the promotion significance for meeting various demands of the market is achieved.
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.
The absolute ethanol in the following examples is of analytical grade.
Example 1
A preparation method of aerogel felt heat insulation material comprises the following steps:
(1) taking tetraethoxysilane, absolute ethyl alcohol and water to be uniformly mixed, and then sequentially adding 2 mol/L NH4Uniformly stirring the solution F and 0.2 moL/L ammonia water to obtain silica sol A;
(2) according to the parts by weight, 20 parts of resin, 0.04 part of initiator, 3 parts of coupling agent and 100 parts of hollow glass beads are stirred and mixed uniformly in a sealable container to obtain slurry B;
(3) soaking the glass fiber mat in the silica sol A obtained in the step (1) for 6 hours, taking out the glass fiber mat and then soaking the glass fiber mat in the freshly prepared slurry B for 3 hours;
(4) repeating the process of the step (3) for 4 times, wherein the silica sol A is always in a stirring state when the glass fiber mat is soaked in the slurry B, and then taking out the glass fiber mat and placing the glass fiber mat under a vacuum condition for sealing and standing for 2 hours;
(5) aging the glass fiber mat obtained in the step (4) under heating conditions, wherein the aging heating temperature is 60 ℃ and the aging time is 20 h, then soaking the glass fiber mat in a mixed solution of hexamethyldisiloxane and absolute ethyl alcohol for modification treatment (in terms of molar ratio, hexamethyldisiloxane: absolute ethyl alcohol = 1: 5) for 12 h, performing solvent replacement for 2 times by absolute ethyl alcohol, wherein the replacement time is 24 h each time, and then performing normal-pressure drying treatment to obtain an aerogel heat insulation mat;
(6) carrying out heat treatment on the aerogel heat insulation felt obtained in the step (5) at 600 ℃ for 1.5 h to obtain an aerogel felt heat insulation material;
wherein, in the step (1): in a molar ratio, tetraethoxysilane, absolute ethyl alcohol and water are = 1: 10: 4; NH (NH)4The amount of the F solution added is such that the molar ratio of NH is4Ethyl orthosilicate = 0.006: 1; the addition of ammonia water ensures that NH is calculated by molar ratio3Tetraethoxysilane = 0.014: 1; in the step (2), the resin is epoxy resin, the initiator is methyl ethyl ketone peroxide, the coupling agent is KH-560, and the hollow glass beads are products of K20 from 3M company and have a density of 0.20 g/cm3。
Example 2
A preparation method of aerogel felt heat insulation material comprises the following steps:
(1) taking tetraethoxysilane, absolute ethyl alcohol and water to be uniformly mixed, and then sequentially adding 2 mol/L NH4Uniformly stirring the solution F and 0.2 moL/L ammonia water to obtain silica sol A;
(2) according to the parts by weight, stirring and mixing 18 parts of resin, 0.05 part of initiator, 4 parts of coupling agent and 100 parts of hollow glass beads uniformly in a sealable container to obtain slurry B;
(3) soaking the glass fiber mat in the silica sol A obtained in the step (1) for 5 hours, taking out the glass fiber mat and then soaking the glass fiber mat in the freshly prepared slurry B for 3 hours;
(4) repeating the process of the step (3) for 3 times, wherein the silica sol A is always in a stirring state when the glass fiber mat is soaked in the slurry B, and then taking out the glass fiber mat and placing the glass fiber mat under a vacuum condition for sealing and standing for 2 hours;
(5) aging the glass fiber mat obtained in the step (4) under heating conditions, wherein the aging heating temperature is 50 ℃ and the aging time is 18 h, then soaking the glass fiber mat in a mixed solution of hexamethyldisiloxane and absolute ethyl alcohol for modification treatment (in terms of molar ratio, hexamethyldisiloxane: absolute ethyl alcohol = 1: 4) for 20 h, performing solvent replacement for 3 times by absolute ethyl alcohol, wherein the replacement time is 20 h each time, and then performing normal-pressure drying treatment to obtain an aerogel heat insulation mat;
(6) carrying out heat treatment on the aerogel heat insulation felt obtained in the step (5) at 650 ℃ for 0.5 h to obtain an aerogel felt heat insulation material;
wherein, in the step (1): in a molar ratio, tetraethoxysilane, absolute ethyl alcohol and water are = 1: 12: 3; NH (NH)4The amount of the F solution added is such that the molar ratio of NH is4F, tetraethoxysilane = 0.008: 1; the addition of ammonia water ensures that NH is calculated by molar ratio3Ethyl orthosilicate = 0.008: 1; in the step (2), the resin is unsaturated polyester resin No. 191, the initiator is BPO, the coupling agent is KH-560, and the hollow glass microspheres are XLD3000 products of 3M company, and the density of the hollow glass microspheres is 0.23 g/cm3。
Example 3
A preparation method of aerogel felt heat insulation material comprises the following steps:
(1) taking tetraethoxysilane, absolute ethyl alcohol and water to be uniformly mixed, and then sequentially adding 2 mol/L NH4Uniformly stirring the solution F and 0.2 moL/L ammonia water to obtain silica sol A;
(2) according to the parts by weight, stirring and mixing 15 parts of resin, 0.02 part of initiator, 2 parts of coupling agent and 100 parts of hollow glass beads uniformly in a sealable container to obtain slurry B;
(3) soaking the glass fiber mat in the silica sol A obtained in the step (1) for 6 hours, taking out the glass fiber mat and then soaking the glass fiber mat in the freshly prepared slurry B for 2 hours;
(4) repeating the process of the step (3) for 3 times, wherein the silica sol A is always in a stirring state when the glass fiber mat is soaked in the slurry B, and then taking out the glass fiber mat and placing the glass fiber mat under a vacuum condition for sealing and standing for 3 hours;
(5) aging the glass fiber mat obtained in the step (4) under heating conditions, wherein the aging heating temperature is 40 ℃, the aging time is 24 h, then soaking the glass fiber mat in a mixed solution of hexamethyldisiloxane and absolute ethyl alcohol for modification treatment (in terms of molar ratio, hexamethyldisiloxane: absolute ethyl alcohol = 1: 3) for 24 h, performing solvent replacement for 3 times by absolute ethyl alcohol, wherein the replacement time is 15 h each time, and then performing normal-pressure drying treatment to obtain an aerogel heat insulation mat;
(6) carrying out heat treatment on the aerogel heat insulation felt obtained in the step (5) at 650 ℃ for 1 h to obtain an aerogel felt heat insulation material;
wherein, in the step (1): in a molar ratio, tetraethoxysilane, absolute ethyl alcohol and water are = 1: 8: 2; NH (NH)4The amount of the F solution added is such that the molar ratio of NH is4F, tetraethoxysilane = 0.01: 1; the addition of ammonia water ensures that NH is calculated by molar ratio3Ethyl orthosilicate = 0.013: 1; in the step (2), the resin is vinyl resin MFE-2, the initiator is cobalt naphthenate, the coupling agent is KH-560, the hollow glass microsphere is a VS5500 product of 3M company, and the density of the hollow glass microsphere is 0.38 g/cm3。
The thermal performance test results of the aerogel felt thermal insulation materials obtained in examples 1 to 3 are shown in the following table:
from the above table, it can be seen that: the aerogel felt heat insulation material prepared by the invention has excellent heat insulation performance.
Claims (8)
1. The preparation method of the aerogel felt heat insulation material is characterized by comprising the following steps:
(1) mixing orthosilicate ester, ethanol and water uniformly, and then adding NH in sequence4Uniformly stirring the solution F and ammonia water to obtain silica sol A;
(2) according to parts by weight, stirring and mixing 2-20 parts of resin, 0.02-0.05 part of initiator, 0.5-5 parts of coupling agent and 100 parts of hollow glass beads uniformly in a sealable container to obtain slurry B; (3) soaking a fibrofelt in the silica sol A obtained in the step (1), taking out the fibrofelt, and soaking the fibrofelt in a freshly prepared slurry B;
(4) repeating the process of the step (3) for 3-4 times, wherein the silica sol A is always in a stirring state when the fibrofelt is soaked in the slurry B, and then taking out the fibrofelt and placing the fibrofelt under a vacuum condition for sealing and standing for 1-3 hours;
(5) aging the fibrofelt obtained in the step (4), soaking the aged fibrofelt in a modification solution, performing solvent replacement by using absolute ethyl alcohol, and drying to obtain an aerogel heat insulation felt;
(6) carrying out heat treatment on the aerogel heat insulation felt obtained in the step (5) to obtain an aerogel felt heat insulation material;
wherein in the step (1), in terms of molar ratio, orthosilicate ester, ethanol and water are = 1: 4-12: 2-4; NH (NH)4The amount of the F solution added is such that the molar ratio of NH is4F, orthosilicate ester = (0.002-0.01): 1; the addition of ammonia water ensures that NH is calculated by molar ratio3Orthosilicate = (0.005-0.015) 1;
in the step (2), the resin is epoxy resin or unsaturated resin, and the unsaturated resin is one or a mixture of more than two of unsaturated polyester resin 191#, unsaturated polyester resin 197#, vinyl resin MFE-2 and vinyl resin VER-2;
in the step (4), the modification liquid is a mixed liquid formed by mixing hexamethyldisiloxane and absolute ethyl alcohol according to the molar ratio of 1: 2-5;
in the step (6), the temperature of the heat treatment is 600-650 ℃, and the time is 0.5-2 h.
2. The method of claim 1, wherein: in the step (1), the orthosilicate is tetraethoxysilane or methyl orthosilicate.
3. The method of claim 1, wherein: in the step (2), the initiator is one or a mixture of more than two of methyl ethyl ketone peroxide, cobalt naphthenate, BPO and AIBN.
4. The method of claim 1, wherein: in the step (2), the coupling agent is a silane coupling agent, and the density of the hollow glass beads is 0.15-0.60 g/cm3。
5. The method of claim 1, wherein: in the step (3), the fiber felt is soaked in the silica sol A for 4-6 hours each time, and is soaked in the slurry B for 2-3 hours each time.
6. The method of claim 1, wherein: in the step (5), aging is carried out under the heating condition, wherein the heating temperature of the aging is 30-60 ℃, and the aging time is 8-24 hours.
7. The method of claim 1, wherein: in the step (5), the aged fiber felt is soaked in the modification liquid for 12-24 hours.
8. The method of claim 1, wherein: in the step (5), the number of times of solvent replacement is 2-3, and the time of each replacement is 12-36 h.
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| CN109503116B (en) * | 2018-12-17 | 2020-12-11 | 山东鲁阳节能材料股份有限公司 | Preparation method of aerogel composite thermal insulation material |
| CN110922095B (en) * | 2019-11-07 | 2021-07-09 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of composite silica aerogel felt |
| CN111825423A (en) * | 2020-07-28 | 2020-10-27 | 巩义市泛锐熠辉复合材料有限公司 | Efficient heat insulation sheet and preparation method thereof |
| CN113651592A (en) * | 2021-08-20 | 2021-11-16 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of anti-buffering silicon dioxide aerogel heat insulation sheet |
| CN113603423A (en) * | 2021-08-24 | 2021-11-05 | 杭州金鼎实业有限公司 | Foam concrete and preparation method thereof |
| CN114033922A (en) * | 2021-11-18 | 2022-02-11 | 青海省水文地质工程地质环境地质调查院 | Preparation method of heat-insulating combined material suitable for hot dry rock single-hole heat-taking steam-discharging device |
| CN115110311B (en) * | 2022-07-08 | 2024-01-12 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of high-temperature-resistant alumina aerogel felt and alumina aerogel felt |
| CN116199522A (en) * | 2023-01-17 | 2023-06-02 | 武汉中科先进材料科技有限公司 | PU sponge-based silicon aerogel felt and preparation method thereof |
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| CN106007635A (en) * | 2015-03-24 | 2016-10-12 | 金承黎 | Aerogel composite material with surface subjected to dust-free treatment and preparation method |
| CN105645921B (en) * | 2016-03-10 | 2018-03-06 | 深圳中凝科技有限公司 | One kind prepares composite S iO2The method of aerogel blanket |
| CN106631154A (en) * | 2016-11-24 | 2017-05-10 | 纳诺科技有限公司 | Non-shedding aerogel composite material and production technique thereof |
| CN106700773A (en) * | 2016-12-01 | 2017-05-24 | 湖北硅金凝节能减排科技有限公司 | Anti-dusting coating and preparation method thereof |
| CN108610000B (en) * | 2017-04-25 | 2021-04-30 | 天津朗华睿博科技有限公司 | Preparation method of anti-falling powder aerogel composite heat-preservation felt |
| CN107021496A (en) * | 2017-05-27 | 2017-08-08 | 航天特种材料及工艺技术研究所 | A kind of ultra-low density silicon dioxide aerogel material and preparation method thereof |
| CN108569912A (en) * | 2018-04-29 | 2018-09-25 | 浙江工业大学 | A kind of preparation method of hydrophobic type aerosil composite fibre felt material |
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