CN114801360B - Wet fiber sheet reinforced aerogel film-covered product and preparation method thereof - Google Patents

Wet fiber sheet reinforced aerogel film-covered product and preparation method thereof Download PDF

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Publication number
CN114801360B
CN114801360B CN202210668982.6A CN202210668982A CN114801360B CN 114801360 B CN114801360 B CN 114801360B CN 202210668982 A CN202210668982 A CN 202210668982A CN 114801360 B CN114801360 B CN 114801360B
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fiber sheet
film
wet
aerogel
wet fiber
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CN114801360A (en
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张东生
张继承
刘喜宗
何凤霞
杨超
杜重辉
曹二伟
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Gongyi Van Research Yihui Composite Material Co Ltd
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Gongyi Van Research Yihui Composite Material Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • 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
    • B32B5/02—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 structural features of a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
    • B29D7/00—Producing flat articles, e.g. films or sheets
    • B29D7/01—Films or sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/12—Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
    • B32B27/281—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyimides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • B32B27/302—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising aromatic vinyl (co)polymers, e.g. styrenic (co)polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • B32B27/304—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl halide (co)polymers, e.g. PVC, PVDC, PVF, PVDF
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
    • B32B27/322—Layered products comprising a layer of synthetic resin comprising polyolefins comprising halogenated polyolefins, e.g. PTFE
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
    • B32B27/365—Layered products comprising a layer of synthetic resin comprising polyesters comprising polycarbonates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/40—Layered products comprising a layer of synthetic resin comprising polyurethanes
    • 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
    • C04B30/00—Compositions for artificial stone, not containing binders
    • C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
    • B32B2260/02—Composition of the impregnated, bonded or embedded layer
    • B32B2260/021—Fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
    • B32B2260/04—Impregnation, embedding, or binder material
    • B32B2260/044—Water-setting substance, e.g. concrete, plaster
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B32B2262/101—Glass fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2457/00—Electrical equipment
    • B32B2457/10—Batteries

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Laminated Bodies (AREA)

Abstract

The invention relates to a wet fiber sheet reinforced aerogel coated product and a preparation method thereof. The preparation method of the wet fiber sheet reinforced aerogel film product comprises the following steps: step one: dipping the wet fiber sheet into sol, and obtaining a gel sheet after gel; step two: respectively placing film coating materials with the peripheral sizes larger than those of the gel sheets on the upper surface and the lower surface of the gel sheets, placing the gel sheets after film coating in a frame body, and performing supercritical drying treatment to obtain aerogel-wet fiber sheets; step three: performing hot pressing treatment on the aerogel-wet fiber sheet obtained in the step two to obtain an aerogel film-covered product; the wet fiber sheet reinforced aerogel film product is prepared by the method. According to the invention, when the wet fiber sheet reinforced aerogel film-coated product is prepared, films are coated on the upper surface and the lower surface of the gel sheet, on one hand, a packaging layer is formed, and felt powder falling is avoided; on the other hand, the organic adhesive avoiding overflowing is adhered in the tooling equipment.

Description

Wet fiber sheet reinforced aerogel film-covered product and preparation method thereof
Technical Field
The invention relates to a wet fiber sheet reinforced aerogel coated product and a preparation method thereof.
Background
The aerogel is a solid structure which is not collapsed after liquid in a gel structure is replaced by gas, and the silica aerogel is a continuous three-dimensional network structure formed by mutually polymerizing nano-scale particles, and has effective limits on heat conductivity efficiency, convection heat transfer efficiency and radiation heat transfer efficiency due to the special nano-scale micropores and skeleton structure, so the aerogel has very low heat conductivity coefficient and is a solid material with the lowest heat conductivity coefficient in the world at present. However, because the pure aerogel has poor mechanical properties and is very brittle, the fiber material is generally used for impregnating the sol to prepare the aerogel composite material so as to enhance the mechanical properties of the aerogel.
At present, when a wet fiber material is used as a reinforcing material of aerogel, an organic adhesive is required to be used in the preparation process of the wet fiber material, so that the gel-out phenomenon can occur in the hydrophobic and drying process of the aerogel composite material, and the composite performance of the aerogel is reduced; on the other hand, the "glue" overflowed from the wet fiber material can be stuck in the drying equipment and the tooling, and each batch of product needs to be cleaned once when being prepared, otherwise, the quality of the next batch of gel material in drying can be affected. Furthermore, due to its own cause, siO 2 The aerogel blanket generally has the condition that the blanket body drops aerogel powder in transportation, construction and use, and the condition that falls powder not only brings inconvenience for the construction, has brought threat to constructor health, also can reduce the performance of aerogel blanket itself simultaneously.
Disclosure of Invention
In view of the above, the present invention aims to provide a wet fiber sheet reinforced aerogel coated product and a preparation method thereof, so as to solve the technical problem that in the prior art, in the process of reinforcing aerogel by adopting wet fiber materials, organic adhesives in the wet fiber sheets are easy to overflow and adhere to tooling equipment, and influence the quality of the next batch of aerogel materials to be dried.
In order to achieve the above purpose, the technical scheme of the wet fiber sheet reinforced aerogel coated product of the invention is as follows:
a wet fiber sheet reinforced aerogel coated product comprises an aerogel-wet fiber sheet and coated materials arranged on the upper surface and the lower surface of the aerogel-wet fiber sheet, wherein the wet fiber sheet comprises an organic adhesive; the aerogel-wet fiber sheet and the coating material are fixed by an organic adhesive overflowed from the wet fiber sheet in the supercritical drying process, and the periphery of the coating material is reserved beyond the edge of the aerogel-wet fiber sheet and is subjected to hot-pressing plastic package.
Preferably, the organic adhesive comprises more than one of phenolic resin adhesive, epoxy resin adhesive, urea resin adhesive, polyacrylic resin adhesive, melamine-formaldehyde adhesive and polyurethane adhesive.
The technical scheme adopted by the preparation method of the wet fiber sheet reinforced aerogel film product is as follows:
the preparation method of the wet fiber sheet reinforced aerogel film product comprises the following steps:
step one: dipping the wet fiber sheet into sol for treatment, and obtaining a gel sheet after gel;
step two: the method comprises the steps of respectively arranging a film coating material on the upper surface and the lower surface of a gel sheet, placing the gel sheet after film coating in a frame body with a clamping function, and performing supercritical drying treatment to obtain an aerogel-wet fiber sheet, wherein the peripheral size of the film coating material is larger than that of the gel sheet;
step three: and (3) carrying out hot pressing treatment on the aerogel-wet fiber sheet obtained in the step (II) to obtain an aerogel tectorial membrane product.
Preferably, in the first step, the sol adopts one of silica sol, aluminum sol or silicon-aluminum composite sol.
Further, the silica sol configuration step includes: uniformly mixing a silicon source, ethanol and water, and then adding a catalyst and uniformly stirring to obtain silicon dioxide sol; wherein, the silicon source, ethanol and water are mixed according to the molar ratio of 1: (2-60): (0.05-30); the silicon source is one or more of ethyl orthosilicate, methyl orthosilicate, butyl orthosilicate, isopropyl orthosilicate and alkyl alkoxy silane; the alkyl alkoxy silane comprises one or more of methyl trimethoxy silane, dimethyl dimethoxy silane, methyl triethoxy silane, dimethyl diethoxy silane, vinyl triethoxy silane, propyl trimethoxy silane and propyl triethoxy silane; the catalyst comprises an alkaline catalyst, wherein the alkaline catalyst is one or the combination of two of sodium hydroxide, potassium hydroxide, ammonia water, ammonium fluoride, ammonium bicarbonate, sodium carbonate, sodium bicarbonate, ethanolamine, diethanolamine, methylamine, dimethylamine, ethylamine, diethylamine, propylamine, dipropylamine, isopropanolamine, aniline, o-phenylenediamine, m-phenylenediamine and p-phenylenediamine;
the preparation method of the aluminum sol comprises the following steps: preparing an aluminum source, a chelating agent, a solvent for aluminum sol, water and a catalyst for aluminum sol to obtain aluminum sol, wherein the molar ratio of the aluminum source to the chelating agent to the solvent for aluminum sol to the water to the catalyst for aluminum sol is 1: (0.001 to 0.06): (4-32): (0.6 to 4): (0.0001-1); the aluminum source is one or the combination of more than two of aluminum isopropoxide, aluminum sec-butoxide and aluminum nitrate; the chelating agent is one of acetylacetone and ethyl acetoacetate; the solvent for aluminum sol is selected from one or more than two of the group consisting of ethanol, isopropanol and n-butanol; the catalyst for the aluminum sol is one or the combination of more than two of sodium hydroxide, potassium hydroxide, ammonia water and ammonium fluoride;
the preparation of the silicon-aluminum composite sol is to uniformly mix the silicon dioxide sol and the aluminum sol or directly uniformly mix the precursor solution used for the silicon-aluminum composite sol.
Preferably, in the second step, the frame body is provided with a plurality of holes through which the supercritical fluid can pass, and the holes on the frame body can be arranged on the frame body and/or the frame walls between the frame bodies.
Preferably, the multi-layer gel sheets are stacked and placed in the frame body, and a layer of film coating material is arranged on the upper surface and the lower surface of each layer of gel sheet in the stacking process.
Preferably, the wet fiber sheet is one of an aluminum silicate fiber sheet, a glass fiber sheet, a basalt fiber sheet, a mullite fiber sheet, a quartz fiber sheet and an aluminum oxide fiber sheet.
Preferably, the film coating material is one of PI film, PET film, PVC film, PTFE film, TPU film, PC film, PE film, PS film and PP film.
Preferably, the temperature of the supercritical drying is 40-55 ℃, and the pressure is 7-20 MPa.
Preferably, the temperature of the hot pressing treatment is 80-300 ℃, the time of the hot pressing treatment is 20-100 s, and the pressure is 1 kg/cm 2 ~100 kg/cm 2 。
The beneficial effects of the invention are as follows:
1. in the process of preparing the laminated product, the upper surface and the lower surface of the gel sheet are covered with the laminated material with the size larger than that of the gel sheet, and the size of the laminated material is larger than that of the gel sheet because the organic adhesive in the wet fiber sheet overflows the wet fiber sheet in the supercritical drying process, so that the laminated material has a blocking effect on the overflowed organic adhesive, the pollution of the overflowed organic adhesive to the product and tooling equipment is avoided, the time consumption and labor for cleaning the tooling equipment are reduced, and the production efficiency is improved; the overflowed organic adhesive can prevent dislocation between the aerogel-wet fiber sheet and the laminating material in the material transferring and hot-pressing plastic packaging process.
2. In the supercritical drying process, a plurality of groups of gel sheets with laminated films can be stacked up and down, and at the moment, a laminated film material is arranged between any two adjacent gel sheets, and a separation layer is formed between a plurality of gel sheets by the laminated film material, so that the condition of poor drying effect caused by too close lamination between the gel sheets is avoided. In addition, the frame and the frame wall of the frame body are provided with holes, which is favorable for the flow of supercritical fluid in the supercritical drying process and shortens the drying time.
3. Because the size of the coating material is larger than that of the gel sheet, after the supercritical drying, the coating material forms a packaging layer on the surface of the gel sheet, and the organic adhesive overflowed from the wet fiber felt in the supercritical drying process is packaged in the product through the coating material, so that the overflow organic adhesive is prevented from adhering to adjacent aerogel fiber products, and the product quality control is improved; in the supercritical drying process, the gel sheet and the film-coated material are combined together through the organic adhesive of the wet fiber, and certain positioning effect is realized on the gel sheet and the film-coated material in the supercritical drying process; if the aerogel-wet fiber sheet is prepared first and then is subjected to plastic packaging, the appearance and performance of the aerogel-wet fiber sheet can be influenced in the scraping process due to the fact that the organic adhesive of the wet fiber material overflows, and the powder falling phenomenon exists on the surface of the prepared aerogel-wet fiber sheet, when the plastic packaging is carried out, layering can be generated between the aerogel-wet fiber sheet and a plastic packaging film due to dust on the surface of the prepared aerogel-wet fiber sheet, so that the plastic packaging effect is poor.
4. The film-coated product prepared by the invention can be applied to the field of new energy, the battery packs are mutually isolated, and the safety and the reliability of the new energy battery pack during working are improved.
Detailed Description
The invention is described in further detail below in connection with specific embodiments.
Specific examples of the preparation method of the wet fiber sheet reinforced aerogel coated product of the present invention:
in the invention, the wet fiber sheet is a wet fiber mat in a sheet shape, and the wet fiber mat is a fiber mat prepared by using a non-woven wet technology. The non-woven wet method technology refers to a technology that fibers are molded by a wet molding instrument after being added with an organic adhesive, a dispersing agent and a thickening agent, wherein the wet molding instrument can be a wet fiber net rapid molding instrument or other molding instruments.
Example 1
In this embodiment, the preparation method of the wet fiber sheet reinforced aerogel film product includes the following steps:
step one: dipping the wet fiber sheet into silica sol for treatment, and obtaining a gel sheet after gel; in this step, the impregnation treatment is to pour the silica sol onto the wet fiber sheet.
Step two: and (3) respectively arranging the coating materials on the upper surface and the lower surface of the gel sheet obtained in the step (I), then placing the coated gel sheet in a frame with a clamping function, and performing supercritical drying treatment to obtain the aerogel-wet fiber sheet.
Step three: and (3) carrying out hot pressing treatment on the aerogel-wet fiber sheet obtained in the step two, so as to obtain an aerogel tectorial membrane product.
In the first step, the wet fiber sheet is a wet aluminum silicate fiber sheet, and the configuration step of the silica sol comprises the following steps: and (3) taking a silicon source, ethanol and water according to a molar ratio, uniformly mixing the silicon source, the ethanol and the water according to a ratio of silicon source to ethanol to water=1:30:12, and then adding an alkaline catalyst and uniformly stirring to obtain the silicon dioxide sol. The silicon source adopts methyltrimethoxysilane, and the alkaline catalyst adopts a mixed solution of ammonia water and ammonium fluoride.
In the second step, the PI film (polyimide film) is adopted as the film coating material, the peripheral size of the film coating material is larger than that of the gel sheet material by 3mm, and the film coating material on the upper surface and the lower surface of the gel sheet material can wrap the gel sheet material. The frame body is of a box-shaped structure with a bottom plate and surrounding baffles integrally formed around the bottom plate, and holes are formed in the surrounding baffles. When the film is coated, the PI film for hot pressing is directly coated on the upper surface and the lower surface of the gel sheet, and an organic adhesive is not required. Directly placing the gel sheet after film coating in a frame body, and adopting CO 2 The supercritical drying mode has the drying temperature of 40 ℃, the drying pressure of 8MPa, the heating speed of 5 ℃/min, the replacement time of 5h and the air release time of 5h. Because the enclosing wall is provided with holes, the supercritical fluid can flow in the supercritical drying process, and the drying time is shortened.
In the third step, the aerogel-wet fiber sheet material covered with the film is hot pressed in a hot press, the temperature of the hot pressing treatment is 100 ℃, and the hot pressing treatment is carried outFor 30s, the autoclave pressure was 10 kg/cm 2 . The hot pressing by the hot press belongs to the prior art, and specific hot pressing principles are not described in detail herein.
In this embodiment, the frame having the holding function is the frame for holding the upper and lower surfaces of the gel sheet after the film coating. The frame body is reserved with a frame body with a cavity for placing the single-group coated gel sheets, and the cavity of the frame body is matched with the coated gel sheets. The opposite inner walls of the frame body are contacted with the upper and lower surfaces of the gel sheet after being coated, and can prevent the gel sheet from slipping. And (5) respectively carrying out supercritical drying on the gel sheets after the film coating after the gel sheets are respectively contained in the frame body. Multiple groups of frames can be simultaneously subjected to supercritical drying.
In this embodiment, in the supercritical drying process, the organic adhesive in the aluminum silicate fiber sheet overflows and overflows between the PI film and the gel sheet, and since the size of the PI film is larger than that of the gel sheet, the organic adhesive cannot continuously overflow from the PI film and wash into the supercritical equipment and the tooling, so that a certain adhesive effect exists between the gel sheet and the PI film, dislocation between the PI film and the gel sheet is prevented, and the quality of the aerogel material to be dried in the next batch is not affected. In addition, the size of the PI film is larger than that of the gel sheet, so that the PI film can form packaging on the periphery of the gel sheet in the hot pressing process, and the phenomenon of powder falling of a formed film-covered product is avoided.
Example 2
In this embodiment, the preparation method of the wet fiber sheet reinforced aerogel film product includes the following steps:
step one: dipping the wet fiber sheet into aluminum sol for treatment, and obtaining a gel sheet after gel; in this step, the impregnation treatment is to brush an alumina sol on the wet fiber sheet.
Step two: and (3) respectively arranging the coating materials on the upper surface and the lower surface of the gel sheet obtained in the step (I), then placing the coated gel sheet in a frame with a clamping function, and performing supercritical drying treatment to obtain the aerogel-wet fiber sheet.
Step three: and (3) carrying out hot pressing treatment on the aerogel-wet fiber sheet obtained in the step two, so as to obtain an aerogel tectorial membrane product.
In the first step, the wet fiber sheet is a wet glass fiber sheet, and the aluminum sol configuration step comprises the following steps: preparing an aluminum source, a chelating agent, a solvent for aluminum sol, water and a catalyst for aluminum sol to obtain aluminum sol, wherein the molar ratio of the aluminum source, the chelating agent, the solvent for aluminum sol, the water and the catalyst for aluminum sol is 1:0.001:4:0.6:0.0001; the preparation method comprises the following specific preparation steps: firstly, uniformly mixing aluminum source sec-butyl alcohol aluminum and chelating agent ethyl acetoacetate, then adding solvent ethanol for aluminum sol, uniformly mixing, then adding water and catalyst acetic acid for aluminum sol, uniformly mixing, and obtaining aluminum sol.
In the second step, PC film (polycarbonate film) is adopted as the film coating material, the peripheral size of the film coating material is larger than that of the gel sheet material by 4mm, and the film coating material on the upper surface and the lower surface of the gel sheet material can wrap the gel sheet material. The frame body is still a box-shaped structure with a bottom plate and surrounding baffles integrally formed around the bottom plate, and holes are formed in the surrounding baffles. When the film is coated, the PC film for hot pressing is directly coated on the upper surface and the lower surface of the gel sheet, and an organic adhesive is not required. And directly placing the gel sheet after film coating in a frame body, and adopting an ethanol supercritical drying mode, wherein the drying temperature is 250 ℃, the drying pressure is 10MPa, the heating rate is 15 ℃/min, the supercritical state holding time is 3 hours, and the air release time is 5 hours.
In the third step, the aerogel-wet fiber sheet material covered by the film is hot pressed in a hot press, the temperature of the hot pressing treatment is 200 ℃, the time of the hot pressing treatment is 50s, and the pressure of the hot pressing treatment is 20 kg/cm 2 。
In this embodiment, the frame having the holding function is the frame for holding the upper and lower surfaces of the gel sheet after the film coating. The frame body is reserved with a cavity in which the gel sheets coated by a single group are placed, and a resilient spring plate is arranged in the cavity of the frame body. The gel sheet after the coating is put into the cavity and then clamped by the elastic sheet, and the inner walls of the elastic sheet and the frame body are respectively contacted with the upper surface and the lower surface of the gel sheet after the coating, so that the gel sheet can be prevented from slipping. And (5) respectively carrying out supercritical drying on the gel sheets after the film coating after the gel sheets are respectively contained in the frame body.
In this embodiment, although the manner of using wet fiber sheets, sol and coating materials and supercritical drying is changed, in the supercritical drying process, the organic adhesive in the glass fiber sheets still overflows between the PC film and the gel sheet, and cannot overflow from the PC film to wash into supercritical equipment and tools, so that a certain adhesive effect exists between the gel sheet and the PI film, dislocation between the PC film and the gel sheet is prevented, and the quality of the aerogel material to be dried in the next batch is not affected. In addition, in the hot pressing process, the PC film can form packaging on the periphery of the gel sheet, so that the phenomenon of powder falling of a formed film-covered product is avoided.
Example 3
In this embodiment, the preparation method of the wet fiber sheet reinforced aerogel film product includes the following steps:
step one: dipping the wet fiber sheet into silicon-aluminum composite sol for treatment, and obtaining a gel sheet after gel; in this step, the impregnation treatment is to spray an aluminum sol on the wet fiber sheet.
Step two: and (3) coating films on the upper surface and the lower surface of the gel sheet obtained in the step one, then placing the coated gel sheet in a frame with a clamping function, and performing supercritical drying treatment to obtain the aerogel-wet fiber sheet.
Step three: and (3) carrying out hot pressing treatment on the aerogel-wet fiber sheet obtained in the step two, so as to obtain an aerogel tectorial membrane product.
Specifically, in the first step, the wet fiber sheet adopts a wet quartz fiber sheet, and the configuration step of the silica-alumina composite sol comprises the following steps: (1) in terms of mole ratio, according to the silicon source: ethanol: uniformly mixing water=1:40:15, then adding an ammonium fluoride aqueous solution, and uniformly stirring to obtain silicon dioxide sol, wherein a silicon source is a mixed silicon source of methyltrimethoxysilane, dimethyldimethoxysilane and methyltriethoxysilane, and an alkali catalyst is the ammonium fluoride aqueous solution; (2) Preparing an aluminum source, a chelating agent, a solvent for aluminum sol, water and a catalyst for aluminum sol to obtain the aluminum sol, wherein the molar ratio of the aluminum source, the chelating agent, the solvent for aluminum sol, the water and the catalyst for aluminum sol is 1:0.06: 32:4:1, a step of; (3) And (3) uniformly mixing the silica sol obtained in the step (1) and the aluminum sol obtained in the step (2) to obtain the silicon-aluminum composite sol.
In the second step, the TPU film (thermoplastic polyurethane film) is adopted as the film coating material, the peripheral size of the film coating material is larger than that of the gel sheet material by 3mm, and the film coating material positioned on the upper surface and the lower surface of the gel sheet material can wrap the gel sheet material. The frame body is still a box-shaped structure with a bottom plate and surrounding baffles integrally formed around the bottom plate, and holes are formed in the surrounding baffles. When the film is coated, the TPU film for hot pressing is directly coated on the upper surface and the lower surface of the gel sheet, and an organic adhesive is not required. Directly placing the gel sheet after film coating in a frame body, and adopting CO 2 The supercritical drying mode has the drying temperature of 55 ℃, the drying pressure of 14MPa, the heating speed of 3 ℃/min, the supercritical state maintaining time of 12h and the air release time of 12h.
In the third step, the aerogel-wet fiber sheet covered with the TPU film is hot pressed in a hot press, the hot pressing temperature is 300 ℃, the hot pressing time is 100s, and the hot pressing pressure is 100 kg/cm 2 。
Example 4
This embodiment differs from embodiment 1 described above only in that: in this embodiment, more than two layers of gel sheets are stacked and placed in a frame, the film coating material is a PVC film, and the wet fiber sheet is a wet basalt fiber sheet.
In this embodiment, the frame having the holding function is a frame for holding the side surface of the laminated film-coated gel sheet. The frame body is reserved with a cavity for placing more than two layers of laminated gel sheets, and the cavity of the frame body is matched with the laminated gel sheets. The two opposite inner walls of the frame body are contacted with the two opposite side surfaces of the laminated film-covered gel sheet, and can prevent the laminated film-covered gel sheet from slipping. And (5) respectively carrying out supercritical drying on the gel sheets after the film coating after the gel sheets are respectively contained in the frame body. The side faces refer to the side edges of the superimposed gel sheets.
At this time, when carrying out supercritical drying, the organic adhesive that overflows from basalt fiber sheet can spill over towards the PVC membrane of both sides simultaneously, makes the PVC membrane that is in between two-layer adjacent gel sheets can bond with two-layer adjacent gel sheet simultaneously, and the PVC membrane forms the separate layer between polylith gel sheet to the condition that the drying effect that causes is bad is too laminated between the gel sheet to avoid appearing.
In summary, the preparation method of the wet fiber sheet reinforced aerogel coated product of the present invention is not limited to the above 4 embodiments, and includes various other embodiments, such as:
1. the wet fiber sheet may also be one of a wet mullite fiber sheet and a wet alumina fiber sheet.
2. The coating material can also adopt one of PET film, PTFE film, PE film, PS film and PP film.
3. In the preparation of the silica sol, the silica sol obtained by mixing is satisfactory as long as the ratio of the silicon source to the ethanol to the water is within the range of 1: (2-60) to (1-30). The silicon source can also be one of butyl orthosilicate, isopropyl orthosilicate and alkylalkoxy silane, and the alkylalkoxy silane comprises one or more of methyltrimethoxysilane, dimethyldimethoxysilane, methyltriethoxysilane, dimethyldiethoxysilane, vinyltriethoxysilane, propyltrimethoxysilane and propyltriethoxysilane; the basic catalyst can also be one or two of sodium hydroxide, potassium hydroxide, ammonia water, ammonium fluoride, ammonium bicarbonate, sodium carbonate, sodium bicarbonate, ethanolamine, diethanolamine, methylamine, dimethylamine, ethylamine, diethylamine, propylamine, dipropylamine, isopropanolamine, aniline, o-phenylenediamine, m-phenylenediamine and p-phenylenediamine. Of course, an acidic catalyst may be additionally added to the silica sol.
In the preparation of the aluminum sol, the molar ratio of the aluminum source, the chelating agent, the solvent for aluminum sol, water and the catalyst for aluminum sol is 1: (0.001 to 0.06): (4-32): (0.6 to 4): in the ratio range of (0.0001-1), the mixed aluminum sol meets the requirements; the aluminum source can be one or the combination of more than two of aluminum isopropoxide, aluminum sec-butoxide and aluminum nitrate; the chelating agent comprises one of acetylacetone and ethyl acetoacetate; the solvent for aluminum sol may be one or a combination of two or more selected from the group consisting of ethanol, isopropanol and n-butanol; the catalyst for aluminum sol may be one or a combination of more than two of sodium hydroxide, potassium hydroxide, ammonia water and ammonium fluoride.
4. When ethanol supercritical drying is adopted, the drying temperature is within 245-260 ℃, the drying pressure is within 8-14 MPa, the heating rate is within 5-20 ℃/min, the supercritical state holding time is within 0.5-3 h, and the air release time is within 3-9 h, so that the preparation requirements can be met.
Similarly, when CO2 supercritical drying is adopted, the drying temperature is within the range of 40-55 ℃, the drying pressure is within the range of 8-14 MPa, the heating speed is within the range of 1-5 ℃/min, the replacement time is within the range of 3-12 h, and the air release time is within the range of 3-12 h, so that the preparation requirements can be met.
5. The temperature of the hot pressing treatment is 80-300 ℃, the time of the hot pressing treatment is 20-100 s, and the pressure is 1 kg/cm 2 ~100 kg/ cm 2 Can meet the hot pressing requirement in the range.
Examples of wet laid fiber sheet reinforced aerogel coated products of the invention:
the wet fiber sheet reinforced aerogel coated product is produced by the method for producing the wet fiber sheet reinforced aerogel coated product described in each of the above embodiments, and will not be described in detail herein. The prepared wet fiber sheet reinforced aerogel film product comprises an aerogel-wet fiber sheet and film materials arranged on the upper surface and the lower surface of the aerogel-wet fiber sheet, wherein the wet fiber sheet comprises an organic adhesive; the aerogel-wet fiber sheet and the coating material are fixed by an organic adhesive overflowed from the wet fiber sheet in the supercritical drying process, and the periphery of the coating material is reserved beyond the edge of the aerogel-wet fiber sheet and is subjected to hot-pressing plastic package. Wherein the organic adhesive comprises more than one of phenolic resin adhesive, epoxy resin adhesive, urea-formaldehyde resin adhesive, polyacrylic resin adhesive, melamine-formaldehyde adhesive and polyurethane adhesive.
The embodiments of the present invention described above do not limit the scope of the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the scope of the present invention as set forth in the appended claims.

Claims (9)

1. A wet fiber sheet reinforced aerogel coated product, characterized by: the laminated product comprises an aerogel-wet fiber sheet and laminated materials arranged on the upper surface and the lower surface of the aerogel-wet fiber sheet, wherein the wet fiber sheet contains an organic adhesive; the aerogel-wet fiber sheet and the coating material are fixed by an organic adhesive overflowed from the wet fiber sheet in the supercritical drying process, and the periphery of the coating material is reserved beyond the edge of the aerogel-wet fiber sheet and is subjected to hot-pressing plastic package;
the preparation method of the film-covered product comprises the following steps:
step one: dipping the wet fiber sheet into sol, and obtaining a gel sheet after gel;
step two: the method comprises the steps of respectively arranging a film coating material on the upper surface and the lower surface of a gel sheet, placing the gel sheet after film coating in a frame body with a clamping function, and performing supercritical drying treatment to obtain an aerogel-wet fiber sheet, wherein the peripheral size of the film coating material is larger than that of the gel sheet;
step three: performing hot pressing treatment on the aerogel-wet fiber sheet obtained in the step two to obtain an aerogel film-covered product;
in the second step, a plurality of holes for the supercritical fluid to pass through are formed in the frame body.
2. A wet laid fiber sheet reinforced aerogel coated product as set forth in claim 1 wherein: the organic adhesive comprises more than one of phenolic resin adhesive, epoxy resin adhesive, urea-formaldehyde resin adhesive, polyacrylic resin adhesive, melamine-formaldehyde adhesive and polyurethane adhesive.
3. A method of preparing a wet laid fiber sheet reinforced aerogel coated product as claimed in claim 1 or 2, comprising the steps of:
step one: dipping the wet fiber sheet into sol, and obtaining a gel sheet after gel;
step two: the method comprises the steps of respectively arranging a film coating material on the upper surface and the lower surface of a gel sheet, placing the gel sheet after film coating in a frame body with a clamping function, and performing supercritical drying treatment to obtain an aerogel-wet fiber sheet, wherein the peripheral size of the film coating material is larger than that of the gel sheet;
step three: performing hot pressing treatment on the aerogel-wet fiber sheet obtained in the step two to obtain an aerogel film-covered product;
in the second step, a plurality of holes for the supercritical fluid to pass through are formed in the frame body.
4. A method of preparing a wet fiber sheet reinforced aerogel coated product as claimed in claim 3, wherein in step one, the impregnating applies the sol to the wet fiber sheet by pouring, spraying, brushing, dipping, or any combination thereof.
5. A method of preparing a wet laid fiber sheet reinforced aerogel coated product as claimed in claim 3, wherein in step one, the sol is one of silica sol, alumina sol or silica alumina composite sol.
6. The method of preparing a wet fiber sheet reinforced aerogel coated product of claim 3, wherein the wet fiber sheet is one of a wet aluminum silicate fiber sheet, a wet glass fiber sheet, a wet basalt fiber sheet, a wet mullite fiber sheet, a wet quartz fiber sheet, and a wet aluminum oxide fiber sheet.
7. A method of preparing a wet laid fiber sheet reinforced aerogel coated product according to claim 3, wherein the coating material used is one of PI film, PET film, PVC film, PTFE film, TPU film, PC film, PE film, PS film and PP film.
8. The method for preparing a wet fiber sheet reinforced aerogel film product according to claim 3, wherein the supercritical drying temperature is 40-55 ℃ and the pressure is 7-20 mpa.
9. The method for preparing a wet fiber sheet reinforced aerogel coated product according to claim 3, wherein the hot pressing temperature is 80 ℃ to 300 ℃, the hot pressing time is 20s to 100s, and the pressure is 1 kg/cm 2 ~100 kg/cm 2 。
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107035008A (en) * 2017-04-05 2017-08-11 天津市建筑材料科学研究院 A kind of cladding aeroge fibrofelt and its wet method composite preparation process
CN113443889A (en) * 2020-03-27 2021-09-28 江苏泛亚微透科技股份有限公司 Silicon dioxide aerogel glass fiber felt composite material sheet for electric vehicle storage battery, heat insulation pad product and application of silicon dioxide aerogel glass fiber felt composite material sheet
CN113620643A (en) * 2021-09-18 2021-11-09 巩义市泛锐熠辉复合材料有限公司 Preparation method of powder falling prevention silicon dioxide aerogel felt
CN113651592A (en) * 2021-08-20 2021-11-16 巩义市泛锐熠辉复合材料有限公司 Preparation method of anti-buffering silicon dioxide aerogel heat insulation sheet

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107035008A (en) * 2017-04-05 2017-08-11 天津市建筑材料科学研究院 A kind of cladding aeroge fibrofelt and its wet method composite preparation process
CN113443889A (en) * 2020-03-27 2021-09-28 江苏泛亚微透科技股份有限公司 Silicon dioxide aerogel glass fiber felt composite material sheet for electric vehicle storage battery, heat insulation pad product and application of silicon dioxide aerogel glass fiber felt composite material sheet
CN113651592A (en) * 2021-08-20 2021-11-16 巩义市泛锐熠辉复合材料有限公司 Preparation method of anti-buffering silicon dioxide aerogel heat insulation sheet
CN113620643A (en) * 2021-09-18 2021-11-09 巩义市泛锐熠辉复合材料有限公司 Preparation method of powder falling prevention silicon dioxide aerogel felt

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