CN115501826B - Integrated device and method for preparing aerogel composite material - Google Patents
Integrated device and method for preparing aerogel composite material Download PDFInfo
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- CN115501826B CN115501826B CN202211310931.2A CN202211310931A CN115501826B CN 115501826 B CN115501826 B CN 115501826B CN 202211310931 A CN202211310931 A CN 202211310931A CN 115501826 B CN115501826 B CN 115501826B
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- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 239000004964 aerogel Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 98
- 239000002904 solvent Substances 0.000 claims abstract description 87
- 239000007788 liquid Substances 0.000 claims abstract description 83
- 239000000463 material Substances 0.000 claims abstract description 56
- 239000000835 fiber Substances 0.000 claims abstract description 50
- 239000011229 interlayer Substances 0.000 claims abstract description 49
- 238000004804 winding Methods 0.000 claims abstract description 19
- 238000003860 storage Methods 0.000 claims abstract description 17
- 230000032683 aging Effects 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 84
- 239000007789 gas Substances 0.000 claims description 43
- 230000001105 regulatory effect Effects 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 19
- 239000010410 layer Substances 0.000 claims description 10
- 239000003365 glass fiber Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 239000000919 ceramic Substances 0.000 claims description 6
- 230000004888 barrier function Effects 0.000 claims description 5
- 230000001276 controlling effect Effects 0.000 claims description 5
- 239000006260 foam Substances 0.000 claims description 4
- 238000005192 partition Methods 0.000 claims description 4
- BJCUGTXVRQRMCX-UHFFFAOYSA-N C[Si](N[Si](C)(C)C)(C)C.[N] Chemical compound C[Si](N[Si](C)(C)C)(C)C.[N] BJCUGTXVRQRMCX-UHFFFAOYSA-N 0.000 claims description 3
- IFNWVFPCPUMCLE-UHFFFAOYSA-N C[Si](OCC)(OCC)OCC.C(C)O Chemical compound C[Si](OCC)(OCC)OCC.C(C)O IFNWVFPCPUMCLE-UHFFFAOYSA-N 0.000 claims description 3
- HGTUTWRGZCKKAH-UHFFFAOYSA-N [dimethyl-(trimethylsilylamino)silyl]methane;ethanol Chemical compound CCO.C[Si](C)(C)N[Si](C)(C)C HGTUTWRGZCKKAH-UHFFFAOYSA-N 0.000 claims description 3
- VBXGBCLDYZCIRT-UHFFFAOYSA-N chloro(trimethyl)silane ethanol Chemical compound CCO.C[Si](C)(C)Cl VBXGBCLDYZCIRT-UHFFFAOYSA-N 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- DLPFFZOABYKWRI-UHFFFAOYSA-N C[Si](Cl)(C)C.[N] Chemical compound C[Si](Cl)(C)C.[N] DLPFFZOABYKWRI-UHFFFAOYSA-N 0.000 claims description 2
- -1 methyltriethoxysilane-nitrogen Chemical compound 0.000 claims description 2
- 238000006073 displacement reaction Methods 0.000 claims 2
- 238000012986 modification Methods 0.000 abstract description 27
- 230000004048 modification Effects 0.000 abstract description 27
- 238000001035 drying Methods 0.000 abstract description 22
- 238000007598 dipping method Methods 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 4
- 239000000499 gel Substances 0.000 description 34
- 230000002209 hydrophobic effect Effects 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 7
- 239000004965 Silica aerogel Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 7
- 239000002253 acid Substances 0.000 description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 238000011084 recovery Methods 0.000 description 7
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 6
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 238000001879 gelation Methods 0.000 description 4
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 4
- 125000004122 cyclic group Chemical group 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000002787 reinforcement Effects 0.000 description 3
- 239000005051 trimethylchlorosilane Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000000352 supercritical drying Methods 0.000 description 2
- 239000011240 wet gel Substances 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007791 dehumidification Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229920001821 foam rubber Polymers 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 239000007783 nanoporous material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses an integrated device and a method for preparing an aerogel composite material, wherein the integrated device comprises a reaction kettle, a reel, a sol tank, a solvent replacement tank and a gas storage tank; the top of the reaction kettle is provided with a kettle cover which can be opened and closed, and the scroll is detachably arranged at the bottom of the kettle cover and used for winding fiber reinforced materials; a material pipe with a valve is arranged in the center of the kettle cover, the upper end of the material pipe is communicated with the sol groove, and the lower end of the material pipe is communicated with the reel; the scroll is of a hollow structure, the bottom end of the scroll is sealed, and the side wall of the scroll is provided with a liquid hole; an emptying pipe with a valve is arranged at the bottom of the reaction kettle and is detachably connected with a solvent replacement tank and a gas storage tank; the side wall of the reaction kettle is provided with an interlayer, and heat tracing circulating liquid is communicated in the interlayer and used for controlling the temperature of materials in the reaction kettle. The device can realize the integrated preparation of the aerogel composite material by circulating gum dipping, gel aging, solvent replacement, modification and drying.
Description
Technical Field
The invention belongs to the field of new materials, and particularly relates to an aerogel composite material, in particular to an integrated device and method for preparing the aerogel composite material.
Background
Aerogel is a nano porous material, has excellent heat insulation performance, and is a solid material with the lowest heat conductivity at present. Aerogel materials used as insulation materials are typically composites of aerogel and continuous fiber preforms. Currently, the aerogel composite material has been applied to industrialization and engineering, the preparation of the aerogel composite material generally realizes the composition of aerogel and fiber by impregnating a fiber preform with sol, and then the production and manufacture of the aerogel composite material product are realized by performing the processes of gelation, aging, solvent replacement, drying and the like. Most of the production processes need to unreel and roll the fiber preform for multiple times and transfer the fiber composite gel in multiple tools, which results in complex production process and easy damage to the fiber composite gel transfer process.
Disclosure of Invention
The invention aims to: the invention aims to solve the technical problem of providing a circulating gum dipping-gel-aging-solvent replacement-drying integrated device for preparing an aerogel composite material aiming at the defects of the prior art.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
an integrated device for preparing aerogel composite materials comprises a reaction kettle, a reel, a sol tank, a solvent replacement tank and a gas storage tank;
the top of the reaction kettle is provided with a kettle cover which can be opened and closed, and the scroll is detachably arranged at the bottom of the kettle cover and used for winding fiber reinforced materials; a material pipe with a valve is arranged in the center of the kettle cover, the upper end of the material pipe is communicated with the sol groove, and the lower end of the material pipe is communicated with the reel; the scroll is of a hollow structure, the bottom end of the scroll is sealed, and the side wall of the scroll is provided with a liquid hole;
an emptying pipe with a valve is arranged at the bottom of the reaction kettle and is detachably connected with a solvent replacement tank and a gas storage tank;
the side wall of the reaction kettle is provided with an interlayer, and heat tracing circulating liquid is communicated in the interlayer and used for controlling the temperature of materials in the reaction kettle.
Specifically, the sol tank is connected with the kettle cover central material pipe through a sol conveying pipe, and a sol pump is arranged on the sol conveying pipe;
the replacement solvent tank is connected with an emptying pipe at the bottom of the reaction kettle through a replacement solvent conveying pipe, and a replacement solvent conveying pump is arranged on the replacement solvent conveying pipe;
the gas storage tank is connected with the emptying pipe at the bottom of the reaction kettle through a gas conveying pipe, and a fan is arranged on the gas conveying pipe.
Further, a pressure regulating valve is further arranged on the kettle cover and is connected to the sol tank through a detachable sol return pipe, so that the circulation of sol in the reaction kettle is realized;
the top end of the central material pipe of the kettle cover is connected to the replacement solvent tank through a detachable replacement solvent return pipe, so that circulation in the replacement solvent reaction kettle is realized.
Specifically, a first porous plate and a second porous plate are sequentially arranged below the inside of the reaction kettle, and a reel mounting hole for mounting a reel is formed in the center of the first porous plate;
the circulating liquid inlet is arranged below the interlayer of the side wall of the reaction kettle, the circulating liquid outlet is arranged above the interlayer, and the spiral partition plate/fins are arranged inside the interlayer.
Specifically, the kettle cover central material pipe comprises a kettle cover upper end pipeline, a kettle cover lower end pipeline and a material pipe valve, wherein the material pipe valve is arranged in the center of the kettle cover, the upper end of the material pipe valve is connected with the kettle cover lower end pipeline, and the lower end of the material pipe valve is connected with the kettle cover lower end pipeline; the upper end pipeline of the kettle cover is communicated with the sol tank, and the lower end pipeline of the kettle cover is connected with the top end of the scroll.
Further, the invention also provides a method for preparing the aerogel composite material by the integrated device, which comprises the following steps:
s1: winding the fiber reinforced material on a reel, then installing the reel on a kettle cover, closing the kettle cover on the reaction kettle, and keeping the kettle sealed;
s2: introducing heat tracing circulating liquid into the interlayer of the side wall of the reaction kettle, and maintaining the temperature in the kettle to be lower than the sol-gel temperature;
s3: feeding the sol stored in the sol tank into a reaction kettle through a central pipe of a kettle cover and a hollow reel, uniformly diffusing the sol into the fiber reinforced material through liquid holes formed in the side wall of the reel, and then discharging the redundant sol through an emptying pipe;
s4: introducing heat-tracing circulating liquid into the interlayer of the side wall of the reaction kettle to enable the temperature in the kettle to reach the sol-gel temperature, and maintaining the sol to gel and gel aging;
s5: the emptying pipe is communicated with a replacement solvent tank, the replacement solvent is introduced into the reaction kettle for solvent replacement, and the solvent in the kettle is emptied after the replacement is completed;
s6: and connecting the emptying pipe with a gas storage tank, and sending gas into the reaction kettle to dry the product.
In the step S5, the replacement solvent is ethanol or a modified liquid; the modified liquid is a trimethylchlorosilane-ethanol mixed liquid, a hexamethyldisilazane-ethanol mixed liquid or a methyltriethoxysilane-ethanol mixed liquid.
In step S6, the gas is nitrogen or modified gas; the modified gas is trimethylchlorosilane-nitrogen mixed gas, hexamethyldisilazane-nitrogen mixed gas or methyltriethoxysilane-nitrogen mixed gas.
In the step S1, the fiber reinforced material is one or a combination of more of glass fiber felt, glass fiber paper, pre-oxidized fiber felt, ceramic fiber paper and high polymer foam; when winding up a plurality of layers of fiber reinforced material, two adjacent layers of fiber reinforced material are separated by a breathable barrier layer.
In step S3 and step S5, the sol or the replacement solvent circulates inside and outside the reaction kettle by arranging corresponding pipelines.
The beneficial effects are that:
(1) The device can realize the integrated preparation of the aerogel composite material through cyclic gum dipping, gel aging, solvent replacement, modification and drying, has a simple structure and high integration degree, can meet the technological requirements of the aerogel composite material production processes such as sol dipping, gel reaction, aging, solvent replacement, gel modification, gel drying, aerogel modification and the like, can randomly select one or more processes to carry out operations such as dipping, solvent replacement, aging, modification, drying and the like in the aerogel composite material preparation process, and can also select certain processes to carry out any combination operation, such as taking out a sample after the solvent replacement or modification to carry out supercritical drying, bypassing the gel modification after the solvent replacement to directly carry out gel drying, placing the dried sample into the device to carry out modification and drying, placing the wet gel sample into the device to carry out modification, placing the wet gel sample into the device to carry out solvent replacement, placing the aerogel product into the device to carry out drying, dehumidification and impurity removal and the like.
(2) The cyclic gum dipping can fully ensure that the pores in the fiber preform are uniformly and completely filled with the aerogel, and ensure the quality of the aerogel composite material. The circulating replacement solvent can ensure that water, unreacted precursor and other impurities in the gel are completely replaced by ethanol, so that the damage of the impurities to the aerogel structure in the drying process is avoided, and the quality of the aerogel is ensured. The cyclic gel modification can ensure the modification effect, so that the modification is more sufficient and uniform, and the modification degree can be controlled by controlling the modification time, the amount of the modifying liquid and the concentration of the modifying agent in the modifying liquid. The temperature control during the gel and aging process can allow the aging process to be controllably performed. The temperature control in the dipping process can avoid the early gelation reaction or the abrupt change of the viscosity of the sol before the sol is fully dipped and compounded with the fiber preform, thereby being beneficial to the full compounding of the fiber preform and the sol. The gel drying provides another novel drying mode except for the drying modes of supercritical drying, tunnel drying, microwave drying and the like, has higher drying efficiency and more controllable volatilization and emission of the organic solvent, and ensures the economy, safety and environmental protection of the gel drying process.
Drawings
The foregoing and/or other advantages of the invention will become more apparent from the following detailed description of the invention when taken in conjunction with the accompanying drawings and detailed description.
Fig. 1 is a schematic view of the overall structure of the integrated device of the present invention.
FIG. 2 is a schematic view of the internal structure of the reaction vessel in the integrated device of the invention.
FIG. 3 is a schematic structural view of a part of a cover of a reaction kettle in the integrated device of the invention.
Fig. 4 is a state diagram of the reel-wound fiber reinforced material in the integrated device of the present invention.
Wherein each reference numeral represents:
1-a reaction kettle; 2-a kettle cover; 3-a reel; 4-sol pump; 5-a sol tank; 51-sol conveying pipe; 52-sol return pipe; 6-a replacement solvent delivery pump; 7-a replacement solvent tank; 71-a replacement solvent delivery tube; 72-displacing solvent return line; 8-a fan; 9-a gas storage tank; 91-a gas delivery tube; 10, a circulating liquid outlet; 11-a circulating liquid inlet; 12-an interlayer; 13-heat tracing circulating liquid; 14-helical baffles/fins; 15-a first porous plate; 16-a spool mounting hole; 17-a second porous plate; 18-emptying the pipe; 19-a pipeline at the upper end of the kettle cover; 20-a pipeline at the lower end of the kettle cover; 21-a pressure regulating valve; 22-a material pipe valve; 23-upper end of the reel; 24-lower end of the reel; 25-liquid hole; 26-fibrous reinforcement; 27-a breathable barrier layer.
Detailed Description
The invention will be better understood from the following examples.
As shown in fig. 1 to 4, the integrated apparatus of the present invention comprises a reaction vessel 1, a reel 3, a sol tank 5, a replacement solvent tank 7, and a gas storage tank 9.
Wherein, the top of reation kettle 1 is equipped with can open and shut the cover 2, spool 3 detachably installs in the cover 2 bottom for coiling fibre reinforced material 26. A material pipe with a valve is arranged in the center of the kettle cover 2, the upper end of the material pipe is communicated with a sol groove 5 and is used for introducing sol into the reaction kettle 1, and the lower end of the material pipe is communicated with a reel 3; the scroll 3 is hollow structure, and the bottom is sealed, and the lateral wall is opened has liquid hole 25. The sol in the sol tank 5 is fed into the hollow scroll 3 through the central pipe of the kettle cover 2, and uniformly diffused into the fiber reinforced material 26 through the liquid holes 25.
The bottom of the reaction kettle 1 is provided with an emptying pipe 18 with a valve, and the emptying pipe 18 is detachably connected with the replacement solvent tank 7 and the gas storage tank 9. When the emptying pipe 18 is connected with the replacement solvent tank 7, the replacement solvent can be conveyed into the reaction kettle 1; when the emptying pipe 18 is connected with the gas storage tank 9, dry gas can be conveyed into the reaction kettle 1; and when the two are not connected, the device can be used for discharging materials in the reaction kettle 1.
As shown in fig. 2, the side wall of the reaction kettle 1 is provided with an interlayer 12, and a heat tracing circulating liquid 13 is led into the interlayer 12 and used for controlling the temperature of materials in the reaction kettle 1, mainly controlling the materials in the reaction kettle 1 in the early stage of reaction to avoid premature gelation below the sol-gel temperature and promoting gelation above the sol-gel temperature in the later stage.
As shown in fig. 1, the sol tank 5 is connected with the central pipe of the kettle cover 2 through a sol conveying pipe 51, the sol conveying pipe 51 is provided with a sol pump 4, and conveying power is provided by the sol pump 4.
The replacement solvent tank 7 is connected to the evacuation pipe 18 at the bottom of the reaction vessel 1 via a replacement solvent transfer pipe 71, and the replacement solvent transfer pipe 71 is provided with a replacement solvent transfer pump 6, and the replacement solvent transfer pump 6 supplies the transfer power.
The gas storage tank 9 is connected with the emptying pipe 18 at the bottom of the reaction kettle 1 through a gas conveying pipe 91, a fan 8 is arranged on the gas conveying pipe 91, and conveying power is provided through the fan 8 and the pressure inside the storage tank.
Referring to fig. 1 and 3, the kettle cover 2 is further provided with a pressure regulating valve 21, and the pressure regulating valve 21 is connected to the sol tank 5 through a detachable sol return pipe 52, so that the circulation of sol in the reaction kettle 1 is realized.
The top end of the central pipe of the kettle cover 2 is connected to the replacement solvent tank 7 through a detachable replacement solvent return pipe 72, so that the circulation in the replacement solvent reaction kettle 1 is realized.
As shown in fig. 2, a first porous plate 15 and a second porous plate 17 are sequentially arranged below the inner part of the reaction kettle 1, and a reel mounting hole 16 for mounting the reel 3 is arranged in the center of the first porous plate 15; the through holes in the first perforated plate 15 and the second perforated plate 17 serve to promote uniform distribution of the fluid material or gas.
The circulating liquid inlet 11 is arranged below the interlayer 12 on the side wall of the reaction kettle 1, the circulating liquid outlet 10 is arranged above the interlayer 12, the spiral partition plate/fins 14 are arranged in the interlayer 12, the heat tracing effect of the circulating liquid is promoted through the spiral partition plate/fins 14, and the temperature of the material reaction in the kettle is controlled.
As shown in fig. 3, the central pipe of the kettle cover 2 comprises a kettle cover upper end pipe 19, a kettle cover lower end pipe 20 and a pipe valve 22, wherein the pipe valve 22 is arranged in the center of the kettle cover 2, the upper end of the pipe valve 22 is connected with the kettle cover lower end pipe 20, and the lower end is connected with the kettle cover lower end pipe 20; the upper end pipeline 19 of the kettle cover is communicated with the sol tank 5, and the lower end pipeline 20 of the kettle cover is connected with the top end of the scroll 3.
In this embodiment, the emptying pipe 18 is connected with the replacement solvent conveying pipe 71 and the gas conveying pipe 91 by quick-release flanges in a sealing manner. The upper end pipeline 19 of the kettle cover is in sealing connection with the sol conveying pipe 51 and the replacement solvent return pipe 72 by adopting a quick-dismantling flange. The lower end pipeline 20 of the kettle cover is connected with the upper end 23 of the scroll by adopting a bolt flange.
As shown in fig. 4, the upper end 23 of the reel is installed at the center of the tank cover 2, and the lower end 24 of the reel is installed in the reel installation hole 16 at the center of the first porous plate 15, thereby fixing the reel 3 wound with the fiber reinforced material 26. Meanwhile, when a plurality of layers of fiber-reinforced material are wound on the reel 3, a ventilation barrier 27 may be selectively provided between the layers of fiber-reinforced material to separate the layers of fiber-reinforced material. The fiber reinforcement 26 is one or a combination of a plurality of glass fiber mats, glass fiber paper, pre-oxidized fiber mats, ceramic fiber paper or polymer foam with the thickness of 0.5-10 mm. The air-permeable barrier 27 may be a porous mesh cloth, a porous plastic net or a porous foam rubber with a thickness of 0.5 to 3 mm.
The method for preparing the aerogel composite material by adopting the integrated device comprises the following steps:
s1: the fiber reinforcement 26 is wound on the reel 3, and then the reel 3 is mounted to the tank cover 2, the tank cover 2 is covered to the reaction tank 1 and the inside of the tank is kept sealed.
S2: introducing heat-tracing circulating liquid 13 into the interlayer 12 on the side wall of the reaction kettle 1, and maintaining the temperature in the kettle to be lower than the sol-gel temperature, and generally at 0-30 ℃; meanwhile, the pressure regulating valve 21 is set to be 0.01-0.2 MPa of gauge pressure, and the evacuation valve on the evacuation pipe 18 is closed.
S3: starting a sol pump 4, conveying sol stored in a sol tank 5 into a reaction kettle 1 through a central pipe of a kettle cover 2 and a hollow reel 3, uniformly diffusing the sol into a fiber reinforced material through a liquid hole 25 formed in the side wall of the reel 3, when liquid escapes from a pressure regulating valve 21, switching on a sol return pipe 52 to continuously circularly input the sol for 1-30 minutes, stopping the sol pump 4, switching off a pipeline 19 at the upper end of the kettle cover from being connected with the sol pump, switching off the pressure regulating valve 21 and switching off the connection of the sol and the sol tank 5, switching on a bottom exhaust valve of the reaction kettle 1 to discharge sol which is not compounded with the fiber reinforced material in the kettle, switching off the exhaust valve, and switching off a pipe valve 22;
s4: introducing heat-tracing circulating liquid 13 into the interlayer 12 on the side wall of the reaction kettle 1, so that the temperature in the kettle reaches the sol-gel temperature of 20-50 ℃ and is kept constant for 6-24 hours, and maintaining the sol to gel and gel aging;
s5: maintaining the temperature in the kettle at 20-50 ℃, communicating the emptying pipe 18 with the replacement solvent tank 7, introducing the replacement solvent into the reaction kettle 1 for solvent replacement, simultaneously connecting the pipeline 19 at the upper end of the kettle cover with the replacement solvent return pipe 72, circulating the replacement solvent for 1-6 hours, replacing the replacement solvent every 1-2 hours,
s6: when the material is needed, the replacement solvent (mainly ethanol) in the replacement solvent tank 7 can be replaced by a modified liquid (mainly a trimethylchlorosilane-ethanol mixed liquid, a hexamethyldisilazane-ethanol mixed liquid or a methyltriethoxysilane-ethanol mixed liquid), the temperature in the tank is maintained at 20-50 ℃, and the modified liquid is sent into the reaction tank 1 to carry out modification treatment on the material; after finishing modification, recycling ethanol for 1-6 hours to replace the solvent, wherein the ethanol is replaced every 1-2 hours;
s7: and stopping introducing the heat tracing circulating liquid 13 into the interlayer 12, evacuating the liquid material in the kettle, connecting the evacuating pipe 18 with the gas storage tank 9, and feeding gas into the reaction kettle 1 to dry the product. If the gas is mainly nitrogen with the temperature of 50-120 ℃, and the modification treatment is not performed in the step S6, trimethylchlorosilane, hexamethyldisilazane or methyltriethoxysilane can be mixed in the gas, and modification and drying can be realized by introducing modification gas into the reaction kettle 1.
Example 1
Winding 10mm thick glass fiber felt on a winding shaft 3, arranging an air-permeable interlayer 26 when winding the fiber, connecting the winding shaft 3 with the lower end of a kettle cover 2 through a pipeline, putting the kettle cover 2 into a reaction kettle 1, sealing the kettle cover 2, introducing 30 ℃ heat-tracing circulating liquid 13 into the interlayer 12, and setting the pressure of a pressure regulating valve 21 to be 0.01MPa.
30 parts of tetraethoxysilane, 80 parts of ethanol and 12 parts of water are mixed by volume at 30 ℃, added with acid to adjust the pH value to 2, stirred for 60 minutes, added with ammonia water to adjust the pH value to 8, and stirred for 5 minutes to obtain sol.
Opening a sol pump 4 to input the sol into the reel 3, when the liquid escapes from the pressure regulating valve 21, connecting a sol return pipe 52 to continue circulating the sol for 15 minutes, and emptying the sol which is not compounded with the fiber in the reaction kettle 1; and introducing a heat-tracing circulating liquid 13 at 50 ℃ into the interlayer 12, and keeping the temperature for 6 hours to gel and age the sol in the kettle.
Continuously circulating the heat-tracing circulating liquid 13 at 50 ℃ into the interlayer 12, circularly conveying ethanol into the reaction kettle 1 for 1 hour to perform solvent replacement, then circulating the mixture of hexamethyldisilazane and ethanol for 1 hour, maintaining the mixture for 12 hours to perform gel modification, and then circulating the mixture of hexamethyldisilazane and ethanol for 1 hour again to perform solvent replacement, and evacuating ethanol.
Stopping introducing the heat-tracing circulating liquid 13, introducing the upper end pipeline of the kettle cover 2 into a solvent recovery device, introducing 120 ℃ nitrogen into the kettle through a fan 8, and drying the product to obtain the density of 0.22g/cm 3 A hydrophobic silica aerogel composite having a hydrophobicity of 98% and a thermal conductivity of 0.026W/(mK) at 25 ℃.
Example 2
The high molecular foam cotton with the thickness of 2mm is wound on the reel 3, the reel 3 is connected with the lower end of the kettle cover 2 through a pipeline and then is placed into the reaction kettle 1, the kettle cover 2 is covered and kept to be sealed in the reaction kettle 1, the heat tracing circulating liquid 13 with the temperature of 20 ℃ is introduced into the interlayer 12, and the pressure of the pressure regulating valve 21 is set to be 0.2MPa.
30 parts of tetraethoxysilane, 80 parts of ethanol and 12 parts of water are mixed by volume at 20 ℃ and added with acid to adjust the pH value to 2, then stirred for 60 minutes, then added with ammonia water to adjust the pH value to 6.8, and stirred for 15 minutes to obtain sol.
Opening a sol pump 4 to input the sol into the reel 3, when the liquid escapes from the pressure regulating valve 21, connecting a sol return pipe 52 to continue circulating the sol for 30 minutes, and emptying the sol which is not compounded with the fiber in the reaction kettle 1; the interlayer 12 is filled with a heat-tracing circulating liquid 13 at 20 ℃ and kept at constant temperature for 24 hours to gel and age the sol.
Continuously circulating 20 ℃ heat-tracing circulating liquid 13 into the interlayer 12, circularly conveying ethanol into the reaction kettle 1 for 6 hours to replace the solvent, wherein the ethanol is replaced every 2 hours, then circulating the mixture of trimethylchlorosilane and ethanol for 6 hours, then maintaining for 4 hours to carry out gel modification, and then circulating the mixture of trimethylchlorosilane and ethanol for 6 hours again to replace the solvent, wherein the ethanol is replaced every 2 hours, and evacuating the ethanol.
Stopping introducing the heat tracing circulating liquid 13, introducing the upper end pipeline of the kettle cover 2 into the solvent recovery device, and passing through a fan8 introducing nitrogen gas at 50 ℃ into the charging barrel to dry the product, thereby obtaining the density of 0.12g/cm 3 A hydrophobic silica aerogel composite having a hydrophobicity of 99% and a thermal conductivity of 0.025W/(mK) at 25 ℃.
Example 3
Winding 3mm thick pre-oxidized fiber felt and 0.5mm thick ceramic fiber paper on a winding shaft 3, separating the two fibers by an air-permeable interlayer 26 during winding, connecting the winding shaft 3 with a pipeline at the lower end of a kettle cover 2, putting the kettle cover 2 into a reaction kettle 1, covering the kettle cover 2, sealing the reaction kettle 1, introducing 20 ℃ heat tracing circulating liquid 13 into an interlayer 12, and setting the pressure of a pressure regulating valve 21 to be 0.1MPa.
30 parts of tetraethoxysilane, 80 parts of ethanol and 12 parts of water are mixed by volume at 20 ℃ and added with acid to adjust the pH value to 2, then stirred for 60 minutes, then added with ammonia water to adjust the pH value to 7, and stirred for 10 minutes to obtain sol.
Opening a sol pump 4 to input the sol into the reel 3, when the liquid escapes from the pressure regulating valve 21, connecting a sol return pipe 52 to continue circulating the sol for 15 minutes, and emptying the sol which is not compounded with the fiber in the reaction kettle 1; and introducing 40 ℃ heat-tracing circulating liquid 13 into the interlayer 12, and keeping the temperature for 12 hours to gel and age the sol.
Continuously circulating the heat-tracing circulating liquid 13 at 40 ℃ into the interlayer 12, circularly conveying the ethanol into the reaction kettle 1 for 3 hours to replace the solvent, replacing the ethanol every 1 hour, then circulating the mixed solution of methyltriethoxysilane and the ethanol for 3 hours, maintaining for 8 hours to carry out gel modification, and then circulating the ethanol for 2 hours again to replace the solvent, replacing the ethanol every 1 hour, and evacuating the ethanol.
Stopping introducing the heat-tracing circulating liquid 13, introducing the upper end pipeline of the kettle cover 2 into a solvent recovery device, introducing 80 ℃ nitrogen into the kettle through a fan 8, and drying the product to obtain the density of 0.19g/cm 3 Pre-oxidized fiber-reinforced hydrophobic silica aerogel composite having a hydrophobicity of 95% and a thermal conductivity of 0.027W/(mK) at 25 ℃ and a density of 0.29g/cm 3 The hydrophobic rate is 95%, and the thermal conductivity at 25 ℃ is 0.024W/(m.K).
Example 4
The ceramic fiber felt with the thickness of 10mm is wound on a reel 3, the reel 3 is connected with the lower end of a kettle cover 2 through a pipeline and then is placed into a reaction kettle 1, the kettle cover 2 is covered and kept to be sealed in the reaction kettle 1, a heat-tracing circulating liquid 13 with the temperature of 20 ℃ is introduced into an interlayer 12, and the pressure of a pressure regulating valve 21 is set to be 0.05MPa.
30 parts of tetraethoxysilane, 80 parts of ethanol and 12 parts of water are mixed by volume at 20 ℃ and added with acid to adjust the pH value to 2, then stirred for 60 minutes, then added with ammonia water to adjust the pH value to 7, and stirred for 10 minutes to obtain sol.
Opening a sol pump 4 to input the sol into the reel 3, when the liquid escapes from the pressure regulating valve 21, connecting a sol return pipe 52 to continue circulating the sol for 15 minutes, and emptying the sol which is not compounded with the fiber in the reaction kettle 1; and introducing 40 ℃ heat-tracing circulating liquid 13 into the interlayer 12, and keeping the temperature for 12 hours to gel and age the sol in the kettle.
Continuously circulating the heat-tracing circulating liquid 13 at 40 ℃ into the interlayer 12, circularly conveying the ethanol into the reaction kettle 1 for 3 hours to replace the solvent, replacing the ethanol every 1 hour, then circulating the mixed solution of methyltriethoxysilane and the ethanol for 3 hours, maintaining for 8 hours to carry out gel modification, and then circulating the ethanol for 2 hours again to replace the solvent, replacing the ethanol every 1 hour, and evacuating the ethanol.
Stopping introducing the heat-tracing circulating liquid 13, introducing the upper end pipeline of the kettle cover 2 into a solvent recovery device, introducing 100 ℃ nitrogen into the kettle through a fan 8, and drying the product to obtain the density of 0.32g/cm 3 Hydrophobic silica aerogel composite material with a hydrophobic rate of 95% and a thermal conductivity of 0.026W/(mK) at 25 ℃.
Example 5
The ceramic fiber paper with the thickness of 3mm is wound on the reel 3, the reel 3 is connected with the lower end of the kettle cover 2 through a pipeline and then is placed into the reaction kettle 1, the kettle cover 2 is covered and the reaction kettle 1 is kept sealed, the interlayer 12 is filled with the heat-tracing circulating liquid 13 with the temperature of 20 ℃, and the pressure of the pressure regulating valve 21 is set to be 0.05MPa.
30 parts of tetraethoxysilane, 80 parts of ethanol and 12 parts of water are mixed by volume at 20 ℃ and added with acid to adjust the pH value to 2, then stirred for 60 minutes, then added with ammonia water to adjust the pH value to 7, and stirred for 10 minutes to obtain sol.
Opening a sol pump 4 to input the sol into the reel 3, when the liquid escapes from the pressure regulating valve 21, connecting a sol return pipe 52 to continue circulating the sol for 15 minutes, and emptying the sol which is not compounded with the fiber in the reaction kettle 1; and introducing 40 ℃ heat-tracing circulating liquid 13 into the interlayer 12, and keeping the temperature for 12 hours to gel and age the sol in the kettle.
Continuously circulating the heat-tracing circulating liquid 13 at 40 ℃ into the interlayer 12, and circularly conveying the ethanol into the reaction kettle 1 for 3 hours to replace the solvent, wherein the ethanol is replaced every 1 hour, and the ethanol is emptied.
Stopping introducing the heat-tracing circulating liquid 13, introducing the upper end pipeline of the kettle cover 2 into a solvent recovery device, introducing 100 ℃ nitrogen into the kettle through a fan 8, and drying the product to obtain the density of 0.29g/cm 3 Silica aerogel composite having a thermal conductivity of 0.024W/(mK) at 25 ℃.
Example 6
Winding glass fiber paper with the thickness of 1mm on a winding shaft 3, arranging an air-permeable interlayer 26 when winding the fiber, connecting the winding shaft 3 with the lower end of a kettle cover 2 through a pipeline, putting the kettle cover 2 into a reaction kettle 1, sealing the kettle cover 2, introducing 20 ℃ heat-tracing circulating liquid 13 into the interlayer 12, and setting the pressure of a pressure regulating valve 21 to be 0.1MPa.
12 parts of tetraethoxysilane, 18 parts of methyltriethoxysilane, 80 parts of ethanol and 12 parts of water are mixed by volume at 20 ℃ and stirred for 60 minutes after the pH value is adjusted to 2.5 by adding acid, then ammonia water is added to adjust the pH value to 7.2, and the mixture is stirred for 10 minutes to obtain sol.
Opening a sol pump 4 to input the sol into the reel 3, when the liquid escapes from the pressure regulating valve 21, connecting a sol return pipe 52 to continue circulating the sol for 15 minutes, and emptying the sol which is not compounded with the fiber in the reaction kettle 1; and introducing a heat-tracing circulating liquid 13 at 20 ℃ into the interlayer 12, and keeping the temperature for 24 hours to gel and age the sol in the kettle.
Continuously circulating the heat-tracing circulating liquid 13 at 20 ℃ into the interlayer 12, and circularly conveying the ethanol into the reaction kettle 1 for 6 hours to replace the solvent, wherein the ethanol is replaced every 1 hour.
And stopping introducing the heat tracing circulating liquid 13, introducing a pipeline at the upper end of the kettle cover 2 into a solvent recovery device, and introducing nitrogen at 100 ℃ into the kettle through a fan 8 to dry the product, thereby obtaining the density 0.23g/cm 3 A hydrophobic silica aerogel composite having a hydrophobicity of 98% and a thermal conductivity of 0.027W/(mK) at 25 ℃.
Example 7
The glass fiber felt with the thickness of 6mm is wound on a reel 3, the reel 3 is connected with the lower end of a kettle cover 2 through a pipeline and then is placed into a reaction kettle 1, the kettle cover 2 is covered and kept to be sealed in the reaction kettle 1, a heat-tracing circulating liquid 13 with the temperature of 20 ℃ is introduced into an interlayer 12, and the pressure of a pressure regulating valve 21 is set to be 0.05MPa.
30 parts of tetraethoxysilane, 80 parts of ethanol and 12 parts of water are mixed by volume at 20 ℃ and added with acid to adjust the pH value to 2, then stirred for 60 minutes, then added with ammonia water to adjust the pH value to 7, and stirred for 10 minutes to obtain sol.
Opening a sol pump 4 to input the sol into the reel 3, when the liquid escapes from the pressure regulating valve 21, connecting a sol return pipe 52 to continue circulating the sol for 15 minutes, and emptying the sol which is not compounded with the fiber in the reaction kettle 1; and introducing a heat-tracing circulating liquid 13 at 20 ℃ into the interlayer 12, and keeping the temperature for 24 hours to gel and age the sol in the kettle.
Continuously circulating the heat-tracing circulating liquid 13 at 20 ℃ into the interlayer 12, and circularly conveying the ethanol into the reaction kettle 1 for 6 hours to replace the solvent, wherein the ethanol is replaced every 1 hour.
Stopping introducing the heat tracing circulating liquid 13, introducing a pipeline at the upper end of the kettle cover 2 into a solvent recovery device, introducing 80 ℃ nitrogen-hexamethyldisilazane mixed gas into the kettle through a fan 8 to carry out hydrophobic modification on the silica aerogel composite material, and purging with 120 ℃ nitrogen after modification to obtain the density of 0.22g/cm 3 A hydrophobic modified aerogel composite with a hydrophobicity of 99% and a thermal conductivity of 0.026W/(mK) at 25 ℃.
The present invention provides an integrated device and method for preparing aerogel composite, and the method for realizing the technical scheme is a plurality of methods and approaches, the above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several improvements and modifications can be made without departing from the principles of the present invention, and these improvements and modifications should also be regarded as the protection scope of the present invention. The components not explicitly described in this embodiment can be implemented by using the prior art.
Claims (6)
1. An integrated device for preparing an aerogel composite material is characterized by comprising a reaction kettle (1), a reel (3), a sol tank (5), a replacement solvent tank (7) and a gas storage tank (9);
the top of the reaction kettle (1) is provided with a kettle cover (2) which can be opened and closed, and the scroll (3) is detachably arranged at the bottom of the kettle cover (2) and is used for winding fiber reinforced materials; a material pipe with a valve is arranged in the center of the kettle cover (2), the upper end of the material pipe is communicated with the sol groove (5), and the lower end of the material pipe is communicated with the reel (3); the scroll (3) is of a hollow structure, the bottom end is sealed, and the side wall is provided with a liquid hole (25);
an emptying pipe (18) with a valve is arranged at the bottom of the reaction kettle (1), and the emptying pipe (18) is detachably connected with the replacement solvent tank (7) and the gas storage tank (9);
an interlayer (12) is arranged on the side wall of the reaction kettle (1), and heat tracing circulating liquid (13) is led into the interlayer (12) and used for controlling the temperature of materials in the reaction kettle (1);
the sol tank (5) is connected with the central material pipe of the kettle cover (2) through a sol conveying pipe (51), and a sol pump (4) is arranged on the sol conveying pipe (51);
the replacement solvent tank (7) is connected with an emptying pipe (18) at the bottom of the reaction kettle (1) through a replacement solvent conveying pipe (71), and a replacement solvent conveying pump (6) is arranged on the replacement solvent conveying pipe (71);
the gas storage tank (9) is connected with an emptying pipe (18) at the bottom of the reaction kettle (1) through a gas conveying pipe (91), and a fan (8) is arranged on the gas conveying pipe (91);
the kettle cover (2) is also provided with a pressure regulating valve (21), and the pressure regulating valve (21) is connected to the sol tank (5) through a detachable sol return pipe (52) to realize circulation of sol in the reaction kettle (1);
the top end of the central material pipe of the kettle cover (2) is connected to a replacement solvent tank (7) through a detachable replacement solvent return pipe (72), so that circulation in the replacement solvent reaction kettle (1) is realized;
a first porous plate (15) and a second porous plate (17) are sequentially arranged below the inner part of the reaction kettle (1), and a reel mounting hole (16) for mounting a reel (3) is formed in the center of the first porous plate (15);
a circulating liquid inlet (11) is arranged below an interlayer (12) on the side wall of the reaction kettle (1), a circulating liquid outlet (10) is arranged above the interlayer (12), and a spiral partition plate/fin (14) is arranged inside the interlayer (12);
the center pipe of the kettle cover (2) comprises a kettle cover upper end pipe (19), a kettle cover lower end pipe (20) and a pipe valve (22), wherein the pipe valve (22) is arranged in the center of the kettle cover (2), the upper end of the pipe valve (22) is connected with the kettle cover lower end pipe (20), and the lower end is connected with the kettle cover lower end pipe (20); the upper end pipeline (19) of the kettle cover is communicated with the sol tank (5), and the lower end pipeline (20) of the kettle cover is connected with the top end of the scroll (3).
2. A method of preparing an aerogel composite using the integrated apparatus of claim 1, comprising the steps of:
s1: winding the fiber reinforced material on a reel (3), then installing the reel (3) on a kettle cover (2), covering the kettle cover (2) on a reaction kettle (1) and keeping the kettle inside sealed;
s2: introducing heat tracing circulating liquid (13) into an interlayer (12) on the side wall of the reaction kettle (1), and maintaining the temperature in the kettle to be lower than the sol-gel temperature;
s3: feeding the sol stored in the sol tank (5) into the reaction kettle (1) through a central pipe of the kettle cover (2) and through a hollow reel (3), uniformly diffusing the sol into the fiber reinforced material through a liquid hole (25) formed in the side wall of the reel (3), and then discharging the redundant sol through an emptying pipe (18);
s4: introducing heat-tracing circulating liquid (13) into an interlayer (12) on the side wall of the reaction kettle (1) to enable the temperature in the kettle to reach the sol-gel temperature, and maintaining the sol to gel and gel aging;
s5: the emptying pipe (18) is communicated with the replacement solvent tank (7), the replacement solvent is introduced into the reaction kettle (1) for solvent replacement, and the solvent in the kettle is emptied after the replacement is completed;
s6: connecting the emptying pipe (18) with a gas storage tank (9), and feeding gas into the reaction kettle (1) to dry the product.
3. The method of preparing an aerogel composite according to claim 2, wherein in step S5, the displacement solvent is ethanol, or a modifying liquid; the modified liquid is a trimethylchlorosilane-ethanol mixed liquid, a hexamethyldisilazane-ethanol mixed liquid or a methyltriethoxysilane-ethanol mixed liquid.
4. The method of preparing an aerogel composite as claimed in claim 2, wherein in step S6, the gas is nitrogen or a modifying gas; the modified gas is trimethylchlorosilane-nitrogen mixed gas, hexamethyldisilazane-nitrogen mixed gas or methyltriethoxysilane-nitrogen mixed gas.
5. The method of preparing an aerogel composite as claimed in claim 2, wherein in step S1, the fiber reinforced material is one or more of glass fiber mat, glass fiber paper, pre-oxidized fiber mat, ceramic fiber paper, and polymer foam; when winding up a plurality of layers of fiber reinforced material, two adjacent layers of fiber reinforced material are separated by a breathable barrier layer.
6. The method for preparing an aerogel composite according to claim 2, wherein in step S3, step S5, the sol or the displacement solvent is circulated inside and outside the reaction vessel (1) by providing corresponding pipes.
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| CN202211310931.2A CN115501826B (en) | 2022-10-24 | 2022-10-24 | Integrated device and method for preparing aerogel composite material |
| PCT/CN2023/119364 WO2024087937A1 (en) | 2022-10-24 | 2023-09-18 | Integrated device for preparing aerogel composite material and method |
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| CN202211310931.2A CN115501826B (en) | 2022-10-24 | 2022-10-24 | Integrated device and method for preparing aerogel composite material |
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| CN115501826B (en) * | 2022-10-24 | 2024-03-08 | 江苏安珈新材料科技有限公司 | Integrated device and method for preparing aerogel composite material |
| CN115709037B (en) * | 2022-11-29 | 2024-04-02 | 翌江新材(江苏)有限公司 | Coiled material aerogel material preparation system and method |
| CN116163140A (en) * | 2022-12-30 | 2023-05-26 | 航天海鹰(镇江)特种材料有限公司 | High-efficiency liquid phase hydrophobic modification method for aerogel material |
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| US5160562A (en) * | 1990-09-08 | 1992-11-03 | Daimler-Benz Ag | Process for producing a hollow fiber-composite body |
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| KR101654795B1 (en) * | 2016-02-05 | 2016-09-06 | 김현철 | Method for Preparing High-insulation Aerogel - Impregnated Mat |
| CN111167386B (en) * | 2019-11-18 | 2024-09-24 | 宁波圣润新材料有限公司 | Method and equipment for rapidly preparing aerogel by radio frequency radiation |
| CN111778649B (en) * | 2020-06-18 | 2024-04-26 | 中化学华陆新材料有限公司 | Method for rapidly preparing nano heat insulation material by supercritical drying |
| CN115501826B (en) * | 2022-10-24 | 2024-03-08 | 江苏安珈新材料科技有限公司 | Integrated device and method for preparing aerogel composite material |
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| US5160562A (en) * | 1990-09-08 | 1992-11-03 | Daimler-Benz Ag | Process for producing a hollow fiber-composite body |
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| WO2024087937A1 (en) | 2024-05-02 |
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