CN115501826A - 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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- CN115501826A CN115501826A CN202211310931.2A CN202211310931A CN115501826A CN 115501826 A CN115501826 A CN 115501826A CN 202211310931 A CN202211310931 A CN 202211310931A CN 115501826 A CN115501826 A CN 115501826A
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- sol
- kettle
- reaction kettle
- pipe
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- 239000004964 aerogel Substances 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 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 88
- 239000007788 liquid Substances 0.000 claims abstract description 80
- 239000000463 material Substances 0.000 claims abstract description 64
- 239000011229 interlayer Substances 0.000 claims abstract description 50
- 239000000835 fiber Substances 0.000 claims abstract description 45
- 238000003860 storage Methods 0.000 claims abstract description 17
- 238000004804 winding Methods 0.000 claims abstract description 14
- 230000032683 aging Effects 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 80
- 239000007789 gas Substances 0.000 claims description 37
- 230000001105 regulatory effect Effects 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 239000003365 glass fiber Substances 0.000 claims description 9
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 8
- 238000006073 displacement reaction Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 230000002787 reinforcement Effects 0.000 claims description 8
- 238000001879 gelation Methods 0.000 claims description 7
- 238000006467 substitution reaction Methods 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 6
- 239000010410 layer Substances 0.000 claims description 6
- 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 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 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 4
- 230000004888 barrier function Effects 0.000 claims description 4
- VBXGBCLDYZCIRT-UHFFFAOYSA-N chloro(trimethyl)silane ethanol Chemical compound CCO.C[Si](C)(C)Cl VBXGBCLDYZCIRT-UHFFFAOYSA-N 0.000 claims description 4
- 230000001276 controlling effect Effects 0.000 claims description 4
- 239000006260 foam Substances 0.000 claims description 4
- 238000005192 partition Methods 0.000 claims description 4
- 229920000642 polymer Polymers 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
- -1 methyl triethoxysilane-nitrogen Chemical compound 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
- 239000003054 catalyst Substances 0.000 claims description 2
- 238000012986 modification Methods 0.000 abstract description 29
- 230000004048 modification Effects 0.000 abstract description 29
- 238000001035 drying Methods 0.000 abstract description 17
- 238000007598 dipping method Methods 0.000 abstract description 5
- 239000000499 gel Substances 0.000 description 31
- 230000002209 hydrophobic effect Effects 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-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
- 238000011084 recovery Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 239000004965 Silica aerogel Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 3
- 239000012779 reinforcing material Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000002028 premature Effects 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 238000000352 supercritical drying Methods 0.000 description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000009826 distribution Methods 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
- 238000005470 impregnation 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
- 239000011344 liquid material Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 230000035772 mutation Effects 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
- 239000002243 precursor Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- 239000011240 wet gel Substances 0.000 description 1
Images
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
Abstract
The invention discloses an integrated device and a method for preparing aerogel composite materials, wherein the integrated device comprises a reaction kettle, a scroll, a sol tank, a replacement solvent tank and a gas storage tank; the top of the reaction kettle is provided with a kettle cover capable of being opened and closed, and the reel is detachably arranged at the bottom of the kettle cover and used for winding the fiber reinforced material; 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 tank, and the lower end of the material pipe is communicated with the scroll; 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; the bottom of the reaction kettle is provided with an emptying pipe with a valve, and the emptying pipe is detachably connected with the replacement solvent tank and the gas storage tank; the side wall of the reaction kettle is provided with an interlayer, and heat tracing circulation liquid is introduced into 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, gelling, aging, solvent replacement, modification and drying.
Description
Technical Field
The invention belongs to the field of new materials, particularly relates to an aerogel composite material, and particularly relates to an integrated device and a 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 thermal conductivity at present. Aerogel materials used as thermal insulation materials are typically composites of aerogel and a preform of continuous fibers. Currently, the aerogel composite materials have been used in industrial and engineering applications, and the preparation of the aerogel composite materials generally includes the steps of impregnating a fiber preform with a sol to composite the aerogel and the fiber, and then performing gelation, aging, solvent replacement, drying, and the like to produce and manufacture aerogel composite materials. Most of the production processes need to unreel and roll the fiber preform for multiple times, and need to transfer the fiber composite gel at multiple tools, which results in complex production process and easy damage to the transfer process of the fiber composite gel.
Disclosure of Invention
The invention aims to: the invention aims to solve the technical problem of the prior art and provides a circulating gum dipping-gel-aging-solvent replacement-drying integrated device for preparing an aerogel composite material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
an integrated device for preparing aerogel composite materials comprises a reaction kettle, a scroll, a sol tank, a replacement solvent tank and a gas storage tank;
the top of the reaction kettle is provided with a kettle cover capable of being opened and closed, and the reel is detachably arranged at the bottom of the kettle cover and used for winding the fiber reinforced material; 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 tank, and the lower end of the material pipe is communicated with the scroll; 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;
the bottom of the reaction kettle is provided with an emptying pipe with a valve, and the emptying pipe is detachably connected with the replacement solvent tank and the 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 central material pipe of the kettle cover through a sol conveying pipe, and a sol pump is arranged on the sol conveying pipe;
the displacement solvent tank is connected with the emptying pipe at the bottom of the reaction kettle through a displacement solvent conveying pipe, and a displacement solvent conveying pump is arranged on the displacement solvent conveying pipe;
and 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 also arranged on the kettle cover and connected to the sol tank through a detachable sol return pipe, so that the circulation of the sol in the reaction kettle is realized;
the top end of the kettle cover central material pipe 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 inner part of the reaction kettle, and a scroll mounting hole for mounting a scroll is formed in the center of the first porous plate;
a circulating liquid inlet is arranged below an interlayer on the side wall of the reaction kettle, a circulating liquid outlet is arranged above the interlayer, and a spiral partition plate/fin is arranged inside the interlayer.
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 pipeline at the lower end of the kettle cover, and the lower end of the material pipe valve is connected with the pipeline at the lower end of the kettle cover; the kettle cover upper end pipeline is communicated with the sol tank, and the kettle cover lower end pipeline 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, covering the kettle cover on the reaction kettle, and keeping the interior of the kettle sealed;
s2: introducing heat tracing circulation liquid into an interlayer on the side wall of the reaction kettle, and maintaining the temperature in the kettle to be lower than the temperature of sol-gel;
s3: feeding the sol stored in the sol tank into a reaction kettle through a central material 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 discharging redundant sol through an emptying pipe;
s4: introducing heat tracing circulation liquid into an interlayer on the side wall of the reaction kettle to enable the temperature in the kettle to reach the sol-gel temperature, and maintaining the sol gelation and gel aging;
s5: communicating an emptying pipe with a replacement solvent tank, introducing a replacement solvent into the reaction kettle for solvent replacement, and emptying the solvent in the kettle after the replacement is finished;
s6: and connecting the emptying pipe with a gas storage tank, and feeding gas into the reaction kettle to dry the product to obtain the catalyst.
In the step S5, the replacement solvent is ethanol or modified liquid; the modified liquid is a trimethylchlorosilane-ethanol mixed liquid, a hexamethyldisilazane-ethanol mixed liquid or a methyltriethoxysilane-ethanol mixed liquid.
In the step S6, the gas is nitrogen or modified gas; the modified gas is trimethyl chlorosilane-nitrogen gas mixture, hexamethyldisilazane-nitrogen gas mixture or methyl triethoxysilane-nitrogen gas mixture.
In the step S1, the fiber reinforced material is one or a combination of a plurality of glass fiber mats, glass fiber paper, pre-oxidized fiber mats, ceramic fiber paper and polymer foam; when multiple layers of fibrous reinforcement are wound, adjacent layers of fibrous reinforcement are separated by an air-permeable barrier.
In the step S3 and the step S5, the sol or the replacement solvent circulates inside and outside the reaction kettle through corresponding pipelines.
Has the beneficial effects that:
(1) The device can realize the integrated preparation of the aerogel composite material by circulating gum dipping, gel, aging, solvent replacement, modification and drying, has simple structure and high integration degree, can meet the process 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 of the processes to carry out the operations of dipping, solvent replacement, aging, modification, drying and the like in the preparation process of the aerogel composite material, and can also select certain of the processes to randomly combine the operations, such as taking out a sample after the solvent replacement or modification for supercritical drying, directly carrying out gel drying after the solvent replacement by skipping the gel modification, putting the dried sample into the device for modification, putting the wet gel sample into the device for solvent replacement, putting the aerogel sample into the device for solvent replacement, and putting the aerogel product into the device for drying, dehumidifying, removing impurities and the like.
(2) The invention can fully ensure that the pores in the fiber preform are uniformly and completely filled with the aerogel through the circulating impregnation, thereby ensuring the quality of the aerogel composite material. The cyclic replacement solvent can ensure that water, unreacted precursors 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 complete and uniform, and the control of the modification degree can be realized by controlling the modification time, the dosage of the modification liquid and the concentration of the modifier in the modification liquid. The temperature control during the gelling and aging process allows the aging process to be controlled. The temperature control in the dipping process can avoid premature gelation reaction or viscosity mutation of the sol before the sol and the fiber preform are fully dipped and compounded, and is beneficial to the full compounding of the fiber preform and the sol. The gel drying provides another novel drying mode except supercritical drying, tunnel drying, microwave drying and other drying modes, the drying efficiency is higher, the volatilization emission of the organic solvent is more controllable, and the economical efficiency, the safety and the environmental protection performance of the gel drying process are ensured.
Drawings
The foregoing and/or other advantages of the invention will become further apparent from the following detailed description of the invention when taken in conjunction with the accompanying drawings.
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 a reaction vessel in the integration apparatus of the present invention.
FIG. 3 is a schematic view of the structure of a part of the reaction kettle cover in the integrated device of the present invention.
FIG. 4 is a view showing a state where the fiber-reinforced material is wound around the reel in the integrating device of the present invention.
Wherein each reference numeral represents:
1-a reaction kettle; 2-kettle cover; 3-a reel; 4-a sol pump; 5-a sol tank; 51-a sol delivery pipe; 52-sol reflux tube; 6-a replacement solvent delivery pump; 7-a replacement solvent tank; 71-a replacement solvent delivery line; 72-replacement solvent reflux pipe; 8, a fan; 9-a gas storage tank; 91-a gas delivery pipe; 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 perforated plate; 16-reel mounting holes; 17-a second perforated plate; 18-evacuation 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-pipe valve; 23-upper end of reel; 24-spool lower end; 25-liquid pore; 26-a fibrous reinforcement; 27-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 substitution solvent tank 7, and a gas storage tank 9.
Wherein, reation kettle 1's top is equipped with the kettle cover 2 that can open and shut, spool 3 detachably installs in kettle cover 2 bottom for convolute fiber reinforcement 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 the sol tank 5 and is used for introducing sol into the reaction kettle 1, and the lower end of the material pipe is communicated with the scroll 3; the scroll 3 is a hollow structure, the bottom end is sealed, and the side wall is provided with a liquid hole 25. The sol in the sol tank 5 is sent into the hollow scroll 3 through the central material pipe of the kettle cover 2 and is uniformly diffused into the fiber reinforced material 26 through the liquid hole 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 evacuation pipe 18 is connected to the replacement solvent tank 7, the replacement solvent can be fed into the reaction vessel 1; when the emptying pipe 18 is connected with the gas storage tank 9, dry gas can be conveyed into the reaction kettle 1; when not connected, can be used for discharging materials in the reaction kettle 1.
As shown in fig. 2, an interlayer 12 is disposed on a side wall of the reaction kettle 1, and a heat tracing circulation liquid 13 is introduced into the interlayer 12 for controlling the temperature of the materials in the reaction kettle 1, wherein the materials in the reaction kettle 1 are controlled below the sol-gel temperature in the early stage of the reaction to avoid premature gelation, and the materials are promoted to gel above the sol-gel temperature in the later stage.
As shown in fig. 1, the sol tank 5 is connected with the central material pipe of the kettle cover 2 through a sol delivery pipe 51, and a sol pump 4 is arranged on the sol delivery pipe 51 and provides delivery power through the sol pump 4.
The substitution solvent tank 7 is connected to the evacuation pipe 18 at the bottom of the reaction vessel 1 via a substitution solvent transfer pipe 71, and a substitution solvent transfer pump 6 is provided on the substitution solvent transfer pipe 71, and transfer power is supplied by the substitution solvent transfer pump 6.
Between gas storage tank 9 and reation kettle 1 bottom evacuation pipe 18, connect through gas delivery pipe 91, be equipped with fan 8 on the gas delivery pipe 91, provide through fan 8 and storage tank internal pressure and carry power.
Referring to fig. 1 and 3, a pressure regulating valve 21 is further disposed on the kettle cover 2, and the pressure regulating valve 21 is connected to the sol tank 5 through a detachable sol return pipe 52, so as to realize circulation of the sol in the reaction kettle 1.
The top end of the central material pipe of the kettle cover 2 is connected to the replacement solvent tank 7 through a detachable replacement solvent return pipe 72, so that circulation in the replacement solvent reaction kettle 1 is realized.
As shown in fig. 2, a first perforated plate 15 and a second perforated 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 at the center of the first perforated plate 15; the through holes in the first perforated plate 15 and the second perforated plate 17 are used to promote an even distribution of the fluid material or gas.
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, a spiral partition plate/fin 14 is arranged inside the interlayer 12, the heat tracing effect of the circulating liquid is promoted through the spiral partition plate/fin 14, and the temperature of material reaction in the kettle is controlled.
As shown in fig. 3, the material pipe in the center of the kettle cover 2 comprises a pipeline 19 at the upper end of the kettle cover, a pipeline 20 at the lower end of the kettle cover, and a material pipe valve 22, wherein the material pipe valve 22 is installed in the center of the kettle cover 2, the upper end of the material pipe valve 22 is connected with the pipeline 20 at the lower end of the kettle cover, and the lower end is connected with the pipeline 20 at the lower end of the kettle cover; kettle cover upper end pipeline 19 and sol groove 5 intercommunication, kettle cover lower extreme pipeline 20 is connected with 3 tops of spool.
In this embodiment, the evacuation pipe 18 is connected to the replacement solvent delivery pipe 71 and the gas delivery pipe 91 by quick-release flanges. The pipeline 19 at the upper end of the kettle cover is hermetically connected with the sol delivery pipe 51 and the replacement solvent return pipe 72 by adopting quick-release flanges. The pipeline 20 at the lower end of the kettle cover is connected with the upper end 23 of the scroll by a bolt flange.
As shown in fig. 4, the upper end 23 of the reel is installed at the center of the vessel 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. Also, air-permeable barrier layers 27 may optionally be provided between the layers of fibrous reinforcing material to space the layers of fibrous reinforcing material apart when multiple layers of fibrous reinforcing material are wound on spool 3. The fiber reinforced material 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 interlayer 27 can be porous mesh cloth with the thickness of 0.5-3 mm, a porous plastic net or porous foamed rubber.
The method for preparing the aerogel composite material by adopting the integrated device comprises the following steps:
s1: fiber reinforcement material 26 is wound on reel 3, then reel 3 is mounted to kettle cover 2, kettle cover 2 is closed to reaction kettle 1 and the interior of the kettle is kept sealed.
S2: introducing a 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, generally at 0-30 ℃; meanwhile, the pressure regulating valve 21 is set to gauge pressure of 0.01-0.2 MPa, and the emptying valve on the emptying pipe 18 is closed.
S3: the sol pump 4 is started, the sol stored in the sol tank 5 is sent into the reaction kettle 1 through the central material pipe of the kettle cover 2 and the hollow scroll 3, the sol is uniformly diffused into the fiber reinforced material through the liquid holes 25 formed in the side wall of the scroll 3, when the liquid escapes from the pressure regulating valve 21, the sol return pipe 52 is connected to continue to circularly input the sol for 1 to 30 minutes, then the sol pump 4 is stopped, the connection between the pipeline 19 at the upper end of the kettle cover and the sol pump is disconnected, the pressure regulating valve 21 is closed and is disconnected from the sol tank 5, the bottom emptying valve of the reaction kettle 1 is opened, the sol which is not compounded with the fiber reinforced material in the kettle is discharged, the emptying valve is closed, and the material pipe 22 is closed;
s4: introducing a heat tracing circulating liquid 13 into an interlayer 12 on the side wall of the reaction kettle 1 to ensure 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 gelation 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 communicating the pipeline 19 at the upper end of the kettle cover with a replacement solvent return pipe 72, circularly replacing the solvent for 1-6 hours, wherein the replacement solvent can be replaced once every 1-2 hours,
s6: when needed, replacing a replacement solvent (mainly ethanol) in the replacement solvent tank 7 with a modification solution (mainly trimethylchlorosilane-ethanol mixed solution, hexamethyldisilazane-ethanol mixed solution or methyltriethoxysilane-ethanol mixed solution), maintaining the temperature in the kettle at 20-50 ℃, and feeding the modification solution into the reaction kettle 1 to modify the material; after the modification is finished, the solvent is replaced by circulating ethanol for 1 to 6 hours, and the ethanol is replaced every 1 to 2 hours in the process;
s7: stopping introducing the heat tracing circulation liquid 13 into the interlayer 12, emptying the liquid material in the kettle, connecting the emptying pipe 18 with the gas storage tank 9, and feeding gas into the reaction kettle 1 to dry the product to obtain the product. The gas is mainly nitrogen at 50-120 ℃, and if the modification treatment is not performed in the step S6, trimethylchlorosilane, hexamethyldisilazane or methyltriethoxysilane can be mixed in the gas, and the modification and drying can be realized by introducing the modification gas into the reaction kettle 1.
Example 1
Winding a 10mm thick glass fiber felt on a reel 3, arranging an air-permeable interlayer 26 during fiber winding, connecting the reel 3 with a pipeline at the lower end of a kettle cover 2, then placing the connected reel into a reaction kettle 1, covering the kettle cover 2 and keeping the reaction kettle 1 sealed, introducing 30 ℃ heat tracing circulation liquid 13 into an interlayer 12, and setting the pressure of a pressure regulating valve 21 to be gauge pressure of 0.01MPa.
30 parts of ethyl orthosilicate, 80 parts of ethanol and 12 parts of water are mixed according to the volume at the temperature of 30 ℃, acid is added to adjust the pH value to 2, then the mixture is stirred for 60 minutes, then ammonia water is added to adjust the pH value to 8, and the mixture is stirred for 5 minutes to obtain sol.
Opening a sol pump 4 to input the sol into the reel 3, connecting a sol return pipe 52 to continue circulating the sol for 15 minutes when liquid escapes from the pressure regulating valve 21, and emptying the sol which is not compounded with the fibers in the reaction kettle 1; 50 ℃ heat tracing circulating liquid 13 is introduced into the interlayer 12, and the temperature is kept for 6 hours to gelatinize the sol in the kettle and age the gel.
And continuously circulating the 50 ℃ heat tracing circulation liquid 13 into the interlayer 12, circularly conveying ethanol into the reaction kettle 1 for 1 hour for solvent replacement, then circulating the mixed liquid for 1 hour by using hexamethyldisilazane-ethanol, keeping the mixed liquid for 12 hours for gel modification, then circulating the mixed liquid for 1 hour by using ethanol again for solvent replacement, and emptying the ethanol.
Stopping introducing the heat tracing circulation liquid 13, introducing a solvent recovery device into the upper end pipeline of the kettle cover 2, introducing nitrogen gas of 120 ℃ into the kettle through a fan 8 to dry the product, and obtaining the product with the density of 0.22g/cm 3 The hydrophobic silica aerogel composite material has the hydrophobic rate of 98 percent and the thermal conductivity at 25 ℃ of 0.026W/(m.K).
Example 2
High polymer foam with the thickness of 2mm is wound on a reel 3, the reel 3 is connected with a pipeline at the lower end of a kettle cover 2 and then is placed into a reaction kettle 1, the kettle cover 2 is covered and the reaction kettle 1 is kept sealed, 20 ℃ heat tracing circulation liquid 13 is introduced into an interlayer 12, and the pressure of a pressure regulating valve 21 is set to be 0.2MPa of gauge pressure.
30 parts of ethyl orthosilicate, 80 parts of ethanol and 12 parts of water are mixed according to the volume at the temperature of 20 ℃, acid is added to adjust the pH value to 2, then the mixture is stirred for 60 minutes, then ammonia water is added to adjust the pH value to 6.8, and the mixture is stirred for 15 minutes to obtain sol.
The sol pump 4 is opened to input the sol into the scroll 3, when the liquid escapes from the pressure regulating valve 21, the sol return pipe 52 is connected to continue to circulate the sol for 30 minutes, and the sol which is not compounded with the fiber in the reaction kettle 1 is emptied; and (3) introducing a 20 ℃ heat tracing circulating liquid 13 into the interlayer 12, and keeping the temperature for 24 hours to gelatinize the sol and age the gel.
And continuously circulating the 20 ℃ heat tracing circulation liquid 13 into the interlayer 12, circularly conveying ethanol into the reaction kettle 1 for 6 hours for solvent replacement, replacing the ethanol once every 2 hours, circulating the ethanol for 6 hours by using a trimethylchlorosilane-ethanol mixed solution, keeping the solution for 4 hours for gel modification, then circulating the ethanol for 6 hours again for solvent replacement, replacing the ethanol once every 2 hours, and emptying the ethanol.
Stopping introducing the heat tracing circulation liquid 13, introducing a pipeline at the upper end of the kettle cover 2 into a solvent recovery device, introducing nitrogen gas at 50 ℃ into the charging barrel through a fan 8 to dry the product, and obtaining the product with the density of 0.12g/cm 3 The hydrophobic silica aerogel composite material has the hydrophobic rate of 99 percent and the thermal conductivity at 25 ℃ of 0.025W/(m.K).
Example 3
Winding a pre-oxidized fiber felt with the thickness of 3mm and a ceramic fiber paper with the thickness of 0.5mm on a reel 3, separating the two fibers by using a ventilating interlayer 26 during winding, connecting the reel 3 with a pipeline at the lower end of a kettle cover 2, then placing the reel 3 into a reaction kettle 1, covering the kettle cover 2, keeping the reaction kettle 1 sealed, introducing a heat tracing circulation liquid 13 with the temperature of 20 ℃ into an interlayer 12, and setting the pressure of a pressure regulating valve 21 to be 0.1MPa of gauge pressure.
30 parts of tetraethoxysilane, 80 parts of ethanol and 12 parts of water are mixed according to the volume at the temperature of 20 ℃, acid is added to regulate the pH value to be 2, then the mixture is stirred for 60 minutes, then ammonia water is added to regulate the pH value to be 7, and the mixture is stirred for 10 minutes to obtain the sol.
Opening a sol pump 4 to input the sol into the reel 3, connecting a sol return pipe 52 to continue circulating the sol for 15 minutes when liquid escapes from the pressure regulating valve 21, and emptying the sol which is not compounded with the fibers in the reaction kettle 1; 40 ℃ heat tracing circulating liquid 13 is introduced into the interlayer 12, and the sol gelation and gel aging are carried out at constant temperature for 12 hours.
And continuously circulating the 40 ℃ heat tracing circulation liquid 13 into the interlayer 12, circularly conveying ethanol into the reaction kettle 1 for 3 hours to perform solvent replacement, replacing the ethanol every 1 hour in the period, circulating the solution for 3 hours by using a methyltriethoxysilane-ethanol mixed solution, keeping the solution for 8 hours to perform gel modification, then circulating the solution for 2 hours again by using the ethanol to perform solvent replacement, replacing the ethanol every 1 hour in the period, and emptying the ethanol.
Stopping introducing the heat tracing circulation liquid 13, introducing a pipeline at the upper end of the kettle cover 2 into a solvent recovery device, introducing nitrogen at 80 ℃ into the kettle through a fan 8 to dry the product to obtain the product with the density of 0.19g/cm 3 The hydrophobic rate is 95 percent, the thermal conductivity at 25 ℃ is 0.027W/(m.K), and the density is 0.29g/cm 3 95 percent of hydrophobic property and 0.024W/(m.K) of thermal conductivity at 25 ℃.
Example 4
Winding a ceramic fiber felt with the thickness of 10mm on a reel 3, connecting the reel 3 with a pipeline at the lower end of a kettle cover 2, then placing the reel 3 into a reaction kettle 1, covering the kettle cover 2 and keeping the reaction kettle 1 sealed, introducing a 20 ℃ heat tracing circulation liquid 13 into an interlayer 12, and setting the pressure of a pressure regulating valve 21 to be the gauge pressure of 0.05MPa.
30 parts of ethyl orthosilicate, 80 parts of ethanol and 12 parts of water are mixed according to the volume at the temperature of 20 ℃, acid is added to adjust the pH value to 2, then the mixture is stirred for 60 minutes, then ammonia water is added to adjust the pH value to 7, and the mixture is stirred for 10 minutes to obtain sol.
The sol pump 4 is opened to input the sol into the scroll 3, when the liquid escapes from the pressure regulating valve 21, the sol return pipe 52 is connected to continue to circulate the sol for 15 minutes, and the sol which is not compounded with the fiber in the reaction kettle 1 is emptied; 40 ℃ heat tracing circulating liquid 13 is introduced into the interlayer 12, and the temperature is kept for 12 hours to lead sol in the kettle to be gelatinized and gel to be aged.
And continuously circulating the heat tracing circulation liquid 13 at 40 ℃ into the interlayer 12, circularly conveying ethanol into the reaction kettle 1 for 3 hours for solvent replacement, replacing the ethanol once every 1 hour in the period, then circulating the ethanol for 3 hours by using a methyl triethoxysilane-ethanol mixed solution, keeping the solution for 8 hours for gel modification, then circulating the ethanol for 2 hours again for solvent replacement, replacing the ethanol once every 1 hour in the period, and emptying the ethanol.
Stopping introducing the heat tracing circulation liquid 13, and placing the upper end of the kettle cover 2The pipeline is connected with a solvent recovery device, nitrogen with the temperature of 100 ℃ is introduced into the kettle through a fan 8 to dry the product, and the density of the product is 0.32g/cm 3 The hydrophobic silica aerogel composite material has the hydrophobic rate of 95 percent and the thermal conductivity at 25 ℃ of 0.026W/(m.K).
Example 5
Winding a ceramic fiber paper with the thickness of 3mm on a reel 3, connecting the reel 3 with a pipeline at the lower end of a kettle cover 2, then placing the reel 3 into a reaction kettle 1, covering the kettle cover 2, keeping the reaction kettle 1 sealed, introducing a 20 ℃ heat tracing circulation liquid 13 into an interlayer 12, and setting the pressure of a pressure regulating valve 21 to be the gauge pressure of 0.05MPa.
30 parts of ethyl orthosilicate, 80 parts of ethanol and 12 parts of water are mixed according to the volume at the temperature of 20 ℃, acid is added to adjust the pH value to 2, then the mixture is stirred for 60 minutes, then ammonia water is added to adjust the pH value to 7, and the mixture is stirred for 10 minutes to obtain sol.
Opening a sol pump 4 to input the sol into the reel 3, connecting a sol return pipe 52 to continue circulating the sol for 15 minutes when liquid escapes from the pressure regulating valve 21, and emptying the sol which is not compounded with the fibers in the reaction kettle 1; 40 ℃ heat tracing circulating liquid 13 is introduced into the interlayer 12, and the temperature is kept for 12 hours to lead the sol in the kettle to be gelatinized and aged.
And continuously circulating the 40 ℃ heat tracing circulation liquid 13 into the interlayer 12, circularly conveying ethanol into the reaction kettle 1 for 3 hours for solvent replacement, replacing the ethanol every 1 hour in the process, and emptying the ethanol.
Stopping introducing the heat tracing circulation liquid 13, introducing a solvent recovery device into the upper end pipeline of the kettle cover 2, introducing 100 ℃ nitrogen into the kettle through a fan 8 to dry the product, and obtaining the product with the density of 0.29g/cm 3 And a thermal conductivity at 25 ℃ of 0.024W/(m.K).
Example 6
Winding a glass fiber paper with the thickness of 1mm on a reel 3, arranging a ventilating interlayer 26 during fiber winding, connecting the reel 3 with a pipeline at the lower end of a kettle cover 2, then placing the connected reel into a reaction kettle 1, covering the kettle cover 2 and keeping the reaction kettle 1 sealed, introducing a 20 ℃ heat tracing circulation liquid 13 into an interlayer 12, and setting the pressure of a pressure regulating valve 21 to be gage pressure of 0.1MPa.
12 parts of tetraethoxysilane, 18 parts of methyltriethoxysilane, 80 parts of ethanol and 12 parts of water are mixed according to volume at the temperature of 20 ℃, acid is added to adjust the pH value to 2.5, then the mixture is stirred for 60 minutes, then ammonia water is added to adjust the pH value to 7.2, and the mixture is stirred for 10 minutes to obtain the sol.
Opening a sol pump 4 to input the sol into the reel 3, connecting a sol return pipe 52 to continue circulating the sol for 15 minutes when liquid escapes from the pressure regulating valve 21, and emptying the sol which is not compounded with the fibers in the reaction kettle 1; 20 ℃ heat tracing circulating liquid 13 is introduced into the interlayer 12, and the temperature is kept for 24 hours to lead sol in the kettle to be gelatinized and gel to be aged.
And continuously circulating the 20 ℃ heat tracing circulation liquid 13 into the interlayer 12, and circularly conveying ethanol into the reaction kettle 1 for 6 hours for solvent replacement, wherein the ethanol is replaced once every 1 hour.
Stopping introducing the heat tracing circulation liquid 13, introducing a pipeline at the upper end of the kettle cover 2 into a solvent recovery device, introducing 100 ℃ nitrogen into the kettle through a fan 8 to dry the product, and obtaining the product with the density of 0.23g/cm 3 The hydrophobic silica aerogel composite material has the water repellency rate of 98 percent and the thermal conductivity at 25 ℃ of 0.027W/(m.K).
Example 7
Winding a 6mm thick glass fiber felt on a reel 3, connecting the reel 3 with a pipeline at the lower end of a kettle cover 2, then placing the reel 3 into a reaction kettle 1, covering the kettle cover 2 and keeping the reaction kettle 1 sealed, introducing a 20 ℃ heat tracing circulation liquid 13 into an interlayer 12, and setting the pressure of a pressure regulating valve 21 to be gage pressure of 0.05MPa.
30 parts of tetraethoxysilane, 80 parts of ethanol and 12 parts of water are mixed according to the volume at the temperature of 20 ℃, acid is added to regulate the pH value to be 2, then the mixture is stirred for 60 minutes, then ammonia water is added to regulate the pH value to be 7, and the mixture is stirred for 10 minutes to obtain the sol.
The sol pump 4 is opened to input the sol into the scroll 3, when the liquid escapes from the pressure regulating valve 21, the sol return pipe 52 is connected to continue to circulate the sol for 15 minutes, and the sol which is not compounded with the fiber in the reaction kettle 1 is emptied; 20 ℃ heat tracing circulating liquid 13 is introduced into the interlayer 12, and the temperature is kept for 24 hours to lead sol in the kettle to be gelatinized and gel to be aged.
And continuously circulating the 20 ℃ heat tracing circulation liquid 13 into the interlayer 12, and circularly conveying ethanol into the reaction kettle 1 for 6 hours for solvent replacement, wherein the ethanol is replaced once every 1 hour.
Stopping introducing the heat tracing circulating liquid 13, and covering the kettle2, connecting a solvent recovery device to an upper end pipeline, introducing 80 ℃ nitrogen-hexamethyldisilazane mixed gas into the kettle through a fan 8 to perform hydrophobic modification on the silica aerogel composite material, and blowing the nitrogen at 120 ℃ after the modification is finished to obtain the silica aerogel composite material with the density of 0.22g/cm 3 The hydrophobic modified aerogel composite material has the hydrophobic rate of 99 percent and the thermal conductivity at 25 ℃ of 0.026W/(m.K).
While the present invention provides an integrated apparatus and method for preparing aerogel composite, and a number of methods and approaches for implementing the same, it is noted that the above description is merely a preferred embodiment of the present invention, and it should be understood that those skilled in the art can make various modifications and enhancements without departing from the principles of the present invention, and such modifications and enhancements are also considered to be within the scope of the present invention. All the components not specified in the present embodiment can be realized by the prior art.
Claims (10)
1. An integrated device for preparing aerogel composite materials is characterized by comprising a reaction kettle (1), a scroll (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) capable of being opened and closed, and the reel (3) is detachably arranged at the bottom of the kettle cover (2) and 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 tank (5), and the lower end of the material pipe is communicated with the scroll (3); the scroll (3) 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 (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);
the side wall of the reaction kettle (1) is provided with an interlayer (12), and a heat tracing circulation liquid (13) is communicated in the interlayer (12) and used for controlling the temperature of materials in the reaction kettle (1).
2. The integrated device for preparing aerogel composites according to claim 1, wherein 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 displacement solvent tank (7) is connected with a emptying pipe (18) at the bottom of the reaction kettle (1) through a displacement solvent conveying pipe (71), and a displacement solvent conveying pump (6) is arranged on the displacement solvent conveying pipe (71);
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), and a fan (8) is arranged on the gas conveying pipe (91).
3. The integrated device for preparing aerogel composite materials according to claim 2, wherein the kettle cover (2) is further provided with a pressure regulating valve (21), the pressure regulating valve (21) is connected to the sol tank (5) through a detachable sol return pipe (52), and circulation of sol in the reaction kettle (1) is realized;
the top end of the central material pipe of the kettle cover (2) is connected to the replacement solvent tank (7) through a detachable replacement solvent return pipe (72), so that circulation in the replacement solvent reaction kettle (1) is realized.
4. The integrated apparatus for preparing aerogel composite according to claim 1, wherein a first porous plate (15) and a second porous plate (17) are sequentially arranged below the inside 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).
5. The integrated device for preparing aerogel composite materials according to claim 1, wherein the material pipe in the center of the kettle cover (2) comprises a pipeline (19) at the upper end of the kettle cover, a pipeline (20) at the lower end of the kettle cover and a material pipe valve (22), the material pipe valve (22) is installed in the center of the kettle cover (2), the upper end of the material pipe valve (22) is connected with the pipeline (20) at the lower end of the kettle cover, and the lower end of the material pipe valve is connected with the pipeline (20) at the lower end of the kettle cover; kettle cover upper end pipeline (19) and sol groove (5) intercommunication, kettle cover lower extreme pipeline (20) are connected with spool (3) top.
6. A method of making 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 the reaction kettle (1) and keeping the interior of the kettle sealed;
s2: introducing heat tracing circulation 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: the sol stored in the sol groove (5) is sent into the reaction kettle (1) through a central material pipe of the kettle cover (2) and a hollow scroll (3), the sol is uniformly diffused into the fiber reinforced material through liquid holes (25) formed in the side wall of the scroll (3), and then the redundant sol is discharged through a discharge pipe (18);
s4: introducing heat tracing circulation 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 maintain the sol gelation and gel aging;
s5: communicating an emptying pipe (18) with a replacement solvent tank (7), introducing a replacement solvent into the reaction kettle (1) for solvent replacement, and emptying the solvent in the kettle after the replacement is finished;
s6: and (3) connecting the emptying pipe (18) with a gas storage tank (9), and feeding gas into the reaction kettle (1) to dry the product to obtain the catalyst.
7. The method for preparing aerogel composite of claim 6, wherein in step S5, the displacing solvent is ethanol or a modifying solution; the modified liquid is a trimethylchlorosilane-ethanol mixed liquid, a hexamethyldisilazane-ethanol mixed liquid or a methyltriethoxysilane-ethanol mixed liquid.
8. The method of preparing an aerogel composite of claim 6, wherein in step S6, the gas is nitrogen or a modifying gas; the modified gas is trimethyl chlorosilane-nitrogen gas mixture, hexamethyldisilazane-nitrogen gas mixture or methyl triethoxysilane-nitrogen gas mixture.
9. The method for preparing aerogel composite of claim 6, wherein in step S1, the fiber reinforcement material is one or more of glass fiber mat, glass fiber paper, pre-oxidized fiber mat, ceramic fiber paper, and polymer foam; when multiple layers of fibrous reinforcement are wound, adjacent layers of fibrous reinforcement are separated by an air-permeable barrier.
10. Method for the preparation of aerogel composites according to claim 6, characterized in that in step S3, step S5, the sol or the substitution solvent is circulated inside and outside the reactor (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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Cited By (2)
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| CN115709037A (en) * | 2022-11-29 | 2023-02-24 | 翌江新材(江苏)有限公司 | Preparation system and method of coiled material aerogel material |
| WO2024087937A1 (en) * | 2022-10-24 | 2024-05-02 | 江苏安珈新材料科技有限公司 | Integrated device for preparing aerogel composite material and method |
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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 |
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