CN110918008A - Foam-reinforced SiO2-TiO2Preparation method of composite aerogel - Google Patents
Foam-reinforced SiO2-TiO2Preparation method of composite aerogel Download PDFInfo
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- CN110918008A CN110918008A CN201911194736.6A CN201911194736A CN110918008A CN 110918008 A CN110918008 A CN 110918008A CN 201911194736 A CN201911194736 A CN 201911194736A CN 110918008 A CN110918008 A CN 110918008A
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
Abstract
The invention discloses foam-reinforced SiO2‑TiO2The preparation method of the composite aerogel comprises the steps of mixing tetraethyl orthosilicate and tetrabutyl titanate according to a certain proportion, sequentially adding absolute ethyl alcohol and deionized water for stirring, adding a catalyst after a period of time, and soaking foam into prepared SiO2‑TiO2And (4) gelling and aging the glue solution, and finally performing supercritical drying. The invention is only used for preparing SiO2‑TiO2The one-step catalyst is used in the composite sol, so that the one-step catalytic method for preparing the foam-enhanced SiO is realized2‑TiO2And (3) compounding the aerogel. In addition, TiO in the composite aerogel prepared by the method of the invention2Possess excellent shading performance, possess the effect of solar radiation protection when the aerogel insulates against heat, can reduce the high temperature thermal conductivity of aerogel effectively. Meanwhile, the foam can effectively solve SiO problem as a reinforcement2‑TiO2The fragility of aerogels. Through testing, the prepared foam-enhanced SiO2‑TiO2The normal-temperature thermal conductivity of the composite aerogel is less than or equal to 0.015W/(m ∙ K).
Description
Technical Field
The invention relates to foam reinforced SiO2-TiO2A preparation method of the composite aerogel.
Background
SiO2Aerogel materials are the most excellent materials in heat preservation and heat insulation performance at present, but the heat radiation prevention effect of the aerogel materials is poor along with the continuous increase of temperature, and the nano TiO materials2As an infrared opacifier with excellent performance, the infrared opacifier can effectively shield the radiant heat, thereby improving SiO2High temperature thermal insulation performance of aerogel. At present, SiO2-TiO2The preparation method of the aerogel mainly comprises a doping method and an in-situ generation method. The doping method is to mix TiO2The nanoparticles are added to the SiO2 sol, but the SiO prepared by this method2-TiO2Aerogel in the presence of TiO2The nano particles are easy to agglomerate and are distributed unevenly. The in-situ generation method is to mix TiO2The precursor is added to SiO in the form of a solution2In sol, SiO prepared by the method2-TiO2TiO in aerogel2The dispersion is uniform. Currently, SiO is prepared by in situ generation2-TiO2The process of the aerogel is mainly a sol-gel process of an acid-base two-step catalysis method, and the strong acid-base reagent can corrode equipment to a certain extent and damage human bodies to a certain extent in the preparation process of the aerogel. Therefore, a new SiO is needed2-TiO2Aerogel production methods to overcome the above problems.
Therefore, the invention provides a method for preparing SiO by adopting a one-step catalysis method2-TiO2The sol-gel process of the method for compounding the aerogel is simple and convenient, and the used catalyst is ammonium salt, thereby avoiding the damage to equipment and human bodies. In addition, foam is a porous and lightweight material, and can effectively solve the problem of fragility of the aerogel as a reinforcing material. Thus, it is possible to provideThe invention provides foam-reinforced SiO2-TiO2The preparation method of the composite aerogel adopts a one-step catalysis method, the process is simple and convenient, and the prepared foam reinforced SiO is2-TiO2The composite aerogel material has the advantages of good heat insulation performance, flame retardance, light weight, energy conservation, environmental protection and the like, can be applied to various fields such as lithium batteries, automobiles and the like, and has wide market prospect.
Disclosure of Invention
Aiming at the problems, the invention provides a foam-reinforced SiO2-TiO2The preparation method of the composite aerogel adopts a one-step catalysis method to prepare SiO2-TiO2The composite aerogel has simple process, avoids the damage to equipment and human body, and the prepared foam-reinforced SiO2-TiO2The composite aerogel material has the advantages of good heat insulation performance, flame retardance, light weight, energy conservation, environmental protection and the like. The specific technical scheme is as follows:
foam-reinforced SiO2-TiO2The preparation method of the composite aerogel comprises the following steps:
（1）SiO2-TiO2preparation of composite sols
Tetraethyl orthosilicate and tetrabutyl titanate are mixed according to a certain proportion, and then absolute ethyl alcohol is added to stir for 15 min; after stirring uniformly, slowly dripping deionized water, and continuously stirring for 15 min; then dropwise adding a catalyst, and continuously stirring uniformly to form SiO2-TiO2Compounding sol;
(2) impregnated composite foam
Placing a foam substrate into a container, and placing the SiO prepared in the step (1)2-TiO2Pouring the composite sol into a container, and pouring SiO2-TiO2The amount of the composite sol is that the foam substrate is completely immersed; then covering the container with a preservative film, and obtaining foam enhanced SiO after the glue solution forms gel2-TiO2A composite aerogel sample;
(3) gel aging and hydrophobic modification
Adding the foam obtained in the step (2)Strong SiO2-TiO2Soaking the composite aerogel sample in an ethanol solvent, and performing gel aging and solvent replacement processes; after the aging of the gel is finished, performing a hydrophobic modification process;
(4) supercritical drying
The foam modified in the step (3) is subjected to hydrophobic modification to enhance SiO2-TiO2Carrying out supercritical drying on the composite aerogel sample to obtain foam reinforced SiO2-TiO2Compounding aerogel materials.
In a preferred embodiment, in the step (1), the mixing ratio of the tetraethyl orthosilicate to the tetrabutyl titanate is 1: 0-0.5; the catalyst is ammonium fluoride solution, and the concentration of the ammonium fluoride solution is 0.1-5 mol/L.
In a preferred embodiment, in the step (2), the foam substrate is melamine foam or PU foam; more preferably, the density of the foam base material is 8Kg/m 3-30 Kg/m3, and the thickness is 0.1-10 mm.
In a preferable embodiment, in the step (3), the aging process is performed for 24 to 48 hours, and the number of times of the ethanol solvent replacement is 3 to 5; in the hydrophobic modification process, the used modification reagent is a mixed solution of dimethyl diethoxy silane and ammonium fluoride, the mass ratio of the dimethyl diethoxy silane to the ammonium fluoride is 500:1, and the hydrophobic modification time is 48-72 hours.
As a preferred embodiment, in the step (4), the supercritical drying is CO2And (5) supercritical drying.
The invention has the beneficial effects that:
compared with the prior art, the invention has at least the following advantages:
(1) the method of the invention is only used for preparing SiO2-TiO2When the composite sol is prepared, a catalyst is used, namely a one-step catalysis method is used for preparing SiO2-TiO2The composite aerogel has simple and convenient process, and compared with the existing acid-base two-step method, the method disclosed by the invention reduces the corrosion to equipment and the damage to human bodies.
(2) The method of the invention prepares titaniumThe tetrabutyl titanate is directly mixed with tetraethyl orthosilicate to make TiO2The components are uniformly dispersed in SiO2In the aerogel, TiO is utilized2Preventing thermal radiation effect, improving SiO2High temperature thermal insulation performance of aerogel.
(3) The method of the invention uses foam as the matrix, can make the aerogel have certain strength, further broadens the application range thereof, and is similar to the traditional fiber reinforced SiO2-TiO2Compared with aerogel, foam-reinforced SiO2-TiO2The density of the composite aerogel material is reduced by 50%, and the normal-temperature thermal conductivity is reduced by 40%.
Drawings
FIG. 1 shows the foam-reinforced SiO prepared by the method of the present invention2-TiO2High resolution transmission electron microscopy of composite aerogel materials.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the present embodiment, belong to the protection scope of the present invention.
Example 1
This example is to prepare foam-reinforced SiO2-TiO2And (3) compounding the aerogel. Adding 10g of tetraethyl orthosilicate (TEOS) and 1g of tetrabutyl titanate (TBOT) into a beaker, mixing, adding 56g of absolute ethyl alcohol into the beaker, and stirring at the rotating speed of 500r/min for 20 min; then weighing 2.48g of deionized water by using an electronic balance, slowly adding the deionized water into the mixed solution by using a dropper, and continuously stirring for 15 min; then weighing 1g of 2mol/L ammonium fluoride solution, dropwise adding the ammonium fluoride solution into the solution by using a dropper, and stirring the solution at the rotating speed of 200r/min for 1min to obtain SiO2-TiO2And (4) compounding the sol. The thickness of the mixture is 1mm, and the density is 15Kg/m3The melamine foam is put into a mould container, the prepared composite sol is poured into the mould container, the sol is over the melamine foam, and then the mould is covered by a preservative film to wait for the sol to formForming gel for about 30min to obtain foam reinforced SiO2-TiO2Composite aerogel samples. Then the prepared foam is used for enhancing SiO2-TiO2And (3) soaking the composite aerogel sample in absolute ethyl alcohol for aging, and replacing the aging solution (absolute ethyl alcohol) once every 24 hours for 3 times. And after the aging is finished, immersing the sample into a solution containing ammonium fluoride and dimethyl diethoxy for hydrophobic modification, wherein the modification time is 48 h. Finally, the hydrophobically modified sample is subjected to CO2Supercritical drying for 13h to obtain foam reinforced SiO2-TiO2Compounding aerogel materials. Tests show that the prepared composite material has the normal-temperature heat conductivity coefficient of 0.0139W/(m ∙ K) and the density of 104Kg/m3The specific surface area of the composite aerogel is 535.2m2The flame retardant rating of the product is 94-V0.
Example 2
This example is to prepare foam-reinforced SiO2-TiO2And (3) compounding the aerogel. Adding 10g of tetraethyl orthosilicate (TEOS) and 2g of tetrabutyl titanate (TBOT) into a beaker, mixing, adding 39g of absolute ethyl alcohol into the beaker, and stirring at the rotating speed of 500r/min for 20 min; then weighing 2.48g of deionized water by using an electronic balance, slowly adding the deionized water into the mixed solution by using a dropper, and continuously stirring for 15 min; then weighing 1.5g of 2mol/L ammonium fluoride solution, dropwise adding the ammonium fluoride solution into the solution by using a dropper, and stirring the solution at the rotating speed of 200r/min for 1min to obtain SiO2-TiO2And (4) compounding the sol. The thickness of the mixture is 2mm, and the density is 20Kg/m3The melamine foam is put into a mould container, the prepared composite sol is poured into the mould container, the sol is over the melamine foam, then the mould is covered by a preservative film to wait for the sol to form gel, the gel time is about 40min, and the foam-enhanced SiO is obtained2-TiO2Composite aerogel samples. Then the prepared foam is used for enhancing SiO2-TiO2And (3) soaking the composite aerogel sample in absolute ethyl alcohol for aging, and replacing the aging solution once every 48 hours for 4 times. And after the aging is finished, immersing the sample into a solution containing ammonium fluoride and dimethyl diethoxy for hydrophobic modification, wherein the modification time is 56 h. Finally, the hydrophobic is modifiedSubjecting the sample of (1) to CO2Supercritical drying for 13h to obtain foam reinforced SiO2-TiO2Compounding aerogel materials. Tests show that the prepared composite material has the normal-temperature heat conductivity coefficient of 0.0143W/(m ∙ K) and the density of 135Kg/m3The specific surface area of the composite aerogel is 503.5m2The flame retardant rating of the product is 94-V0.
Example 3
This example is to prepare foam-reinforced SiO2-TiO2And (3) compounding the aerogel. Adding 10g of tetraethyl orthosilicate (TEOS) and 3g of tetrabutyl titanate (TBOT) into a beaker, mixing, adding 28.5g of absolute ethyl alcohol into the beaker, and stirring at the rotating speed of 500r/min for 20 min; then weighing 2.48g of deionized water by using an electronic balance, slowly adding the deionized water into the mixed solution by using a dropper, and continuously stirring for 15 min; then 2g of 2mol/L ammonium fluoride solution is weighed, the ammonium fluoride solution is added into the solution drop by a dropper, and the solution is stirred for 1min at the rotating speed of 200r/min to obtain SiO2-TiO2And (4) compounding the sol. The thickness of the mixture is 3mm, and the density is 15Kg/m3The melamine foam is put into a mould container, the prepared composite sol is poured into the mould container, the sol is over the melamine foam, then the mould is covered by a preservative film to wait for the sol to form gel, the gel time is about 45min, and the foam-reinforced SiO is obtained2-TiO2Composite aerogel samples. Then the prepared foam is used for enhancing SiO2-TiO2And (3) soaking the composite aerogel sample in absolute ethyl alcohol for aging, and replacing the aging solution once every 24 hours for 5 times. And after the aging is finished, immersing the sample into a solution containing ammonium fluoride and dimethyl diethoxy for hydrophobic modification, wherein the modification time is 72 h. Finally, the hydrophobically modified sample is subjected to CO2Supercritical drying for 13h to obtain foam reinforced SiO2-TiO2Compounding aerogel materials. Tests show that the prepared composite material has the normal-temperature heat conductivity coefficient of 0.0148W/(m ∙ K) and the density of 160Kg/m3The specific surface area of the composite aerogel is 489.6m2The flame retardant rating of the product is 94-V0.
Example 4
This example is the preparation of a blisterCotton reinforced SiO2-TiO2And (3) compounding the aerogel. Adding 10g of tetraethyl orthosilicate (TEOS) and 4g of tetrabutyl titanate (TBOT) into a beaker, mixing, adding 28.5g of absolute ethyl alcohol into the beaker, and stirring at the rotating speed of 500r/min for 20 min; then weighing 2.48g of deionized water by using an electronic balance, slowly adding the deionized water into the mixed solution by using a dropper, and continuously stirring for 15 min; then 2.6g of 2mol/L ammonium fluoride solution is weighed, the ammonium fluoride solution is added into the solution drop by a dropper, and the solution is stirred for 1min at the rotating speed of 200r/min to obtain SiO2-TiO2And (4) compounding the sol. The thickness of the mixture is 1mm, and the density is 30Kg/m3Putting the PU foam into a mold container, pouring the prepared composite sol into the mold container, covering the PU foam with a preservative film, waiting for the sol to form gel, and allowing the gel time to be about 38min to obtain foam-reinforced SiO2-TiO2Composite aerogel samples. Then the prepared foam is used for enhancing SiO2-TiO2And (3) soaking the composite aerogel sample in absolute ethyl alcohol for aging, and replacing the aging solution once every 48 hours for 3 times. And after the aging is finished, immersing the sample into a solution containing ammonium fluoride and dimethyl diethoxy for hydrophobic modification, wherein the modification time is 72 h. Finally, the hydrophobically modified sample is subjected to CO2Supercritical drying for 13h to obtain foam reinforced SiO2-TiO2Compounding aerogel materials. Tests show that the prepared composite material has the normal-temperature heat conductivity coefficient of 0.0153W/(m ∙ K) and the density of 142Kg/m3The specific surface area of the composite aerogel is 423.2m2The flame retardant rating of the product is 94-V0.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. Furthermore, it should be understood that the above-described are only preferred embodiments of the present invention, and are not intended to limit the invention in any way, so that any person skilled in the art can change or modify the technical content of the above-described disclosure into an equivalent embodiment with equivalent changes. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (8)
1. Foam-reinforced SiO2-TiO2The preparation method of the composite aerogel is characterized by comprising the following steps: the method comprises the following steps:
（1）SiO2-TiO2preparation of composite sols
Tetraethyl orthosilicate and tetrabutyl titanate are mixed according to a certain proportion, and then absolute ethyl alcohol is added to stir for 20 min; after stirring uniformly, slowly dripping deionized water, and continuously stirring for 15 min; then dropwise adding a catalyst, and continuously stirring uniformly to form SiO2-TiO2Compounding sol;
(2) impregnated composite foam
Placing a foam substrate into a container, and placing the SiO prepared in the step (1)2-TiO2Pouring the composite sol into a container, and pouring SiO2-TiO2The amount of the composite sol is that the foam substrate is completely immersed; then covering the container with a preservative film, and obtaining foam enhanced SiO after the glue solution forms gel2-TiO2A composite aerogel sample;
(3) gel aging and hydrophobic modification
Reinforcing the foam obtained in the step (2) with SiO2-TiO2Soaking the composite aerogel sample in an ethanol solvent, and performing gel aging and solvent replacement processes; after the aging of the gel is finished, performing a hydrophobic modification process;
(4) supercritical drying
The foam modified in the step (3) is subjected to hydrophobic modification to enhance SiO2-TiO2Carrying out supercritical drying on the composite aerogel sample to obtain foam reinforced SiO2-TiO2Compounding aerogel materials.
2. Foam reinforced SiO according to claim 12-TiO2The preparation method of the composite aerogel is characterized by comprising the following steps:in the step (1), the mixing ratio of the tetraethyl orthosilicate to the tetrabutyl titanate is 1: 0.1-0.5 by mass.
3. Foam reinforced SiO according to claim 12-TiO2The preparation method of the composite aerogel is characterized by comprising the following steps: in the step (1), the catalyst is ammonium fluoride solution, and the concentration of the ammonium fluoride solution is 0.1-5 mol/L.
4. Foam reinforced SiO according to claim 12-TiO2The preparation method of the composite aerogel is characterized by comprising the following steps: in the step (2), the foam base material is melamine foam or PU foam.
5. Foam reinforced SiO according to claim 1 or 42-TiO2The preparation method of the composite aerogel is characterized by comprising the following steps: the density of the foam base material is 8Kg/m3～30Kg/m3The thickness is 0.1-10 mm.
6. Foam reinforced SiO according to claim 12-TiO2The preparation method of the composite aerogel is characterized by comprising the following steps: in the step (3), in the aging process, the aging time is 24-48 h, and the number of times of ethanol solvent replacement is 3-5.
7. Foam reinforced SiO according to claim 12-TiO2The preparation method of the composite aerogel is characterized by comprising the following steps: in the hydrophobic modification process, the used modification reagent is a mixed solution of dimethyl diethoxy silane and ammonium fluoride, the mass ratio of the dimethyl diethoxy silane to the ammonium fluoride is 500:1, and the hydrophobic modification time is 48-72 hours.
8. Foam reinforced SiO according to claim 12-TiO2The preparation method of the composite aerogel is characterized by comprising the following steps: in the step (4), the supercritical drying is CO2And (5) supercritical drying.
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Cited By (5)
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| CN111848114A (en) * | 2020-07-31 | 2020-10-30 | 航天海鹰(镇江)特种材料有限公司 | Super heat-insulating aerogel composite material and preparation process thereof |
| CN113462078A (en) * | 2021-07-14 | 2021-10-01 | 湖北祥源新材科技股份有限公司 | Aerogel composite foaming sheet, preparation method and application |
| CN113895101A (en) * | 2021-08-25 | 2022-01-07 | 河南爱彼爱和新材料有限公司 | Flexible hydrophobic aerogel heat insulation sheet with energy storage characteristic and preparation method thereof |
| CN115926243A (en) * | 2022-08-17 | 2023-04-07 | 常州威斯双联科技有限公司 | Flame-retardant heat-insulation foam aerogel and preparation method thereof |
| DE102022121099A1 (en) | 2022-08-22 | 2024-02-22 | Deutsches Zentrum für Luft- und Raumfahrt e.V. | Preparation of carbon-containing crystalline titanium oxide aerogels with large surface area and large pore volume |
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| DE102022121099A1 (en) | 2022-08-22 | 2024-02-22 | Deutsches Zentrum für Luft- und Raumfahrt e.V. | Preparation of carbon-containing crystalline titanium oxide aerogels with large surface area and large pore volume |
| WO2024042031A1 (en) | 2022-08-22 | 2024-02-29 | Deutsches Zentrum für Luft- und Raumfahrt e.V. | Production of carbon-containing crystalline titanium oxide aerogels with large surface and large pore volume |
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Application publication date: 20200327 |