CN112876195A - Preparation method of graphene composite silicon aerogel thermal insulation material - Google Patents
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
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- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
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- 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
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Abstract
The invention relates to the technical field of graphene and heat insulation materials, in particular to a preparation method of a graphene composite silicon aerogel heat insulation material, which comprises the following four steps of fully hydrolyzing ethyl orthosilicate and ethanol to obtain silicon precursor liquid; mixing graphene oxide with a silicon precursor solution; impregnating the fiber felt in the obtained graphene-SiO2Sol and heating for forming; aging and modifying the fibrofelt, and drying; the production flow of the existing silica aerogel felt can not be changed by adding the Graphene Oxide (GO), and only the graphene oxide is added before silica gel forming, so that the process is simple to operate, and when the composite aerogel is combined with reinforcements such as glass fibers, a large amount of powder is not easy to fall off due to factors such as external force, and the problem of powder falling of the aerogel felt is greatly improved.
Description
Technical Field
The invention relates to the technical field of graphene and heat insulation materials, in particular to a preparation method of a graphene composite silicon aerogel heat insulation material.
Background
With the popularization of the 5G era, the performance of electronic products such as smart phones is further improved, but in the use process of the products, more heat is generated in the structure of the products than before, generally, technicians can adopt corresponding technologies to perform heat dissipation treatment on parts of the products, however, corresponding heat insulation treatment needs to be performed on special parts of some products, and as the electronic products such as smart phones are developed to be lighter and thinner and the materials of the electronic products are strict and special, when heat insulation treatment is performed on some parts, the requirements (such as thickness) of the selected heat insulation materials are higher than before.
SiO2The aerogel is used as a novel heat insulation material, the porosity of the aerogel is as high as 80% -99.8%, and the specific surface area of the aerogel is 200-1000 m2A density of at least 0.03 g/cm3The material has ultralow thermal conductivity (0.015W/(m.K)) at room temperature; SiO due to its preparation method and its structural characteristics2The strength and toughness of the aerogel are low, and the aerogel can be combined with a series of reinforcements such as fiber mats and the like in practical heat insulation application; however, these SiO2The aerogel felt can have the problem that aerogel micropowder falls off (namely powder falls off), the problem is solved, the existing effective technology is to attach a layer of glass fiber cloth or aluminum foil with a certain thickness to the surface of the aerogel felt, however, if the material with excellent heat insulation effect is used as electronic products such as mobile phones, the thickness of the heat insulation material can be greatly increased by the method, and obviously, the method does not accord with the development trend of the existing electronic products.
Disclosure of Invention
The invention provides a preparation method of a graphene composite silicon aerogel heat-insulating material aiming at the market demands.
The technical scheme of the invention is as follows:
a preparation method of a graphene composite silicon aerogel thermal insulation material comprises the following steps:
taking ethyl orthosilicate, ethanol and water according to a molar ratio of 1: (1.5-10): (1-4) uniformly stirring and mixing by magnetic force, adding hydrochloric acid to enable the pH value of the solution to be 3.0-5.0, stirring, standing at room temperature, and fully hydrolyzing to obtain a silicon precursor solution;
step two, taking a certain solid contentUltrasonically mixing the graphene oxide solution with the amount and the pH value with the silicon precursor solution obtained in the step one uniformly; then, gradually dropwise adding ammonia water until the pH value of the mixed solution is 7.0-9.0; adding a small amount of N, N-dimethylformamide to obtain graphene-SiO2Sol;
step three, dipping the fibrofelt in the graphene-SiO obtained in the step two2After sol dissolving, taking out, placing in a heating table, heating for 10-100 min at the temperature of 70 ℃, and obtaining a formed graphene-silica gel composite felt;
step four, adding the absolute ethyl alcohol/water mixed solution and the absolute ethyl alcohol/ethyl orthosilicate mixed solution into the graphene-silicon gel composite felt obtained in the step three in sequence, and respectively carrying out aging treatment; adding n-hexane for solvent replacement; then placing the mixture in a trimethylchlorosilane/normal hexane mixed solution for modification treatment; and drying at normal pressure to obtain the graphene composite silicon aerogel heat insulation felt.
Preferably, the graphene oxide solution in the second step is a solution after centrifugal cleaning; the solid content of the graphene oxide solution is 1% -20%, and preferably 5% -10%; the pH value of the graphene oxide solution is 5.0-6.0.
Preferably, the ultrasonic mixing time in the second step is 10-60 min.
Preferably, the fiber mat in the third step is a glass chopped strand mat or a glass fiber surface mat or a prefabricated oxidized fiber mat, and more preferably, the glass fiber surface mat.
Preferably, the aging treatment in the fourth step is carried out, wherein the volume ratio of the mixed solution to the graphene-silicon gel composite felt is (2-5): 1, and the aging treatment is carried out for 8-36 h at room temperature.
Preferably, the n-hexane solvent in the fourth step is replaced for 1-3 times, and the time of each replacement is 12-36 hours.
Preferably, the modification treatment time in the fourth step is 24-84 h, and the volume ratio of the trimethylchlorosilane/n-hexane mixed solution is 1: 9.
preferably, the drying treatment in the fourth step is divided into two times, and the first time is dried for 4-12 hours at the temperature of 60 ℃; and the second drying is carried out for 4-12 h at the temperature of 80 ℃.
The invention has the beneficial effects that:
the production flow of the existing silica aerogel felt can not be changed by adding the Graphene Oxide (GO), and the graphene oxide can be added before silica gel forming, so that the process operation is simple; meanwhile, the surface of GO contains a large number of oxygen-containing functional groups such as hydroxyl and carboxyl, when GO is added into a silicon precursor liquid as a nano filler in a very small amount, GO can be effectively combined with silicic acid micromolecules in the process of micromolecule polycondensation, and the excellent mechanical property of GO helps to obtain a porous framework with a larger block and better mechanical property, so that when the composite aerogel is combined with reinforcements such as glass fibers, a large number of powder bodies are not easy to fall off due to factors such as external force, and the problem of powder falling of the aerogel felt is greatly improved.
Drawings
Fig. 1 is an appearance schematic diagram of a graphene composite silicon aerogel thermal insulation material.
Detailed Description
The following describes the embodiment of the present invention in detail with reference to fig. 1.
Example 1:
the graphene composite silicon aerogel thermal insulation material is prepared by the following steps:
(1) taking ethyl orthosilicate, absolute ethyl alcohol and water according to a molar ratio of 1: 7: 3, uniformly mixing, adding 3% hydrochloric acid by mass to adjust the pH value of the solution to 3.0, stirring, standing, and fully hydrolyzing to obtain a silicon precursor solution;
(2) taking a GO (graphene oxide) solution subjected to centrifugal cleaning treatment, mixing the GO solution with a solid content and a pH value of 5% and 6.0 respectively with the silicon precursor solution obtained in the step (1), and performing ultrasonic treatment for 10 min; then gradually dropwise adding 0.3 mol/L ammonia water to make the pH value of the mixed solution neutral, adding a small amount of DMF (N, N-dimethylformamide) and uniformly mixing to obtain graphene-SiO 2 sol;
(3) dipping the glass fiber surface felt in the graphene-SiO 2 sol obtained in the step (2), placing the glass fiber surface felt on a heating table after ultrasonic treatment, and heating the glass fiber surface felt at a constant temperature of 70 ℃ for 20 min to obtain a graphene-silicon gel composite felt;
(4) sequentially aging the graphene-silicon gel composite felt obtained in the step (3) for 24 hours in a mixed solution with the volume ratio of absolute ethyl alcohol/water to absolute ethyl alcohol/tetraethyl orthosilicate being 4:1 at room temperature; adding excessive n-hexane for solvent replacement for 24 h, and performing replacement for 3 times; then, mixing the components in a volume ratio of 1: 9, modifying for 72 hours in a trimethylchlorosilane/normal hexane mixed solution; and drying at 60 ℃ and 80 ℃ for 4h and 8h respectively under normal pressure to finally obtain the graphene composite silicon aerogel heat insulation felt.
The finished product of the graphene composite silicon aerogel heat insulation felt is tested, the appearance of the finished product is shown in figure 1, the graphene-silicon aerogel is well combined with the glass fiber felt, and no obvious powder falls; the density of the material was found to be 0.235 g/cm3The sample thickness is 0.92 mm, and the thermal conductivity is 0.035W/(m.K).
Example 2:
the graphene composite silicon aerogel thermal insulation material is prepared by the following steps:
taking tetraethoxysilane, anhydrous ethanol and water according to a molar ratio of 1: 5: 2, uniformly mixing, adding 3% hydrochloric acid by mass to adjust the pH value of the solution to 3.0, stirring, standing, and fully hydrolyzing to obtain a silicon precursor solution;
mixing a GO (graphene oxide) solution subjected to centrifugal cleaning treatment, wherein the solid content and the pH value of the GO solution are respectively 5% and 6.0, and performing ultrasonic treatment for 20 min; then gradually dropwise adding 0.3 mol/L ammonia water to make the pH value of the mixed solution neutral, adding a small amount of DMF (N, N-dimethylformamide) and uniformly mixing to obtain graphene-SiO 2 sol;
thirdly, dipping the glass fiber surface felt in the graphene-SiO 2 sol obtained in the step (2), placing the glass fiber surface felt on a heating table after ultrasonic treatment, and heating the glass fiber surface felt at the constant temperature of 70 ℃ for 50 min to obtain a graphene-silicon gel composite felt;
fourthly, sequentially aging the graphene-silicon gel composite felt obtained in the step (3) for 20 hours in a mixed solution with the volume ratio of absolute ethyl alcohol/water to absolute ethyl alcohol/tetraethyl orthosilicate being 3:1 at room temperature; adding excessive n-hexane for solvent replacement for 36 h, and performing replacement for 2 times; then, mixing the components in a volume ratio of 1: 9, carrying out modification treatment in a trimethylchlorosilane/n-hexane mixed solution for 36 hours; and drying the obtained product for 8 hours and 4 hours at the temperature of 60 ℃ and 80 ℃ respectively under the normal pressure condition to finally obtain the graphene composite silicon aerogel heat insulation felt.
The foregoing is merely a preferred embodiment of the invention and all such equivalent alterations and permutations and derivations thereof are intended to be included within the scope of the invention.
Claims (8)
1. A preparation method of a graphene composite silicon aerogel thermal insulation material is characterized by comprising the following steps:
taking ethyl orthosilicate, ethanol and water according to a molar ratio of 1: (1.5-10): (1-4) uniformly stirring and mixing by magnetic force, adding hydrochloric acid to enable the pH value of the solution to be 3.0-5.0, stirring, standing at room temperature, and fully hydrolyzing to obtain a silicon precursor solution;
step two, taking a graphene oxide solution with certain solid content and pH value, and ultrasonically mixing the graphene oxide solution with the silicon precursor solution obtained in the step one uniformly; then, gradually dropwise adding ammonia water until the pH value of the mixed solution is 7.0-9.0; adding a small amount of N, N-dimethylformamide to obtain graphene-SiO2Sol;
step three, dipping the fibrofelt in the graphene-SiO obtained in the step two2After sol dissolving, taking out, placing in a heating table, heating for 10-100 min at the temperature of 70 ℃, and obtaining a formed graphene-silica gel composite felt;
step four, adding the absolute ethyl alcohol/water mixed solution and the absolute ethyl alcohol/ethyl orthosilicate mixed solution into the graphene-silicon gel composite felt obtained in the step three in sequence, and respectively carrying out aging treatment; adding n-hexane for solvent replacement; then placing the mixture in a trimethylchlorosilane/normal hexane mixed solution for modification treatment; and drying at normal pressure to obtain the graphene composite silicon aerogel heat insulation felt.
2. The preparation method of the graphene composite silicon aerogel thermal insulation material according to claim 1, characterized in that: step two, the graphene oxide solution is a solution after centrifugal cleaning; the solid content of the graphene oxide solution is 1% -20%, and preferably 5% -10%; the pH value of the graphene oxide solution is 5.0-6.0.
3. The preparation method of the graphene composite silicon aerogel thermal insulation material according to claim 1, characterized in that: and step two, the ultrasonic mixing time is 10-60 min.
4. The preparation method of the graphene composite silicon aerogel thermal insulation material according to claim 1, characterized in that: and step three, the fiber mat is a glass chopped strand mat or a glass surface mat or a prefabricated oxidized fiber mat, and the glass surface mat is more preferably selected.
5. The preparation method of the graphene composite silicon aerogel thermal insulation material according to claim 1, characterized in that: and step four, carrying out aging treatment, wherein the volume ratio of the mixed solution to the graphene-silicon gel composite felt is (2-5): 1, and the aging treatment is carried out for 8-36 h at room temperature.
6. The preparation method of the graphene composite silicon aerogel thermal insulation material according to claim 1, characterized in that: and fourthly, replacing the n-hexane solvent for 1-3 times, wherein the time of each replacement is 12-36 hours.
7. The preparation method of the graphene composite silicon aerogel thermal insulation material according to claim 1, characterized in that: the modification treatment time is 24-84 h, and the volume ratio of the trimethylchlorosilane/n-hexane mixed solution is 1: 9.
8. the preparation method of the graphene composite silicon aerogel thermal insulation material according to claim 1, characterized in that: the drying treatment is divided into two times, and the first time is dried for 4-12 hours at the temperature of 60 ℃; and the second drying is carried out for 4-12 h at the temperature of 80 ℃.
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Cited By (5)
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| CN114106561A (en) * | 2021-10-20 | 2022-03-01 | 东莞市道睿石墨烯研究院 | Graphene foam heat-conducting gasket and preparation method thereof |
| CN114775298A (en) * | 2022-03-11 | 2022-07-22 | 广东机电职业技术学院 | Composite material containing graphene aerogel and preparation method and application thereof |
| CN116396056A (en) * | 2023-04-14 | 2023-07-07 | 南京工业大学 | High-strength wave-absorbing heat-insulating integrated silicon-carbon hybrid aerogel and preparation method thereof |
| CN116393053A (en) * | 2023-06-02 | 2023-07-07 | 江苏珈云新材料有限公司 | Modified nano SiO 2 Aerogel and preparation method thereof |
| CN117003543A (en) * | 2023-06-16 | 2023-11-07 | 天津轻快未来科技有限公司 | Preparation method and device of graphene composite silicon aerogel heat insulation material |
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| CN116396056A (en) * | 2023-04-14 | 2023-07-07 | 南京工业大学 | High-strength wave-absorbing heat-insulating integrated silicon-carbon hybrid aerogel and preparation method thereof |
| CN116393053A (en) * | 2023-06-02 | 2023-07-07 | 江苏珈云新材料有限公司 | Modified nano SiO 2 Aerogel and preparation method thereof |
| CN116393053B (en) * | 2023-06-02 | 2023-09-05 | 江苏珈云新材料有限公司 | Modified nano SiO 2 Aerogel and preparation method thereof |
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