CN114454574A - Sheet aerogel/polystyrene composite material and preparation method thereof - Google Patents
Sheet aerogel/polystyrene composite material and preparation method thereof Download PDFInfo
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- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/18—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer of foamed material
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/065—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of foam
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- 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
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- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- B32B2266/00—Composition of foam
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2266/00—Composition of foam
- B32B2266/12—Gel
- B32B2266/126—Aerogel, i.e. a supercritically dried gel
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- C08J2205/00—Foams characterised by their properties
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/026—Aerogel, i.e. a supercritically dried gel
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
- C08J2361/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols with monohydric phenols
- C08J2361/10—Phenol-formaldehyde condensates
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Abstract
The invention discloses a preparation method of a flaky aerogel/polystyrene composite material, which specifically comprises the following steps: step 1, mixing resorcinol, formaldehyde water solution, sodium carbonate and water; step 2, transferring the obtained mixed solution to a thermostat and standing; step 3, washing and soaking the glass mold with dilute ammonia water; step 4, pouring the sol obtained in the step 2 into the glass mold obtained in the step 3, filling the container with the sol, and standing in a thermostat; step 5, soaking and washing the wet gel obtained in the step with absolute ethyl alcohol to obtain alcogel; step 6, performing carbon dioxide supercritical drying on the obtained alcohol gel; step 7, preparing a polystyrene film; step 8, placing the obtained flaky aerogel on a glass slide, and then placing the obtained polystyrene film; and 9, transferring the mold together with the aerogel and the polystyrene into a thermostat, heating and cooling to obtain the aerogel-polystyrene composite material. The invention also discloses the flaky aerogel/polystyrene composite material prepared by the method.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to a flaky aerogel/polystyrene composite material and a preparation method of the flaky aerogel/polystyrene composite material.
Background
Aerogel is a nano-porous material with integrated structure and function. Since the first invention of silica aerogels by Kistler et al in 1931, aerogels have attracted the interest of a wide range of researchers. There are many types of aerogels, including silicon-based, carbon-based, sulfur-based, metal oxide-based, and metal-based ones.
In engineering practices such as inertial confinement nuclear fusion, low-temperature and high-pressure equation of state experiments, hydrodynamics instability experiments and the like, aerogel and polystyrene need to be compounded. Although the thickness of the polystyrene film can be accurately regulated and controlled by adopting the spin coating method, the problems of surface wrinkles, uneven thickness and the like of the film can be caused in the solvent volatilization process. The adhesive is adopted for sticking, but unnecessary impurities are introduced.
Houvance et al (national invention patent publication No. CN113248229A) disclose a graphite inorganic composite polystyrene foam insulation board and a preparation method thereof, wherein the insulation board is mainly prepared from the following raw materials in parts by weight: 600-800 parts of magnesium sulfate, 100-120 parts of magnesium oxide, 1-5 parts of retarder, 80-120 parts of polystyrene foam particles, 370-425 parts of water, 5-10 parts of silica aerogel and 0-20 parts of graphite; the preparation method comprises the following steps: adding magnesium sulfate into water, then adding magnesium oxide to obtain a gel system, adding the raw materials except the polystyrene foam particles into the gel system, finally adding the polystyrene foam particles, and carrying out pressure molding.
Chen Guozhong et al (national invention patent publication No. CN113416020A) disclose a wall heat insulation slurry, which comprises the following raw materials by weight percent: 15-25% of aerogel compound, 22-28% of vitrified micro bubbles, 5-10% of polymer emulsion, 12-20% of heavy calcium carbonate powder, 3-6% of barium sulfate, 2-4% of modifier, 1-2% of flame retardant, 0.3-0.5% of wetting agent and the balance of water; the aerogel compound is added in the formula, the preparation process of the aerogel is optimized, the dry density of the slurry can be reduced, the phase-change material and the polystyrene microspheres serving as modifiers are added in the preparation process, the phase-change material and the polystyrene microspheres can be doped into a fragile network system of the aerogel while the heat insulation performance of the slurry is improved, the structural continuity of the aerogel is improved, and the phase-change material and the polystyrene microspheres filled in the aerogel can cooperatively maintain higher heat insulation and heat storage capacities relative to gaps in the aerogel; the strength of the aerogel can be improved to a certain extent by adding the polystyrene microspheres.
Sun Lei et al (national invention patent publication No. CN113356391A) discloses an aerogel polyurethane foam inner wall heat and sound insulation system, which comprises an inner wall body, a silica aerogel-polyurethane foam composite material layer and an integrated wallboard, wherein the inner wall body, the silica aerogel-polyurethane foam composite material layer and the integrated wallboard are distributed from inside to outside in a layered mode. The wall body and the integrated wallboard are fixed through the integrated wallboard fixing piece to form a space structure, and the silicon dioxide aerogel-polyurethane foam adhesive composite material layer is bonded with the wall body and the integrated wallboard to provide heat preservation and sound insulation performance simultaneously. The technology of the invention realizes excellent heat insulation performance and sound insulation performance through the silicon dioxide aerogel-polyurethane material with high doping proportion.
Xupei et al (national invention patent publication No. CN113133297A) disclose a hypercrosslinked polystyrene-based composite carbon aerogel electromagnetic shielding material and a preparation method thereof, which comprises the steps of firstly using nickel-coated multi-walled carbon nanotubes and multi-walled carbon nanotubes as mixed fillers, obtaining polystyrene-carbon nanotube composite aerogel with a high surface area, interconnected macroporous structure and nanofiber-like structure by adopting a high internal phase emulsion template method, and then carrying out hypercrosslinking and carbonization on the polystyrene-carbon nanotube composite aerogel to obtain a target product.
Tangwei et al (national invention patent publication No. CN113105191A) discloses a preparation method of an assembled environment-friendly and energy-saving insulation board based on urban solid waste garbage production, which comprises the following steps: mixing cement, fly ash, polypropylene fiber, polystyrene foam particles, cellulose acetate/polyacrylamide/silk fibroin/graphene oxide composite aerogel fibers and deionized water, then adding polymer modified solid waste particles, stirring uniformly, adding a vegetable protein foaming agent, sodium carboxymethylcellulose and calcium stearate, stirring and mixing, pouring the prepared slurry into a mold, carrying out constant-temperature maintenance treatment, finally demolding, and continuing natural maintenance treatment in the air to obtain the heat-insulating plate.
Wupekoe et al (national invention patent publication No. CN112959781A) disclose an optical film substrate comprising a polyester film (3) and an acrylic coating layer (2) formed on at least one side of the polyester film (3), wherein the polyester film (3) has a single-layer or multi-layer composite structure. In addition, the invention also provides a preparation method of the optical film substrate, which comprises a preparation step of the polyester film (3) and a step of forming the acrylic coating (2) on the surface of the polyester film (3) after the polyester film (3) is obtained.
Xu Sha fei et al (national invention patent publication No. CN112761283A) disclose a lightweight, fireproof, low thermal conductivity integrated non-dismantling composite thermal insulation template and a preparation process thereof; the concrete pouring wall comprises an inner protective layer connected with a concrete pouring wall body, wherein a heat insulation material layer, an inorganic material protective layer and an outer anti-cracking layer are sequentially arranged outside the inner protective layer, the inner protective layer is connected with the heat insulation material layer, the inorganic material protective layer and the outer anti-cracking layer in a reinforcing mode through a mortise and tenon reinforced structure, and the outer anti-cracking layer, the inorganic material protective layer, the heat insulation material layer and the inner protective layer are fixedly connected with the concrete pouring wall body through connecting anchor bolts; has the advantages of reasonable structural design, small heat conductivity coefficient, light weight, convenient construction and good fireproof performance.
Storage and construction front et al (national invention patent publication No. CN111907169A) disclose an A-level flame-retardant polystyrene heat-insulating template, which comprises a polystyrene plate and a casting slurry between the polystyrene plate, wherein the casting slurry comprises 100 parts by weight of water, 5-20 parts by weight of a binder, 20-50 parts by weight of a hydroxide flame retardant, 5-20 parts by weight of a silicate char forming agent and 0.5-5 parts by weight of a foaming agent. The invention also comprises a preparation method of the A-grade flame-retardant polystyrene heat-insulation template, which comprises the steps of preparing the casting slurry and bonding and pressing the plates, wherein the bonding agent comprises the following components: 5-15 parts of aerogel matrix, 0-10 parts of aerogel cross-linking agent, 10-50 parts of nano clay, 15-30 parts of aluminum dihydrogen phosphate and 15-30 parts of silica sol.
However, it remains a challenge to use simple means to composite the sheet-like aerogel with polystyrene.
Disclosure of Invention
The invention aims to provide a sheet aerogel/polystyrene composite material which has the advantages of good flatness, tight interlayer connection and controllable thickness.
Another object of the present invention is to provide a method for preparing a sheet-like aerogel/polystyrene composite, which is simple and easy to implement.
The first technical scheme adopted by the invention is that the preparation method of the flaky aerogel/polystyrene composite material specifically comprises the following steps:
step 2, transferring the mixed solution obtained in the step 1 to a thermostat and standing for 1-2d to obtain sol;
step 3, washing and soaking the glass mold with dilute ammonia water, washing with deionized water, and drying to obtain a hydrophilic glass mold;
step 4, pouring the sol obtained in the step 2 into the hydrophilic glass mold obtained in the step 3, filling the container with the sol, covering a hydrophilic glass cover, sealing, and placing the container in a thermostat for standing to obtain wet gel;
step 5, soaking and washing the wet gel obtained in the step with absolute ethyl alcohol to obtain alcogel;
step 6, carrying out carbon dioxide supercritical drying on the alcogel obtained in the step 5 to obtain a sheet-shaped aerogel;
step 7, preparing a polystyrene solution, and preparing polystyrene films with different thicknesses by using a spin-coating method;
step 8, placing the flaky aerogel obtained in the step 6 on a glass slide, placing the polystyrene film obtained in the step 7, covering the polystyrene film with the glass slide, supporting two sides of the glass slide by gaskets with proper thickness to enable the glass slide to be aligned up and down, and clamping two ends of the glass slide by using a long-tail clamp to form a mold;
and 9, transferring the mold in the step 8 together with the aerogel and the polystyrene into a thermostat for heating, cooling, and opening the mold to obtain the flaky aerogel/polystyrene composite material.
The present invention is also characterized in that,
in the step 1, the formaldehyde aqueous solution is 38% by mass, and the mass ratio of the resorcinol to the formaldehyde aqueous solution to the sodium carbonate to the water is 1:1.5:0.001-0.01: 1-10;
in step 2, the temperature of the incubator is 45-50 ℃.
In the step 3, the concentration of the dilute ammonia water is 0.5-1M, and the soaking time is 12-24 h.
In step 4, the temperature of the incubator is 45-50 ℃.
In step 5, soaking and washing the mixture for 3-4 days by using absolute ethyl alcohol, and replacing the solvent once every 1 day.
In step 6, the temperature of supercritical drying is set to be 40-42 ℃, the air pressure is set to be 10-11MPa, the heating rate is set to be 0.5-1 ℃/min, the constant temperature time is 3-4h, and the decompression rate is 1-3 MPa/h.
In step 7, the prepared polystyrene solution has a mass fraction of 5-10%, the used solvent is chloroform, and the rotation speed of a spin coater is 5000-10000 r/min; in step 9, the temperature of the thermostat is 145-150 ℃, and the heating time is 30-45 min.
In step 8, the thickness of the spacer is 100-500 μm, the length is 25-30mm, and the width is 10-12 mm.
The second technical scheme adopted by the invention is that the flaky aerogel/polystyrene composite material is characterized by being prepared by the preparation method.
The invention has the beneficial effects that:
(1) the method provided by the invention is simple and feasible, the preparation equipment is cheap and easy to obtain, the aerogel and polystyrene can be effectively compounded, and the method has important significance in engineering practices such as inertial confinement nuclear fusion, low-temperature and high-pressure state equation experiments, fluid mechanics instability experiments and the like.
(2) The sheet aerogel/polystyrene composite material prepared by the method disclosed by the invention is good in flatness, tight in interlayer connection and controllable in thickness.
Drawings
FIG. 1 is a flow chart of the production process of the present invention;
FIG. 2 is an SEM image (scale: 100 μm) of a cross section of a portion of the sheet-like aerogel/polystyrene composite prepared in example 1 of the present invention;
FIG. 3 is an SEM image (scale: 100 μm) of a second cross section of a portion of the flaky aerogel/polystyrene composite prepared in example 1 of the present invention;
FIG. 4 is an SEM image (scale bar is 100 μm) of a three-section area of a sheet-like aerogel/polystyrene composite material prepared in example 1 of the present invention;
FIG. 5 is an SEM image (scale bar is 100 μm) of the four cross sections of the part of the flaky aerogel/polystyrene composite material prepared in example 1 of the present invention;
FIG. 6 is an SEM image (scale bar is 100 μm) of a cross section of five parts of the sheet-like aerogel/polystyrene composite prepared in example 1 of the present invention;
FIG. 7 is an SEM image (scale: 100 μm) of a six-section of a portion of a flaky aerogel/polystyrene composite prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention provides a preparation method of a sheet-shaped aerogel/polystyrene composite material, which specifically comprises the following steps as shown in figure 1:
step 2, transferring the mixed solution obtained in the step 1 to a thermostat and standing for 1-2d to obtain sol;
step 3, washing and soaking the glass mold with dilute ammonia water, washing the glass mold with deionized water, and drying the glass mold to obtain a hydrophilic glass mold;
step 4, pouring the sol obtained in the step 2 into the hydrophilic glass mold obtained in the step 3, filling the container with the sol, covering a hydrophilic glass cover, sealing, and placing the container in a thermostat for standing to obtain wet gel;
step 5, soaking and washing the wet gel obtained in the step with absolute ethyl alcohol to obtain alcogel;
step 6, carrying out carbon dioxide supercritical drying on the alcogel obtained in the step 5 to obtain a sheet-shaped aerogel;
step 7, preparing a polystyrene solution, and preparing polystyrene films with different thicknesses by using a spin-coating method;
step 8, placing the flaky aerogel obtained in the step 6 on a glass slide, placing the polystyrene film obtained in the step 7, covering the polystyrene film with the glass slide, supporting two sides of the glass slide by gaskets with proper thickness to enable the glass slide to be aligned up and down, and clamping two ends of the glass slide by using a long-tail clamp to form a mold;
and 9, transferring the mold in the step 8 together with the aerogel and the polystyrene into a thermostat for heating, cooling, and opening the mold to obtain the flaky aerogel/polystyrene composite material.
In the step 1, the formaldehyde aqueous solution is 38% by mass, and the mass ratio of the resorcinol to the formaldehyde aqueous solution to the sodium carbonate to the water is 1:1.5:0.001-0.01: 1-10.
In step 2, the temperature of the incubator is 45-50 ℃.
In the step 3, the concentration of the dilute ammonia water is 0.5-1M, and the soaking time is 12-24 h.
In step 4, the temperature of the incubator is 45-50 ℃.
In step 5, soaking and washing the mixture for 3-4 days by using absolute ethyl alcohol, and replacing the solvent once every 1 day.
In step 6, the temperature of supercritical drying is set to be 40-42 ℃, the air pressure is set to be 10-11MPa, the heating rate is set to be 0.5-1 ℃/min, the constant temperature time is 3-4h, and the pressure reduction rate is 1-3 MPa/h.
In step 7, the mass fraction of the prepared polystyrene solution is 5-10%, the used solvent is chloroform, and the rotation speed of the spin coater is 5000-10000 r/min.
In step 8, the thickness of the spacer is 100-500 μm, the length is 25-30mm, and the width is 10-12 mm.
In step 9, the temperature of the thermostat is 145-150 ℃, and the heating time is 30-45 min.
The invention also provides a flaky aerogel/polystyrene composite material prepared by the preparation method.
Example 1
A sheet-like aerogel/polystyrene composite having a thickness of 250 μm.
Firstly, uniformly mixing resorcinol, a formaldehyde aqueous solution with the mass fraction of 38%, sodium carbonate and water according to the mass ratio of 1:1.5:0.002:2, and stirring for 2 hours by magnetic force to form a mixed solution;
secondly, transferring the mixed solution into a thermostat with the temperature of 50 ℃ and standing for 1d to obtain sol;
thirdly, soaking the glass mold in 0.5M dilute ammonia water for 24 hours, washing with deionized water, and drying to obtain a hydrophilic glass mold;
fourthly, pouring the sol obtained in the step 2 into the hydrophilic glass mold obtained in the step 3, filling the container with the sol, covering a hydrophilic glass cover, sealing, and standing in a thermostat at 50 ℃ for 2d to obtain hydrogel;
fifthly, soaking and washing the hydrogel with absolute ethyl alcohol for 3d, and replacing the solvent once every 1d to obtain alcogel;
sixthly, carrying out carbon dioxide supercritical drying on the alcogel, setting the temperature of the supercritical drying to be 40 ℃, setting the air pressure to be 10MPa, setting the heating rate to be 1 ℃/min, setting the constant temperature time to be 4h, and setting the decompression rate to be 3MPa/h, and drying to obtain the sheet aerogel;
seventhly, preparing a polystyrene solution with the mass fraction of 10%, wherein the used solvent is trichloromethane, and preparing a polystyrene film by using a spin coating method, wherein the rotating speed of a spin coater is 5000 r/min;
eighthly, placing the flaky aerogel on a glass slide, placing a polystyrene film, covering the polystyrene film with the glass slide, supporting two sides of the glass slide by gaskets with proper thickness to enable the glass slide to be aligned up and down, clamping two ends of the glass slide by using a long tail clamp to form a mold, wherein the thickness of each gasket is 250 micrometers, the length of each gasket is 30mm, the width of each gasket is 10mm, and the total thickness of the polystyrene film and the flaky aerogel is 10-20 micrometers higher than the thickness of each gasket;
and finally, transferring the die together with the aerogel and the polystyrene into a thermostat for heating at 146 ℃ for 32min, and opening the die after cooling to obtain the flaky aerogel/polystyrene composite material. FIGS. 2 to 7 are SEM images of cross sections of different parts of the sheet-like aerogel/polystyrene composite prepared in example 1 of the present invention. As can be seen from the figure, the prepared sheet aerogel/polystyrene composite material has good flatness, tight interlayer connection and controllable thickness.
Example 2
A sheet-like aerogel/polystyrene composite having a thickness of 150 μm.
Firstly, uniformly mixing resorcinol, a formaldehyde water solution with the mass fraction of 38%, sodium carbonate and water according to the mass ratio of 1:1.5:0.002:2, and magnetically stirring for 2 hours to form a mixed solution;
secondly, transferring the mixed solution into a thermostat with the temperature of 50 ℃ and standing for 1d to obtain sol;
thirdly, soaking the glass mold in 0.5M dilute ammonia water for 24 hours, washing with deionized water, and drying to obtain a hydrophilic glass mold;
fourthly, pouring the sol obtained in the step 2 into the hydrophilic glass mold obtained in the step 3, filling the container with the sol, covering the container with a hydrophilic glass cover, sealing the container, and standing the container in a thermostat at 50 ℃ for 2d to obtain hydrogel;
fifthly, soaking and washing the hydrogel for 3 days by using absolute ethyl alcohol, and replacing the solvent once every 1 day to obtain alcogel;
sixthly, carrying out carbon dioxide supercritical drying on the alcogel, setting the temperature of the supercritical drying to be 40 ℃, setting the air pressure to be 10MPa, setting the heating rate to be 1 ℃/min, setting the constant temperature time to be 4h, and setting the decompression rate to be 3MPa/h, and drying to obtain the sheet aerogel;
seventhly, preparing a polystyrene solution with the mass fraction of 10%, wherein the used solvent is trichloromethane, and preparing a polystyrene film by using a spin coating method, wherein the rotating speed of a spin coater is 5000 r/min;
eighthly, placing the flaky aerogel on a glass slide, placing a polystyrene film, covering the polystyrene film with the glass slide, supporting two sides of the glass slide by gaskets with proper thickness to enable the glass slide to be aligned up and down, clamping two ends of the glass slide by using a long tail clamp to form a mold, wherein the thickness of each gasket is 150 micrometers, the length of each gasket is 30mm, the width of each gasket is 10mm, and the total thickness of the polystyrene film and the flaky aerogel is 10-20 micrometers higher than the thickness of each gasket;
and finally, transferring the die together with the aerogel and the polystyrene into a thermostat for heating at 145 ℃ for 30min, and opening the die after cooling to obtain the flaky aerogel/polystyrene composite material.
Example 3
A sheet-like aerogel/polystyrene composite having a thickness of 300 μm.
Firstly, uniformly mixing resorcinol, a formaldehyde water solution with the mass fraction of 38%, sodium carbonate and water according to the mass ratio of 1:1.5:0.002:2, and magnetically stirring for 2 hours to form a mixed solution;
secondly, transferring the mixed solution into a thermostat with the temperature of 50 ℃ and standing for 1d to obtain sol;
thirdly, soaking the glass mold in 0.5M dilute ammonia water for 24 hours, washing with deionized water, and drying to obtain a hydrophilic glass mold;
fourthly, pouring the sol obtained in the step 2 into the hydrophilic glass mold obtained in the step 3, filling the container with the sol, covering a hydrophilic glass cover, sealing, and standing in a thermostat at 50 ℃ for 2d to obtain hydrogel;
fifthly, soaking and washing the hydrogel for 3 days by using absolute ethyl alcohol, and replacing the solvent once every 1 day to obtain alcogel;
sixthly, carrying out carbon dioxide supercritical drying on the alcogel, setting the temperature of the supercritical drying to be 40 ℃, setting the air pressure to be 10MPa, setting the heating rate to be 1 ℃/min, setting the constant temperature time to be 4h, setting the decompression rate to be 3MPa/h, and drying to obtain the flaky aerogel;
seventhly, preparing a polystyrene solution with the mass fraction of 10%, wherein the used solvent is trichloromethane, and preparing a polystyrene film by using a spin coating method, wherein the rotating speed of a spin coater is 5000 r/min;
eighthly, placing the flaky aerogel on a glass slide, placing a polystyrene film, covering the polystyrene film with the glass slide, supporting two sides of the glass slide by gaskets with proper thickness to enable the glass slide to be aligned up and down, clamping two ends of the glass slide by using a long tail clamp to form a mold, wherein the thickness of each gasket is 300 microns, the length of each gasket is 30mm, the width of each gasket is 10mm, and the total thickness of the polystyrene film and the flaky aerogel is 10-20 microns higher than the thickness of each gasket;
and finally, transferring the die together with the aerogel and the polystyrene into a thermostat for heating at the temperature of 150 ℃ for 30min, and opening the die after cooling to obtain the flaky aerogel/polystyrene composite material.
Example 4
A sheet-like aerogel/polystyrene composite having a thickness of 350 μm.
Firstly, uniformly mixing resorcinol, a formaldehyde water solution with the mass fraction of 38%, sodium carbonate and water according to the mass ratio of 1:1.5:0.005:8, and magnetically stirring for 2 hours to form a mixed solution;
secondly, transferring the mixed solution into a thermostat with the temperature of 48 ℃ and standing for 1.5d to obtain sol;
thirdly, soaking the glass mold in 0.6M dilute ammonia water for 22 hours, washing with deionized water, and drying to obtain a hydrophilic glass mold;
fourthly, pouring the sol obtained in the step 2 into the hydrophilic glass mold obtained in the step 3, filling the container with the sol, covering a hydrophilic glass cover, sealing, and standing in a thermostat at 59 ℃ for 2d to obtain hydrogel;
fifthly, soaking and washing the hydrogel for 3 days by using absolute ethyl alcohol, and replacing the solvent once every 1 day to obtain alcogel;
sixthly, carrying out carbon dioxide supercritical drying on the alcogel, setting the temperature of the supercritical drying to be 41 ℃, setting the air pressure to be 10.5MPa, setting the heating rate to be 0.6 ℃/min, setting the constant temperature time to be 3.5h and the decompression rate to be 2MPa/h, and drying to obtain the flaky aerogel;
seventhly, preparing a polystyrene solution with the mass fraction of 8%, wherein the used solvent is trichloromethane, and preparing a polystyrene film by using a spin coating method, wherein the rotating speed of a spin coating machine is 6000 r/min;
eighthly, placing the flaky aerogel on a glass slide, placing a polystyrene film, covering the polystyrene film with the glass slide, supporting two sides of the glass slide by gaskets with proper thickness to enable the glass slide to be aligned up and down, clamping two ends of the glass slide by using a long tail clamp to form a mold, wherein the thickness of each gasket is 350 microns, the length of each gasket is 30mm, the width of each gasket is 10mm, and the total thickness of the polystyrene film and the flaky aerogel is 10-20 microns higher than the thickness of each gasket;
and finally, transferring the die together with the aerogel and the polystyrene into a thermostat for heating at the temperature of 146 ℃ for 35min, and opening the die after cooling to obtain the flaky aerogel/polystyrene composite material.
Example 5
A sheet-like aerogel/polystyrene composite having a thickness of 400 μm.
Firstly, uniformly mixing resorcinol, a formaldehyde water solution with the mass fraction of 38%, sodium carbonate and water according to the mass ratio of 1:1.5:0.001:10, and magnetically stirring for 2 hours to form a mixed solution;
secondly, transferring the mixed solution into a thermostat at 45 ℃ and standing for 1d to obtain sol;
thirdly, soaking the glass mold in 1M dilute ammonia water for 12 hours, washing with deionized water, and drying to obtain a hydrophilic glass mold;
fourthly, pouring the sol obtained in the step 2 into the hydrophilic glass mold obtained in the step 3, filling the container with the sol, covering a hydrophilic glass cover, sealing, and standing in a thermostat at 45 ℃ for 2d to obtain hydrogel;
fifthly, soaking and washing the hydrogel with absolute ethyl alcohol for 4 days, and replacing the solvent once every 1 day to obtain alcogel;
sixthly, carrying out carbon dioxide supercritical drying on the alcogel, setting the temperature of the supercritical drying to be 42 ℃, setting the air pressure to be 11MPa, setting the heating rate to be 0.5 ℃/min, setting the constant temperature time to be 3h and the decompression rate to be 1MPa/h, and drying to obtain the sheet aerogel;
seventhly, preparing a polystyrene solution with the mass fraction of 5%, wherein the used solvent is trichloromethane, and preparing a polystyrene film by using a spin coating method, wherein the rotating speed of a spin coating machine is 10000 r/min;
eighthly, placing the flaky aerogel on a glass slide, placing a polystyrene film, covering the polystyrene film with the glass slide, supporting two sides of the glass slide by gaskets with proper thickness to enable the glass slide to be aligned up and down, clamping two ends of the glass slide by using a long tail clamp to form a mold, wherein the thickness of each gasket is 400 microns, the length of each gasket is 30mm, the width of each gasket is 10mm, and the total thickness of the polystyrene film and the flaky aerogel is 10-20 microns higher than the thickness of each gasket;
and finally, transferring the die together with the aerogel and the polystyrene into a thermostat for heating at the temperature of 150 ℃ for 45min, and opening the die after cooling to obtain the flaky aerogel/polystyrene composite material.
Example 6
A sheet-like aerogel/polystyrene composite having a thickness of 450 μm.
Firstly, uniformly mixing resorcinol, a formaldehyde water solution with the mass fraction of 38%, sodium carbonate and water according to the mass ratio of 1:1.5:0.001:1, and magnetically stirring for 2 hours to form a mixed solution;
secondly, transferring the mixed solution into a thermostat with the temperature of 50 ℃ and standing for 1d to obtain sol;
thirdly, soaking the glass mold in 0.5M dilute ammonia water for 24 hours, washing with deionized water, and drying to obtain a hydrophilic glass mold;
fourthly, pouring the sol obtained in the step 2 into the hydrophilic glass mold obtained in the step 3, filling the container with the sol, covering a hydrophilic glass cover, sealing, and standing in a thermostat at 50 ℃ for 2d to obtain hydrogel;
fifthly, soaking and washing the hydrogel with absolute ethyl alcohol for 4 days, and replacing the solvent once every 1 day to obtain alcogel;
sixthly, carrying out carbon dioxide supercritical drying on the alcogel, setting the temperature of the supercritical drying to be 40 ℃, setting the air pressure to be 10MPa, setting the heating rate to be 1 ℃/min, setting the constant temperature time to be 4h, and setting the decompression rate to be 3MPa/h, and drying to obtain the sheet aerogel;
seventhly, preparing a polystyrene solution with the mass fraction of 10%, wherein the used solvent is trichloromethane, and preparing a polystyrene film by using a spin coating method, wherein the rotating speed of a spin coater is 5000 r/min;
eighthly, placing the flaky aerogel on a glass slide, placing a polystyrene film, covering the polystyrene film with the glass slide, supporting two sides of the glass slide by gaskets with proper thickness to enable the glass slide to be aligned up and down, clamping two ends of the glass slide by using a long tail clamp to form a mold, wherein the thickness of each gasket is 450 micrometers, the length of each gasket is 30mm, the width of each gasket is 10mm, and the total thickness of the polystyrene film and the flaky aerogel is 10-20 micrometers higher than the thickness of each gasket;
and finally, transferring the die together with the aerogel and the polystyrene into a thermostat for heating at 145 ℃ for 30min, and opening the die after cooling to obtain the flaky aerogel/polystyrene composite material.
Example 7
A sheet-like aerogel/polystyrene composite having a thickness of 500 μm.
Firstly, uniformly mixing resorcinol, a formaldehyde aqueous solution with the mass fraction of 38%, sodium carbonate and water according to the mass ratio of 1:1.5:0.002:2, and stirring for 2 hours by magnetic force to form a mixed solution;
secondly, transferring the mixed solution into a thermostat with the temperature of 50 ℃ and standing for 1d to obtain sol;
thirdly, soaking the glass mold in 0.5M dilute ammonia water for 24 hours, washing with deionized water, and drying to obtain a hydrophilic glass mold;
fourthly, pouring the sol obtained in the step 2 into the hydrophilic glass mold obtained in the step 3, filling the container with the sol, covering a hydrophilic glass cover, sealing, and standing in a thermostat at 50 ℃ for 2d to obtain hydrogel;
fifthly, soaking and washing the hydrogel for 3 days by using absolute ethyl alcohol, and replacing the solvent once every 1 day to obtain alcogel;
sixthly, carrying out carbon dioxide supercritical drying on the alcogel, setting the temperature of the supercritical drying to be 40 ℃, setting the air pressure to be 10MPa, setting the heating rate to be 1 ℃/min, setting the constant temperature time to be 4h, and setting the decompression rate to be 3MPa/h, and drying to obtain the sheet aerogel;
seventhly, preparing a polystyrene solution with the mass fraction of 10%, wherein the used solvent is trichloromethane, and preparing a polystyrene film by using a spin coating method, wherein the rotating speed of a spin coater is 5000 r/min;
eighthly, placing the flaky aerogel on a glass slide, placing a polystyrene film, covering the polystyrene film with the glass slide, supporting two sides of the glass slide by gaskets with proper thickness to enable the glass slide to be aligned up and down, clamping two ends of the glass slide by using a long tail clamp to form a mold, wherein the thickness of each gasket is 500 micrometers, the length of each gasket is 30mm, the width of each gasket is 10mm, and the total thickness of the polystyrene film and the flaky aerogel is 10-20 micrometers higher than the thickness of each gasket;
and finally, transferring the mold together with the aerogel and the polystyrene into a thermostat for heating at the temperature of 150 ℃ for 30-45min, and opening the mold after cooling to obtain the flaky aerogel/polystyrene composite material.
The structure of the glass mold of examples 1 to 7 was a slide-glass gasket-slide laminated structure.
Claims (10)
1. The preparation method of the flaky aerogel/polystyrene composite material is characterized by comprising the following steps:
step 1, uniformly mixing resorcinol, formalin, sodium carbonate and water, and magnetically stirring for 1-2 hours to form a mixed solution;
step 2, transferring the mixed solution obtained in the step 1 to a thermostat and standing for 1-2d to obtain sol;
step 3, washing and soaking the glass mold with dilute ammonia water, washing with deionized water, and drying to obtain a hydrophilic glass mold;
step 4, pouring the sol obtained in the step 2 into the hydrophilic glass mold obtained in the step 3, filling the container with the sol, covering a hydrophilic glass cover, sealing, and placing the container in a thermostat for standing to obtain wet gel;
step 5, soaking and washing the wet gel obtained in the step with absolute ethyl alcohol to obtain alcogel;
step 6, carrying out carbon dioxide supercritical drying on the alcogel obtained in the step 5 to obtain a sheet-shaped aerogel;
step 7, preparing a polystyrene solution, and preparing polystyrene films with different thicknesses by using a spin-coating method;
step 8, placing the flaky aerogel obtained in the step 6 on a glass slide, placing the polystyrene film obtained in the step 7, covering the polystyrene film with the glass slide, supporting two sides of the glass slide by gaskets with proper thickness to enable the glass slide to be aligned up and down, and clamping two ends of the glass slide by using a long-tail clamp to form a mold;
and 9, transferring the mold in the step 8 together with the aerogel and the polystyrene into a thermostat for heating, cooling, and opening the mold to obtain the flaky aerogel/polystyrene composite material.
2. The preparation method of the flaky aerogel/polystyrene composite material according to claim 1, wherein in the step 1, the aqueous formaldehyde solution is 38% by mass, and the mass ratio of the resorcinol, the aqueous formaldehyde solution, the sodium carbonate and the water is 1:1.5:0.001-0.01: 1-10.
3. The method for preparing a sheet-like aerogel/polystyrene composite according to claim 1, wherein the temperature of the incubator in step 2 is 45-50 ℃.
4. The method for preparing the sheet-like aerogel/polystyrene composite material according to claim 1, wherein in the step 3, the concentration of the dilute ammonia water is 0.5-1M, and the soaking time is 12-24 h.
5. The method for preparing a sheet-like aerogel/polystyrene composite according to claim 1, wherein the temperature of the incubator in step 4 is 45-50 ℃.
6. The method for preparing a flaky aerogel/polystyrene composite material according to claim 1, wherein in the step 5, the solvent is replaced every 1d by soaking and washing with absolute ethyl alcohol for 3-4 d.
7. The method for preparing a sheet-like aerogel/polystyrene composite according to claim 1, wherein in step 6, the temperature of supercritical drying is set to 40-42 ℃, the air pressure is set to 10-11MPa, the temperature rise rate is set to 0.5-1 ℃/min, the constant temperature time is 3-4h, and the pressure reduction rate is 1-3 MPa/h.
8. The preparation method of the sheet-like aerogel/polystyrene composite material as claimed in claim 1, wherein in step 7, the prepared polystyrene solution has a mass fraction of 5-10%, the solvent used is chloroform, and the rotation speed of the spin coater is 5000-10000 r/min; in step 9, the temperature of the thermostat is 145-150 ℃, and the heating time is 30-45 min.
9. The method for preparing a sheet-like aerogel/polystyrene composite as claimed in claim 1, wherein in step 8, the thickness of the gasket is 100 μm, the length is 25-30mm, and the width is 10-12 mm.
10. A sheet-like aerogel/polystyrene composite, characterized in that it is obtained by the preparation method according to any one of claims 1 to 9.
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