CN113045257B - Aerogel heat-insulation composite material and preparation method thereof - Google Patents
Aerogel heat-insulation composite material and preparation method thereof Download PDFInfo
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- CN113045257B CN113045257B CN202110525144.9A CN202110525144A CN113045257B CN 113045257 B CN113045257 B CN 113045257B CN 202110525144 A CN202110525144 A CN 202110525144A CN 113045257 B CN113045257 B CN 113045257B
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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Abstract
Discloses a composite aerogel, which is obtained by gelatinizing a mixed solution of SiC nano particles, silica sol, ethanol, water and dimethylformamide and then drying the mixed solution at normal pressure; the SiC nanoparticles are selected from KH-570 modified SiC nanoparticles. In addition, a preparation method of the composite aerogel, an aerogel heat insulation composite material obtained from the composite aerogel and a preparation method of the aerogel heat insulation composite material are also disclosed. The composite material has better heat insulation effect; meanwhile, the mechanical property is better.
Description
Technical Field
The invention belongs to the technical field of aerogel nano materials; relates to an aerogel heat insulation composite material and a preparation method thereof.
Background
SiO 2 Aerogel is a porous heat insulating material, has high porosity (more than 99.8%), pore diameter in a nanoscale range, and lower thermal conductivity (0.013W/(mK)) than room-temperature air, so that SiO 2 Aerogel is also called super heat insulation material, and is widely applied in the fields of heat preservation and heat insulation of industrial and building materials.
At present, the silicon aerogel prepared at home and abroad mainly takes tetraethoxysilane organic matters as silicon sources and is prepared by a supercritical drying process. The silica aerogel prepared by using water glass as a silicon source easily contains impurities such as sodium ions and the like, and needs to be subjected to treatment such as ion exchange and the like. However, the supercritical fluid drying technology can maintain the integrity and excellent pore structure characteristics of the aerogel material, but has the disadvantages of complex operation, high risk and high cost, and further limits the large-scale application of the silicon aerogel material.
Chinese patent application CN107858050A discloses a SiO 2 The aerogel heat insulation coating comprises the following components in parts by weight: 50-100 parts of base paint and 5-20 parts of SiO 2 Aerogel, 2-10 parts of hollow glass beads with titanium dioxide coatings, 0.05-0.2 part of dimethyl hydroxyl silicone oil, 0.05-0.2 part of hexadecyl trimethyl ammonium bromide, 10-25 parts of curing agents and 2-10 parts of auxiliaries; the auxiliary agent comprises a dispersing agent, a wetting agent, a defoaming agent and a flatting agent. The SiO 2 In the aerogel heat-insulating and heat-preserving coating, SiO 2 The aerogel is matched with the hollow glass beads with the coating, and the heat preservation and insulation effects are improved in a synergistic mode.
However, in this patent application, SiO 2 The aerogel is not subjected to any surface modification, belongs to a hydrophobic substance and has poor compatibility with an acrylic emulsion used as a matrix paint; at the same time, SiO 2 The aerogel has higher surface energy, is easy to agglomerate, and has smaller connecting area of secondary particles, thus leading to poor heat insulation effect and poor mechanical property of the coating.
Aiming at the defects in the prior art, an aerogel heat insulation composite material with better heat insulation and heat preservation effects and mechanical properties and a preparation method thereof are urgently needed to be found.
Disclosure of Invention
The invention aims to provide an aerogel heat insulation composite material and a preparation method thereof. The aerogel heat insulation composite material has better heat insulation effect; meanwhile, the mechanical property is better.
In order to achieve the purpose, the invention firstly provides a composite aerogel, which is obtained by gelatinizing a mixed solution of SiC nano-particles, silica sol, ethanol, water and dimethylformamide and then drying the mixture at normal pressure; characterized in that the SiC nanoparticles are selected from KH-570 modified SiC nanoparticles.
The composite aerogel according to the present invention, wherein the SiC nanoparticles have an average particle size of 20 to 60 nm.
The composite aerogel provided by the invention is characterized in that the average particle size of the silica sol is 10-20nm, and the solid content is 20-40%.
The composite aerogel provided by the invention is prepared from SiC nanoparticles and silica sol, wherein the weight-volume ratio of the SiC nanoparticles to the silica sol is (2-4) g: 100 mL.
The composite aerogel provided by the invention is characterized in that the volume ratio of silica sol, ethanol and water is (6-10): (12-20): 1.
the composite aerogel provided by the invention is prepared by adding 0.5-1.5% of dimethylformamide by volume of a mixed solution.
In another aspect, the present invention also provides a preparation method of the composite aerogel according to the present invention, the preparation method comprising:
dispersing SiC nano particles in ethanol to obtain SiC dispersion liquid;
adding silica sol, ethanol, water and dimethylformamide into the SiC dispersion liquid to obtain a mixed liquid;
gelatinizing the mixed solution;
optionally, aging, solvent exchange;
drying under normal pressure.
Secondly, the invention also provides an aerogel heat insulation composite material, which is characterized in that the material is obtained by reacting the KH-570 modified composite aerogel and the acrylic acid monomer.
The aerogel thermal insulation composite material is characterized in that the weight-volume ratio of the KH-570 modified composite aerogel to the acrylic monomer is 1 g: (0.1-0.3) mL.
In yet another aspect, the present invention also provides a method for preparing the aerogel thermal insulation composite according to the present invention, the method comprising:
KH-570 modification is carried out on the composite aerogel;
the modified composite aerogel is reacted with an acrylic monomer.
The invention has the beneficial effects that: compared with the prior art, the aerogel heat insulation composite material has better heat insulation effect; meanwhile, the mechanical property is better.
Detailed Description
The present invention will be further described with reference to the following examples, but the invention is not limited to the application thereof.
In the specific embodiment of the invention, the SiC nano-particles are purchased from Beijing Deke island gold science and technology Co., Ltd, and the product model is DK-SiC-001; the average particle diameter is 40nm, and the bulk density is 0.11g/cm 3 Specific surface area of 39.8m 2 /g。
The silica sol is purchased from Beijing Deke island gold science and technology Limited, and has a product model of JL-SiO2-Z15, an average particle size of 15nm and a solid content of 30 percent.
KH-570 was obtained from Shanghai permanent research chemical technology Co.
The flexible acrylic emulsion (film-forming emulsion) is purchased from Shanghai Baolijia chemical company Limited, and has the product model of BLJ-963M and the solid content of 54 percent.
Ammonium polyacrylate salt (dispersant OROTAN 1124) was purchased from Rohm and Haas, China, USA, and has a solid content of 50%.
The polyether modified polydimethylsiloxane solution (wetting agent BYK-306) was purchased from BYK, Germany.
Silicone antifoam (ADEKA NATE B-199) was purchased from Shanghai Edisco Fine chemical Co., Ltd at a viscosity of 2500 cP.
The rutile type titanium dioxide nanoparticles are obtained from Beijing Deke island gold science and technology Limited, and have a product model of DK405-3, an average particle diameter of 200nm and a specific surface area of 15m 2 /g。
The hollow glass beads are purchased from Shanghai Hui Jing sub-nanometer new material Co Ltd, the product model is S-38, the 50 percent particle size is below 40nm, and the volume density is 0.38g/cm 3 。
Anionic thickener (TT-935) was purchased from Rohm and Haas China, USA, and has a solid content of 30%.
Coalescing agent alcohol ester-12 was purchased from Istmann chemical Co., Ltd.
Modification of SiC nanoparticles
50mL of a 2% by volume KH-570 ethanol solution was prepared, and the pH was adjusted to 4.0 using acetic acid. 10g of SiC nanoparticles are added into the KH-570 ethanol solution, and modification reaction is carried out at the temperature of 55 ℃. After the reaction was completed, the reaction mixture was centrifuged at 12000rpm for 10min to obtain a solid precipitate. Washed 3 times with absolute ethanol and dried at 80 ℃ to obtain modified SiC nanoparticles (a 1).
SiC-SiO 2 Preparation of composite aerogels
1.2g of modified SiC nanoparticles are added into 80mL of absolute ethanol, and the mixture is subjected to ultrasonic treatment to be uniformly dispersed, so that SiC ethanol dispersion liquid is obtained. 40mL of silica sol (with a solid content of 30%) and 5mL of deionized water were added to the SiC ethanol dispersion, and then 1mL of dimethylformamide DMF was added, and the mixture was dispersed uniformly by sonication. Standing at room temperature to obtain SiC-SiO 2 Compounding the wet gel. Aging at room temperature for 24h after wet gel formation; and then respectively soaking the mixture for 24 hours by using ethanol water solution with the volume concentration of 50% and absolute ethanol, and replacing the corresponding solution once in 8 hours. Finally, drying for 48h at 60 ℃ to obtain SiC-SiO 2 Composite aerogel (a 2).
SiC-SiO 2 Modification of composite aerogels
5g of SiC-SiO 2 The composite aerogel is placed in 60mL of ethanol, then 0.5mL of 25% ammonia water solution is added, and the mixture is subjected to ultrasonic treatment to be uniformly dispersed. Then adding 1gKH-570, uniformly dispersing by ultrasonic waves, and reacting for 36 hours at 70 ℃ under a closed condition; then the opening is heated for 4 h. After the reaction was completed, the reaction mixture was centrifuged at 12000rpm for 10min to obtain a solid precipitate. Washing with anhydrous ethanol for 3 times, and drying at 80 deg.C to obtain KH-570 modified SiC-SiO 2 Composite aerogel (a 3). Then 1g of KH-570 modified SiC-SiO 2 The composite aerogel is dispersed in 9mL of absolute ethyl alcohol, 10mL of 2% acrylic monomer ethanol solution with volume concentration and 10mL of 0.015g of potassium persulfate aqueous solution are sequentially added in a nitrogen atmosphere, and the mixture reacts for 12 hours at the temperature of 80 ℃. After the reaction was completed, the reaction mixture was centrifuged at 12000rpm for 10min to obtain a solid precipitate. Washing with anhydrous ethanol for 3 times, and drying at 80 deg.C to obtain polyacrylic acid modified SiC-SiO 2 Composite aerogel (a 4).
Preparation of aerogel heat insulation coating
The aerogel thermal insulation coating comprises the following formula: 40 wt% of BLJ-963M; polyacrylic acid modified SiC-SiO 2 15 wt% of composite aerogel (a 4); OROTAN 11242 wt%; BYK-3060.2 wt%; 2371ADEKA NATE B-1990.3 wt%; DK405-34 wt%; s-384%; TT-9352 wt%; alcohol ester-121 wt%; 0.5 wt% of ammonia water; the balance of deionized water.
Adding OROTAN 1124, BYK-306 and B-199 in the formula amount of 1/2 into deionized water, and stirring to mix them uniformly; then adding formula amount of polyacrylic acid modified SiC-SiO 2 Homogenizing the composite aerogel (A4) at 8000rpm for 10 min; adding DK405-3 with the formula amount, and stirring to uniformly mix; then adding BLJ-963M, alcohol ester-12 and S-38 with the formula ratio, and stirring to uniformly mix; then adding ammonia water and 1/2 formula amount of B-199, stirring to mix them uniformly; and finally, adding TT-935, and stirring to uniformly mix the mixture to obtain the aerogel thermal insulation coating.
Thermal insulation test
The heat insulation test is carried out according to the national standard GB/T25261-2018. The heat insulation temperature difference testing device comprises a heating device (250W infrared lamp), a temperature testing device (a Pt resistance probe and an automatic temperature display instrument) and a heat insulation box (which is formed by six polyethylene foam plates of 36cmX36cmX3cm, the heat conductivity coefficient of the polyethylene foam plates is 0.023W/mK; a square hole of 15cmX7.5cmX3cm is cut in the polyethylene foam plate at the top for placing a test sample plate or a blank sample plate); the heating device is positioned at a position 30cm above the center of the test sample plate; the Pt resistance probe was in contact with the bottom of the test panel. The test panels were coated with 1mm thick aerogel thermal barrier coating. The temperature of the blank and test panels after 60min heating were recorded separately. The difference value is used as the insulation temperature difference. The thermal insulation temperature difference of the aerogel thermal insulation coating is 18.6 ℃.
Adhesion test
The adhesion test was performed according to the cross-hatch method of the national standard GB/T1720-.
The adhesive force of the aerogel heat insulation coating is grade 1.
Comparative test
With SiC-SiO 2 Composite aerogel (A2) and KH-570 modified SiC-SiO 2 Replacement of polyacrylic acid modified SiC-SiO by composite aerogel (A3) 2 And (3) preparing the aerogel thermal insulation coating according to the same method, and respectively carrying out a thermal insulation test and an adhesion test on the composite aerogel (A4). The results show that the adiabatic temperature differences of (A2) and (A3) are 12.7 ℃ and 11.4 ℃ respectively; the adhesive force is 2 grades.
The SiC-SiO was carried out sequentially by replacing the modified SiC nanoparticles (A1) with the unmodified SiC nanoparticles (A1') 2 Composite aerogel (A2'), KH-570 modified SiC-SiO 2 Composite aerogel (A3') and polyacrylic acid modified SiC-SiO 2 Composite aerogel (a4 '), prepared by replacing (a4) with (a 4') according to the same method, and subjected to heat insulation test and adhesion test, respectively. The results showed that the adiabatic temperature differences of (A4') were 16.9 ℃ respectively; the adhesive force is 1 grade.
Without wishing to be bound by any theory, the use of the particular aerogels of the invention improves SiO 2 The surface energy of the aerogel and the connection area of the secondary particles, thereby improving mechanical properties and heat insulation properties.
It should be understood that the detailed description of the invention is merely illustrative of the spirit and principles of the invention and is not intended to limit the scope of the invention. Furthermore, it should be understood that various changes, substitutions, deletions, modifications or adjustments may be made by those skilled in the art after reading the disclosure of the present invention, and such equivalents are also within the scope of the invention as defined in the appended claims.
Claims (2)
1. The aerogel heat insulation composite material is characterized by being obtained by reacting KH-570 modified composite aerogel with acrylic acid monomers;
(1) modification of SiC nanoparticles
Preparing 50mL of KH-570 ethanol solution with the volume concentration of 2%, and adjusting the pH value to be 4.0 by using acetic acid; adding 10g of SiC nano-particles into the KH-570 ethanol solution, and carrying out modification reaction at the temperature of 55 ℃; after the reaction is finished, centrifuging the reaction mixture for 10min at the rotating speed of 12000rpm to obtain solid precipitate; washing with absolute ethyl alcohol for 3 times, and drying at 80 ℃ to obtain modified SiC nano particles;
(2) SiC-SiO 2 preparation of composite aerogels
Adding 1.2g of modified SiC nano particles into 80mL of absolute ethanol, and performing ultrasonic treatment to uniformly disperse the modified SiC nano particles to obtain SiC ethanol dispersion liquid; sequentially adding 40mL of silica sol with the solid content of 30% and 5mL of deionized water into the SiC ethanol dispersion liquid, adding 1mL of dimethyl formamide DMF, and performing ultrasonic treatment to uniformly disperse the dimethyl formamide DMF; standing at room temperature to obtain SiC-SiO 2 Compounding the wet gel; aging at room temperature for 24h after wet gel formation; respectively soaking the mixture in 50% ethanol aqueous solution and absolute ethanol for 24h, and replacing the corresponding solutions once in 8 h; finally, drying for 48h at 60 ℃ to obtain SiC-SiO 2 Compounding aerogel; SiC-SiO 2 Modification of composite aerogel, namely, adding 5g of SiC-SiO 2 Putting the composite aerogel into 60mL of ethanol, adding 0.5mL of 25% ammonia water solution, and performing ultrasonic treatment to uniformly disperse the composite aerogel; adding 1gKH-570, dispersing uniformly by ultrasonic, and reacting for 36h at 70 ℃ under a closed condition; then opening and heating for 4 h; after the reaction is finished, centrifuging the reaction mixture for 10min at the rotating speed of 12000rpm to obtain solid precipitate; washing with anhydrous ethanol for 3 times, and drying at 80 deg.C to obtain KH-570 modified SiC-SiO 2 Compounding aerogel; then 1g of KH-570 modified SiC-SiO 2 The composite aerogel is dispersed in 9mL of absolute ethyl alcohol and is added with nitrogenIn the atmosphere, 10mL of 2% acrylic monomer ethanol solution with volume concentration and 10mL of 0.015g potassium persulfate aqueous solution are sequentially added, and the mixture reacts for 12 hours at the temperature of 80 ℃; after the reaction is finished, centrifuging the reaction mixture for 10min at the rotating speed of 12000rpm to obtain solid precipitate; washing with anhydrous ethanol for 3 times, and drying at 80 deg.C to obtain polyacrylic acid modified SiC-SiO 2 And (3) compounding the aerogel.
2. A method of making the aerogel thermal insulation composite of claim 1, the method comprising:
KH-570 modification is carried out on the composite aerogel;
the modified composite aerogel is reacted with an acrylic monomer.
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Denomination of invention: Aerogel thermal insulation composite and its preparation method Effective date of registration: 20221210 Granted publication date: 20220902 Pledgee: Xuzhou Rural Commercial Bank Co.,Ltd. Pledgor: ANHUA FIRE-FIGHTING NEW MATERIAL TECHNOLOGY (JIANGSU) Co.,Ltd. Registration number: Y2022320000784 |
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Address after: 221100 east of Yinshan road and south of Lijiang Road, No.2 Industrial Park, Tongshan District, Xuzhou City, Jiangsu Province, 1st floor, building A9, Safety Technology Industrial Park Patentee after: Anhua New Materials Technology (Jiangsu) Co.,Ltd. Address before: 221100 east of Yinshan road and south of Lijiang Road, No.2 Industrial Park, Tongshan District, Xuzhou City, Jiangsu Province, 1st floor, building A9, Safety Technology Industrial Park Patentee before: ANHUA FIRE-FIGHTING NEW MATERIAL TECHNOLOGY (JIANGSU) Co.,Ltd. |
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