CN110745835B - Preparation method of silicon dioxide/graphene composite aerogel and composite aerogel obtained by preparation method - Google Patents
Preparation method of silicon dioxide/graphene composite aerogel and composite aerogel obtained by preparation method Download PDFInfo
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Abstract
The invention relates to the technical field of aerogels, in particular to a preparation method of a silicon dioxide/graphene composite aerogel and the composite aerogel obtained by the preparation method. Reacting graphene oxide with amino trialkoxysilane to obtain alkoxy silanized graphene, ultrasonically dispersing the alkoxy silanized graphene in an organic solvent for hydrolysis to obtain a hydrolysate A, hydrolyzing a conventional silicon source to obtain a hydrolysate B, uniformly mixing the hydrolysate A and the hydrolysate B, performing alkaline condensation to obtain wet gel, aging, replacing the solvent, performing surface modification, and drying to obtain the silicon dioxide/graphene composite aerogel. The silicon dioxide/graphene composite aerogel disclosed by the invention has higher mechanical strength, and the existence of graphene reduces the high-temperature heat conductivity coefficient of the silicon dioxide aerogel, so that the silicon dioxide/graphene composite aerogel can be applied to the fields of heat insulation materials and the like.
Description
Technical Field
The invention relates to the technical field of aerogels, in particular to a preparation method of a silicon dioxide/graphene composite aerogel and the composite aerogel obtained by the preparation method.
Background
The silica aerogel has attracted the extensive attention of developers in the industry due to the unique properties of high specific surface area, low thermal conductivity, low density and electric conductivity, and the most important application prospect is heat insulation and heat preservation material. However, as the temperature increases, the silica aerogel has an increased infrared radiation transmittance, and in order to further reduce the high-temperature infrared radiation, an opacifier such as carbon black, titanium dioxide, etc. is usually added to the silica aerogel, but this leads to a reduction in other properties of the silica.
The graphene aerogel is another aerogel, also has the properties of high specific surface area, low density and the like, and has good elasticity. The preparation of the composite aerogel with more excellent performance is very meaningful work by combining the advantages of the silica aerogel and the graphene aerogel.
There have been some reports in the prior art of preparing silica/graphene composite aerogels. There are two main methods, one is to coat silicon dioxide on the surface of graphene aerogel, such as CN107117608B, CN108083262A, and CN107235744A, which has long steps and high cost, and needs to prepare graphene aerogel first; another method is to compound graphene oxide and a silicon source together in a sol-gel, such as CN107032360B, CN107032360B, CN108218386A, and CN107304052A, but the obtained silica/graphene composite aerogel has poor thermal insulation performance at high temperature.
Through a large number of experiments, the inventor of the application finds a method capable of reducing the thermal conductivity coefficient of the silicon dioxide aerogel at high temperature.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of silicon dioxide/graphene composite aerogel.
The invention also aims to provide the silicon dioxide/graphene composite aerogel, wherein the graphene can effectively shield infrared radiation, reduce the heat conductivity coefficient of the silicon dioxide aerogel at high temperature and improve the heat insulation performance of the silicon dioxide aerogel at high temperature.
The invention adopts the following technical scheme:
a preparation method of silicon dioxide/graphene composite aerogel comprises the following steps:
s1, ultrasonically dispersing alkoxy silanized graphene in a first organic solvent, and hydrolyzing under an acidic condition to obtain a hydrolysate A;
s2, hydrolyzing a silicon source in a second organic solvent under an acidic condition to obtain a hydrolysate B;
s3, uniformly mixing the hydrolysate A in the step S1 and the hydrolysate B in the step S2, condensing under an alkaline condition to obtain wet gel, aging, replacing with absolute ethyl alcohol, carrying out surface modification, and drying to obtain the silicon dioxide/graphene composite aerogel.
Preferably, the alkoxy silanized graphene in step S1 is obtained by reacting graphene oxide with amino trialkoxysilane. The graphene oxide is preferably graphene oxide by a Hummers method or graphene oxide by a modified Hummers method.
The surface of graphene oxide has abundant active groups, including hydroxyl, carboxyl and epoxy groups, and can further react with amino groups. The paper, "thermal stability of graphene oxide/polybutylmethacrylate composite material" (advanced chemical bulletin, 2014,35(11),2466-2471), CN106311185B and CN107746054A all disclose that graphene oxide can react with amino-containing triethoxysilane, wherein amino groups can react with carboxyl groups to form amide bonds and amino groups can also react with epoxy groups to form addition reactions, and by using absolute ethyl alcohol as a reaction medium, alkoxy groups in amino-containing trialkoxysilane can not undergo hydrolytic condensation and can participate in subsequent hydrolysis reactions.
More preferably, the amino-containing trialkoxysilane is selected from the group consisting of 3-aminopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, N-phenyl-gamma-aminopropyltriethoxysilane, N-methyl-3-aminopropyltrimethoxysilane, N-methyl-3-aminopropyltriethoxysilane, N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane, N-beta- (aminoethyl) -gamma-aminopropyltriethoxysilane, gamma-divinyltriaminopropyltrimethoxysilane, gamma-divinyltriaminopropyltriethoxysilane, bis- (gamma-trimethoxysilylpropyl) amine, bis- (gamma-aminopropyl) trimethoxysilane, bis- (gamma-aminopropyl) amine, bis- (gamma-aminopropyl, One or more of bis- (gamma-triethoxysilylpropyl) amine, 3- (phenylamino) propyltrimethoxysilane, 3- (phenylamino) propyltriethoxysilane, p-aminophenyltrimethoxysilane, p-aminophenyltriethoxysilane, m-aminophenyltrimethoxysilane, m-aminophenyltriethoxysilane, 2-aminoethylaminomethyltrimethoxysilane, 2-aminoethylaminomethyltriethoxysilane, 3- (N-allylamino) propyltrimethoxysilane, 3- (N-allylamino) propyltriethoxysilane, 3- (3-aminophenoxy) propyltrimethoxysilane and 3- (3-aminophenoxy) propyltriethoxysilane.
Preferably, the first organic solvent in step S1 is one or more selected from the group consisting of absolute ethanol, methanol, isopropanol, acetone, tetrahydrofuran, and methyl ethyl ketone.
Preferably, the silicon source in step S2 is selected from one of methyl orthosilicate, ethyl orthosilicate and sodium silicate.
Preferably, the second organic solvent in step S2 is one or more selected from the group consisting of absolute ethanol, methanol, isopropanol, acetone, tetrahydrofuran, and methyl ethyl ketone.
Preferably, the weight ratio of the alkoxy silanized graphene in the step S1 to the silicon source in the step S2 is 0.0001-0.1: 1.
Preferably, the weight ratio of the alkoxy silanized graphene to the silicon source is 0.002-0.02: 1.
The acidic hydrolysis and alkaline condensation is a common method for preparing silicon dioxide wet gel, and specifically comprises the steps of adding an acidic substance to enable the pH of a reaction system to be 2-4, respectively hydrolyzing the alkoxy silanized graphene and a silicon source, uniformly mixing, adding an alkaline substance, adjusting the pH of the reaction system to be 8-12, promoting the co-condensation to obtain the wet gel, wherein the acidic substance can be at least one of sulfuric acid, hydrochloric acid, nitric acid, oxalic acid, formic acid and acetic acid, and the alkaline substance can be at least one of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, barium hydroxide, ammonia water and tetramethyl ammonium hydroxide.
The aged wet gel in step S3 is maintained at 20-80 deg.C for 1-4 hr.
In the step S3, the absolute ethyl alcohol is replaced by soaking the aged wet gel in the absolute ethyl alcohol for 1-2 hours, and then removing the redundant solvent.
Preferably, the surface modifier used for surface modification in step S3 is trimethylchlorosilane or hexamethyldisilazane. The surface modifier is dissolved in the normal hexane for use according to the volume ratio of the modifier to the normal hexane of 1:5-10, and the surface modification time is 1-5 hours at normal temperature.
A silica/graphene composite aerogel obtained by the preparation method of any one of the above embodiments.
The invention has the beneficial effects that:
(1) according to the method, the amino group containing the amino trialkoxysilane reacts with the active carboxyl, epoxy and the like on the surface of the graphene oxide to obtain the alkoxy silanized graphene with the alkoxysilane grafted on the surface. The conventional silicon source of the alkoxy silanization graphene and the silicon dioxide aerogel can be hydrolyzed under an acidic condition, mixed and subjected to condensation reaction under an alkaline condition, and the silicon dioxide/graphene composite aerogel is obtained through post-treatment.
(2) The obtained silicon dioxide/graphene composite aerogel has the tensile strength of more than 0.22MPa, can be dried under the normal pressure through further optimization of a formula, saves equipment investment, improves the production efficiency and reduces the production cost, and the tensile strength can reach more than 0.7 MPa.
(3) The obtained silicon dioxide/graphene composite aerogel has a low high-temperature thermal conductivity coefficient which can be as low as 0.020W/(m.k) when tested at 650 ℃, is lower than that of the conventional silicon dioxide aerogel by about 47 percent, and improves the heat preservation and insulation performance at high temperature.
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description.
Detailed description of the preferred embodiments
According to the paper "thermal stability of graphene oxide/polybutylmethacrylate composite material", 3-aminopropyltriethoxysilane, N- β - (aminoethyl) - γ -aminopropyltriethoxysilane, and γ -diethylenetriaminopropyltriethoxysilane were respectively used to react with graphene oxide by Hummers method, so as to obtain ethoxysilanized graphene 1, ethoxysilanized graphene 2, and ethoxysilanized graphene 3, respectively.
Example 1
Ultrasonically dispersing 0.05g of ethoxysilanized graphene 1 in 50ml of acetone at room temperature, adding an oxalic acid aqueous solution with the concentration of 0.1mol/L to adjust the pH value to 3.5, and hydrolyzing to obtain a hydrolysate 1A.
100g of ethyl orthosilicate, 600g of acetone and 35g of deionized water were mixed at room temperature, and oxalic acid was added to adjust the pH to 3.5 for hydrolysis, to obtain a hydrolysate 1B.
Uniformly mixing and stirring the hydrolysate 1A and the hydrolysate 1B, adding ammonia water to adjust the pH value to 11.0, and condensing to obtain wet gel; and aging the wet gel in a water bath at 30 ℃ for 4 hours, taking out the wet gel, soaking the wet gel in absolute ethyl alcohol for 2 hours for solvent replacement, performing solvent replacement for 3 times, taking out the wet gel, soaking the wet gel in an n-hexane solution of trimethylchlorosilane (the volume ratio of the trimethylchlorosilane to the n-hexane is 1:7) for 3 hours, taking out the wet gel, and drying by adopting a freeze drying method to obtain the silicon dioxide graphene composite aerogel 1.
Example 2
Ultrasonically dispersing 0.2g of ethoxy silanized graphene 2 in 60ml of absolute ethyl alcohol at room temperature, adding oxalic acid aqueous solution with the concentration of 0.1mol/L to adjust the pH value to 3.0, and hydrolyzing to obtain a hydrolysate 2A.
At room temperature, 100g of ethyl orthosilicate, 600g of absolute ethanol and 35g of deionized water were mixed, and oxalic acid was added to adjust the pH to 3.5 for hydrolysis, to obtain hydrolysate 2B.
Uniformly mixing and stirring the hydrolysate 2A and the hydrolysate 2B, adding ammonia water to adjust the pH value to 11.0, and condensing to obtain wet gel; and aging the wet gel in a water bath at 30 ℃ for 4 hours, taking out the wet gel, soaking the wet gel in absolute ethyl alcohol for 1.5 hours for solvent replacement, performing solvent replacement for 3 times, taking out the wet gel, soaking the wet gel in an n-hexane solution of trimethylchlorosilane (the volume ratio of the trimethylchlorosilane to the n-hexane is 1:7) for 3 hours, taking out the wet gel, sequentially drying the wet gel in a forced air drying oven at 40 ℃ for 2.5 hours, a forced air drying oven at 80 ℃ for 2.5 hours and a forced air drying oven at 120 ℃ for 1.5 hours to obtain the silicon dioxide graphene composite aerogel 2.
Example 3
Ultrasonically dispersing 0.4g of ethoxy silanized graphene 3 in 70ml of absolute ethyl alcohol at room temperature, adding oxalic acid aqueous solution with the concentration of 0.1mol/L to adjust the pH value to 3.0, and hydrolyzing to obtain a hydrolysate 3A.
Uniformly mixing and stirring the hydrolysate 3A and the hydrolysate 2B, adding ammonia water to adjust the pH value to 11.0, and condensing to obtain wet gel; and aging the wet gel in a water bath at 40 ℃ for 3.5 hours, taking out the wet gel, soaking the wet gel in absolute ethyl alcohol for 2 hours for solvent replacement, performing solvent replacement for 3 times, taking out the wet gel, soaking the wet gel in an n-hexane solution of trimethylchlorosilane (the volume ratio of the trimethylchlorosilane to the n-hexane is 1:7) for 3 hours, taking out the wet gel, sequentially drying the wet gel in a forced air drying oven at 40 ℃ for 2.5 hours, a forced air drying oven at 80 ℃ for 2.5 hours and a forced air drying oven at 120 ℃ for 1.5 hours to obtain the silicon dioxide graphene composite aerogel 3.
Example 4
Ultrasonically dispersing 0.8g of ethoxy silanized graphene 2 in 100ml of acetone at room temperature, adding oxalic acid aqueous solution with the concentration of 0.1mol/L to adjust the pH value to 3.0, and hydrolyzing to obtain a hydrolysate 4A.
Uniformly mixing and stirring the hydrolysate 4A and the hydrolysate 1B, adding ammonia water to adjust the pH value to 10.0, and condensing to obtain wet gel; and aging the wet gel in a water bath at 40 ℃ for 3.5 hours, taking out the wet gel, soaking the wet gel in absolute ethyl alcohol for 2 hours for solvent replacement, performing solvent replacement for 3 times, taking out the wet gel, soaking the wet gel in an n-hexane solution of trimethylchlorosilane (the volume ratio of the trimethylchlorosilane to the n-hexane is 1:7) for 3 hours, taking out the wet gel, sequentially drying the wet gel in a forced air drying oven at 40 ℃ for 2.5 hours, a forced air drying oven at 80 ℃ for 2.5 hours and a forced air drying oven at 120 ℃ for 1.5 hours to obtain the silicon dioxide graphene composite aerogel 4.
Example 5
Ultrasonically dispersing 1.5g of ethoxysilanized graphene 1 in 120ml of absolute ethyl alcohol at room temperature, adding an oxalic acid aqueous solution with the concentration of 0.1mol/L to adjust the pH value to 3.0, and hydrolyzing to obtain a hydrolysate 5A.
Uniformly mixing and stirring the hydrolysate 5A and the hydrolysate 2B, adding ammonia water to adjust the pH value to 11.0, and condensing to obtain wet gel; and aging the wet gel in a water bath at 40 ℃ for 3.5 hours, taking out the wet gel, soaking the wet gel in absolute ethyl alcohol for 2 hours for solvent replacement, performing solvent replacement for 3 times, taking out the wet gel, soaking the wet gel in an n-hexane solution of trimethylchlorosilane (the volume ratio of the trimethylchlorosilane to the n-hexane is 1:7) for 3 hours, taking out the wet gel, drying the wet gel in a forced air drying oven at 40 ℃ for 3 hours, drying the wet gel in a forced air drying oven at 80 ℃ for 2 hours, and drying the wet gel in a forced air drying oven at 120 ℃ for 1.5 hours to obtain the silicon dioxide graphene composite aerogel 5.
Example 6
Ultrasonically dispersing 2.5g of ethoxy silanized graphene 3 in 200ml of absolute ethyl alcohol at room temperature, adding oxalic acid aqueous solution with the concentration of 0.1mol/L to adjust the pH value to 3.0, and hydrolyzing to obtain a hydrolysate 6A.
Uniformly mixing and stirring the hydrolysate 6A and the hydrolysate 2B, adding ammonia water to adjust the pH value to 11.0, and condensing to obtain wet gel; and aging the wet gel in a water bath at 40 ℃ for 3.5 hours, taking out the wet gel, soaking the wet gel in absolute ethyl alcohol for 2 hours for solvent replacement, performing solvent replacement for 3 times, taking out the wet gel, soaking the wet gel in an n-hexane solution of trimethylchlorosilane (the volume ratio of the trimethylchlorosilane to the n-hexane is 1:7) for 3 hours, taking out the wet gel, and drying by adopting a freeze drying method to obtain the silicon dioxide graphene composite aerogel 6.
Comparative example 1
Ultrasonically dispersing 0.4g of ethoxy silanized graphene 2 in 600ml of absolute ethyl alcohol at room temperature, adding 100g of tetraethoxysilane and 36g of deionized water, mixing, adding oxalic acid to adjust the pH value to 3.5, hydrolyzing, adding ammonia water to adjust the pH value to 11.0, and condensing to obtain wet gel; and aging the wet gel in a water bath at 30 ℃ for 4 hours, taking out the wet gel, soaking the wet gel in absolute ethyl alcohol for 1.5 hours for solvent replacement, performing solvent replacement for 3 times, taking out the wet gel, soaking the wet gel in an n-hexane solution of trimethylchlorosilane (the volume ratio of the trimethylchlorosilane to the n-hexane is 1:7) for 3 hours, taking out the wet gel, and drying by adopting a freeze-drying method to obtain the silicon dioxide graphene composite aerogel 7.
Comparative example 2
Commercially available silica aerogels.
Results of Performance testing
The results of the performance tests are shown in table 1.
Table 1 results of performance testing
Remarking: 1. the specific surface area is measured by a BET method; 2. testing the heat conductivity coefficient at room temperature by a hot wire method; 3. the high temperature thermal conductivity was measured at 650 ℃ using a hot plate method.
Therefore, as can be seen from the results in table 1, the silica/graphene composite aerogel of the present invention not only has high compressive strength, but also has low thermal conductivity at high temperature, and is more suitable for application in high temperature.
The foregoing has shown and described the fundamental principles, major features and advantages of the invention. It should be understood by those skilled in the art that the present invention is not limited by the foregoing embodiments, which are merely preferred embodiments of the present invention, and the scope of the present invention should not be limited thereby, and that equivalent changes and modifications made within the scope of the present invention and the specification should be covered thereby. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The preparation method of the silicon dioxide/graphene composite aerogel is characterized by comprising the following steps:
s1, ultrasonically dispersing alkoxy silanized graphene in a first organic solvent, and hydrolyzing under an acidic condition to obtain a hydrolysate A;
s2, hydrolyzing a silicon source in a second organic solvent under an acidic condition to obtain a hydrolysate B;
s3, uniformly mixing the hydrolysate A in the step S1 and the hydrolysate B in the step S2, condensing under an alkaline condition to obtain wet gel, aging, replacing with absolute ethyl alcohol, carrying out surface modification, and drying to obtain the silicon dioxide/graphene composite aerogel.
2. The method according to claim 1, wherein the alkoxysilanized graphene in step S1 is obtained by reacting graphene oxide with an amino-containing trialkoxysilane.
3. The method according to claim 2, wherein the amino group-containing trialkoxysilane is selected from the group consisting of γ -aminopropyltriethoxysilane, γ -aminopropyltrimethoxysilane, N-phenyl- γ -aminopropyltriethoxysilane, N-methyl-3-aminopropyltrimethoxysilane, N-methyl-3-aminopropyltriethoxysilane, N- β - (aminoethyl) - γ -aminopropyltrimethoxysilane, N- β - (aminoethyl) - γ -aminopropyltriethoxysilane, γ -divinyltriaminopropyltrimethoxysilane, γ -divinyltriaminopropyltriethoxysilane, bis- (γ -trimethoxysilylpropyl) amine, bis- (γ -aminopropyl) amine, bis (γ -aminopropyl) amine, and a mixture thereof, One or more of bis- (gamma-triethoxysilylpropyl) amine, 3- (phenylamino) propyltrimethoxysilane, 3- (phenylamino) propyltriethoxysilane, p-aminophenyltrimethoxysilane, p-aminophenyltriethoxysilane, m-aminophenyltrimethoxysilane, m-aminophenyltriethoxysilane, 2-aminoethylaminomethyltrimethoxysilane, 2-aminoethylaminomethyltriethoxysilane, 3- (N-allylamino) propyltrimethoxysilane, 3- (N-allylamino) propyltriethoxysilane, 3- (3-aminophenoxy) propyltrimethoxysilane and 3- (3-aminophenoxy) propyltriethoxysilane.
4. The method according to claim 1, wherein the first organic solvent in step S1 is one or more selected from the group consisting of absolute ethanol, methanol, isopropanol, acetone, tetrahydrofuran, and methyl ethyl ketone.
5. The method as claimed in claim 1, wherein the silicon source in step S2 is selected from one of methyl orthosilicate, ethyl orthosilicate and sodium silicate.
6. The method according to claim 1, wherein the second organic solvent in step S2 is one or more selected from the group consisting of absolute ethanol, methanol, isopropanol, acetone, tetrahydrofuran, and methyl ethyl ketone.
7. The method of claim 1, wherein the weight ratio of the alkoxylated silanized graphene in step S1 to the silicon source in step S2 is 0.0001-0.1: 1.
8. The preparation method according to claim 7, wherein the weight ratio of the alkoxy silanized graphene to the silicon source is 0.002-0.02: 1.
9. The method according to claim 1, wherein the surface modifier used for surface modification in step S3 is trimethylchlorosilane or hexamethyldisilazane.
10. A silica/graphene composite aerogel obtained by the preparation method according to any one of claims 1 to 9.
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| CN108927112A (en) * | 2018-09-21 | 2018-12-04 | 佛山皖和新能源科技有限公司 | A kind of graphene composite aerogel adsorbent |
| CN110127705A (en) * | 2019-05-14 | 2019-08-16 | 杭州师范大学 | A kind of preparation method for the fire-retardant silica aerogel that graphene oxide is modified |
| CN110422850A (en) * | 2019-06-25 | 2019-11-08 | 华南理工大学 | High-specific surface area strong-hydrophobicity graphene oxide/silicon dioxide composite aerogel atmospheric preparation method |
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