CN113683343A - High-flexibility aerogel felt and preparation method thereof - Google Patents
High-flexibility aerogel felt and preparation method thereof Download PDFInfo
- Publication number
- CN113683343A CN113683343A CN202111033703.0A CN202111033703A CN113683343A CN 113683343 A CN113683343 A CN 113683343A CN 202111033703 A CN202111033703 A CN 202111033703A CN 113683343 A CN113683343 A CN 113683343A
- Authority
- CN
- China
- Prior art keywords
- felt
- water
- gel
- silica
- wet gel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/04—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/10—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B26/14—Polyepoxides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/52—Sound-insulating materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to a preparation method of aerogel felt, which comprises the steps of attaching a water-absorbing expansion type adhesive to the surface of a fiber felt body, then combining silica sol catalyzed by a gel catalyst with the fiber felt, carrying out gelation to form a silica wet gel felt, and then carrying out drying treatment; the water-absorbing expansion type resin absorbs water and expands in the gelation process of the silica sol to generate cracks among gel pore structures, the introduction of the cracks enables the gel in the silica gel felt to deform, the flexibility of the aerogel can be improved, and the aerogel felt can be used as a flexible thermal insulation material or a flexible sound absorption material.
Description
Technical Field
The invention relates to a preparation method of an aerogel felt, in particular to a high-flexibility anti-dusting aerogel felt and a preparation method thereof.
Background
The silica aerogel is a continuous three-dimensional network structure formed by mutually polymerizing nano-scale particles, and the thermal conductivity efficiency, the convection heat transfer efficiency and the radiation heat transfer efficiency of the silica aerogel are effectively limited due to the special nano-scale micropores and a skeleton structure, so that the silica aerogel has very low thermal conductivity coefficient and is a solid material with the lowest thermal conductivity coefficient in the world at present.
Generally, aerogels are obtained by preparing a hydrogel from a silica precursor such as water glass or Tetraethylorthosilicate (TEOS) and removing the liquid component from the hydrogel without destroying the microstructure. Silica aerogels include three conventional forms of powder, granule and monolith. The aerogel felt or aerogel sheet is prepared by compounding the silica aerogel and the fibers, and is applied to the fields of industrial heat preservation and the like.
However, the largest disadvantage of aerogel in practical application is that dust is generated, and the adhesion between aerogel and felt is weak, so that the felt is separated from aerogel in use. At present, most of the existing powder falling prevention schemes adopt glass fiber cloth, aluminum foil cloth and the like to be pasted on the surface of aerogel felt, the flexibility of products produced in the mode is reduced, the products are not easy to curl and bend, and the products are not suitable for heat insulation and sound absorption materials requiring flexible forms.
Patent CN107735385A discloses a method for preparing aerogel felt with low dust and high thermal insulation, which uses acid to etch the surface of felt body, activates the surface of felt body to improve the adhesion with silica aerogel, and improves the mechanical flexibility of aerogel itself by repeating the gel deformation process of winding the felt body impregnated with silica gel along a cylinder to introduce cracks into silica gel to reduce the generation of dust. However, the felt body is etched with acid, and the felt body needs to be washed many times after etching, which results in a long production period, an increase in production cost, and environmental pollution.
Disclosure of Invention
The invention aims to provide a preparation method of a high-flexibility aerogel felt, which is used for solving the technical problem of powder falling of the aerogel felt with poor flexibility at present.
The preparation method of the high-flexibility aerogel felt adopts the following technical scheme:
a) attaching a water-absorbing and expanding type adhesive to the surface of the fiber felt body;
b) combining the fiber felt with the water-absorbing expansion type adhesive attached to the surface with silica sol catalyzed by a gel catalyst, and gelling the fiber felt and the catalyzed silica sol to form a silica wet gel felt;
c) the silica wet gel mat is dried.
Has the advantages that: in the preparation method, the water-absorbing expansion type adhesive is attached to the surface of the felt body to improve the adhesion between the felt body and the silica gel, so that the adhesion between aerogel particles and the felt body is improved, the generation of aerogel dust can be reduced, and the problem of powder falling caused by the separation of aerogel and the felt body when the aerogel felt is used can be effectively solved; after the adhesive is formed into a film, the aerogel powder compounded by the felt body is sealed to reduce the powder falling condition of the aerogel powder; the expansion type resin expands in the gelation process of the silica sol to generate cracks among gel hole structures, the introduction of the cracks enables the gel in the silica gel felt to deform, the flexibility of the aerogel can be improved, the mechanical flexibility of the aerogel felt is further improved, the aerogel felt is used as a flexible thermal insulation material or a sound absorption material, and the high-flexibility aerogel felt can relieve the powder falling problem when the aerogel felt is bent for use.
Further, the attaching of the water-swellable adhesive to the surface of the fibrous felt body includes applying a water-swellable resin to the surface of the fibrous felt body or spraying a water-swellable resin to the surface of the fibrous felt body.
Further, in the step a), the water-absorbing and expanding type adhesive is preferably styrene-butadiene emulsion, the styrene-butadiene emulsion is obtained by copolymerizing butadiene and styrene monomers and has good adhesive force and adhesive force, both butadiene and styrene are hydrophobic monomers, the prepared styrene-butadiene emulsion is a hydrophobic polymer and has water resistance, the styrene-butadiene emulsion has the flexibility of rubber and has lower water absorption and water-absorbing expansion rate, the styrene-butadiene emulsion can be cured to form a film after being kept at 30-70 ℃ for 4-24 h, the styrene-butadiene emulsion is used as the water-absorbing and expanding type adhesive, the styrene-butadiene emulsion is coated or sprayed on the surface of a fiber felt body and is combined with silica sol catalyzed by a gel catalyst before being cured to form a film, the water resistance of the styrene-butadiene emulsion avoids that water in the silica sol influences the adhesive performance, the water absorption of the styrene-butadiene emulsion for 1 day is lower than 2%, the water absorption of the styrene-butadiene emulsion used in the application has low influence on the silica gel reaction due to the water absorption of the adhesive, the styrene-butadiene latex with low water swelling rate swells in the gel to introduce cracks between the pore structures of the silica gel and avoid collapse of the pore structures of the silica gel caused by excessive swelling.
Further, in the step a), the water-swellable adhesive is formed by mixing an adhesive and a water-swellable swelling agent, wherein the adhesive is liquid epoxy resin, the liquid epoxy resin is liquid epoxy resin added with a curing agent, and the swelling agent is nano magnesium oxide. The nano magnesium oxide is added into liquid epoxy resin to be mixed as a water-absorbing expansion type adhesive, the liquid epoxy resin mixed with the nano magnesium oxide is coated or sprayed on the surface of a fibrofelt body, the liquid epoxy resin is combined with silica sol catalyzed by a gel catalyst before the liquid epoxy resin is cured into a film, and the nano magnesium oxide reacts with water to generate magnesium hydroxide, so that volume expansion is generated and cracks are introduced between pore structures of the silica gel. Heating 15-30 parts of sodium alginate to 50-65 ℃, preserving heat for 15-30min, slowly adding 5-10 parts of polytetrafluoroethylene and 5-10 parts of chitosan in the process of preserving heat, uniformly stirring, cooling to room temperature, adding 25-40 parts of nano magnesium oxide, and uniformly stirring. Sodium alginate is used as a film forming agent, a mixture of chitosan and polytetrafluoroethylene soluble film is formed on the surface of the nano magnesium oxide, the thickness of the soluble film can be adjusted by adjusting the part ratio, the reaction expansion time of the nano magnesium oxide and water is controlled, and the time for introducing cracks in the silica wet gel is better controlled.
Further, in the step a), the fibers in the fiber mat are one or a combination of two or more of the following fiber materials: quartz fibers, glass fibers, high silica fibers, carbon fibers, pre-oxidized fiber, mullite fibers, basalt fibers, silicon carbide fibers, silicon nitride fibers, alumina fibers, and boron nitride fibers. The fiber in the fiber felt is preferably one or the combination of more than two of glass fiber, high silica fiber or pre-oxidized fiber.
In the step a), the fiber felt comprises a sheet felt in a sheet shape and a rolling felt formed by rolling a continuous felt body.
Further, in the step b), the silica sol catalyzed by the gel catalyst is prepared by adding the gel catalyst into the silica sol; the silica sol is prepared by mixing a silicon source, ethanol and water in a molar ratio of 1 to (2-60) to (1-30); the silicon source is one or more than two of ethyl orthosilicate, methyl orthosilicate, butyl orthosilicate, isopropyl orthosilicate or alkyl alkoxy silane; the alkyl alkoxy silane comprises one or more than two of methyl trimethoxy silane, dimethyl dimethoxy silane, methyl triethoxy silane, dimethyl diethoxy silane, vinyl triethoxy silane, propyl trimethoxy silane or propyl triethoxy silane; the gel catalyst is one or two of alkaline catalyst such as sodium hydroxide, potassium hydroxide, ammonia water and ammonium fluoride aqueous solution; the gel catalyst adjusts the pH of the silica sol to 6-8.
Further, in the step b), the preparation of the silica sol further comprises adding an acidic catalyst for catalyzing a sol reaction, wherein the acidic catalyst adjusts the pH of the mixed solution of the silicon source, the ethanol and the water to 2-6, and the mixed solution is catalyzed by the acidic catalyst to form the silica sol.
Further, the acidic catalyst is one or a combination of more than two of sulfuric acid, hydrochloric acid, hydrofluoric acid, oxalic acid, acetic acid or benzenesulfonic acid.
Further, in the step b), the silica sol catalyzed by the gel catalyst is combined with the fiber felt with the water-absorbing and expanding type binder attached to the surface, generally adopting: the first method is as follows: the catalyzed silica sol is immersed into the fiber mat in a spray form, or mode two: and (3) placing the catalyzed silica sol into a dipping tank, and dipping the fiber felt into the dipping tank to dip the catalyzed silica sol into the fiber felt.
Further, the step b) also comprises an aging step, wherein the silica wet gel felt is kept at the temperature of 30-70 ℃ for 4-24 hours, more Si-O-Si bonds can be formed in the aging step, the formed gel network structure of the wet gel is more stable, the maintenance of the pore structure in the subsequent drying process is promoted, and the mechanical stability of the aerogel felt is improved. Aging is performed in a proper temperature range to enhance the optimum pore structure, and when the aging temperature is lower than 30 ℃, the aging time is lengthened, and when the aging temperature is higher than 70 ℃, the temperature exceeds the boiling point of ethanol, and evaporation is caused to cause solvent loss.
Further, the silica wet gel felt obtained by the step b) is subjected to surface hydrophobic modification treatment before the step c). The surface of the wet gel contains a large number of hydrophilic groups, the hydrophilic groups are replaced by hydrophobic groups in the modification process of the surface of the wet gel, and the hydrophobic modification can relieve the problems of gel framework shrinkage caused in the drying process of the aerogel and moisture absorption from the environment in the use process. Surface-hydrophobization modification, surface modification is carried out using an organosilane compound including trimethylchlorosilane, hexamethyldisilazane, methyltrimethoxysilane, trimethylethoxysilane, ethyltriethoxysilane, phenyltriethoxysilane, etc. Mixing an organosilane compound with ethanol in a molar ratio of 1: 2-1: 5 mixing to obtain a modified solution, and soaking the wet gel felt in the modified solution for modification. And (3) washing for 1-2 times after modification, wherein the washing is used for removing impurities such as unreacted products and byproducts generated in the modification reaction process.
Further, the step c) further comprises solvent replacement, wherein the wet gel felt is subjected to solvent replacement for 1-3 times and then dried, and a nonpolar organic solvent is used for replacing alcohol and water in the pore structure of the wet gel felt in the solvent replacement. The nonpolar organic solvent is usually mixed liquid of normal hexane and ethanol, the wet gel felt is placed in the mixed liquid for dipping and replacement, dipping is carried out for 4-6 hours, and solvent replacement is repeated for 1-3 times. Drying is carried out by removing the solvent within the pore structure while maintaining the pore structure of the aged silica gel, typically by supercritical drying or atmospheric drying processes.
In addition, the invention also provides the aerogel felt prepared by the method. The aerogel felt prepared by the method has high flexibility, and when the aerogel felt is used as a flexible thermal insulation material or a sound absorption material, the problem of powder falling caused by separation of aerogel and a felt body can be effectively relieved, so that the aerogel felt is a high-flexibility aerogel felt.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1:
the invention provides a preparation method of a high-flexibility aerogel felt, which comprises the following steps:
1) attaching a water-swellable adhesive to the surface of the fibrous felt body: the fiber felt is a glass fiber roll felt, the fiber felt is unreeled and is conveyed by a conveying device, the surface of the fiber felt is coated with the butylbenzene emulsion, and the butylbenzene emulsion is used as a water-absorbing expansion type adhesive.
2) Preparation of wet gel felt with silica wet gel bonded: uniformly mixing a silicon source, ethanol and water, wherein the molar ratio of the silicon source to the ethanol to the water is = 1: 6: 2, the silicon source is tetraethoxysilane, then sequentially adding a gel catalyst to make the pH of the solution be 7, the gel catalyst is ammonia water, uniformly stirring to obtain a catalyzed silica sol, continuously inputting the catalyzed silica sol into a gel storage tank, conveying a fibrofelt with butylbenzene emulsion attached to the surface by a conveying device into the gel storage tank to be impregnated with the catalyzed silica sol, combining the fibrofelt with the butylbenzene emulsion attached to the surface with the silica sol catalyzed by the gel catalyst before the butylbenzene emulsion is cured to form a film, conveying the fibrofelt with the butylbenzene emulsion attached to the surface by the conveying device after impregnation and gelling the silica sol on the conveying device to form a silica wet gel felt, rolling the silica wet gel felt at the tail end of the conveying device, standing and keeping the silica wet gel felt at 30 ℃ for 24 hours for aging, the styrene-butadiene emulsion is gradually solidified into a film in the aging process, and cracks are formed between gel pore structures due to the fact that the styrene-butadiene emulsion absorbs water and expands in the sol gelation and aging processes.
3) Carrying out surface hydrophobization modification on the silicon dioxide wet gel felt after the crack is introduced, mixing hexamethyldisilazane and absolute ethyl alcohol according to a molar ratio of 1:5 to form a modification solution, soaking the silicon dioxide wet gel felt in the modification solution, and washing the silicon dioxide wet gel with the absolute ethyl alcohol after the soaking is finished so as to remove impurities generated in the modification reaction process.
4) And (3) carrying out solvent replacement on the silica wet gel felt for 3 times, then carrying out drying treatment, mixing normal hexane and ethanol, placing the silica wet gel felt in the mixed solution for soaking for 6 hours, taking out the silica wet gel felt after the soaking is finished, drying the silica wet gel felt by adopting supercritical drying, and drying to obtain the silica aerogel felt with high flexibility.
Example 2:
a method of making a highly flexible aerogel blanket comprising:
1) attaching a water-swellable adhesive to the surface of the fibrous felt body: the fiber felt is a glass fiber sheet felt, the surface of the fiber felt is coated with the butylbenzene emulsion, and the butylbenzene emulsion is used as a water-absorbing expansion type adhesive.
2) Preparation of wet gel felt with silica wet gel bonded: uniformly mixing a silicon source, ethanol and water according to a molar ratio of the silicon source to the ethanol to the water = 1: 10: 4, the silicon source is methyl orthosilicate, then gel catalyst is added in sequence to ensure that the pH value of the solution is 6, the gel catalyst is ammonium fluoride, the gel catalyst is uniformly stirred to obtain catalyzed silica sol, the catalyzed silica sol is placed in a gel storage tank, placing the fibrofelt with the butylbenzene emulsion attached to the surface into a glue storage tank, dipping the catalyzed silica sol, combining the fibrofelt with the butylbenzene emulsion attached to the surface with the silica sol catalyzed by a gel catalyst before the butylbenzene emulsion is cured to form a film, and forming a silica wet gel felt after the silica sol is gelatinized, and the silica wet gel felt is kept standing for 5 hours at 50 ℃ for aging, the butylbenzene emulsion is gradually solidified into a film in the aging process, the styrene-butadiene emulsion absorbs water to expand in the sol gelation and aging processes to form cracks among gel pore structures.
3) Carrying out surface hydrophobization modification on the silicon dioxide wet gel felt after the crack is introduced, mixing trimethylchlorosilane and absolute ethyl alcohol according to a molar ratio of 1:2 to form a modification solution, soaking the silicon dioxide wet gel felt in the modification solution, and washing the silicon dioxide wet gel with the absolute ethyl alcohol after the soaking is finished so as to remove impurities generated in the modification reaction process.
4) And (3) carrying out solvent replacement on the silica wet gel felt for 1 time, then carrying out drying treatment, mixing normal hexane and ethanol, placing the silica wet gel felt in the mixed solution for soaking for 5 hours, taking out the silica wet gel felt after the soaking is finished, drying the silica wet gel felt by adopting supercritical drying, and drying to obtain the silica aerogel felt with high flexibility.
Example 3:
a method of making a highly flexible aerogel blanket comprising:
1) attaching a water-swellable adhesive to the surface of the fibrous felt body: the fiber felt is pre-oxidized fiber sheet felt, the surface of the fiber felt is coated with styrene-butadiene emulsion, and the styrene-butadiene emulsion is used as a water-absorbing expansion type adhesive.
2) Preparation of wet gel felt with silica wet gel bonded: mixing tetraethoxysilane, ethanol and water uniformly, wherein the molar ratio of tetraethoxysilane: ethanol: water = 1: 35: 30, of a nitrogen-containing gas; adding sulfuric acid to enable the pH to be 5, uniformly stirring to form silicon dioxide sol, then sequentially adding an ammonium fluoride solution and ammonia water, and uniformly stirring, wherein the molar ratio of ammonium fluoride to tetraethoxysilane is ammonium fluoride: tetraethoxysilane = 0.01: 1, adding amount of ammonia water in molar ratio: tetraethoxysilane = 0.015: 1, adjusting the pH value of the solution to 7 to obtain silica sol catalyzed by a gel catalyst, placing the catalyzed silica sol in a gel storage tank, placing a fiber felt with styrene-butadiene emulsion attached to the surface in the gel storage tank to be soaked in the catalyzed silica sol, combining the fiber felt with the styrene-butadiene emulsion attached to the surface with the silica sol catalyzed by the gel catalyst before the styrene-butadiene emulsion is cured to form a film, standing the silica sol at 70 ℃ for 4 hours for aging, gradually curing the styrene-butadiene emulsion to form a film in the aging process, and forming cracks between gel pore structures due to the expansion of the styrene-butadiene emulsion in the gelation and aging processes of the sol.
3) Carrying out surface hydrophobization modification on the silicon dioxide wet gel felt after the crack is introduced, mixing hexamethyldisilazane and absolute ethyl alcohol according to a molar ratio of 1:3 to form a modification solution, soaking the silicon dioxide wet gel felt in the modification solution, and washing the silicon dioxide wet gel with the absolute ethyl alcohol after the soaking is finished so as to remove impurities generated in the modification reaction process.
4) And (3) carrying out solvent replacement on the silica wet gel felt for 3 times, then carrying out drying treatment, mixing normal hexane and ethanol, placing the silica wet gel felt in the mixed solution for soaking for 4 hours, taking out the silica wet gel felt after the soaking is finished, drying the silica wet gel felt by adopting supercritical drying, and drying to obtain the silica aerogel felt with high flexibility.
Example 4:
a method of making a highly flexible aerogel blanket comprising:
1) attaching a water-swellable adhesive to the surface of the fibrous felt body: the fiber felt is high silica fiber rolled felt, the fiber felt is rolled and conveyed by a conveying device, the surface of the fiber felt is coated with butylbenzene emulsion, and the butylbenzene emulsion is used as a water-absorbing expansion type adhesive.
2) Preparation of wet gel felt with silica wet gel bonded: uniformly mixing a silicon source, ethanol and water, wherein the molar ratio of the silicon source to the ethanol to the water is = 1: 60: 10, the silicon source is methyltriethoxysilane, then sequentially adding a gel catalyst to make the pH of the solution be 8, the gel catalyst is ammonia water, uniformly stirring to obtain a catalyzed silica sol, continuously inputting the catalyzed silica sol into a gel storage tank, conveying a fibrofelt with butylbenzene emulsion attached to the surface by a conveying device into the gel storage tank to be impregnated with the catalyzed silica sol, combining the fibrofelt with the butylbenzene emulsion attached to the surface with the silica sol catalyzed by the gel catalyst before the butylbenzene emulsion is cured to form a film, conveying the fibrofelt with the butylbenzene emulsion attached to the surface by the conveying device after impregnation to be gelatinized on the conveying device to form a silica wet gel felt, rolling the silica wet gel felt at the tail end of the conveying device, standing the silica wet gel felt at 50 ℃ for 20 hours for aging, the styrene-butadiene emulsion is gradually solidified into a film in the aging process, and cracks are formed between gel pore structures due to the fact that the styrene-butadiene emulsion absorbs water and expands in the sol gelation and aging processes.
3) Carrying out surface hydrophobization modification on the silicon dioxide wet gel felt after the crack is introduced, mixing hexamethyldisilazane and absolute ethyl alcohol according to a molar ratio of 1:3 to form a modification solution, soaking the silicon dioxide wet gel felt in the modification solution, and washing the silicon dioxide wet gel with the absolute ethyl alcohol after the soaking is finished so as to remove impurities generated in the modification reaction process.
4) And (3) carrying out solvent replacement on the silica wet gel felt for 1 time, then carrying out drying treatment, carrying out solvent replacement by adopting ethanol, soaking the silica wet gel felt in the ethanol for 6 hours, taking out the silica wet gel felt after the soaking is finished, drying the gel felt by adopting supercritical drying, and drying to obtain the silica aerogel felt with high flexibility.
Example 5:
a method of making a highly flexible aerogel blanket comprising:
1) attaching a water-swellable adhesive to the surface of the fibrous felt body: the fiber mat is a glass fiber mat, 15 parts of sodium alginate by mass are heated to 55 ℃, the temperature is kept for 30min, 5 parts of polytetrafluoroethylene and 6 parts of chitosan are slowly added in the heat preservation process, the mixture is uniformly stirred, and after the mixture is cooled to the room temperature, 15 parts of nano magnesium oxide is added and uniformly stirred, so that the water-swelling expanding agent is prepared; and then mixing an expanding agent with liquid epoxy resin, wherein the liquid epoxy resin is added with a curing agent, mixing 150 parts by mass of the liquid epoxy resin with 30 parts by mass of the expanding agent to prepare a water-absorbing expansion type adhesive, and spraying the water-absorbing expansion type adhesive on the surface of the fiber felt in a spraying manner.
2) Preparation of wet gel felt with silica wet gel bonded: mixing tetraethoxysilane, ethanol and water uniformly, wherein the molar ratio of tetraethoxysilane: ethanol: water = 1: 60: 20; adding sulfuric acid to enable the pH value to be 2, uniformly stirring to form silica sol, then sequentially adding ammonia water to uniformly stir to enable the pH value of the solution to be 7, obtaining silica sol catalyzed by a gel catalyst, placing the catalyzed silica sol in a gel storage tank, placing a fiber felt with a water-absorbing expansion type adhesive attached to the surface in the gel storage tank to be soaked in the catalyzed silica sol, after the silica sol is gelatinized to form silica wet gel felt, dissolving a film on the surface of nano magnesium oxide in the gelatinization process, reacting and expanding the nano magnesium oxide with water to form cracks between wet gel pore structures, and solidifying liquid epoxy resin into a film in the gelatinization process.
3) Carrying out surface hydrophobization modification on the silicon dioxide wet gel felt after the crack is introduced, mixing trimethylethoxysilane and absolute ethyl alcohol according to a molar ratio of 1:2 to form a modification solution, and soaking the silicon dioxide wet gel felt in the modification solution.
4) And (3) carrying out solvent replacement on the silica wet gel felt for 3 times, then carrying out drying treatment, carrying out solvent replacement by adopting ethanol, soaking the silica wet gel felt in the ethanol for 5 hours, taking out the silica wet gel felt after the soaking is finished, drying the gel felt by adopting supercritical drying, and drying to obtain the silica aerogel felt with high flexibility.
Example 6:
a method of making a highly flexible aerogel blanket comprising:
1) attaching a water-swellable adhesive to the surface of the fibrous felt body: the fiber felt is a high silica fiber felt, 30 parts of sodium alginate is heated to 65 ℃ according to the parts by mass, the temperature is kept for 15min, 10 parts of polytetrafluoroethylene and 10 parts of chitosan are slowly added in the heat preservation process, the mixture is uniformly stirred, 25 parts of nano magnesium oxide is added after the mixture is cooled to the room temperature, and the mixture is uniformly stirred to prepare the water-swelling expanding agent; and then mixing an expanding agent with liquid epoxy resin, wherein the liquid epoxy resin is added with a curing agent, mixing 200 parts by mass of the liquid epoxy resin with 50 parts by mass of the expanding agent to prepare a water-absorbing expansion type adhesive, and coating the water-absorbing expansion type adhesive on the surface of the fiber felt.
2) Preparation of wet gel felt with silica wet gel bonded: uniformly mixing methyl orthosilicate, ethanol and water, wherein the molar ratio of methyl orthosilicate: ethanol: water = 1: 50: 10; adding sulfuric acid to enable the pH value to be 3, uniformly stirring to form a silicon dioxide sol, then sequentially adding ammonia water to uniformly stir to enable the pH value of the solution to be 8, obtaining the silicon dioxide sol catalyzed by a gel catalyst, placing the catalyzed silicon dioxide sol in a gel storage tank, placing a fiber felt with a water-absorbing expansion type adhesive attached to the surface in the gel storage tank to be soaked in the catalyzed silicon dioxide sol, standing the silicon sol at 40 ℃ to form a silicon dioxide wet gel felt, aging the silicon dioxide wet gel felt for 24 hours, dissolving a film on the surface of nano magnesium oxide in the aging process, reacting and expanding the nano magnesium oxide with water to form cracks between wet gel pore structures, and gradually curing liquid epoxy resin to form a film in the gelation and aging processes.
3) And (3) carrying out surface hydrophobization modification on the silicon dioxide wet gel felt after the crack is introduced, mixing trimethylchlorosilane and absolute ethyl alcohol according to a molar ratio of 1:3 to form a modification solution, and soaking the silicon dioxide wet gel felt in the modification solution to carry out surface hydrophobization modification.
4) And drying the silicon dioxide wet gel felt with the surface subjected to hydrophobic modification, drying the gel felt by adopting normal-pressure drying, and drying to obtain the high-flexibility silicon dioxide aerogel felt.
And (3) performance testing: the silica aerogel felts prepared in the above examples 1 to 6 were tested for hydrophobic property, thermal conductivity, mechanical strength and appearance, and the test results are shown in table 1.
Claims (10)
1. A preparation method of high-flexibility aerogel felt is characterized by comprising the following steps: the method comprises the following steps:
a) attaching a water-absorbing and expanding type adhesive to the surface of the fiber felt body;
b) combining the fiber felt with the water-absorbing expansion type adhesive attached to the surface with silica sol catalyzed by a gel catalyst, and gelling the fiber felt and the catalyzed silica sol to form a silica wet gel felt;
c) the silica wet gel mat is dried.
2. The method of making a highly flexible aerogel blanket according to claim 1, wherein: in the step a), the water-swellable adhesive is styrene-butadiene emulsion.
3. The method of making a highly flexible aerogel blanket according to claim 1, wherein: in the step a), the water-swelling type adhesive is formed by mixing an adhesive and a water-swelling agent.
4. The method of making a highly flexible aerogel blanket according to claim 1, wherein: in the step a), the fibers in the fiber felt are one or more of the following fiber materials: quartz fibers, glass fibers, high silica fibers, carbon fibers, pre-oxidized fiber, mullite fibers, basalt fibers, silicon carbide fibers, silicon nitride fibers, alumina fibers, and boron nitride fibers.
5. The method of making a highly flexible aerogel blanket according to claim 1, wherein: in the step b), the silica sol catalyzed by the gel catalyst is prepared by adding the gel catalyst into the silica sol; the silica sol is prepared by mixing a silicon source, ethanol and water in a molar ratio of 1 to (2-60) to (1-30); the silicon source is one or more than two of ethyl orthosilicate, methyl orthosilicate, butyl orthosilicate, isopropyl orthosilicate or alkyl alkoxy silane; the alkyl alkoxy silane comprises one or more than two of methyl trimethoxy silane, dimethyl dimethoxy silane, methyl triethoxy silane, dimethyl diethoxy silane, vinyl triethoxy silane, propyl trimethoxy silane or propyl triethoxy silane; the gel catalyst is one or two of alkaline catalyst such as sodium hydroxide, potassium hydroxide, ammonia water and ammonium fluoride aqueous solution; the gel catalyst adjusts the pH of the silica sol to 6-8.
6. The method of making a highly flexible aerogel blanket according to claim 5, wherein: adding an acid catalyst for catalyzing sol reaction, wherein the acid catalyst adjusts the pH value of the mixed solution of the silicon source, the ethanol and the water to be 2-6, and the acid catalyst catalyzes the reaction to enable the mixed solution to form silica sol; the acidic catalyst is one or the combination of more than two of sulfuric acid, hydrochloric acid, hydrofluoric acid, oxalic acid, acetic acid or benzenesulfonic acid.
7. The method of making a highly flexible aerogel blanket according to claim 1, wherein: the step b) further comprises an aging step, wherein the aging step is carried out by keeping the silica wet gel felt at the temperature of 30-70 ℃ for 4-24 hours.
8. The method of making a highly flexible aerogel blanket according to claim 1, wherein: the silica wet gel felt obtained by the step b) is subjected to surface hydrophobic modification treatment before the step c).
9. The method of making a highly flexible aerogel blanket according to claim 1, wherein: and c) performing solvent replacement on the wet gel felt for 1-3 times, and then drying, wherein the non-polar organic solvent is used for replacing alcohol and water in the pore structure of the wet gel felt, the non-polar organic solvent is a mixed solution of n-hexane and ethanol, the wet gel felt is placed in the mixed solution for dipping replacement, the dipping is performed for 4-6 hours, and the solvent replacement is repeated for 1-3 times.
10. An aerogel blanket prepared by the method of any of claims 1-9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111033703.0A CN113683343B (en) | 2021-09-03 | 2021-09-03 | High-flexibility aerogel felt and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111033703.0A CN113683343B (en) | 2021-09-03 | 2021-09-03 | High-flexibility aerogel felt and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113683343A true CN113683343A (en) | 2021-11-23 |
| CN113683343B CN113683343B (en) | 2023-01-17 |
Family
ID=78585538
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111033703.0A Active CN113683343B (en) | 2021-09-03 | 2021-09-03 | High-flexibility aerogel felt and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113683343B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114213156A (en) * | 2021-12-28 | 2022-03-22 | 山东工业陶瓷研究设计院有限公司 | Preparation method of ceramic heat insulation tile surface coating |
| CN114773027A (en) * | 2022-06-16 | 2022-07-22 | 巩义市泛锐熠辉复合材料有限公司 | Aerogel felt prepared at low cost and preparation method thereof |
| CN114804819A (en) * | 2022-06-14 | 2022-07-29 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of high-temperature-resistant aerogel composite material and composite material thereof |
| CN115043641A (en) * | 2022-06-30 | 2022-09-13 | 巩义市泛锐熠辉复合材料有限公司 | Tough wet-process fibrofelt reinforced aerogel composite material and preparation method thereof |
| CN115043408A (en) * | 2022-07-04 | 2022-09-13 | 巩义市泛锐熠辉复合材料有限公司 | Flexible silicon dioxide aerogel, aerogel felt and preparation method thereof |
| CN115124319A (en) * | 2022-07-04 | 2022-09-30 | 巩义市泛锐熠辉复合材料有限公司 | High-compression silicon dioxide aerogel, aerogel felt and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20130091482A (en) * | 2012-02-08 | 2013-08-19 | (주) 빛과환경 | Porous composite compound, manufacturing method thereof and cement composition containing porous composite compound |
| US20140170350A1 (en) * | 2011-07-12 | 2014-06-19 | Board Of Trustees Of Michigan State University | Porous sol gels and methods and structures related thereto |
| CN105645921A (en) * | 2016-03-10 | 2016-06-08 | 深圳中凝科技有限公司 | Method for preparing composite SiO2 aerogel felt |
| CN108569912A (en) * | 2018-04-29 | 2018-09-25 | 浙江工业大学 | A kind of preparation method of hydrophobic type aerosil composite fibre felt material |
| CN109400105A (en) * | 2018-09-26 | 2019-03-01 | 巩义市泛锐熠辉复合材料有限公司 | A kind of preparation method of anti-picking aerogel blanket |
-
2021
- 2021-09-03 CN CN202111033703.0A patent/CN113683343B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140170350A1 (en) * | 2011-07-12 | 2014-06-19 | Board Of Trustees Of Michigan State University | Porous sol gels and methods and structures related thereto |
| KR20130091482A (en) * | 2012-02-08 | 2013-08-19 | (주) 빛과환경 | Porous composite compound, manufacturing method thereof and cement composition containing porous composite compound |
| CN105645921A (en) * | 2016-03-10 | 2016-06-08 | 深圳中凝科技有限公司 | Method for preparing composite SiO2 aerogel felt |
| CN108569912A (en) * | 2018-04-29 | 2018-09-25 | 浙江工业大学 | A kind of preparation method of hydrophobic type aerosil composite fibre felt material |
| CN109400105A (en) * | 2018-09-26 | 2019-03-01 | 巩义市泛锐熠辉复合材料有限公司 | A kind of preparation method of anti-picking aerogel blanket |
Non-Patent Citations (1)
| Title |
|---|
| 熊刚等: "柔韧性二氧化硅气凝胶的研究进展", 《硅酸盐通报》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114213156A (en) * | 2021-12-28 | 2022-03-22 | 山东工业陶瓷研究设计院有限公司 | Preparation method of ceramic heat insulation tile surface coating |
| CN114213156B (en) * | 2021-12-28 | 2023-06-16 | 山东工业陶瓷研究设计院有限公司 | Preparation method of ceramic heat-insulating tile surface coating |
| CN114804819A (en) * | 2022-06-14 | 2022-07-29 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of high-temperature-resistant aerogel composite material and composite material thereof |
| CN114804819B (en) * | 2022-06-14 | 2023-04-07 | 巩义市泛锐熠辉复合材料有限公司 | Preparation method of high-temperature-resistant aerogel composite material and composite material thereof |
| CN114773027A (en) * | 2022-06-16 | 2022-07-22 | 巩义市泛锐熠辉复合材料有限公司 | Aerogel felt prepared at low cost and preparation method thereof |
| CN115043641A (en) * | 2022-06-30 | 2022-09-13 | 巩义市泛锐熠辉复合材料有限公司 | Tough wet-process fibrofelt reinforced aerogel composite material and preparation method thereof |
| CN115043408A (en) * | 2022-07-04 | 2022-09-13 | 巩义市泛锐熠辉复合材料有限公司 | Flexible silicon dioxide aerogel, aerogel felt and preparation method thereof |
| CN115124319A (en) * | 2022-07-04 | 2022-09-30 | 巩义市泛锐熠辉复合材料有限公司 | High-compression silicon dioxide aerogel, aerogel felt and preparation method thereof |
| CN115124319B (en) * | 2022-07-04 | 2023-03-24 | 巩义市泛锐熠辉复合材料有限公司 | High-compression silicon dioxide aerogel, aerogel felt and preparation method thereof |
| CN115043408B (en) * | 2022-07-04 | 2023-11-10 | 巩义市泛锐熠辉复合材料有限公司 | Flexible silica aerogel, aerogel felt and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113683343B (en) | 2023-01-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113683343B (en) | High-flexibility aerogel felt and preparation method thereof | |
| US10669392B2 (en) | Method of preparing aerogels/nonwoven composites fireproof and heat-insulating materials | |
| CN113896505B (en) | Method for discontinuously producing aerogel felt | |
| CN108383487B (en) | PAN pre-oxidized fiber felt/silicon dioxide aerogel composite material and preparation method thereof | |
| KR101955184B1 (en) | Method of preparing for aerogel blanket with low dust and high thermal insulation | |
| JP7196854B2 (en) | Coating liquid, method for producing coating film, and coating film | |
| CN113135732B (en) | Chopped glass fiber silicon dioxide aerogel composite material and preparation method thereof | |
| KR100710887B1 (en) | Method for manufacturing aerogel blanket | |
| CN111607253B (en) | Preparation method of silica aerogel thermal insulation filler | |
| US20080081014A1 (en) | Rapid preparation process of aerogel | |
| JP7196852B2 (en) | Coating liquid, method for producing coating film, and coating film | |
| CN110723738B (en) | Preparation method of enhanced silica aerogel, enhanced silica aerogel and application thereof | |
| CN107987311A (en) | A kind of preparation method of hydrophobicity melamine sponge enhancing polysilsesquioxane composite aerogel | |
| CN113563048B (en) | Low-dust aerogel felt and preparation method thereof | |
| CN110787745B (en) | Preparation method of silicon dioxide aerogel composite material and silicon dioxide aerogel composite material | |
| CN115124319B (en) | High-compression silicon dioxide aerogel, aerogel felt and preparation method thereof | |
| JPWO2019069494A1 (en) | Coating liquid, coating film manufacturing method and coating film | |
| CN109734412A (en) | A kind of second stage drying method preparing hydrophobic aluminium silica aerogel heat-barrier material | |
| CN104528741A (en) | Organic modified nanoporous silica aerogel and preparation method thereof | |
| CN111348886A (en) | Preparation method of thermal-insulation flexible silica aerogel | |
| CN110092939B (en) | Polyorganoalkoxysilane-reinforced hybrid silica aerogel and method for producing same | |
| CN108484952A (en) | A kind of preparation method of composite heat-insulated material | |
| CN108676360B (en) | Flexible hydrophobic aerogel composite heat insulation film and preparation method thereof | |
| CN115043408B (en) | Flexible silica aerogel, aerogel felt and preparation method thereof | |
| JP7196907B2 (en) | Method for suppressing corrosion under insulation and paste for suppressing corrosion under insulation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |