Fiber-reinforced aerogel fireproof and thermal insulation sheet and preparation method thereof
By dispersing fibers, mixing aerogels, and coating molding, combined with melamine foam, a fiber-reinforced aerogel fireproof and heat-insulating sheet with low density, low thermal conductivity, low water absorption, and high flame retardancy was prepared. This solved the problems of insufficient performance and complex and costly preparation in the existing technology, and is suitable for the construction, industrial, and new energy fields.
Patent Information
- Application Number
- CN202211720721.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-12-30
- Publication Date
- 2025-12-12
- Estimated Expiration
- 2042-12-30
AI Technical Summary
Existing fiber-reinforced aerogel fireproof and heat-insulating sheets have shortcomings in balancing low thermal conductivity, specific heat capacity, density, water absorption and flame retardant properties, and the preparation process is complex and costly.
Fiber-reinforced aerogel fireproof and heat-insulating sheets were prepared by dispersing fibers, mixing aerogels, coating and molding. By using melamine foam to compound with other components, the sintering step was avoided, ensuring the uniformity and adhesion of the aerogel powder.
The prepared fiber-reinforced aerogel fireproof and heat-insulating sheet has low density, low thermal conductivity, low water absorption and high flame retardancy. Its comprehensive performance is superior to similar products on the market, and it is suitable for the construction, industrial and new energy fields.
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the field of fireproof thermal insulation and aerogel, in particular to a kind of fiber reinforced aerogel fireproof thermal insulation sheet and preparation method thereof. BACKGROUND
[0002] Aerogel is widely used in thermal insulation and adsorption due to its low density, low thermal conductivity and high porosity. Currently, aerogel sheets on the market are mainly made by two methods. The first method is to dry the aerogel precursor directly into a large piece of aerogel sheet. This method is extremely high in cost and extremely difficult in technology, and the thickness of the sheet is limited, so few people use it. The second method is to make a sheet by sintering the prepared aerogel powder or to load the aerogel powder on other sheets by coating. Although this method is lower in cost, sintering can damage the structure of the aerogel itself, and coating can easily cause uneven distribution of the aerogel powder. Therefore, the thermal conductivity of this type of material is generally high, and the use of the material is limited.
[0003] For the fiber reinforced aerogel fireproof thermal insulation sheet used in new energy batteries, in addition to the high requirement for its thermal conductivity, the specific heat capacity, density, water absorption and flame retardant performance of the thermal insulation sheet itself also have higher requirements. The same type of product on the market is difficult to achieve a fiber reinforced aerogel fireproof thermal insulation sheet with low thermal conductivity and good performance, and the operation is complex and the preparation cost is high. SUMMARY
[0004] The present application discloses a preparation method of a fiber reinforced aerogel fireproof thermal insulation sheet to solve the above problems and overcome the shortcomings of the prior art. The preparation method is simple and easy to operate, has no sintering step, and the obtained product powder is more uniform and not easy to fall off.
[0005] In order to achieve the above purposes, the specific technical scheme of the present application is as follows:
[0006] A preparation method of a fiber reinforced aerogel fireproof thermal insulation sheet, comprising the following steps:
[0007] S1, dispersing fibers: adding dispersant, adhesive and fibers into a solvent, respectively, and dissolving the mixture at room temperature. After cooling to room temperature, a fiber slurry is obtained and is ready for use;
[0008] S2, mixing aerogel: adding aerogel powder and melamine foam into the fiber slurry prepared in S1, respectively, and stirring to obtain a fiber reinforced aerogel slurry;
[0009] S3, coating: pour the fiber-reinforced aerogel slurry prepared in S2 into a mold with a sheet on the upper and lower surfaces, then scrape the slurry flat and close the mold; or use a coater to spread the fiber-reinforced aerogel slurry prepared in S2 on the sheet;
[0010] S4, molding: heat or vacuum heat the mold or sheet; after demolding or slicing, plastic encapsulation is performed, and finally the fiber-reinforced aerogel fireproof and heat insulation sheet is obtained.
[0011] As a preferred embodiment in the present application, the solvent in S1 is any one or a mixture of multiple of water, n-hexane, cyclohexane, n-pentane, cyclopentane, dioxane, ethanol, methanol, n-propanol or isopropanol.
[0012] As a preferred embodiment in the present application, the dispersing agent in S1 is any one or a mixture of multiple of phytic acid, oleic acid, stearic acid, lauric acid, lanolin acid, polyethylene glycol or polyvinyl alcohol.
[0013] As a preferred embodiment in the present application, the adhesive in S1 is any one or a mixture of multiple of tetraethyl orthosilicate, silane coupling agent KH550, KH560, KH570 or KH580.
[0014] As a preferred embodiment in the present application, the fiber in S1 is any one or multiple of aluminum silicate fiber, zirconia fiber or glass fiber.
[0015] As a preferred embodiment in the present application, the aerogel in S2 is any one or multiple of silica aerogel, alumina aerogel or phenolic aerogel.
[0016] As a preferred embodiment in the present application, the gasket in S3 is any one or multiple of glass fiber, carbon fiber, ceramic fiber, hydroxyapatite paper, natural organic polymer or petroleum-based polymer to make fabric, non-woven fabric or paper.
[0017] As a preferred embodiment in the present application, the specific steps for using a mold for coating in S3 are as follows:
[0018] a. When designing the mold, the mold cavity thickness is controlled to be 4 mm; a sheet is placed on the upper and lower surfaces of the mold;
[0019] b. Pour the fiber-reinforced aerogel slurry into the lower mold of the mold, and use a scraper to spread it flat;
[0020] c. Close the upper and lower molds, and remove the air bubbles between the upper gasket and the slurry, then place the mold in a press machine and apply pressure from top to bottom.
[0021] As a preferred embodiment in the application, the molding is preheated to 90 DEG C under non-vacuum condition, part of the solvent is removed after 30 minutes, and then the temperature is raised to 150 DEG C under non-vacuum condition for 60 minutes.
[0022] Another object of the application is to protect a fiber-reinforced aerogel fireproof and thermal insulation sheet prepared by the above method, which has low density, low thermal conductivity, low water absorption and high flame retardancy.
[0023] Compared with the prior art, the positive effects of the application are reflected in:
[0024] (I) Because melamine foam is used in the formula and other components are well compounded, the water absorption rate is reduced while the thermal conductivity and density are reduced, and the negative effects of using a large amount of aerogel material are reduced.
[0025] (II) The fiber-reinforced aerogel fireproof and thermal insulation sheet prepared by the application has low density, low thermal conductivity, low water absorption and high flame retardancy, and the comprehensive performance is better than that of similar products on the market, and can be widely used in fields requiring fireproofing or thermal insulation such as building, industry and new energy.
[0026] (III) The preparation method does not use sintering or other steps, and the product has better comprehensive performance than the product prepared by sintering, and the powder of the aerogel sheet prepared by the traditional coating method is more uniform and not easy to fall off. DETAILED DESCRIPTION
[0027] In order to better explain the content of the application, the application will be further described by specific examples below, but it should not be understood that the protection scope of the application is limited to this, all the features disclosed in the inventive content of the application, or all the steps in the disclosed method or process, can be combined in any way, except for mutually exclusive features and / or steps. Any feature disclosed in the application can be replaced by other equivalent or similar features unless specifically stated. That is, unless specifically stated, each feature is only an example of a series of equivalent or similar features.
[0028] At the same time, it should be understood that the terms such as "have", "contain" and "include" used in this paper do not exclude the presence or addition of one or more other elements or combinations thereof.
[0029] In addition, it is worth mentioning that the thermal conductivity of the test product obtained by the following examples is determined by FOX200 heat flow meter method of TA company of USA at 25℃ according to the test standard of GB / T10295-2008; the specific heat capacity of the test product is determined by Q200 differential scanning calorimeter of TA company of USA according to the test standard of ASTM E1269-2011; the flame retardant grade is determined by CZF-2 type vertical burning instrument according to UL-94 standard; the water absorption rate is tested and calculated after placing in the environment of relative humidity 50% and temperature 23.0℃±1.0℃ for 24h according to the method in GB / T 1034-2008 standard.
[0030] Example 1:
[0031] A preparation method of a fiber-reinforced aerogel fireproof and thermal insulation sheet, comprising the following steps:
[0032] S1, dispersing fibers: taking water mass as 100 parts (each part can be regarded as 1 kg), adding 0.1 parts of phytic acid, 0.1 parts of tetraethyl orthosilicate and 1 part of aluminum silicate fiber into the water. The mixture is dissociated by a stirrer at a speed of 5000r / min for 3h at room temperature. After cooling to room temperature, it is used.
[0033] S2, mixing aerogel: 1 part of silica aerogel powder and 1 part of melamine foam are added to the dispersed fiber slurry. The fiber-reinforced aerogel slurry is obtained by stirring with a stirrer at a speed of 5000r / min for 0.5h.
[0034] S3, coating: pour the fiber slurry into the mold with glass cloth on the upper and lower surfaces, and then close the mold after scraping the slurry flat. The specific steps are as follows:
[0035] When using the mold for coating:
[0036] a. When designing the mold, the thickness of the mold cavity is controlled at 4mm; the upper and lower surfaces of the mold are padded with a sheet.
[0037] b. Pour the slurry into the lower mold of the mold, and use a scraper to spread it flat.
[0038] c. Close the upper and lower molds, and remove the bubbles between the upper pad and the slurry. Then put the mold into the press and apply pressure from top to bottom.
[0039] S4, molding: the mold or sheet is subjected to non-vacuum heating treatment. After demolding or slicing, it is plastic sealed, and finally the fiber-reinforced aerogel sheet is obtained. The specific steps are as follows: the coated mold is directly placed on the hot press for pressure and temperature rise. First, preheat at 90℃ under non-vacuum condition for 30min to remove part of the solvent, then heat to 150℃ under non-vacuum condition for 60min to form. Then, without removing the pad, vacuum plastic sealing is carried out.
[0040] The density of the obtained fiber-reinforced aerogel thermal insulation sheet is 247 kg / m 3 , the thermal conductivity is 0.034 W / (m·K), the specific heat capacity is 0.21 J / (g·℃), the flame retardant level is UL94 V-0 level, and the water absorption rate is 2.8%.
[0041] Example 2:
[0042] A method for preparing a fiber-reinforced aerogel fireproof thermal insulation sheet, comprising the following steps:
[0043] S1, dispersing fibers: taking the mass of n-hexane as 100 parts, adding 0.1 parts of oleic acid, 0.1 parts of silane coupling agent KH550, and 1 part of zirconium oxide fiber. Dissociate the mixture with a fiber disperser or a stirrer at a speed of 5000 r / min for 3 h at room temperature. After cooling to room temperature, it is used.
[0044] S2, mixing aerogel: taking the mass of the solvent as 100 parts, adding 1 part of aluminum oxide aerogel powder and 1 part of melamine foam to the dispersed fiber slurry. Stir with a stirrer at a speed of 5000 r / min for 0.5 h to obtain a fiber-reinforced aerogel slurry.
[0045] S3, coating: spread the slurry on the carbon fiber cloth with a coating machine. The specific steps are:
[0046] When using a mold to coat:
[0047] a. When designing the mold, control the thickness of the mold cavity to be 4 mm; pad the upper and lower surfaces of the mold with sheet materials.
[0048] b. Pour the slurry into the lower mold of the mold, and use a scraper to spread it flat.
[0049] c. Close the upper and lower molds, and remove the air bubbles between the upper gasket and the slurry. Then put the mold into the press and apply pressure from top to bottom.
[0050] S4, molding: heat treat the mold or sheet material under non-vacuum conditions. After demolding or slicing, it is plastic sealed, and finally the fiber-reinforced aerogel sheet is obtained. The specific steps are: place the coated mold directly on the hot press and apply pressure and heat. First, preheat to 90℃ under non-vacuum conditions for 30 min to remove part of the solvent, then heat to 150℃ under non-vacuum conditions for 60 min to form. Then, without removing the gasket, vacuum plastic sealing is performed.
[0051] The density of the obtained fiber-reinforced aerogel thermal insulation sheet is 235 kg / m 3 , the thermal conductivity is 0.034 W / (m·K), the specific heat capacity is 0.22 J / (g·℃), the flame retardant level is UL94 V-0 level, and the water absorption rate is 2.7%.
[0052] Example 3:
[0053] A method for preparing a fiber-reinforced aerogel fireproof thermal insulation sheet, comprising the following steps:
[0054] S1, dispersing fibers: taking cyclohexane as 100 parts by mass, adding 1 part of stearic acid, 1 part of silane coupling agent KH560, and 10 parts of glass fiber. The mixture is dissociated at room temperature for 3 h by a fiber disperser or a stirrer at a speed of 5000 r / min. After cooling to room temperature, it is used.
[0055] S2, mixing aerogel: taking the solvent as 100 parts by mass, adding 10 parts of phenolic aerogel powder to the dispersed fiber slurry. Stirring is performed at a speed of 5000 r / min for 0.5 h by a stirrer to obtain a fiber-reinforced aerogel slurry.
[0056] S3, coating: the slurry is laid on a ceramic fiber cloth by a coating machine. The specific steps are as follows:
[0057] When using a mold for coating:
[0058] a. When designing the mold, the thickness of the mold cavity is controlled to be 4 mm; the upper and lower surfaces of the mold are padded with a sheet.
[0059] b. Pour the slurry into the lower mold of the mold, and use a scraper to flatten it.
[0060] c. Close the upper and lower molds, and remove the air bubbles between the upper gasket and the slurry. Then place the mold in a press machine and apply pressure from top to bottom.
[0061] S4, molding: the mold or sheet is subjected to non-vacuum heating treatment. After demolding or slicing, it is plastic-wrapped, and finally a fiber-reinforced aerogel sheet is obtained. The specific steps are as follows: the coated mold is directly placed on a hot press for pressure and temperature increase. First, preheat at 90℃ under non-vacuum conditions for 30 min to remove part of the solvent, then heat to 150℃ under non-vacuum conditions for 60 min to form. Then, without removing the gasket, vacuum plastic-wrapped.
[0062] The density of the obtained fiber-reinforced aerogel thermal insulation sheet is 356 kg / m 3 , the thermal conductivity is 0.031 W / (m·K), the specific heat capacity is 0.24 J / (g·℃), the flame retardant level is UL94 V-2 level, and the water absorption rate is 3.5%.
[0063] Example 4:
[0064] A method for preparing a fiber-reinforced aerogel fireproof thermal insulation sheet, comprising the following steps:
[0065] S1, dispersing fibers: taking the mass of n-pentane as 100 parts, adding 1 part of lauric acid, 1 part of silane coupling agent KH570, and 10 parts of aluminum silicate fibers into it. Dissociate the mixture at room temperature with a fiber disperser or a stirrer at a speed of 5000 r / min for 3 h. Use it after it cools down to room temperature.
[0066] S2, mixing aerogel: taking the mass of solvent as 100 parts, adding 5 parts of silica aerogel and 5 parts of alumina aerogel powder and 1 part of melamine foam into the dispersed fiber slurry. Stir it with a stirrer at a speed of 5000 r / min for 0.5 h to obtain a fiber-reinforced aerogel slurry.
[0067] S3, coating: spread the slurry on the ceramic fiber felt with a coating machine. The specific steps are as follows:
[0068] When using a mold to coat:
[0069] a. When designing the mold, control the thickness of the mold cavity to be 4 mm; pad the upper and lower surfaces of the mold with sheets.
[0070] b. Pour the slurry into the lower mold of the mold, and spread it flat with a scraper.
[0071] c. Close the upper and lower molds, and get rid of the air bubbles between the upper gasket and the slurry. Then put the mold into the press and apply pressure from top to bottom.
[0072] S4, forming: heat treat the mold or sheet under non-vacuum conditions. After demolding or slicing, seal it in a plastic bag to obtain a fiber-reinforced aerogel sheet. The specific steps are as follows: place the coated mold directly on the hot press and apply pressure and heat. First, preheat it to 90℃ under non-vacuum conditions for 30 min to remove part of the solvent, then heat it to 150℃ under non-vacuum conditions for 60 min to form. Then, without removing the gasket, perform vacuum sealing.
[0073] The density of the obtained fiber-reinforced aerogel thermal insulation sheet is 368 kg / m 3 , the thermal conductivity is 0.032 W / (m·K), the specific heat capacity is 0.24 J / (g·℃), the flame retardant level is UL94 V-0 level, and the water absorption rate is 3.0%.
[0074] Example 5:
[0075] A method for preparing a fiber-reinforced aerogel fireproof thermal insulation sheet, comprising the following steps:
[0076] S1, dispersing fibers: taking the mass of n-pentane as 100 parts, adding 1 part of lauric acid, 1 part of silane coupling agent KH570, and 10 parts of aluminum silicate fibers into it. Dissociate the mixture at room temperature with a fiber disperser or a stirrer at a speed of 5000 r / min for 3 h. Use it after it cools down to room temperature.
[0077] S2, mixed aerogel: 10 parts of silica aerogel powder and 1 part of melamine foam are added to the dispersed fiber slurry, taking the solvent mass as 100 parts. Stirring is performed at a speed of 5000 r / min for 0.5 h using a stirrer to obtain a fiber-reinforced aerogel slurry.
[0078] S3, coating: the slurry is laid flat on the ceramic fiber paper using a coating machine. The specific steps are as follows:
[0079] When using a mold to coat:
[0080] a. When designing the mold, the thickness of the mold cavity is controlled to be 4 mm; the upper and lower surfaces of the mold are padded with a sheet.
[0081] b. Pour the slurry into the lower mold of the mold, and use a scraper to flatten it.
[0082] c. Close the upper and lower molds, and remove the air bubbles between the upper gasket and the slurry. Then place the mold in the press and apply pressure from top to bottom.
[0083] S4, molding: the mold or sheet is subjected to non-vacuum heating treatment. After demolding or slicing, it is plastic sealed, and finally a fiber-reinforced aerogel sheet is obtained. The specific steps are as follows: the coated mold is directly placed on the hot press for pressure and temperature rise. First, preheat at 90℃ under non-vacuum conditions for 30 min to remove part of the solvent, then heat to 150℃ under non-vacuum conditions for 60 min to form. Then, without removing the gasket, vacuum plastic sealing is performed.
[0084] The density of the obtained fiber-reinforced aerogel thermal insulation sheet is 328 kg / m 3 , the thermal conductivity is 0.026 W / (m·K), the specific heat capacity is 0.27 J / (g·℃), the flame retardant level is UL94 V-0 level, and the water absorption rate is 3.7%.
[0085] Example 6:
[0086] A method for preparing a fiber-reinforced aerogel fireproof thermal insulation sheet, comprising the following steps:
[0087] S1, dispersing fibers: 1 part of polyethylene glycol, 1 part of tetraethyl orthosilicate, and 10 parts of aluminum silicate fiber are added to 1,4-dioxane with a mass of 100 parts. The mixture is dissociated at room temperature using a fiber disperser or a stirrer at a speed of 5000 r / min for 3 h. It is used after cooling to room temperature.
[0088] S2, mixed aerogel: 10 parts of silica aerogel powder and 3 parts of melamine foam are added to the dispersed fiber slurry, taking the solvent mass as 100 parts. Stirring is performed at a speed of 5000 r / min for 0.5 h using a stirrer to obtain a fiber-reinforced aerogel slurry.
[0089] S3, coating: the slurry is spread on the hydroxyapatite paper with a coating machine. The specific steps are:
[0090] When using a mold to coat:
[0091] a. When designing the mold, the cavity thickness is controlled at 4 mm; the upper and lower surfaces of the mold are padded with a sheet.
[0092] b. Pour the slurry into the lower mold of the mold, and use a scraper to spread it flat.
[0093] c. Close the upper and lower molds, and remove the air bubbles between the upper gasket and the slurry. Then put the mold into the press and apply pressure from top to bottom.
[0094] S4, forming: the mold or sheet is subjected to non-vacuum heating treatment. After demolding or slicing, it is plastic sealed, and finally the fiber reinforced aerogel sheet is obtained. The specific steps are: the coated mold is directly placed on the hot press for pressure and temperature rise. First, preheat at 90℃ for 30min to remove part of the solvent, then heat to 150℃ under non-vacuum conditions for 60min to form. Then, without removing the gasket, vacuum plastic sealing is carried out.
[0095] The density of the obtained fiber reinforced aerogel thermal insulation sheet is 382 kg / m 3 , the thermal conductivity is 0.025 W / (m·K), the specific heat capacity is 0.27 J / (g·℃), the flame retardant level is UL94 V-2 level, and the water absorption rate is 4.5%.
[0096] Example 7:
[0097] A method for preparing a fiber reinforced aerogel fireproof thermal insulation sheet, comprising the following steps:
[0098] S1, dispersion of fibers: taking the mass of ethanol as 100 parts, adding polyvinyl alcohol 1 part, silane coupling agent KH550 1 part, and aluminum silicate fiber 1 part. The mixture is dissociated with a fiber disperser or a stirrer at a speed of 5000 r / min for 3h at room temperature. After cooling to room temperature, it is used.
[0099] S2, mixing aerogel: taking the mass of solvent as 100 parts, adding 10 parts of silica aerogel powder and 5 parts of melamine foam to the dispersed fiber slurry. Stir with a stirrer at a speed of 5000 r / min for 0.5h to obtain a fiber reinforced aerogel slurry.
[0100] S3, coating: the slurry is spread on the cotton fiber cloth with a coating machine. The specific steps are:
[0101] When using a mold to coat:
[0102] a. When designing the mold, the cavity thickness is controlled at 4 mm; the upper and lower surfaces of the mold are padded with a sheet.
[0103] b. Pour the slurry into the lower mold of the mold, and use a scraper to flatten it.
[0104] c. Close the upper and lower molds, and remove the air bubbles between the upper pad and the slurry. Then place the mold in the press and apply pressure from above and below.
[0105] S4, molding: the mold or sheet is subjected to non-vacuum heating treatment. After demolding or slicing, it is plasticized and sealed, and finally the fiber reinforced aerogel sheet is obtained. The specific steps are: the coated mold is directly placed on the hot press for pressure and temperature rise. First, preheat at 90℃ under non-vacuum conditions for 30min to remove part of the solvent, then heat to 150℃ under non-vacuum conditions for 60min to form. Then, without removing the pad, vacuum sealing is carried out.
[0106] The density of the obtained fiber reinforced aerogel thermal insulation sheet is 228kg / m 3 , the thermal conductivity is 0.029W / (m·K), the specific heat capacity is 0.26J / (g·℃), the flame retardant level is UL94 N.R. grade, and the water absorption rate is 3.2%.
[0107] Example 8:
[0108] A method for preparing a fiber reinforced aerogel fireproof thermal insulation sheet, comprising the following steps:
[0109] S1, dispersion of fibers: taking methanol as 100 parts by mass, adding 1 part of lanolin acid, 1 part of silane coupling agent KH550, and 10 parts of aluminum silicate fiber. The mixture is dissociated by a fiber disperser or a stirrer at a speed of 5000r / min for 3h at room temperature. After cooling to room temperature, it is used.
[0110] S2, mixing aerogel: taking the solvent as 100 parts by mass, adding 10 parts of silica aerogel powder and 3 parts of melamine foam to the dispersed fiber slurry. Stir with a stirrer at a speed of 5000r / min for 0.5h to obtain a fiber reinforced aerogel slurry.
[0111] S3, coating: the slurry is spread on the terylene cloth with a coating machine. The specific steps are:
[0112] When using a mold for coating:
[0113] a. When designing the mold, the cavity thickness is controlled at 4 mm; the upper and lower surfaces of the mold are padded with a sheet.
[0114] b. Pour the slurry into the lower mold of the mold, and use a scraper to flatten it.
[0115] c. Close the upper and lower molds, and remove the air bubbles between the upper gasket and the slurry. Then put the mold into the press and apply pressure from top and bottom.
[0116] S4, molding: non-vacuum heating treatment is performed on the mold or sheet. After demolding or slicing, it is plastic sealed, and finally the fiber reinforced aerogel sheet is obtained. The specific steps are: the coated mold is directly placed on the hot press for pressure and temperature rise. First, preheat at 90℃ for 30min under non-vacuum conditions to remove part of the solvent, then heat to 150℃ under non-vacuum conditions for 60min to form. Then, without removing the gasket, vacuum plastic sealing is performed.
[0117] The density of the obtained fiber reinforced aerogel thermal insulation sheet is 286kg / m 3 , the thermal conductivity is 0.021W / (m·K), the specific heat capacity is 0.31J / (g·℃), the flame retardant level is UL94 V-2 level, and the water absorption rate is 4.1%.
[0118] Example 9:
[0119] A method for preparing a fiber reinforced aerogel fireproof thermal insulation sheet, comprising the following steps:
[0120] S1, dispersion of fibers: taking the mass of n-propyl alcohol as 100 parts, adding 1 part of lanolin acid, 1 part of silane coupling agent KH560, and 10 parts of aluminum silicate fiber. The mixture is dissociated at a speed of 5000r / min for 3h by using a fiber disperser or a stirrer at room temperature. After cooling to room temperature, it is used.
[0121] S2, mixing aerogel: taking the mass of solvent as 100 parts, adding 10 parts of silica aerogel powder and 3 parts of melamine foam to the dispersed fiber slurry. Stir at a speed of 5000r / min for 0.5h by using a stirrer to obtain a fiber reinforced aerogel slurry.
[0122] S3, coating: the slurry is spread on the polyester-cotton blended fiber cloth by using a coating machine. The specific steps are:
[0123] When using a mold for coating:
[0124] a. When designing the mold, the thickness of the mold cavity is controlled at 4mm; the mold is padded with a sheet on both upper and lower surfaces.
[0125] b. Pour the slurry into the lower mold of the mold, and spread it flat with a scraper.
[0126] c. Close the upper and lower molds, and remove the air bubbles between the upper gasket and the slurry. Then put the mold into the press and apply pressure from top and bottom.
[0127] S4, molding: non-vacuum heating treatment is performed on the mold or sheet. After demolding or slicing, it is plastic sealed, and finally the fiber reinforced aerogel sheet is obtained. The specific steps are: the coated mold is directly placed on the hot press for pressure and temperature rise. First, preheat at 90℃ for 30min under non-vacuum conditions to remove part of the solvent, then heat to 150℃ under non-vacuum conditions for 60min to form. Then, without removing the gasket, vacuum plastic sealing is performed.
[0128] The density of the obtained fiber reinforced aerogel thermal insulation sheet is 271 kg / m 3 , the thermal conductivity is 0.022 W / (m·K), the specific heat capacity is 0.31 J / (g·℃), the flame retardant level is UL94 V-2 level, and the water absorption rate is 5.6%.
[0129] Example 10:
[0130] A method for preparing a fiber reinforced aerogel fireproof thermal insulation sheet, comprising the following steps:
[0131] S1, dispersion of fibers: taking isopropanol as 100 parts by mass, adding 1 part of lanolin acid, 1 part of silane coupling agent KH560, and 10 parts of glass fiber. The mixture is dissociated by a fiber disperser or a stirrer at a speed of 5000r / min for 3h at room temperature. After cooling to room temperature, it is used.
[0132] S2, mixing aerogel: taking the mass of the solvent as 100 parts, adding 10 parts of silica aerogel powder and 1 part of melamine foam to the dispersed fiber slurry. Stirring is performed at a speed of 5000r / min for 0.5h using a stirrer to obtain a fiber reinforced aerogel slurry.
[0133] S3, coating: the slurry is spread on the ceramic fiber cloth by a coating machine. The specific steps are:
[0134] When using a mold for coating:
[0135] a. When designing the mold, the thickness of the mold cavity is controlled at 4mm; the mold is padded with a sheet on the upper and lower surfaces.
[0136] b. Pour the slurry into the lower mold of the mold, and use a scraper to spread it flat.
[0137] c. Close the upper and lower molds, and remove the air bubbles between the upper gasket and the slurry. Then place the mold in the press and apply pressure from top to bottom.
[0138] S4, molding: non-vacuum heating treatment is performed on the mold or sheet. After demolding or slicing, it is plastic sealed, and finally the fiber reinforced aerogel sheet is obtained. The specific steps are: the coated mold is directly placed on the hot press for pressure and temperature rise. First, preheat at 90°C for 30 min under non-vacuum conditions to remove part of the solvent, then heat to 150°C under non-vacuum conditions for 60 min to form. Then, without removing the gasket, vacuum plastic sealing is performed.
[0139] The density of the obtained fiber reinforced aerogel thermal insulation sheet is 334 kg / m 3 , the thermal conductivity is 0.024 W / (m·K), the specific heat capacity is 0.29 J / (g·℃), the flame retardant level is UL94 V-0 level, and the water absorption rate is 3.8%.
[0140] Comparative Example 1:
[0141] The method of Example 1 is used to prepare the fiber reinforced aerogel fireproof thermal insulation sheet, and the preparation method is the same as that of Example 1, except that no melamine foam is added.
[0142] S1, dispersion of fibers: taking water as 100 parts (each part can be regarded as 1 kg), adding phytic acid 0.1 parts, tetraethyl orthosilicate 0.1 parts, and aluminum silicate fiber 1 part. The mixture is dissociated by a stirrer at a speed of 5000 r / min for 3 h at room temperature. After cooling to room temperature, it is used:
[0143] S2, mixing aerogel: 1 part of silica aerogel powder is added to the dispersed fiber slurry. Stir with a stirrer at a speed of 5000 r / min for 0.5 h to obtain a fiber reinforced aerogel slurry.
[0144] S3, coating: pour the fiber slurry into the mold with fiberglass cloth on the upper and lower surfaces, scrape the slurry flat, and then clamp the mold. The specific steps are:
[0145] When using a mold for coating:
[0146] a. When designing the mold, the mold cavity thickness is controlled at 4 mm; the mold is padded with a sheet on the upper and lower surfaces.
[0147] b. Pour the slurry into the lower mold of the mold, and use a scraper to spread it flat.
[0148] c. The upper and lower molds are clamped, and the air bubbles between the upper gasket and the slurry are removed. Then the mold is placed in the press machine to apply pressure from top to bottom.
[0149] S4, molding: non-vacuum heating treatment is performed on the mold or sheet. After demolding or slicing, it is plastic sealed, and finally the fiber reinforced aerogel sheet is obtained. The specific steps are: the coated mold is directly placed on the hot press for pressure and temperature rise. First, preheat at 90°C for 30 min under non-vacuum conditions to remove part of the solvent, then heat to 150°C under non-vacuum conditions for 60 min to form. Then, without removing the gasket, vacuum plastic sealing is performed.
[0150] The density of the obtained fiber reinforced aerogel thermal insulation sheet is 240 kg / m 3 , the thermal conductivity is 0.038 W / (m·K), the specific heat capacity is 0.21 J / (g·℃), the flame retardant level is UL94 V-2 level, and the water absorption rate is 2.7%.
[0151] Comparative Example 2:
[0152] The method of Example 1 is used to prepare the fiber reinforced aerogel fireproof thermal insulation sheet, and the preparation method is General Example 1, the only difference is that the melamine foam is replaced with an equal amount of aerogel:
[0153] S1, dispersion of fibers: taking water as 100 parts (each part can be regarded as 1 kg), adding phytic acid 0.1 parts, tetraethyl orthosilicate 0.1 parts, and aluminum silicate fiber 1 part. The mixture is dissociated by a stirrer at a speed of 5000 r / min for 3 h at room temperature. After cooling to room temperature, it is used.
[0154] S2, mixing aerogel: 1 part of silica aerogel powder and 1 part of melamine foam are added to the dispersed fiber slurry. Stir with a stirrer at a speed of 5000 r / min for 0.5 h to obtain a fiber reinforced aerogel slurry.
[0155] S3, coating: pour the fiber slurry into the mold with fiberglass cloth on the upper and lower surfaces, scrape the slurry flat, and then clamp the mold. The specific steps are:
[0156] When using the mold for coating:
[0157] a. When designing the mold, the mold cavity thickness is controlled at 4 mm; the mold is padded with a sheet on the upper and lower surfaces.
[0158] b. Pour the slurry into the lower mold of the mold, and use a scraper to spread it flat.
[0159] c. The upper and lower molds are clamped, and the air bubbles between the upper gasket and the slurry are removed. Then the mold is placed in the press machine to apply pressure from top to bottom.
[0160] S4, molding: non-vacuum heating treatment is performed on the mold or sheet. After demolding or slicing, it is plastic sealed, and finally the fiber reinforced aerogel sheet is obtained. The specific steps are: the coated mold is directly placed on the hot press for pressure and temperature rise. First, preheat at 90℃ for 30min under non-vacuum conditions to remove part of the solvent, then heat to 150℃ under non-vacuum conditions for 60min to form. Then, without removing the gasket, vacuum plastic sealing is performed.
[0161] The density of the obtained fiber reinforced aerogel thermal insulation sheet is 245kg / m 3 , the thermal conductivity is 0.033W / (m·K), the specific heat capacity is 0.22J / (g·℃), the flame retardant level is UL94 V-2 level, and the water absorption rate is 3.1%.
[0162] Comparative Example 3:
[0163] The method of Example 1 is used to prepare the fiber reinforced aerogel fireproof thermal insulation sheet, and the preparation method is General Example 1, the only difference is that the stirring rate is as low as 500r / min:
[0164] S1, dispersion of fibers: taking water as 100 parts (each part can be regarded as 1kg), adding phytic acid 0.1 parts, tetraethyl orthosilicate 0.1 parts, and aluminum silicate fiber 1 part. The mixture is dissociated by a stirrer at a speed of 500r / min for 3h at room temperature. After cooling to room temperature, it is used.
[0165] S2, mixing aerogel: 1 part of silica aerogel powder is added to the dispersed fiber slurry. Stir with a stirrer at a speed of 500r / min for 0.5h to obtain a fiber reinforced aerogel slurry.
[0166] S3, coating: pour the fiber slurry into the mold with fiberglass cloth on the upper and lower surfaces, scrape the slurry flat, and then clamp the mold. The specific steps are:
[0167] When using the mold for coating:
[0168] a. When designing the mold, the mold cavity thickness is controlled at 4mm; the mold is padded with a sheet on the upper and lower surfaces.
[0169] b. Pour the slurry into the lower mold of the mold, and use a scraper to spread it flat.
[0170] c. The upper and lower molds are clamped, and the air bubbles between the upper gasket and the slurry are removed. Then the mold is placed in the press machine to apply pressure from top to bottom.
[0171] S4, molding: non-vacuum heating treatment is performed on the mold or sheet. After demolding or slicing, it is plastic sealed, and finally the fiber reinforced aerogel sheet is obtained. The specific steps are: the coated mold is directly placed on the hot press for pressure and temperature rise. First, preheat at 90°C for 30 min under non-vacuum conditions to remove part of the solvent, then heat to 150°C under non-vacuum conditions for 60 min to form. Then, without removing the gasket, vacuum plastic sealing is performed.
[0172] The density of the obtained fiber reinforced aerogel thermal insulation sheet is 247 kg / m 3 , the thermal conductivity is 0.037 W / (m·K), the specific heat capacity is 0.21 J / (g·℃), the flame retardant level is UL94 V-2 level, and the water absorption rate is 2.8%.
[0173] Comparative Example 4:
[0174] The method of Example 1 is used to prepare the fiber reinforced aerogel fireproof thermal insulation sheet, and the preparation method is General Example 1, the only difference is that the preheating process is skipped in the S4, molding step, and the temperature is directly raised to 150°C for 60 min to form:
[0175] S1, dispersion of fibers: taking water as 100 parts (each part can be regarded as 1 kg), adding phytic acid 0.1 parts, tetraethyl orthosilicate 0.1 parts, and aluminum silicate fiber 1 part. The mixture is dissociated by a stirrer at a speed of 5000 r / min for 3 h at room temperature. After cooling to room temperature, it is used.
[0176] S2, mixing aerogel: 1 part of silica aerogel powder and 1 part of melamine foam are added to the dispersed fiber slurry. Stir with a stirrer at a speed of 5000 r / min for 0.5 h to obtain a fiber reinforced aerogel slurry.
[0177] S3, coating: pour the fiber slurry into the mold with fiberglass cloth on the upper and lower surfaces, scrape the slurry flat, and then clamp the mold. The specific steps are:
[0178] When using the mold for coating:
[0179] a. When designing the mold, the mold cavity thickness is controlled at 4 mm; the mold is padded with a sheet on the upper and lower surfaces.
[0180] b. Pour the slurry into the lower mold of the mold, and use a scraper to spread it flat.
[0181] c. The upper and lower molds are clamped, and the air bubbles between the upper gasket and the slurry are removed. Then the mold is placed in the press machine to apply pressure from top to bottom.
[0182] S4, molding: non-vacuum heating treatment is performed on the mold or the sheet. After demolding or cutting, it is plastic sealed, and finally the fiber reinforced aerogel sheet is obtained. The specific steps are: the coated mold is directly placed on the hot press for pressure and temperature rise. First, preheat at 90℃ for 30min under non-vacuum conditions to remove part of the solvent, then heat to 150℃ under non-vacuum conditions for 60min to form. Then, without removing the gasket, vacuum plastic sealing is performed.
[0183] The density of the obtained fiber reinforced aerogel thermal insulation sheet is 257 kg / m 3 , the thermal conductivity is 0.038 W / (m·K), the specific heat capacity is 0.23 J / (g·℃), the flame retardant level is UL94 V-2 level, and the water absorption rate is 3.1%.
[0184] The foregoing basic examples and each further selected example of the present application can be freely combined to form a plurality of embodiments, all of which are embodiments that can be used and claimed by the present application. In the present application, each selected example can be arbitrarily combined with any basic example and selected example. Those skilled in the art can know numerous combinations.
[0185] The above only describes the preferred embodiments of the present application and does not limit the present application. Any modification, equivalent replacement and improvement made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims
1. A process for the preparation of a fiber reinforced aerogel fireproof thermal insulation sheet, characterized in that The method comprises the following steps: S1, dispersing fibers: adding dispersant, binder and fibers into solvent respectively, and dissolving the mixture at room temperature, and obtaining fiber slurry after cooling to room temperature, and preparing for use; the dissolving device is a fiber disperser or a stirrer, the rotating speed is 5000 r / min, and the dissolving time is 3 h; S2, mixing aerogel: adding aerogel powder and melamine foam into the fiber slurry prepared in S1 respectively, and obtaining fiber-reinforced aerogel slurry after stirring; S3, coating: pouring the fiber-reinforced aerogel slurry prepared in S2 into a mold with a sheet on the upper and lower surfaces of the mold, and using the mold to coat; Or directly laying the fiber-reinforced aerogel slurry prepared in S2 on the sheet using a coating machine; S4, molding: heating or vacuum heating the mold or the sheet; after demolding or slicing, the product is plastic-wrapped, and finally the fiber-reinforced aerogel fireproof and heat-insulating sheet is obtained; during molding, preheating is first performed under non-vacuum conditions to 90℃, part of the solvent is removed after 30 min, then the temperature is increased to 150℃ under non-vacuum conditions, and molding is performed for 60 min; The solvent in S1 is any one or a mixture of multiple of water, n-hexane, cyclohexane, n-pentane, cyclopentane, dioxane, ethanol, methanol, n-propanol or isopropanol; the dispersant is any one or a mixture of multiple of phytic acid, oleic acid, stearic acid, lauric acid, lanolin acid, polyethylene glycol or polyvinyl alcohol; The binder in S1 is any one or a mixture of multiple of tetraethyl orthosilicate, silane coupling agent KH550, KH560, KH570 or KH580; the fiber is any one or multiple of aluminum silicate fiber, zirconia fiber or glass fiber; the aerogel in S2 is any one or multiple of silica aerogel, alumina aerogel or phenolic aerogel.
2. The process of claim 1 wherein: the fiber reinforced aerogel fire protection and thermal insulation sheet is prepared by the steps of: a) providing a mixture of a silica aerogel and a fibrous material; b) forming the mixture into a sheet; c) drying the sheet; and d) curing the sheet. The mass ratio of the solvent, the dispersant, the binder and the fiber is 100:0.1-1:0.1-2:1-10.
3. The method for preparing the fiber-reinforced aerogel fireproof and heat-insulating sheet as described in claim 1, characterized in that: The gasket in S3 is any one or multiple of fabric, non-woven fabric or paper made of glass fiber, carbon fiber, ceramic fiber, hydroxyapatite paper, natural organic polymer or petroleum-based polymer.
4. The preparation method of the fiber-reinforced aerogel fireproof and heat-insulating sheet as described in claim 1, characterized in that: The specific steps of using the mold to coat in S3 are as follows: a. When designing the mold, the thickness of the mold cavity is controlled to be 4 mm; the mold is padded with a sheet on the upper and lower surfaces; b. Pouring the fiber-reinforced aerogel slurry into the lower mold of the mold, and leveling it with a scraper; c. Clamping the upper and lower molds, and removing the bubbles between the upper gasket and the slurry, and then placing the mold into a press machine to apply pressure from top to bottom.
5. The fiber-reinforced aerogel fireproof and heat-insulating sheet prepared by any one of the methods in claims 1-4.
Citation Information
Patent Citations
Aerogel composite and preparation method thereof
CN109734950A
Aerogel composite insulation board and preparation method thereof
CN114349394A