CN112760024A - Silicon aerogel composite heat-insulating coating and preparation method and application thereof - Google Patents
Silicon aerogel composite heat-insulating coating and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of heat insulation coatings and preparation thereof, in particular to a silicon aerogel composite heat insulation coating and a preparation method and application thereof. The silicon aerogel composite heat insulation coating comprises: 20-40% of polyurethane emulsion, 2-10% of acrylic emulsion, 0-16% of silicon dioxide microspheres, 0-4% of silicon aerogel, 0.1-1% of dispersing agent, 0.5-2% of silane coupling agent, 0.1-1.5% of defoaming agent, 1-3% of film forming agent, 1-4% of flame retardant auxiliary agent and 0.5-2% of thickening agent; the silica aerogel is hydrophobic silica aerogel with a three-dimensional network structure and stacked by porous nanosphere particles; the silicon dioxide microspheres are prepared by a solution-gel method. The composite heat-insulating coating has good adhesive force, larger hardness and bending strength, high hydrophobicity and excellent heat insulating property, and can be applied to application fields of building heat-insulating coatings, pipeline heat insulation and the like.
Description
Technical Field
The invention relates to the technical field of heat insulation coatings and preparation thereof, in particular to a silicon aerogel composite heat insulation coating and a preparation method and application thereof.
Background
The heat-insulating coating is used as a novel functional coating, has the characteristics of heat insulation, energy conservation, convenient construction, strong adaptability and the like, is coated on the surfaces of high-temperature pipelines, containers, equipment, buildings and the like, can form a coating with certain strength and toughness after drying and curing, and can play a role in heat insulation. Because the use of the heat-insulating coating does not need to reconstruct the original wall body, water pipes, electric wire pipes and the like in a house, only the construction is carried out according to the construction process of the common architectural coating, the damage condition of equipment and pipelines is easy to detect, and the system maintenance difficulty and the maintenance cost are greatly reduced. In addition, the coating is simple in construction process, can comprehensively cover special-shaped parts such as elbows, tees and valves, effectively reduces heat dissipation of pipelines, and is widely applied to industries and products such as house buildings, automobiles, petrochemical engineering, military equipment and high-temperature equipment at present.
In the prior art, an organic or inorganic heat-insulating material is mainly added into a coating, wherein the inorganic heat-insulating material comprises a ceramic fiber material, vermiculite, sepiolite, ceramic hollow microspheres and the like, or a reflective material is added, such as ceramic micro powder, aluminum powder, titanium dioxide and other raw materials, and other auxiliary agents are added to prepare the heat-insulating coating.
Disclosure of Invention
Aiming at the problems in the prior art, the invention adopts the silica aerogel and the silica microspheres with unique nano-pore structures as the important raw materials of the heat-insulating coating, and prepares the heat-insulating coating with good heat-insulating effect and good mechanical property by a specific preparation method.
In order to realize the purpose, the invention provides a silicon aerogel composite heat insulation coating, which comprises the following raw materials in percentage by weight:
20-40% of polyurethane emulsion, 2-10% of acrylic emulsion, 0-16% of silicon dioxide microspheres, 0-4% of silicon aerogel, 0.1-1% of dispersing agent, 0.5-2% of silane coupling agent, 0.1-1.5% of defoaming agent, 1-3% of film forming agent, 1-4% of flame retardant auxiliary agent and 0.5-2% of thickening agent;
the silica aerogel is hydrophobic silica aerogel with a three-dimensional network structure and stacked by porous nanosphere particles.
Further, the dispersant is one or the combination of two of organic dispersant SN-5040 and inorganic dispersant sodium hexametaphosphate.
Further, the defoaming agent is one or a combination of more of an organic defoaming agent NXZ, a non-silicon mineral oil defoaming agent J0416 or a water-based defoaming agent JT-910.
Further, the silane coupling agent is 3-aminopropyltriethoxysilane.
Further, the film forming auxiliary agent is one or a combination of a plurality of film forming auxiliary agents such as alcohol ester 12, diethylene glycol monobutyl ether, triethylene glycol monobutyl ether and the like.
Further, the flame retardant auxiliary agent is ammonium polyphosphate.
Further, the thickening agent is one of sodium carboxymethylcellulose, hydroxypropyl methylcellulose or hydroxyethyl cellulose.
Based on the same inventive concept, the invention also provides a preparation method of the silica aerogel composite heat insulation coating, which specifically comprises the following steps:
s1, mixing ammonia water, ethanol and distilled water to obtain a mixed solution A, mixing tetraethyl silicate and ethanol to obtain a mixed solution B, mixing the mixed solution A and the mixed solution B uniformly, carrying out water bath reaction, filtering to obtain filter residue, washing and drying to obtain silicon dioxide microspheres;
s2, dissolving a defoaming agent and a dispersing agent in distilled water, adding the silicon dioxide microspheres, stirring to obtain a white dispersion, adding the emulsion and the defoaming agent, and stirring to obtain white slurry;
and S3, dropwise adding the silica aerogel and the silane coupling agent into the white slurry, stirring until the silica aerogel is completely dispersed, adding the film-forming assistant, the flame-retardant assistant and the thickening agent, stirring and discharging bubbles to obtain the silica aerogel heat-insulating coating.
Further, the process conditions of the water bath reaction in the step S1 are as follows:
the reaction temperature is 5-65 ℃ and the reaction time is 1-4 h.
Based on the same inventive concept, the silicon aerogel composite heat insulation coating is applied to coating heat protection.
Has the advantages that:
(1) the invention adopts the solution-gel method to prepare the silicon dioxide microspheres, the preparation method and the operation instrument are simple and convenient, and the silicon dioxide microspheres have the characteristics of light weight, low density, high mechanical strength, good thermal stability and the like, and can obviously improve the mechanical properties of the coating material.
(2) According to the invention, the silica aerogel is used as a novel heat insulation filler, wherein the nano-pores and the large specific surface area structure of the aerogel can effectively improve the heat insulation performance of the coating. Meanwhile, the high dispersibility and the high compatibility of the aerogel can be uniformly mixed with the emulsion, so that the comprehensive performance of the coating is improved.
(3) The silicon aerogel composite heat insulation coating prepared by the invention has the advantages of higher hardness (the lowest hardness is 1B), good adhesive force (5B), good bending strength (2 mm), high hydrophobicity (WCA is 130.5 degrees) and excellent heat insulation performance (the temperature difference delta T is 10.1-20.4 degrees), and can be applied to the application fields of building heat insulation coatings, pipeline heat insulation and the like.
Drawings
FIG. 1 is an electron microscope scan of silica microspheres of example 1 of the present invention;
FIG. 2 is an electron microscopic scan of a silica aerogel according to example 2 of the present invention;
FIG. 3 is a thermal insulation temperature difference curve of the silica aerogel composite thermal insulation coating in examples 1 to 6 of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to specific embodiments, but the scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
1. Preparation of silica microspheres
Preparing a certain amount of 25mL of ammonia water, 75mL of ethanol and 60mL of distilled water into a mixed solution A, weighing 60mL of tetraethyl silicate and 100mL of ethanol into a mixed solution B, adding the solution B into the solution A at one time, sealing the opening of a beaker by using a preservative film, placing the beaker in a constant-temperature water bath kettle at 30 ℃ for reaction for 2 hours, and adjusting the rotating speed to 600rpm to control the reaction rate. After the reaction was completed, the filtrate was washed with a large amount of distilled water, placed in a petri dish and dried at 60 ℃. As can be seen from fig. 1, the obtained silica microspheres are characterized by micron-sized spherical particles and have good dispersibility.
2. Preparation of silicon aerogel composite heat insulation coating
Firstly, dissolving 1 wt% of organic dispersant SN-5040 and 1 wt% of inorganic dispersant sodium hexametaphosphate in a certain amount of water, uniformly stirring, then adding 8% of silicon spheres, stirring at 1600rpm for 20min to obtain a pure white dispersion, then sequentially adding 40 wt% of polyurethane emulsion, 2 wt% of acrylic emulsion and 0.1 wt% of organic defoamer NXZ, stirring at 400rpm for 20min at a low speed to obtain a milky white slurry, further slowly adding 0.5 wt% of 3-aminopropyltriethoxysilane without adding hydrophobic silicon aerogel, stirring at 1600rpm for 40min at a high speed, after the aerogel is completely dispersed, sequentially adding 2 wt% of film-forming aid alcohol ester 12, 4 wt% of flame-retardant aid ammonium polyphosphate and 0.5 wt% of thickener hydroxyethyl cellulose, stirring at 400rpm for 40min, and obtaining the silicon dioxide composite heat-insulating coating.
Example 2
1. Preparation of silicon aerogel composite heat insulation coating
Firstly, dissolving 1 wt% of organic dispersant SN-5040 and 1 wt% of inorganic dispersant sodium hexametaphosphate in a certain amount of water, uniformly stirring to obtain uniform dispersion liquid, under the condition of not adding silica microspheres, sequentially adding 40 wt% of polyurethane emulsion, 5 wt% of acrylic emulsion and 0.1 wt% of organic defoaming agent NXZ, stirring at low speed of 400rpm for 20min to obtain milk white slurry, further slowly adding 2 wt% of hydrophobic silica aerogel and 0.5 wt% of 3-aminopropyltriethoxysilane, stirring at high speed of 1600rpm for 40min, after the aerogel is completely dispersed, sequentially adding 2 wt% of film-forming aid alcohol ester 12, 4 wt% of flame-retardant aid ammonium polyphosphate and 0.5 wt% of thickener hydroxyethyl cellulose, stirring at low speed of 400rpm for 40min to discharge bubbles, and obtaining the silica composite heat-insulating coating. Wherein, the scanning image of the electron microscope in fig. 2 shows that the silica aerogel is a three-dimensional network structure stacked by the porous nanosphere particles, and the heat insulation performance of the coating can be effectively improved.
Example 3
1. Preparation of silica microspheres
Preparing a certain amount of 25mL of ammonia water, 75mL of ethanol and 60mL of distilled water into a mixed solution A, weighing 60mL of tetraethyl silicate and 100mL of ethanol into a mixed solution B, adding the solution B into the solution A at one time, sealing the opening of a beaker by using a preservative film, placing the beaker in a constant-temperature water bath kettle at 5 ℃ for reaction for 4 hours, and adjusting the rotating speed to 600rpm to control the reaction rate. After the reaction is finished, washing, filtering, washing and filtering by using a large amount of distilled water, placing in a watch glass, and drying at 60 ℃ to obtain the silica microspheres.
2. Preparation of silicon aerogel composite heat insulation coating
Firstly, 0.1 wt% of organic dispersant SN-5040 and 1 wt% of inorganic dispersant sodium hexametaphosphate are dissolved in a certain amount of water and uniformly stirred, then 8% of silicon spheres are added and stirred at 1600rpm for 20min to obtain pure white dispersion liquid, then 40 wt% of polyurethane emulsion, 2 wt% of acrylic emulsion, 0.2 wt% of organic defoamer NXZ and 0.2 wt% of aqueous defoamer JT-910 are sequentially added, and stirred at 400rpm for 20min to obtain milky white slurry, 1 wt% of hydrophobic silica aerogel and 0.5 wt% of 3-aminopropyltriethoxysilane are further slowly added and stirred at 1600rpm for 40min, after the aerogel is completely dispersed, 1 wt% of film-forming aid alcohol ester 12, 4 wt% of flame-retardant aid ammonium polyphosphate and 0.5 wt% of thickener hydroxyethyl cellulose are sequentially added and stirred at 400rpm for 40min to obtain the silica aerogel heat-insulating coating.
Example 4
1. Preparation of silica microspheres
Preparing a certain amount of 25mL of ammonia water, 75mL of ethanol and 60mL of distilled water into a mixed solution A, weighing 60mL of tetraethyl silicate and 100mL of ethanol into a mixed solution B, adding the solution B into the solution A at one time, sealing the opening of a beaker by using a preservative film, placing the beaker in a constant-temperature water bath kettle at 65 ℃ for reaction for 1h, and adjusting the rotating speed to 600rpm to control the reaction rate. After the reaction is finished, washing, filtering, washing and filtering by using a large amount of distilled water, placing in a watch glass, and drying at 60 ℃ to obtain the silica microspheres.
2. Preparation of silicon aerogel composite heat insulation coating
Firstly, dissolving 1 wt% of organic dispersant SN-5040 and 0.1 wt% of inorganic dispersant sodium hexametaphosphate in a certain amount of water, uniformly stirring, then adding 16% of silicon spheres, stirring at 1600rpm for 20min to obtain a pure white dispersion, then sequentially adding 20 wt% of polyurethane emulsion, 10 wt% of acrylic emulsion and 1.5 wt% of non-silicon mineral oil defoamer J0416, stirring at 400rpm for 20min to obtain a milky white slurry, further slowly adding 2 wt% of hydrophobic silica aerogel and 2 wt% of 3-aminopropyltriethoxysilane, stirring at 1600rpm for 40min, after the aerogel is completely dispersed, sequentially adding 3 wt% of film-forming aid alcohol ester 12, 2 wt% of flame-retardant aid ammonium polyphosphate and 2 wt% of thickener hydroxypropyl methyl cellulose, stirring at 400rpm for 40min, and obtaining the silica aerogel heat-insulating coating.
Example 5
1. Preparation of silica microspheres
Preparing a certain amount of 25mL of ammonia water, 75mL of ethanol and 60mL of distilled water into a mixed solution A, weighing 60mL of tetraethyl silicate and 100mL of ethanol into a mixed solution B, adding the solution B into the solution A at one time, sealing the opening of a beaker by using a preservative film, placing the beaker in a constant-temperature water bath kettle at 25 ℃ for reaction for 2 hours, and adjusting the rotating speed to 600rpm to control the reaction rate. After the reaction is finished, washing, filtering, washing and filtering by using a large amount of distilled water, placing in a watch glass, and drying at 60 ℃ to obtain the silica microspheres.
2. Preparation of silicon aerogel composite heat insulation coating
Firstly, 0.5 wt% of organic dispersant SN-5040 and 0.5 wt% of inorganic dispersant sodium hexametaphosphate are dissolved in a certain amount of water and uniformly stirred, then 10% of silicon spheres are added and stirred at 1600rpm for 20min to obtain pure white dispersion liquid, then 30 wt% of polyurethane emulsion, 10 wt% of acrylic emulsion and 0.5 wt% of organic defoaming agent NXZ are sequentially added, and stirred at 400rpm for 20min at low speed to obtain milky white slurry, 3 wt% of hydrophobic silica aerogel and 1 wt% of 3-aminopropyltriethoxysilane are further slowly added and stirred at 1600rpm for 40min at high speed, after the aerogel is completely dispersed, 1 wt% of film-forming aid alcohol ester 12, 2 wt% of flame-retardant aid ammonium polyphosphate and 0.5 wt% of thickener hydroxyethyl cellulose are sequentially added, and stirred at 400rpm for 40min, and the silica aerogel heat-insulating coating is obtained. Wherein, the scanning image of the electron microscope in fig. 2 shows that the silica aerogel is a three-dimensional network structure stacked by the porous nanosphere particles, and the heat insulation performance of the coating can be effectively improved.
Example 6
1. Preparation of silica microspheres
Preparing a certain amount of 25mL of ammonia water, 75mL of ethanol and 60mL of distilled water into a mixed solution A, weighing 60mL of tetraethyl silicate and 100mL of ethanol into a mixed solution B, adding the solution B into the solution A at one time, sealing the opening of a beaker by using a preservative film, placing the beaker in a constant-temperature water bath kettle at 40 ℃ for reaction for 3 hours, and adjusting the rotating speed to 600rpm to control the reaction rate. After the reaction is finished, washing, filtering, washing and filtering by using a large amount of distilled water, placing in a watch glass, and drying at 60 ℃ to obtain the silica microspheres.
2. Preparation of silicon aerogel composite heat insulation coating
Firstly, dissolving 1 wt% of organic dispersant SN-5040 in a certain amount of water, uniformly stirring, adding 12% of silicon balls, stirring at 1600rpm for 20min to obtain a pure white dispersion liquid, then sequentially adding 30 wt% of polyurethane emulsion, 10 wt% of acrylic emulsion and 0.5 wt% of organic defoaming agent NXZ, stirring at 400rpm for 20min to obtain a milky white slurry, further slowly adding 4 wt% of hydrophobic silica aerogel and 1 wt% of 3-aminopropyltriethoxysilane, stirring at 1600rpm for 40min, after the aerogel is completely dispersed, sequentially adding 1 wt% of diethylene glycol monobutyl ether and 1 wt% of triethylene glycol monobutyl ether as film forming aids, 1 wt% of ammonium polyphosphate as flame retardant aids and 1 wt% of carboxymethyl cellulose sodium as thickening agents, stirring at 400rpm for 40min to discharge, and obtaining the silica aerogel heat insulation coating.
The individuality tests obtained in the examples 1 to 6 are carried out, and the temperature rise curve of the back side of the sample along with the change of time under the irradiation of an infrared lamp is tested by adopting a self-made heat insulation temperature difference testing device, wherein the size of the polystyrene foam box is 300mm multiplied by 300mm, the wall thickness is 30mm, and the top end above the cabin is provided with a notch of 150mm multiplied by 150mm for placing a sample plate to be tested. The power of the infrared lamp for testing is 500W, and the distance between the infrared lamp and the sample plate is 25 mm. The test sample is an aluminum plate with the thickness of 150mm multiplied by 1mm, the temperature of the test coating sample and the back sample is collected and tested by a temperature sensor, the temperature which is kept constant within 5min is taken as the stable temperature of the sample, and the difference value of the stable temperature is the heat insulation temperature difference. The results are shown in detail in FIG. 3.
As can be seen from fig. 3 and table 1, the hot surface temperature of the coating layer is 92 ℃, the cold surface temperatures of examples 1 to 6 are 88.5 ℃, 85.1 ℃, 79.3 ℃, 74.6 ℃, 71.6 ℃ and 81.9 ℃, and the temperature differences are 3.5 ℃, 6.9 ℃, 12.7 ℃, 17.4 ℃, 20.4 ℃ and 10.1 ℃, respectively, wherein no silica aerogel is added in example 1, the thermal insulation effect is poor, no silica microspheres are added in example 2, the mechanical properties are poor, and the silica aerogel and the silica microspheres are added in examples 3 to 6, so that the thermal insulation effect and the mechanical properties are good.
The coating layers obtained in examples 1 to 6 were measured for static water contact angle and mechanical properties such as pencil hardness, adhesion and flexural strength, and the results are shown in Table 1.
Table 1 coating performance test results
As can be seen from Table 1, the thermal insulation coating added with the silica aerogel has good hydrophobic property, and the mechanical property of the coating can be obviously enhanced by adding the silica microspheres, so that the thermal insulation coating obtained by adopting the technical scheme of the invention has high hardness, good adhesive force and bending strength, high hydrophobicity and excellent thermal insulation property, and can be applied to application fields of building thermal insulation coatings, pipeline thermal insulation and the like.
The above-mentioned embodiments are only preferred embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical scope of the present invention, and equivalents and modifications of the technical solutions and concepts of the present invention should be covered by the scope of the present invention.
Claims (10)
1. The silicon aerogel composite heat insulation coating is characterized by comprising the following raw materials in percentage by weight:
20-40% of polyurethane emulsion, 2-10% of acrylic emulsion, 0-16% of silicon dioxide microspheres, 0-4% of silicon aerogel, 0.1-1% of dispersing agent, 0.5-2% of silane coupling agent, 0.1-1.5% of defoaming agent, 1-3% of film forming agent, 1-4% of flame retardant auxiliary agent and 0.5-2% of thickening agent;
the silica aerogel is hydrophobic silica aerogel with a three-dimensional network structure and stacked by porous nanosphere particles;
the silicon dioxide microspheres are prepared by a solution-gel method.
2. The silicon aerogel composite thermal insulation coating as claimed in claim 1, wherein the dispersant is one or a combination of two of an organic dispersant SN-5040 and an inorganic dispersant sodium hexametaphosphate.
3. The silicon aerogel composite thermal insulation coating according to claim 1, wherein the defoaming agent is one or a combination of organic defoaming agent NXZ, non-silicon mineral oil defoaming agent J0416 or water-based defoaming agent JT-910.
4. The silicon aerogel composite thermal insulation coating of claim 1, wherein the silane coupling agent is 3-aminopropyltriethoxysilane.
5. The silica aerogel composite thermal insulation coating as claimed in claim 1, wherein the film forming auxiliary agent is one or more of alcohol ester 12, diethylene glycol monobutyl ether, triethylene glycol monobutyl ether and the like.
6. The silicone aerogel composite thermal insulation coating of claim 1, wherein the flame retardant additive is ammonium polyphosphate.
7. The silicone aerogel composite thermal insulation coating of claim 1, wherein the thickener is one of sodium carboxymethylcellulose, hydroxypropyl methylcellulose, or hydroxyethyl cellulose.
8. A preparation method of a silicon aerogel composite heat insulation coating is characterized by specifically comprising the following steps:
s1, mixing ammonia water, ethanol and distilled water to obtain a mixed solution A, mixing tetraethyl silicate and ethanol to obtain a mixed solution B, mixing the mixed solution A and the mixed solution B uniformly, carrying out water bath reaction, filtering to obtain filter residue, washing and drying to obtain silicon dioxide microspheres;
s2, dissolving a defoaming agent and a dispersing agent in distilled water, adding the silicon dioxide microspheres, stirring to obtain a white dispersion, adding the emulsion and the defoaming agent, and stirring to obtain white slurry;
and S3, dropwise adding the silica aerogel and the silane coupling agent into the white slurry, stirring until the silica aerogel is completely dispersed, adding the film-forming assistant, the flame-retardant assistant and the thickening agent, stirring and discharging bubbles to obtain the silica aerogel heat-insulating coating.
9. The preparation method of the silicon aerogel composite thermal insulation coating according to claim 1, wherein the process conditions of the water bath reaction in the step S1 are as follows:
the reaction temperature is 5-65 ℃ and the reaction time is 1-4 h.
10. Use of the silica aerogel composite thermal barrier coating according to any one of claims 1 to 7 or the silica aerogel composite thermal barrier coating prepared by the preparation method according to any one of claims 8 to 9 in thermal protection of coatings.
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| CN113372748A (en) * | 2021-07-05 | 2021-09-10 | 陈杨刚 | Waterproof and fireproof coating and preparation method thereof |
| CN116120811A (en) * | 2023-03-14 | 2023-05-16 | 中国科学院深圳先进技术研究院 | Water-based acrylic resin composite modified aerogel heat-insulating fireproof coating and preparation method thereof |
| CN116237221A (en) * | 2023-03-09 | 2023-06-09 | 东莞市上扬智造科技有限公司 | Silicon dioxide aerogel spraying method of hairdressing equipment |
| CN116120811B (en) * | 2023-03-14 | 2024-06-04 | 中国科学院深圳先进技术研究院 | Water-based acrylic resin composite modified aerogel heat-insulating fireproof coating and preparation method thereof |
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