CN109403023B - Glass fiber nano-pore heat-insulating felt and preparation method thereof - Google Patents

Glass fiber nano-pore heat-insulating felt and preparation method thereof Download PDF

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CN109403023B
CN109403023B CN201811416489.5A CN201811416489A CN109403023B CN 109403023 B CN109403023 B CN 109403023B CN 201811416489 A CN201811416489 A CN 201811416489A CN 109403023 B CN109403023 B CN 109403023B
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felt
glass fiber
nano
silicon dioxide
heat
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CN109403023A (en
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张成贺
任大贵
岳耀辉
刘超
王振宇
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Luyang Energy Saving Materials Co Ltd
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Luyang Energy Saving Materials Co Ltd
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    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/77Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
    • D06M11/79Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/263Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
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    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/564Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
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    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain

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Abstract

The invention provides a glass fiber nano-pore heat-insulating felt and a preparation method thereof. The preparation method provided by the invention comprises the following steps: a) mixing nano silicon dioxide, an organic binding agent, a water repellent and water to obtain silicon dioxide mucilage; b) impregnating a glass fiber felt with the silica gel slurry to obtain a wet blank; c) and carrying out microwave drying after filter pressing on the wet blank to obtain the glass fiber nano-pore heat-insulating felt. The heat-insulating felt prepared by the preparation method has excellent heat-insulating property, high tensile strength, high water-repellent rate, good combustion performance and stable performance.

Description

Glass fiber nano-pore heat-insulating felt and preparation method thereof
Technical Field
The invention relates to the technical field of heat preservation and insulation materials, in particular to a glass fiber nano-pore heat insulation felt and a preparation method thereof.
Background
The heat-insulating felt is a heat-insulating material commonly used for industrial equipment, and is usually used for heat insulation in the fields of industrial pipelines, storage tanks, industrial furnace bodies, power plants, injection molding machines, metal, glass and the like, such as a detachable heat-insulating sleeve and the like.
Currently, aerogel fiber mats are relatively common heat insulation mats, and aerogel fiber mats are heat insulation materials prepared by compounding silica aerogel into fiber mats, wherein the fiber mats (often glass fiber mats) provide excellent strength and toughness, and the silica aerogel provides nano holes, reduces convection heat transfer of materials, and improves heat insulation effects of the fiber mats. The two materials are compounded, the advantages of the two materials are fully combined, the heat-insulating felt has good heat-insulating effect, excellent mechanical properties such as strength and toughness and the like, and the actual construction and use requirements are met.
In the past, processes for making such insulation blankets included both supercritical and non-supercritical processes. The aerogel composite glass fiber mat prepared by the supercritical process has lower heat conductivity coefficient, but has extremely high production cost and higher danger, and is difficult to realize the commercial production. Compared with the prior art, the non-critical process has improved safety, but the product performance such as heat insulation is reduced, and the product is often subjected to aging, aging and other processes, so that the production period is longer and the cost is higher.
In order to overcome the above problems, the prior art proposes some improved preparation methods, for example, patent application with publication number CN105599396A discloses a spray-pressed aerogel felt and a preparation method thereof, the spray-pressed aerogel felt comprises a thermal insulation cloth surface layer and a thermal insulation cloth bottom layer, at least one composite thermal insulation layer is arranged between the thermal insulation cloth surface layer and the thermal insulation cloth bottom layer, the composite thermal insulation layer is composed of a glass fiber layer and an aerogel powder layer, and a thermal insulation synergistic effect is generated, so that the phenomenon that aerogel micro-particles and dust are easy to fall off in the transportation, construction and use processes of the traditional aerogel felt is solved, the service life of the aerogel felt is prolonged, and the spray-pressed aerogel felt has the advantages of moisture resistance, fire resistance, corrosion resistance and the like. Patent application publication No. CN105209248A discloses a method of making a nonwoven wet laid aerogel blanket that can exhibit improved thermal conductivity, lower corrosivity, lower dust generation, and a uniform structure. Different from the traditional supercritical and non-supercritical processes, the preparation method is relatively simple and easy to operate, and provides convenience for industrial production.
However, the method provided by CN105599396A has a certain disadvantage, and only the fiber felt and the aerogel powder are laminated together without any binder, and although the upper and lower layers are provided with the thermal insulation cloth, the powder can be inhibited from falling off, the thermal insulation effect is still not good, and the interlayer strength is poor, and the fiber felt is easy to peel off, especially in the transportation and construction processes, the fiber felt is vibrated to different degrees, so that the aerogel powder migrates to the upper and lower surface layers along the holes where the fibers are interlaced, so that the aerogel powder is unevenly distributed, the thermal insulation effect is more affected, and the hydrophobic effect is poor. CN105209248A prepares aerogel felt through wet process pulping process, though can guarantee that the aerogel powder is evenly distributed in the body, in order to guarantee intensity and toughness of felt body, need introduce a large amount of organic binder, influence its thermal conductivity, and this kind of aerogel felt is under the high temperature environment, and organic binder can burn, causes felt body intensity decay seriously, and volatilizes a large amount of irritative flue gas, seriously influences result in the result of use to cause the harm to the environment. Therefore, it is often difficult to achieve a balance between the thermal insulation properties and the mechanical properties such as strength and toughness of the thermal insulation blanket, and the thermal insulation properties and strength are more likely to be significantly reduced particularly after transportation. How to obtain the heat insulation felt with excellent heat insulation performance, excellent strength performance, environmental protection and good performance retention is a problem to be solved urgently.
Disclosure of Invention
In view of the above, the present invention aims to provide a glass fiber nano-pore heat insulation felt and a preparation method thereof. The heat-insulating felt prepared by the preparation method has excellent heat insulation performance, high tensile strength and stable performance.
The invention provides a preparation method of a glass fiber nano-pore heat-insulating felt, which comprises the following steps:
a) mixing nano silicon dioxide, an organic binding agent, a water repellent and water to obtain silicon dioxide mucilage;
b) impregnating a glass fiber felt with the silica gel slurry to obtain a wet blank;
c) and carrying out microwave drying after filter pressing on the wet blank to obtain the glass fiber nano-pore heat-insulating felt.
Preferably, the organic binder is acrylate emulsion and/or polyurethane emulsion.
Preferably, the solid content of the acrylate emulsion is 52-54%, and the viscosity is 400-1500 mPa.s;
the solid content of the polyurethane emulsion is 28-32%, and the viscosity of the polyurethane emulsion is 400-600 mPa.s.
Preferably, the water repellent is an organosilicon water repellent.
Preferably, the water repellent is hydrogen-containing silicone oil emulsion.
Preferably, the oil content of the hydrogen-containing silicone oil emulsion is more than or equal to 28 percent; the hydrogen content of the hydrogen-containing silicone oil in the hydrogen-containing silicone oil emulsion is 1.5 to 2.5 percent.
Preferably, in the step a), the mass ratio of the water, the nano silicon dioxide, the organic binding agent and the water repellent is 100: 20-25: 2-3: 1-2;
the concentration of the silicon dioxide in the silicon dioxide mucilage is 15-20 wt%.
Preferably, the glass fiber felt is a calcined glass fiber needled felt;
the temperature of the calcination treatment is 350-400 ℃, and the time is 1-2 h.
Preferably, in the step c), the temperature of the microwave drying is 120-150 ℃ and the time is 2-3 h.
The invention also provides the glass fiber nano-pore heat-insulating felt prepared by the preparation method in the technical scheme.
The invention provides a preparation method of a glass fiber nano-pore heat-insulating felt, which comprises the following steps: a) mixing nano silicon dioxide, an organic binding agent, a water repellent and water to obtain silicon dioxide mucilage; b) impregnating a glass fiber felt with the silica gel slurry to obtain a wet blank; c) and carrying out microwave drying after filter pressing on the wet blank to obtain the glass fiber nano-pore heat-insulating felt. Mixing nano silicon dioxide, an organic binding agent, a water repellent and water to prepare silicon dioxide mucilage, impregnating a glass fiber felt with the mucilage, and then performing filter pressing and microwave drying; after the treatment, the nano silicon dioxide, the bonding agent and the water repellent are uniformly distributed in the fibrofelt, and the bonding agent is dried to form a film to bond the fibers and the nano silicon dioxide, so that the bonding strength of the fibers in the felt body is improved; the nano silicon dioxide is more uniformly distributed in the felt body in a microwave drying mode, so that the nano silicon dioxide can play a role in reducing convection heat transfer to the maximum extent, the heat conductivity coefficient is reduced, and the product strength is improved; in addition, the water repellent reacts with silicon hydroxyl on the surface of the fiber, so that the surface of the fiber is connected with organic functional groups with hydrophobicity, and the hydrophobicity of the fiber felt can be obviously improved.
Test results show that the average thermal conductivity coefficient at 25 ℃ of the prepared glass fiber nano-pore thermal insulation felt is less than 0.026W/(m.k), the average thermal conductivity coefficient at 300 ℃ is less than 0.05W/(m.k), and the prepared glass fiber nano-pore thermal insulation felt shows excellent thermal insulation performance; the tensile strength is more than 0.3 MPa; the hydrophobic rate is more than 98 percent; the combustion performance reaches A1 level.
Detailed Description
The invention provides a preparation method of a glass fiber nano-pore heat-insulating felt, which comprises the following steps:
a) mixing nano silicon dioxide, an organic binding agent, a water repellent and water to obtain silicon dioxide mucilage;
b) impregnating a glass fiber felt with the silica gel slurry to obtain a wet blank;
c) and carrying out microwave drying after filter pressing on the wet blank to obtain the glass fiber nano-pore heat-insulating felt.
Mixing nano silicon dioxide, an organic binding agent, a water repellent and water to prepare silicon dioxide mucilage, impregnating a glass fiber felt with the mucilage, and then performing filter pressing and microwave drying; after the treatment, the nano silicon dioxide, the bonding agent and the water repellent are uniformly distributed in the fibrofelt, and the bonding agent is dried to form a film to bond the fibers and the nano silicon dioxide, so that the bonding strength of the fibers in the felt body is improved; the nano silicon dioxide is more uniformly distributed in the felt body in a microwave drying mode, so that the nano silicon dioxide can play a role in reducing convection heat transfer to the maximum extent, the heat conductivity coefficient is reduced, and the product strength is improved; in addition, the water repellent reacts with silicon hydroxyl on the surface of the fiber, so that the surface of the fiber is connected with organic functional groups with hydrophobicity, and the hydrophobicity of the fiber felt can be obviously improved.
According to the invention, the nano silicon dioxide, the organic binding agent, the water repellent and the water are mixed to obtain the silicon dioxide mucilage.
In the invention, the nano-silica is preferably one or more of gas-phase nano-silica and sol-gel nano-silica. The preferred bulk density of the nano silicon dioxide is 20-40 kg/m3. The particle size of the nano silicon dioxide is preferably 20-30 nm.
In the present invention, the organic binder is preferably an acrylate emulsion and/or a polyurethane emulsion. Compared with other organic binders such as starch, cellulose and the like, the two types of emulsions have better film forming property, flexibility and the like after being dried, are beneficial to improving the flexibility of the heat-insulating felt product, are not easy to break when being bent, and improve the tensile strength of the heat-insulating felt product. Wherein the solid content of the acrylate emulsion is preferably 52-54%; the viscosity of the acrylate emulsion is preferably 400-1500 mPa.s. The solid content of the polyurethane emulsion is preferably 28-32%; the viscosity of the polyurethane emulsion is preferably 400-600 mPa.s. In the present invention, the source of the organic binder is not particularly limited, and may be any commercially available product. In one embodiment of the present invention, the organic binder is an acrylate emulsion with a solids content of 54% and a viscosity of 1500mpa.s (provided by york sunrise chemical company, inc.). In one embodiment of the invention, the organic binder is an acrylate emulsion having a solids content of 52% and a viscosity of 400mpa.s (provided by the taiwanghua chemical group, inc.). In one embodiment of the present invention, the organic binder is an aqueous polyurethane emulsion model 2536 (provided by the Nicotiana Vanhua chemical group, Inc.).
In the invention, the water repellent is preferably an organosilicon water repellent, and more preferably a hydrogen-containing silicone oil emulsion. Compared with other water repellents, on one hand, the hydrogen-containing silicone oil emulsion can be well mixed with other components in the silica gel slurry system to form a uniform system, so that the gel slurry and various components in the gel slurry are more easily combined with fibers; furthermore, the hydrogen-containing silicone oil emulsion can generate dehydration condensation reaction with silicon hydroxyl on the surface of the glass fiber, so that organic functional groups are formed on the surface of the glass fiber, and the fiber is endowed with good hydrophobic performance, thereby improving the hydrophobic rate of the heat-insulating felt. In the invention, the oil content of the hydrogen-containing silicone oil emulsion is preferably not less than 28%, and more preferably 28% -32%; if the oil content is too low, the hydrophobic effect is poor, and if the oil content is too high, the difficulty of combining the silica gel slurry and the fibrofelt is greatly increased, the properties of the heat insulation felt, such as strength, heat conductivity and the like, are influenced, and the production efficiency of the product is also influenced. In the invention, the oil content refers to the mass ratio of the hydrogen-containing silicone oil to the whole hydrogen-containing silicone oil emulsion. In the present invention, in the hydrogen-containing silicone oil emulsion, the hydrogen content of the hydrogen-containing silicone oil is preferably 1.5% to 2.5%. In the invention, the pH value of the contained hydrogen silicone oil emulsion is preferably 3-4.
In the invention, the mass ratio of the water, the nano silicon dioxide, the organic binder and the water repellent is preferably 100 to (20-25) to (2-3) to (1-2).
In the invention, the mode of mixing the nano silicon dioxide, the organic binding agent, the water repellent and the water is not particularly limited, and all the components can be uniformly mixed; preferably, under the stirring condition, adding the nano silicon dioxide, the organic binding agent and the water repellent into water in sequence, and continuously stirring; the rotation speed of stirring is preferably 1000-1200 rpm, and the time of continuous stirring is preferably 20-30 min. And uniformly mixing to obtain uniform silicon dioxide mucilage. In the present invention, the concentration of silica in the silica gel slurry is preferably 15 wt% to 20 wt%.
According to the invention, after the silica gel is obtained, the glass fiber mat is impregnated with the silica gel to obtain a wet blank.
In the invention, the volume density of the glass fiber felt is preferably 120-140 kg/m3. The diameter of the fibers in the glass fiber mat is preferably 6-8 mu m.
In the present invention, the glass fiber mat is preferably an alkali-free glass fiber mat. The glass fiber felt is preferably a glass fiber needled felt, and more preferably a glass fiber needled felt after calcination treatment. The glass fiber needled felt is a material obtained by needling a carded chopped glass fiber felt by using a needle, and mutually intertwining felt layers by using a mechanical method, wherein a lubricating material such as lubricating grease is usually added in the process of producing glass fibers for facilitating needling. Compared with the fiber felt which is not calcined, the silica gel slurry can be more easily and uniformly soaked in the felt body after calcination treatment, so that the components can better interact, the strength, the heat conduction performance, the hydrophobicity and the like of the heat insulation felt are favorably improved, the organic content of the felt body can be reduced, the combustion performance of the product is improved, and the combustion performance of the heat insulation felt product reaches A1 level. In the invention, the temperature of the calcination treatment is preferably 350-400 ℃; the time of the calcination treatment is preferably 1-2 h.
The invention has no special limitation on the dipping mode of dipping the glass fiber felt by the silica gel slurry, for example, the glass fiber felt can be dipped in the silica gel slurry. The amount of the silica gel is not particularly limited, and the glass fiber mat can be completely immersed in the gel. In the invention, the time for soaking is preferably 10-30 s. The silica gel slurry system is uniform and good in fluidity, and can easily permeate into a fiber felt and be uniformly dispersed, wherein the organic binding agent is dried to form a film, so that the fiber and the nano-silica are bound, and the bonding strength of the fiber in the felt body is improved; the hydrophobic agent reacts with silicon hydroxyl on the surface of the fiber, so that the surface of the fiber is connected with organic functional groups with hydrophobicity, and the hydrophobicity of the fiber felt can be obviously improved. And (3) fully impregnating the glass fiber felt with the silica gel slurry to obtain a wet blank.
According to the invention, after a wet blank is obtained, the wet blank is subjected to pressure filtration and microwave drying to obtain the glass fiber nano-pore heat-insulating felt.
In the invention, after the wet blank is obtained, the wet blank is subjected to filter pressing for thickness setting, and the blank is dehydrated and pressed to a proper thickness through filter pressing. The filter pressing thickness setting mode is not particularly limited, and the filter pressing thickness setting mode can be implemented according to a conventional filter pressing thickness setting flow known to a person skilled in the art. In the invention, the pressure of the filter pressing is preferably 0.2-0.6 MPa. The filter pressing thickness is preferably 3-15 mm.
After filter pressing, microwave drying is carried out. According to the invention, the nano-silica is more uniformly distributed in the felt body through microwave drying, so that the effect of reducing convection heat transfer is exerted to the maximum extent, and the heat conductivity coefficient is reduced. In the invention, the temperature of the microwave drying is preferably 120-150 ℃; the microwave drying time is preferably 2-3 h. And after the microwave drying, obtaining the glass fiber nano-pore heat-insulating felt.
The invention also provides the glass fiber nano-pore heat-insulating felt prepared by the preparation method in the technical scheme. The obtained heat-insulating felt has excellent bonding strength, lower heat conductivity coefficient, higher hydrophobic rate and good combustion performance.
Test results show that the average thermal conductivity coefficient at 25 ℃ of the prepared glass fiber nano-pore thermal insulation felt is less than 0.026W/(m.k), the average thermal conductivity coefficient at 300 ℃ is less than 0.05W/(m.k), and the prepared glass fiber nano-pore thermal insulation felt shows excellent thermal insulation performance; the tensile strength is more than 0.3 MPa; the hydrophobic rate is more than 98 percent; the combustion performance reaches A1 level.
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims. In the following examples, each raw material was a commercially available product, wherein the acrylic ester emulsion in examples 1 to 2 had a solid content of 54% and a viscosity of 1500mpa.s, and was provided by Jiangsu sunrise chemical Co., Ltd; the acrylic ester emulsion in example 3 had a solid content of 52% and a viscosity of 400mpa.s, and was provided by taiwanhua chemical group ltd; the polyurethane emulsion in example 4 was an aqueous polyurethane emulsion having a model number of 2536, which was supplied by Nicotiana Vanhua chemical group Co., Ltd. The oil content of the hydrogen-containing silicone oil emulsion is 28-32%, the PH value is 3-4, and the hydrogen content of the hydrogen-containing silicone oil in the hydrogen-containing silicone oil emulsion is 1.5-2.5%.
Example 1
Weighing 100 parts by weight of water, injecting the water into a glue preparation tank, starting a high-speed dispersion machine, and setting the stirring speed to be 1000 rpm; and (3) taking 20 parts by weight of fumed silica, 2 parts by weight of acrylate emulsion and 2 parts by weight of hydrogen-containing silicone oil emulsion, slowly adding the materials into a dispersion machine in sequence, and stirring for 30min to obtain the silica mucilage with the concentration of 16.13%.
The thickness is 12mm, the volume weight is 120kg/m3The alkali-free glass fiber mat is calcined by a calcining furnace at 350 ℃ for 2 hours to remove the lubricating grease inside. Conveying the calcined fibrofelt into a slurry dipping pool to be soaked for 30 seconds(ii) a And conveying the wet blank obtained by soaking to a position below a stainless steel compression roller with the diameter of 80mm through a mesh belt, performing filter pressing for thickness setting, wherein the pressure is 0.6MPa, and controlling the thickness of the blank to be 10mm after filter pressing and dehydration.
And conveying the blank subjected to filter pressing and dehydration to a continuous microwave oven for drying at the temperature of 120 ℃ for 3 hours to obtain the glass fiber nano-pore heat-insulating felt.
Example 2
Weighing 100 parts by weight of water, injecting the water into a glue preparation tank, starting a high-speed dispersion machine, and setting the stirring speed to be 1200 rpm; and (3) taking 25 parts by weight of fumed silica, 3 parts by weight of acrylate emulsion and 1 part by weight of hydrogen-containing silicone oil emulsion, slowly adding the materials into a dispersion machine in sequence, and stirring for 30min to obtain the silica mucilage with the concentration of 19.38%.
The thickness is 10mm, the volume weight is 140kg/m3The alkali-free glass fiber mat of (1) was calcined at 400 ℃ for 1 hour by a calcining furnace to remove the grease from the inside. Conveying the calcined fibrofelt into a slurry dipping pool to be dipped for 30 seconds; and conveying the wet blank obtained by soaking to a position below a stainless steel compression roller with the diameter of 90mm through a mesh belt, performing filter pressing for thickness setting, wherein the pressure is 0.2MPa, and controlling the thickness of the blank to be 9mm after filter pressing and dehydration.
And conveying the blank subjected to filter pressing and dehydration to a continuous microwave oven for drying at the temperature of 150 ℃ for 2 hours to obtain the glass fiber nano-pore heat-insulating felt.
Example 3
Weighing 100 parts by weight of water, injecting the water into a glue preparation tank, starting a high-speed dispersion machine, and setting the stirring speed to be 1100 rpm; and (3) taking 23 parts by weight of fumed silica, 3 parts by weight of acrylate emulsion and 2 parts by weight of hydrogen-containing silicone oil emulsion, slowly adding the materials into a dispersion machine in sequence, and stirring for 25min to obtain the silica mucilage with the concentration of 18.00%.
The thickness is 5mm, the volume weight is 130kg/m3The alkali-free glass fiber mat of (1) was calcined at 380 ℃ for 1.5 hours by a calciner to remove the grease from the inside. Conveying the calcined fibrofelt into a slurry dipping pool to be dipped for 10 seconds; conveying the wet blank obtained by soaking to a position below a PP compression roller with the diameter of 80mm through a mesh belt to perform filter pressing for thickness setting, wherein the pressure is 0.4MPa, and the filter pressing is performedControlling the thickness of the blank to be 3mm after dehydration.
And conveying the blank subjected to filter pressing and dehydration to a continuous microwave oven for drying at the temperature of 140 ℃ for 2.5 hours to obtain the glass fiber nano-pore heat-insulating felt.
Example 4
Weighing 100 parts by weight of water, injecting the water into a glue preparation tank, starting a high-speed dispersion machine, and setting the stirring speed to be 1100 rpm; and (3) taking 23 parts by weight of fumed silica, 3 parts by weight of polyurethane emulsion and 2 parts by weight of hydrogen-containing silicone oil emulsion, slowly adding the materials into a dispersion machine in sequence, and stirring for 25min to obtain the silica mucilage with the concentration of 18.00%.
The thickness is 5mm, the volume weight is 130kg/m3The alkali-free glass fiber mat of (1) was calcined at 380 ℃ for 1.5 hours by a calciner to remove the grease from the inside. Conveying the calcined fibrofelt into a slurry dipping pool to be dipped for 10 seconds; and conveying the wet blank obtained by soaking to a position below a PP compression roller with the diameter of 80mm through a mesh belt, performing filter pressing for thickness setting, wherein the pressure is 0.4MPa, and controlling the thickness of the blank to be 3mm after filter pressing and dehydration.
And conveying the blank subjected to filter pressing and dehydration to a continuous microwave oven for drying at the temperature of 140 ℃ for 2.5 hours to obtain the glass fiber nano-pore heat-insulating felt.
Comparative example 1
The insulation felt was prepared according to the method disclosed in CN105599396A, specifically as follows:
A) preparation of the glass fiber layer: cutting the glass fiber into short glass fiber with the length of 60mm, then adding a swelling agent for opening, and carding the fluffy short glass fiber into single fibers by a carding machine to obtain a felt net layer; conveying the felt net layers to a lapping machine for laminating, wherein the stacking height is 1 mm; finally, needling is carried out to obtain the product;
B) preparing fine aerogel powder:
sol-gel: mixing 10ml of industrial water glass with the modulus of 4.0 and the mass concentration of 34% and 80ml of deionized water in a beaker, stirring for 10min to obtain silica sol, adding 0.5mol/ml of ammonia water into the silica sol to adjust the pH to 7.5, adding 0.5ml of formamide, and stirring for 5min to obtain SiO2 hydrogel;
aging: aging the SiO2 hydrogel obtained in the above step at 35 deg.C for 4h, placing in ethanol solution, and aging at 50 deg.C for 24 h;
and (3) solvent fractional replacement: firstly, placing the SiO2 hydrogel obtained in the step into a mixed solution consisting of an ethanol solution and n-hexane for displacement for 2 times, and each time for 5 hours to obtain first-stage displacement SiO2 hydrogel, wherein the volume ratio of the ethanol solution to the n-hexane in the mixed solution is 2: 1; placing the first-stage replacement SiO2 hydrogel in a mixed solution composed of ethanol and n-hexane for replacement for 2 times, wherein each time is 4 hours, so as to obtain a second-stage replacement SiO2 hydrogel, and the volume ratio of the ethanol solution to the n-hexane in the mixed solution is 1: 1; placing the second-stage replacement SiO2 hydrogel in n-hexane solution for replacement for 2 times, and each time for 5 hours to obtain third-stage replacement SiO2 hydrogel;
surface modification treatment: placing the three-stage replacement SiO2 hydrogel in a mixed solution of polyethylene glycol and trimethylchlorosilane in a volume ratio of 1.2:0.3 for surface modification, and cleaning for 6 hours by using a mixed solution of an ethanol solution and n-hexane in a volume ratio of 1:2 after modification;
drying under normal pressure: drying the three-level replacement SiO2 hydrogel treated in the steps at 60 ℃ for 5 hours, then drying at 150 ℃ for 2 hours to obtain aerogel particles, and crushing the aerogel particles into fine powder of 200 meshes for later use;
C) preparing aerogel felt: laying an insulating cloth layer on a coating machine, and laying a glass fiber layer prepared in the step A) on the insulating cloth; uniformly spraying the aerogel fine powder prepared in the step B) on the glass fiber layer to form an aerogel powder layer with the thickness of 1 mm; laying a glass fiber layer on the aerogel powder layer; then evenly spraying the aerogel fine powder on the glass fiber layer to form another aerogel powder layer; continuously circulating the operation to lay 10 composite heat insulating layers, and covering a heat insulating cloth layer after the laying is finished; and (3) conveying the materials to a roller press, and rolling to obtain the aerogel felt with the thickness of 2 cm.
Comparative example 2
The heat insulating felt is prepared according to the preparation method disclosed in CN105209248A, and concretely comprises the following steps:
a polyester laid scrim (5x 5/inch, SG adhesives Dewtex) was placed at the bottom of the mixing tank and the tank was filled with 24 liters of tap water. In a separate blender (
Figure BDA0001879598060000093
Type CB10B), 12g of microfibers B-06 borosilicate glass fibers (Lauscha) were combined with
Figure BDA0001879598060000094
12 wetting agent (lauryl dimethyl amine oxide) and
Figure BDA0001879598060000091
830F silicone antifoam was mixed and the blend was filled 2/3 with tap water. The mixture was blended at low speed for 40 seconds and added to the mixing tank. Aerogel particles were prepared by the following method: 25g of P200 aerogel particles having an average particle size of 1mm (Cabot Corp) were mixed with
Figure BDA0001879598060000092
7768 viscosity modifier (anionic polyacrylamide), 3g Barlox 12i wetting agent and 3g Foamkill830F defoamer. Sufficient water was added to the blender to fill the blender to about 2/3 and the mixture was blended at low speed for 15 seconds. Then 12g of the IR opacifier titanium dioxide (0.8 to 3 μm rutile sand) was added to the same blender and the entire mixture was blended at low speed for 30 seconds. The resulting aerogel/sunscreen dispersion was then added to the mixing tank. Then, by mixing
Figure BDA0001879598060000101
The PSR 300 acrylic polymer latex is added to the mixing tank, and a charged compound, which also acts as a binder, is added to the dispersion of fibers and aerogel. The entire slurry was mixed thoroughly for one minute and a milky white emulsion clearly existed throughout the slurry tank. To destabilize the system, polyamine coagulants are added
Figure BDA0001879598060000102
c 573(Kemira) was added dropwise to the mixing tank until a clear supernatant was visible in the corner of the mixing tank. This occurred after about 3g of coagulant was added to the slurry emulsion. After flocculation, the discharge at the bottom of the mixing tank was opened, allowing the supernatant to drain through the scrim. The majority of the floe is retained by the scrim and eventually distributed throughout. The scrim is then subjected to a vacuum to remove additional water from the aerogel floe. The wire rolls are then rolled over the upper surface of the floc/scrim to soften the irregularities and smooth the surface. The mat was placed in a drying oven at 150 ℃ for one hour until the mat was dry to the touch but not brittle.
Example 5
The heat-insulating felt obtained in examples 1 to 4 and comparative examples 1 to 2 was tested for bulk density, normal temperature thermal conductivity, average 300 ℃ thermal conductivity, tensile strength, combustion performance, and water repellency, respectively, and the test results are shown in table 1.
TABLE 1 Performance test results of examples 1 to 4 and comparative examples 1 to 2
Figure BDA0001879598060000103
From the test results, the thermal conductivity coefficient of the thermal insulation felt at the average temperature of 25 ℃ is less than 0.026W/(m.k), and the thermal conductivity coefficient of the thermal insulation felt at the average temperature of 300 ℃ is less than 0.05W/(m.k); the tensile strength is more than 0.3 MPa; the hydrophobic rate is more than 98 percent; the combustion performance reaches A1 level; all performance indexes of the composite material are obviously superior to those of a comparative example 1 and a comparative example 2, and the composite material shows excellent heat insulation performance, strength, hydrophobic performance and combustion performance.
Example 6
(1) The thermal insulation felt of example 3 and the thermal insulation felt of comparative example 1 were subjected to a vibration test (simulating vibration during transportation and construction) with a vibration frequency of 120 times/min for 100 min; each sample was then tested for thermal conductivity (example 3 treated sample was designated S3-1 and comparative example 1 treated sample was designated D1-1) with the results shown in Table 2.
(2) Respectively carrying out high-temperature treatment (simulating the high-temperature working environment of the heat-insulating felt) on the heat-insulating felt of the example 3 and the heat-insulating felt of the comparative example 2 at the temperature of 600 ℃ for 30 min; each sample was then tested for tensile strength (example 3 treated sample was designated S3-2 and comparative example 2 treated sample was designated D2-2), with the results of the tests being shown in Table 2.
Table 2 results of performance testing of example 6
Figure BDA0001879598060000111
Comparing the thermal conductivity of the samples S3-1 and D1-1 with that of the samples of example 3 and comparative example 1, it can be seen that after the vibration test, the thermal conductivity of the sample S3-1 is equivalent to that of the sample of example 3, while the thermal conductivity of the sample of comparative example 1 is obviously increased, namely the thermal conductivity is greatly reduced; it can be seen that the thermal insulation performance of the sample of comparative example 1 was greatly impaired after vibration of transportation and construction, and the thermal insulation felt of the present invention was still able to maintain high thermal insulation performance.
Comparing the tensile strengths of the samples S3-2 and D2-2 with those of the example 3 and the comparative example 2, it can be seen that the tensile strength of the sample S3-2 is equivalent to that of the example 3, while the tensile strength of the comparative example 2 is obviously reduced after the high temperature treatment; it can be seen that the strength of the comparative example 2 sample was severely attenuated when used in a high temperature environment, while the thermal insulation blanket of the present invention was still able to maintain high tensile strength. It can be seen from the above tests that the thermal insulation felt of the present invention has not only high thermal insulation performance, strength performance, etc., but also better performance stability.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (4)

1. A preparation method of a glass fiber nano-pore heat-insulating felt is characterized by comprising the following steps:
a) mixing nano silicon dioxide, an organic binding agent, a water repellent and water to obtain silicon dioxide mucilage;
b) impregnating a glass fiber felt with the silica gel slurry to obtain a wet blank;
c) carrying out filter pressing on the wet blank, and then carrying out microwave drying to obtain a glass fiber nano-pore heat-insulating felt;
the bulk density of the nano silicon dioxide is 20-40 kg/m3The granularity is 20-30 nm;
the organic binder is acrylate emulsion and/or polyurethane emulsion;
the solid content of the acrylate emulsion is 52-54%, and the viscosity is 400-1500 mPa.s;
the solid content of the polyurethane emulsion is 28-32%, and the viscosity is 400-600 mPa.s;
the water repellent is hydrogen-containing silicone oil emulsion;
the oil content of the hydrogen-containing silicone oil emulsion is 28-32 percent;
the microwave drying temperature is 120-150 ℃, and the time is 2-3 h;
in the step a), the mass ratio of water, nano silicon dioxide, organic binder and water repellent is 100: 20-25: 2-3: 1-2;
the glass fiber felt is a calcined glass fiber needled felt;
the temperature of the calcination treatment is 350-400 ℃, and the time is 1-2 h.
2. The method according to claim 1, wherein the hydrogen content of the hydrogen-containing silicone oil in the hydrogen-containing silicone oil emulsion is 1.5% to 2.5%.
3. The method according to claim 1, wherein the concentration of silica in the silica gel slurry is 15 to 20 wt%.
4. The glass fiber nano-pore heat insulation felt prepared by the preparation method of any one of claims 1 to 3.
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