CN116063812A - Transparent heat insulation aerogel resin and preparation method and application thereof - Google Patents
Transparent heat insulation aerogel resin and preparation method and application thereof Download PDFInfo
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- CN116063812A CN116063812A CN202310270376.3A CN202310270376A CN116063812A CN 116063812 A CN116063812 A CN 116063812A CN 202310270376 A CN202310270376 A CN 202310270376A CN 116063812 A CN116063812 A CN 116063812A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
- C03C27/06—Joining glass to glass by processes other than fusing
- C03C27/10—Joining glass to glass by processes other than fusing with the aid of adhesive specially adapted for that purpose
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
- B32B27/283—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polysiloxanes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
- B32B27/308—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising acrylic (co)polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/38—Layered products comprising a layer of synthetic resin comprising epoxy resins
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/40—Layered products comprising a layer of synthetic resin comprising polyurethanes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B3/00—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
- B32B3/02—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by features of form at particular places, e.g. in edge regions
- B32B3/08—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by features of form at particular places, e.g. in edge regions characterised by added members at particular parts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/0007—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding involving treatment or provisions in order to avoid deformation or air inclusion, e.g. to improve surface quality
- B32B37/003—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding involving treatment or provisions in order to avoid deformation or air inclusion, e.g. to improve surface quality to avoid air inclusion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
- B32B37/1284—Application of adhesive
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
- B32B37/15—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer being manufactured and immediately laminated before reaching its stable state, e.g. in which a layer is extruded and laminated while in semi-molten state
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/16—Drying; Softening; Cleaning
- B32B38/162—Cleaning
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/304—Insulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/40—Properties of the layers or laminate having particular optical properties
- B32B2307/412—Transparent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
- Y02A30/24—Structural elements or technologies for improving thermal insulation
- Y02A30/249—Glazing, e.g. vacuum glazing
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B80/00—Architectural or constructional elements improving the thermal performance of buildings
- Y02B80/22—Glazing, e.g. vaccum glazing
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Abstract
The invention belongs to the technical field of laminated glass. The invention provides a transparent heat insulation aerogel resin, and a preparation method and application thereof. The invention is realized by the method of preparing SiO 2 Performing hydrophobic modification and surface hydrophilic modification on the aerogel powder to obtain modified SiO with an internal hydrophobic layer and surface hydrophilic layer structure 2 Aerogel, and carrying out surface coating treatment, and coating modified SiO of resin on the surface 2 The aerogel, the water-based transparent resin, the infrared shielding material, the dispersing medium and the auxiliary agent are mixed to obtain the transparent heat insulation aerogel resin. And pouring transparent heat insulation aerogel resin into the glass cavity, and covering a second piece of monolithic glass to obtain the transparent heat insulation laminated glass. The transparent heat insulation aerogel resin has fluidity and self-curing capability, a nano porous structure is still maintained after curing, and the added infrared shielding material can isolate near infrared light in sunlight, so that the laminated glass has good transparent heat insulation performance and mechanical property.
Description
Technical Field
The invention relates to the technical field of laminated glass, in particular to transparent heat insulation aerogel resin, and a preparation method and application thereof.
Background
Aerogel is a porous amorphous solid material composed of nano colloid particles or high polymer molecules, and has a three-dimensional network structure, and the space structure is filled with a gas medium, but the appearance is solid. The aerogel has the advantages of low density, low thermal conductivity, high porosity, high temperature resistance, incombustibility and the like, and has very wide application prospect in the fields of aerospace, construction, petrochemical industry, military industry, thermal energy engineering, transportation, household appliances and the like.
The performance of the aerogel has close relation with the particle size, and when the particle size of the aerogel is smaller than the wavelength of visible light and the pore diameter is smaller than 70nm, the aerogel can be a transparent blue solid with excellent heat insulation performance, and has certain application value in building glass. The glass door and window is one of the important focus fields of building energy conservation, and building glass has gradually developed from pure lighting and decorative materials to the directions of heat preservation, heat insulation, sound insulation, noise reduction, light control and the like. The transparent aerogel resin has excellent heat insulation and certain transparency, so that the transparent aerogel resin has high application value in the field of energy-saving glass, in particular to laminated glass. The sandwich layer of the laminated glass is replaced by the composite resin containing aerogel, so that the glass door and window with the functions of transparency and heat preservation can be obtained.
Tungsten bronze (MxWO) 3 M is an alkali metal element) is the latest generation of transparent heat insulating material, which is composed of [ WO ] 6 ]The octahedron co-peaks are connected to form a lattice framework, and alkali metal atoms filled in lattice gaps inject electrons outside the lattice framework into conduction bands to form free electrons, so that the material has intrinsic conductivity (conductivity 10) -5 Omega/cm) and near infrared shielding capability of the full solar spectrum. Photo-thermal simulation evaluation shows that the energy-saving glass coated with the tungsten bronze heat insulation layer can effectively reduce indoor temperature (3-10 ℃) and air conditioner refrigeration energy consumption and improve living comfort under the premise of ensuring enough lighting. The tungsten bronze has high thermodynamic stability, and the contained elements are cheap and nontoxic, so that the tungsten bronze has high competitive advantage when used as an energy-saving glass coating.
The prior aerogel glass preparation process is to fix a prefabricated single or a plurality of transparent aerogel resin sheets between two glass sheets. Patent CN109502997a discloses a preparation method of transparent heat-insulating aerogel glass, in which a block-shaped wet gel after pre-drying treatment is put into a space formed by spacing bars on a lower cover plate, and then an upper cover plate is covered; and (3) pressurizing, heating, drying and edge sealing the packaged aerogel glass to obtain a transparent heat insulation aerogel glass finished product. Although the aerogel glass finished product has good heat insulation and light transmittance, the large-scale aerogel is difficult to prepare, and the aerogel is easy to break in the moving and packaging processes, so that the process is complicated and is not beneficial to large-scale production. And the other process is that transparent aerogel resin with fluidity is injected into a laminated glass cavity with a reserved pouring gate, and the transparent heat-insulating aerogel laminated glass is formed after solidification. Patent CN107267104a discloses a transparent heat-insulating fireproof glue containing aerogel, a preparation method thereof and heat-insulating fireproof glass, and the transparent heat-insulating fireproof glue containing aerogel is poured into a glass cavity of a reserved pouring gate, and the reserved pouring gate is sealed and cured. The heat-insulating fireproof rubber glass has the advantages of being focused on fire resistance, not ideal in heat insulation performance and failing to exert the heat-insulating effect of the air-out gel.
Based on the above, an aerogel resin which can be directly injected into an interlayer and is subjected to flow curing and has good transparency and heat insulation performance is developed, and the aerogel resin is used for laminated glass, so that the transparency and the heat insulation performance of the laminated glass are improved, and has important economic value and significance.
Disclosure of Invention
The invention aims to provide a transparent heat insulation aerogel resin, a preparation method and application thereof, aiming at the defects of the prior art.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of transparent heat insulation aerogel resin, which comprises the following steps:
1) SiO is made of 2 Mixing aerogel powder with surface hydrophilic modification solution, and sequentially carrying out surface hydrophilic modification and drying treatment to obtain modified SiO 2 An aerogel;
2) Modified SiO 2 Sequentially carrying out surface coating and curing treatment on the aerogel to obtain modified SiO of surface coating resin 2 An aerogel;
3) Modified SiO with surface coated with resin 2 The aerogel, the water-based transparent resin, the infrared shielding material, the dispersing medium and the auxiliary agent are mixed to obtain the transparent heat insulation aerogel resin.
Preferably, the SiO of step 1) 2 The aerogel powder has the structure of regular tetrahedron, regular hexahedron, regular octahedron, regular dodecahedron or regular icosahedron, siO 2 The grain diameter of the aerogel powder is 20-200 mu m;
the surface hydrophilic modification solution comprises a surfactant, a low surface tension solvent and water, wherein the mass ratio of the surfactant to the low surface tension solvent to the water is 1:0.1 to 100: 100-300, wherein the surfactant is one or more of fatty alcohol phosphate, fatty alcohol polyoxyethylene ether phosphate, aliphatic ammonium salt, alkyl amino acid, carboxylic acid betaine, aliphatic polyester and alkylphenol polyoxyethylene, and the low-surface tension solvent is one or more of acetone, n-hexane, n-pentane, n-heptane, ethanol, isopropanol, tertiary butanol, propylene glycol and glycerin.
Preferably, in step 1), when SiO 2 When the contact angle between the surface of the aerogel powder and water is smaller than 90 DEG, siO is added into the mixture to form a powder body of the aerogel powder 2 The aerogel powder is subjected to hydrophobic modification in a closed hydrophobic modifier gas-phase environment and then subjected to surface hydrophilic modification, wherein the hydrophobic modifier is one or more of chlorosilane, silazane, siloxane, methoxysilane and ethoxysilane.
Preferably, the SiO of step 1) 2 The volume ratio of the aerogel powder to the surface hydrophilic modification solution is 1:2-5; the surface hydrophilic modification mode is one or more of far infrared radiation, mechanical stirring, ultrasonic treatment and ball milling, and the surface hydrophilic modification time is 5-30 min; the temperature of the drying treatment is 80-150 ℃, and the time of the drying treatment is 0.5-3 h.
Preferably, the surface coating mode in the step 2) is dip-coating or plasma polymerization, wherein the dip-coating resin is aqueous fluorine-containing polyurethane resin, and the dip-coating time of the dip-coating is 10-50 min; the plasma polymerized plasma is fluorine-containing acrylic acid, the discharge air pressure of the plasma polymerization is 10-20 Pa, the power of the plasma polymerization is 30-80W, and the time of the plasma polymerization is 1-3 h;
the temperature of the curing treatment is 100-300 ℃, and the time of the curing treatment is 2-6 h.
Preferably, the water-based transparent resin in the step 3) is one or more of water-based alkyd resin, water-based acrylic resin, water-based polyurethane resin, water-based organic silicon resin, water-based epoxy resin and water-based fluorocarbon resin;
the infrared shielding material is one or more of arsenic trioxide, indium tin oxide, titanium dioxide, tungsten bronze, silicon carbide, titanium pyrosulfate, silica fume and yttrium stabilized zirconia;
the dispersion medium is one or more of water, dimethylbenzene, butyl acetate and alcohol with 2-5 carbon atoms;
the auxiliary agent is one or more of a crosslinking curing agent, a wetting agent, a dispersing agent, a leveling agent, a defoaming agent, a preservative and a film forming agent.
Preferably, step 3) the surface-coated resin-modified SiO 2 The mass ratio of aerogel, water-based transparent resin, infrared shielding material, dispersion medium and auxiliary agent is 10-20: 70-100: 0.1 to 1:100:1 to 5;
the mixing time is 10-60 min.
The invention also provides the transparent heat insulation aerogel resin prepared by the preparation method of the transparent heat insulation aerogel resin.
The invention also provides application of the transparent heat-insulating aerogel resin in laminated glass, borosilicate glass spacer bars are bonded around a first piece of glass to form a cavity with one open surface, the transparent heat-insulating aerogel resin is poured into the cavity, a second piece of glass is covered on the cavity, and curing treatment and sealing treatment are sequentially carried out to obtain the transparent heat-insulating laminated glass.
Preferably, the bonding agent is silicone structural adhesive, and the thickness of the silicone structural adhesive is 0.5-2 mm; the temperature of the curing treatment is 50-80 ℃, and the time of the curing treatment is 1-5 h; the sealing treatment is to seal the periphery of the transparent heat-insulating laminated glass by using the double-component silicone adhesive.
The beneficial effects of the invention include the following points:
1) In the transparent heat insulation aerogel resin, the aerogel keeps a nano porous structure, the water-based transparent resin is paved on the surface of the aerogel, the nano porous structure in the aerogel is not damaged, and the light transmittance and heat insulation performance of the aerogel can be maintained.
2) The transparent heat insulation aerogel resin has fluidity and self-curing capability, after curing, the aerogel still keeps a nano porous structure, and the added infrared shielding material can isolate near infrared light energy in sunlight to a certain extent, so that the laminated glass has good transparent heat insulation performance, good mechanical performance, difficult occurrence of defects such as cracks and the like, simple process, practicability and suitability for industrial production, and can be widely applied to enclosure structures such as heat insulation windows, curtain walls and the like of low-energy buildings.
Detailed Description
The invention provides a preparation method of transparent heat insulation aerogel resin, which comprises the following steps:
1) SiO is made of 2 Mixing aerogel powder with surface hydrophilic modification solution, and sequentially carrying out surface hydrophilic modification and drying treatment to obtain modified SiO 2 An aerogel;
2) Modified SiO 2 Sequentially carrying out surface coating and curing treatment on the aerogel to obtain modified SiO of surface coating resin 2 An aerogel;
3) Modified SiO with surface coated with resin 2 The aerogel, the water-based transparent resin, the infrared shielding material, the dispersing medium and the auxiliary agent are mixed to obtain the transparent heat insulation aerogel resin.
SiO as described in step 1) of the present invention 2 The aerogel powder has a structure of regular tetrahedron, regular hexahedron, regular octahedron, regular dodecahedron or regular icosahedron, or SiO 2 The particle diameter of the aerogel powder is preferably 20 to 200. Mu.m, more preferably 50 to 150. Mu.m, still more preferably 80 to 120. Mu.m;
the surface hydrophilic modification solution comprises a surfactant, a low surface tension solvent and water, wherein the mass ratio of the surfactant to the low surface tension solvent to the water is preferably 1:0.1 to 100:100 to 300, more preferably 1: 10-80: 130 to 260, more preferably 1: 30-50: 150-200; the surfactant is preferably one or more of fatty alcohol phosphate, fatty alcohol polyoxyethylene ether phosphate, aliphatic ammonium salt, alkyl amino acid, carboxylic acid betaine, aliphatic polyester and alkylphenol polyoxyethylene, and the low-surface tension solvent is preferably one or more of acetone, n-hexane, n-pentane, n-heptane, ethanol, isopropanol, tertiary butanol, propylene glycol and glycerin.
According to the invention, the hydrophilic modification treatment is carried out on the aerogel by adopting the aqueous solution of the surfactant and the low-surface-tension solvent, so that the wetting expansion rate of the modified solution on the surface of the aerogel can be obviously improved, and the expansion capacity towards the inside of the aerogel is reduced; the low surface tension solvent has a surface synergistic hydrophilic modification effect with water and a surfactant, and can reduce the capillary force of the modification solution entering the aerogel surface nano-pores, so that the modification solution is easily evaporated through a drying process, the aerogel nano-porous structure is not damaged, and the heat insulation performance of the resin is ensured.
In step 1) of the present invention, when SiO 2 When the contact angle between the surface of the aerogel powder and water is smaller than 90 DEG, siO is added into the mixture to form a powder body of the aerogel powder 2 The aerogel powder is subjected to hydrophobic modification in a closed hydrophobic modifier gas phase environment and then subjected to surface hydrophilic modification, wherein the hydrophobic modifier is preferably one or more of chlorosilane, silazane, siloxane, methoxysilane and ethoxysilane, and more preferably one or more of trimethylchlorosilane, hexamethyldisilazane, hexamethyldisiloxane, methyltrimethoxysilane, methyltriethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, gamma-aminopropyl trimethoxysilane, gamma-aminopropyl triethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma-methacryloxypropyl trimethoxysilane and N- (beta-aminoethyl) -gamma-aminopropyl triethoxysilane; the time for the hydrophobic modification is preferably 1 to 3 hours, more preferably 1.5 to 2 hours.
SiO as described in step 1) of the present invention 2 The volume ratio of the aerogel powder to the surface hydrophilic modification solution is preferably 1:2-5, and more preferably 1:3-4; the surface hydrophilic modification mode is preferably one or more of far infrared radiation, mechanical stirring, ultrasonic treatment and ball milling, and the surface hydrophilic modification time is preferably 5-30 min, more preferably 10-25 min, and even more preferably 15-20 min; the temperature of the drying treatment is preferably 80 to 150 ℃, more preferably 90 to 130 ℃, and even more preferably 100 to 120 ℃; the drying treatment time is preferably 0.5 to 3 hours, more preferably 1 to 2.5 hours, and still more preferably 1.5 to 2 hours.
Modified SiO of the invention 2 The aerogel is composed of an inner hydrophobic layer and a surface hydrophilic layer, so that reflection of visible light on the surface of the aerogel can be reduced, and the transmittance of the visible light in the aerogel is improved.
The surface coating mode in the step 2) is preferably dip-coating or plasma polymerization, the dip-coating resin is preferably aqueous fluorine-containing polyurethane resin, the dip-coating time of the dip-coating is preferably 10-50 min, more preferably 20-40 min, and even more preferably 25-30 min; the plasma of the plasma polymerization is preferably fluorine-containing acrylic acid, and the discharge pressure of the plasma polymerization is preferably 10 to 20Pa, more preferably 12 to 17Pa, and even more preferably 14 to 15Pa; the power of the plasma polymerization is preferably 30 to 80W, more preferably 40 to 70W, still more preferably 50 to 60W; the time for the plasma polymerization is preferably 1 to 3 hours, more preferably 1.2 to 2.5 hours, and still more preferably 1.5 to 2 hours;
the pulling impregnation method of the invention is to immerse the modified aerogel in the water transparent resin, so that the modified aerogel and the water transparent resin are fully contacted and then taken out; the low-temperature plasma polymerization method is to activate the resin material into active particles such as free radicals to form gas-phase free radicals, the gas-phase free radicals are adsorbed on the surface of the aerogel to form surface free radicals, and the surface free radicals and gas-phase original monomers or derivative monomers in the plasma are subjected to polymerization reaction on the surface of the aerogel to form the film. Due to the principle of an antireflection film, the visible light transmittance of the aerogel resin can be improved by coating one or more layers of aqueous resin films with refractive indexes between those of the aerogel and the aqueous resin on the surface of the aerogel.
The temperature of the curing treatment in step 2) of the present invention is preferably 100 to 300 ℃, more preferably 130 to 260 ℃, and even more preferably 150 to 200 ℃; the curing time is preferably 2 to 6 hours, more preferably 3 to 5 hours, and still more preferably 4 hours.
The water-based transparent resin in the step 3) is preferably one or more of water-based alkyd resin, water-based acrylic resin, water-based polyurethane resin, water-based organic silicon resin, water-based epoxy resin and water-based fluorocarbon resin;
the infrared shielding material is preferably one or more of arsenic trioxide, indium tin oxide, titanium dioxide, tungsten bronze, silicon carbide, titanium pyrosulfate, silica fume and yttrium stabilized zirconia;
the dispersion medium is preferably one or more of water, dimethylbenzene, butyl acetate and alcohol with 2-5 carbon atoms, and the alcohol with 2-5 carbon atoms is preferably one or more of ethanol, isopropanol, n-butanol and ethylene glycol;
the auxiliary agent is preferably one or more of a crosslinking curing agent, a wetting agent, a dispersing agent, a leveling agent, a defoaming agent, a preservative and a film forming agent, and the crosslinking curing agent is preferably one or more of sodium fluosilicate, potassium fluosilicate, aluminum fluoride, dimethylethanolamine, divinyl triamine, dicyandiamide, adipic acid dihydrazide and ammonium persulfate; the wetting agent is preferably one or more of sodium dodecyl sulfonate, lauryl sulfate, dialkyl sulfosuccinate, castor oil sulfate, alkyl pyridinium chloride, alkylphenol polyvinyl ether, polyoxyethylene alkyl ether and polyoxyethylene glycol alkyl ester; the dispersing agent is preferably one or more of sodium metasilicate, sodium disilicate, alkyl polyether sulfate, alkylaryl sulfonate, fatty acid amide derivative sulfate, polyvinyl alcohol alkylaryl ether sodium sulfate, sorbitol alkylate, polyoxyethylene alkylphenol ether, trimethyl stearamide chloride, polycarboxylate, polyacrylic acid derivative, polymethacrylic acid derivative and naphthalene sulfonate; the leveling agent is preferably one or more of an acrylic polymer leveling agent, a fluorine modified acrylic ester leveling agent, an organic silicon leveling agent and a fluorocarbon leveling agent; the defoaming agent is preferably one or more of unsaturated alkane defoaming agents without organic silicon, polysiloxane defoaming agents, modified organic silicon defoaming agents, dimethyl polysiloxane and hydrophobic silicon dioxide mixture defoaming agents, organic silicon polymer defoaming agents containing hydrophobic particles and silicon-free nonionic acrylic polymer defoaming agents; the preservative is preferably one or more of 1, 2-benzisothiazolin-3-one, 5-chloro-2-methyl-4-isothiazolin-3-one, hexahydro-1, 3, 5-tris (2-hydroxyethyl) s-triazine and 1,3, 5-triethyl-hexahydro-1, 3, 5-triazine; the film forming agent is preferably one or more of methyl pyrrolidone, 2, 4-trimethyl-1, 3-pentanediol monoisobutyrate, diisobutyl succinate, diisobutyl glutarate, diisobutyl adipate, dipropylene glycol butyl ether and propylene glycol phenyl ether.
According to the invention, the dispersing medium and the auxiliary agent are added into the aerogel resin, so that the transparency, heat insulation, curing conditions, fluidity, weather resistance, ageing resistance, mechanical properties and the like of the resin can be improved.
The step 3) of the invention is to coat the modified SiO of the resin on the surface 2 The mass ratio of aerogel, water-based transparent resin, infrared shielding material, dispersion medium and auxiliary agent is preferably 10-20: 70-100: 0.1 to 1:100:1 to 5, more preferably 12 to 17: 80-95: 0.3 to 0.8:100:2 to 4, more preferably 14 to 15: 85-90: 0.4 to 0.6:100:2 to 3;
the mixing time is preferably 10 to 60 minutes, more preferably 20 to 50 minutes, and still more preferably 30 to 40 minutes.
The invention also provides the transparent heat insulation aerogel resin prepared by the preparation method of the transparent heat insulation aerogel resin.
The invention also provides application of the transparent heat-insulating aerogel resin in laminated glass, borosilicate glass spacer bars are bonded around a first piece of glass to form a cavity with one open surface, the transparent heat-insulating aerogel resin is poured into the cavity, a second piece of glass is covered on the cavity, and curing treatment and sealing treatment are sequentially carried out to obtain the transparent heat-insulating laminated glass.
The first single glass and the second single glass are independently preferably toughened glass, float glass, colored glass, coated glass or embossed glass, and the thickness of the first single glass and the second single glass is independently preferably 3-15 mm, more preferably 7-12 mm, and even more preferably 9-10 mm.
The first single glass and the second single glass are preferably pretreated and then are prepared into transparent heat-insulating laminated glass, the pretreatment is preferably sequentially ultrasonic cleaning by ethanol and water, and the inner surfaces of the glass are treated by a silane coupling agent and then are dried in vacuum; the ultrasonic cleaning time is preferably 10 to 30 minutes, more preferably 15 to 25 minutes, and even more preferably 18 to 20 minutes; the silane coupling agent is preferably KH550; the temperature of the vacuum drying is preferably 50 to 70 ℃, more preferably 55 to 65 ℃, and even more preferably 58 to 60 ℃; the vacuum degree of the vacuum drying is preferably-0.1 to-0.5 MPa, more preferably-0.2 to-0.4 MPa, and still more preferably-0.3 MPa; the time for vacuum drying is preferably 10 to 30 minutes, more preferably 15 to 25 minutes, and still more preferably 20 to 22 minutes. The pretreatment of the single glass can improve the transmittance of the glass and the interface bonding strength between the glass and the transparent heat-insulating resin.
In the invention, after the transparent heat insulation aerogel resin is poured into the cavity, one or more of vibration treatment, ultrasonic treatment, heating treatment and ultraviolet radiation treatment are preferably carried out, so that the fluidity and wettability of the poured resin can be improved, the bonding capability of the aerogel resin and glass can be improved, air bubbles can be reduced or eliminated, and the appearance quality of the product can be improved.
The bonding agent is preferably silicone structural adhesive, and the thickness of the silicone structural adhesive is preferably 0.5-2 mm, more preferably 0.7-1.6 mm, and even more preferably 1.0-1.3 mm; the borosilicate glass spacing bars are preferably 10mm in width and 5mm in thickness; the temperature of the curing treatment is preferably 50 to 80 ℃, more preferably 60 to 75 ℃, still more preferably 65 to 70 ℃; the curing treatment time is preferably 1 to 5 hours, more preferably 2 to 4 hours, and still more preferably 3 hours; the sealing treatment is preferably to seal the periphery of the transparent heat-insulating laminated glass by using a two-component silicone adhesive.
In the invention, the steps of preparing the transparent heat-insulating laminated glass are repeated, so that the multilayer transparent heat-insulating laminated glass can be obtained, wherein the number of layers of the multilayer transparent heat-insulating laminated glass is preferably 2-5, and more preferably 3-4.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
An octahedral structure of SiO with a particle size of 100 μm 2 Hydrophobic modification is carried out on aerogel powder (the contact angle between the surface of the powder and water is 45 ℃) in a closed trimethylchlorosilane gas-phase environment, and the hydrophobic modified SiO is obtained after the reaction for 1.5h 2 Aerogel powder; fatty alcohol polyoxyethylene ether ammonium sulfate AESA, n-hexane, acetone and water were mixed in a ratio of 1:0.4:0.4:130 to obtain a surface hydrophilic modification solution; hydrophobically modified SiO 2 Mixing aerogel powder and surface hydrophilic modification solution according to a volume ratio of 1:3, stirring for 15min at a rotation speed of 2500r/min to carry out surface hydrophilic modification, and drying at 120 ℃ for 0.5h to obtain modified SiO with a surface hydrophilic layer thickness of 11.1 mu m 2 An aerogel; modified SiO 2 Soaking aerogel in aqueous fluorine-containing polyurethane resin for 20min, coating surface by adopting a soaking and pulling method, and curing at 150deg.C for 3h to obtain modified SiO with surface coated resin 2 An aerogel; modified SiO with surface coated with resin 2 Aerogel, aqueous acrylic resin S-70, indium tin oxide ITO and TiO 2 Mixing water, a polydimethylsiloxane defoamer, sodium disilicate, a leveling agent BYK-378 and dimethylethanolamine according to a mass ratio of 15:80:0.3:0.2:100:0.03:2:0.05:1, and stirring for 20min at a rotating speed of 1500r/min to obtain the transparent heat insulation aerogel resin.
Sequentially cleaning cesium potassium glass with the thickness of 6mm with absolute ethyl alcohol and deionized water under 40KHz power for 20min, treating the inner surface of the glass with a silane coupling agent KH550, and vacuum drying at-0.1 MPa and 60 ℃ for 20min; and (3) bonding a borosilicate glass spacer bar with the thickness of 10mm and the thickness of 5mm on the periphery of the pretreated cesium-potassium glass by using a single-component neutral silicone structural adhesive with the thickness of 1mm to form a cavity with one open surface, pouring transparent heat insulation aerogel resin into the cavity, coating the periphery of a second piece of pretreated cesium-potassium glass with the single-component neutral silicone structural adhesive, covering the cavity, curing for 3 hours at the temperature of 60 ℃, and sealing the periphery by using a double-component silicone adhesive to obtain the transparent heat insulation laminated glass.
The performance index of the transparent heat-insulating laminated glass of this example is shown in table 1.
Table 1 performance index of the transparent heat insulating laminated glass of example 1
Wherein B represents glass, and Q represents transparent heat insulation aerogel resin.
Example 2
Mixing fatty alcohol polyoxyethylene ether ammonium sulfate AESA, normal hexane, absolute ethanol and water according to a ratio of 1:0.4:0.3:260 to obtain a surface hydrophilic modification solution; siO with regular icosahedron structure and particle diameter of 89 μm 2 Mixing aerogel powder (the contact angle of the powder surface and water is 145 DEG) with a surface hydrophilic modification solution according to a volume ratio of 1:3, ball milling for 10min at a rotating speed of 500r/min to carry out surface hydrophilic modification, and drying for 0.5h at 120 ℃ to obtain modified SiO with a surface hydrophilic layer thickness of 5.4 mu m 2 An aerogel; under the conditions that the discharge air pressure is 16Pa and the power is 55W, fluorine-containing acrylic acid is taken as plasma, and a plasma polymerization method is adopted to modify SiO 2 The aerogel is coated for 2 hours, cured for 3 hours at 200 ℃ and minus 0.1MPa, and the modified SiO of the surface coating resin is obtained 2 An aerogel; modified SiO with surface coated with resin 2 Aerogel, waterborne acrylic S-70, cesium tungsten bronze (Cs) 0.33 WO 3 ) The transparent heat-insulating air-condensing agent is prepared by stirring water, a polyether modified organic silicon defoamer HY-024, sodium metasilicate, a fluorine modified acrylic ester flatting agent LD-1084 and sodium fluosilicate for 30min at a rotating speed of 1500r/min according to a mass ratio of 15:80:0.2:100:0.03:2:0.05:1And (3) glue resin.
Sequentially cleaning cesium potassium glass with the thickness of 6mm with absolute ethyl alcohol and deionized water under the power of 30KHz for 20min, treating the inner surface of the glass with a silane coupling agent KH550, and vacuum drying at-0.1 MPa and 60 ℃ for 20min; and (3) bonding a borosilicate glass spacer bar with the thickness of 1mm and the thickness of 5mm on the periphery of the pretreated cesium-potassium glass by using a single-component neutral silicone structural adhesive with the thickness of 10mm to form a cavity with one open surface, pouring transparent heat insulation aerogel resin into the cavity, coating the periphery of a second piece of pretreated cesium-potassium glass with the single-component neutral silicone structural adhesive, covering the cavity, curing for 3 hours at the temperature of 60 ℃, repeating the steps, and sealing the periphery of the obtained combined glass by using a double-component silicone adhesive to obtain the three-glass two-cavity transparent heat insulation laminated glass.
The performance index of the transparent heat-insulating laminated glass of this example is shown in table 2.
Table 2 performance index of transparent heat-insulating laminated glass of example 2
Wherein B represents glass, and Q represents transparent heat insulation aerogel resin.
Example 3
Replacement of indium tin oxide ITO, tiO in example 1 with cesium tungsten bronze, silicon carbide 2 Other conditions were the same as in example 1, to obtain a transparent heat insulating aerogel resin.
Sequentially ultrasonically cleaning cesium potassium glass with the thickness of 8mm with absolute ethyl alcohol and deionized water for 30min at the power of 40KHz, treating the inner surface of the glass with a silane coupling agent KH550, and vacuum drying at-0.2 MPa and 70 ℃ for 30min; and (3) bonding a borosilicate glass spacer bar with the thickness of 1mm and the thickness of 5mm on the periphery of the pretreated cesium-potassium glass by using a single-component neutral silicone structural adhesive with the thickness of 10mm to form a cavity with one open surface, pouring transparent heat insulation aerogel resin into the cavity, coating the periphery of a second piece of pretreated cesium-potassium glass with the single-component neutral silicone structural adhesive, covering the cavity, curing for 3 hours at 80 ℃, repeating the steps, and sealing the periphery of the obtained combined glass by using a double-component silicone adhesive to obtain the three-glass two-cavity transparent heat insulation laminated glass.
The performance index of the transparent heat-insulating laminated glass of this example is shown in table 3.
TABLE 3 Performance index of transparent Heat insulating laminated glass of example 3
Wherein B represents glass, and Q represents transparent heat insulation aerogel resin.
Example 4
Replacement of indium tin oxide ITO, tiO in example 1 with titanium pyrosulfate 2 Modified SiO with surface coated with resin 2 Aerogel, aqueous acrylic resin S-70, titanium pyrosulfate, water, polydimethylsiloxane defoamer, sodium disilicate, leveling agent BYK-378 and dimethylethanolamine are mixed according to the mass ratio of 15:80:0.8:100:0.03:2:0.05:1, and other conditions are the same as in example 1, so that transparent heat insulation aerogel resin is obtained.
The performance index of the transparent heat-insulating laminated glass of this example is shown in table 4.
TABLE 4 Performance index of transparent Heat insulating laminated glass of example 4
Wherein B represents glass, and Q represents transparent heat insulation aerogel resin.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. The preparation method of the transparent heat insulation aerogel resin is characterized by comprising the following steps:
1) SiO is made of 2 Mixing aerogel powder with surface hydrophilic modification solution, and sequentially carrying out surface hydrophilic modification and drying treatment to obtain modified SiO 2 An aerogel;
2) Modified SiO 2 Sequentially carrying out surface coating and curing treatment on the aerogel to obtain modified SiO of surface coating resin 2 An aerogel;
3) Modified SiO with surface coated with resin 2 The aerogel, the water-based transparent resin, the infrared shielding material, the dispersing medium and the auxiliary agent are mixed to obtain the transparent heat insulation aerogel resin.
2. The method according to claim 1, wherein the SiO of step 1) is 2 The aerogel powder has the structure of regular tetrahedron, regular hexahedron, regular octahedron, regular dodecahedron or regular icosahedron, siO 2 The grain diameter of the aerogel powder is 20-200 mu m;
the surface hydrophilic modification solution comprises a surfactant, a low surface tension solvent and water, wherein the mass ratio of the surfactant to the low surface tension solvent to the water is 1:0.1 to 100: 100-300, wherein the surfactant is one or more of fatty alcohol phosphate, fatty alcohol polyoxyethylene ether phosphate, aliphatic ammonium salt, alkyl amino acid, carboxylic acid betaine, aliphatic polyester and alkylphenol polyoxyethylene, and the low-surface tension solvent is one or more of acetone, n-hexane, n-pentane, n-heptane, ethanol, isopropanol, tertiary butanol, propylene glycol and glycerin.
3. The method according to claim 2, wherein in step 1), when SiO 2 When the contact angle between the surface of the aerogel powder and water is smaller than 90 DEG, siO is added into the mixture to form a powder body of the aerogel powder 2 The aerogel powder is subjected to hydrophobic modification in a closed hydrophobic modifier gas-phase environment and then subjected to surface hydrophilic modification, wherein the hydrophobic modifier is one or more of chlorosilane, silazane, siloxane, methoxysilane and ethoxysilane.
4. Root of Chinese characterA method according to claim 2 or 3, wherein the SiO of step 1) is prepared by 2 The volume ratio of the aerogel powder to the surface hydrophilic modification solution is 1:2-5; the surface hydrophilic modification mode is one or more of far infrared radiation, mechanical stirring, ultrasonic treatment and ball milling, and the surface hydrophilic modification time is 5-30 min; the temperature of the drying treatment is 80-150 ℃, and the time of the drying treatment is 0.5-3 h.
5. The preparation method according to claim 4, wherein the surface coating mode in the step 2) is dip-coating or plasma polymerization, the dip-coating resin is aqueous fluorine-containing polyurethane resin, and the dip-coating time is 10-50 min; the plasma polymerized plasma is fluorine-containing acrylic acid, the discharge air pressure of the plasma polymerization is 10-20 Pa, the power of the plasma polymerization is 30-80W, and the time of the plasma polymerization is 1-3 h;
the temperature of the curing treatment is 100-300 ℃, and the time of the curing treatment is 2-6 h.
6. The preparation method according to claim 5, wherein the aqueous transparent resin in step 3) is one or more of aqueous alkyd resin, aqueous acrylic resin, aqueous polyurethane resin, aqueous silicone resin, aqueous epoxy resin and aqueous fluorocarbon resin;
the infrared shielding material is one or more of arsenic trioxide, indium tin oxide, titanium dioxide, tungsten bronze, silicon carbide, titanium pyrosulfate, silica fume and yttrium stabilized zirconia;
the dispersion medium is one or more of water, dimethylbenzene, butyl acetate and alcohol with 2-5 carbon atoms;
the auxiliary agent is one or more of a crosslinking curing agent, a wetting agent, a dispersing agent, a leveling agent, a defoaming agent, a preservative and a film forming agent.
7. The method of claim 6, wherein the surface coating resin of step 3)Modified SiO of (2) 2 The mass ratio of aerogel, water-based transparent resin, infrared shielding material, dispersion medium and auxiliary agent is 10-20: 70-100: 0.1 to 1:100:1 to 5;
the mixing time is 10-60 min.
8. A transparent heat insulation aerogel resin produced by the method for producing a transparent heat insulation aerogel resin according to any one of claims 1 to 7.
9. The use of the transparent insulating aerogel resin in laminated glass as claimed in claim 8, wherein borosilicate glass spacer bars are bonded around the first monolithic glass to form a cavity with one open surface, the transparent insulating aerogel resin is poured into the cavity, and the second monolithic glass is covered on the cavity, and the transparent insulating laminated glass is obtained by sequentially performing curing treatment and sealing treatment.
10. The use according to claim 9, wherein the bonding agent is a silicone structural adhesive having a thickness of 0.5-2 mm; the temperature of the curing treatment is 50-80 ℃, and the time of the curing treatment is 1-5 h; the sealing treatment is to seal the periphery of the transparent heat-insulating laminated glass by using the double-component silicone adhesive.
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