WO2017142244A1 - Procédé et appareil de fabrication de feuille composite comprenant une feuille d'aérogel - Google Patents

Procédé et appareil de fabrication de feuille composite comprenant une feuille d'aérogel Download PDF

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Publication number
WO2017142244A1
WO2017142244A1 PCT/KR2017/001327 KR2017001327W WO2017142244A1 WO 2017142244 A1 WO2017142244 A1 WO 2017142244A1 KR 2017001327 W KR2017001327 W KR 2017001327W WO 2017142244 A1 WO2017142244 A1 WO 2017142244A1
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WIPO (PCT)
Prior art keywords
sheet
airgel
composite
gel
manufacturing
Prior art date
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Ceased
Application number
PCT/KR2017/001327
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English (en)
Korean (ko)
Inventor
김예훈
이제균
오경실
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LG Chem Ltd
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LG Chem Ltd
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Publication date
Priority claimed from KR1020160095254A external-priority patent/KR101962206B1/ko
Application filed by LG Chem Ltd filed Critical LG Chem Ltd
Priority to EP17753405.4A priority Critical patent/EP3326810B1/fr
Priority to JP2018520558A priority patent/JP6612443B2/ja
Priority to US15/755,500 priority patent/US10682839B2/en
Priority to CN201780003197.6A priority patent/CN108136749B/zh
Publication of WO2017142244A1 publication Critical patent/WO2017142244A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/12—Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B38/00—Ancillary operations in connection with laminating processes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/157—After-treatment of gels
    • C01B33/158—Purification; Drying; Dehydrating

Definitions

  • the present invention relates to a composite sheet manufacturing method and manufacturing apparatus comprising an airgel sheet, and more particularly, to a composite sheet manufacturing method and manufacturing apparatus comprising an airgel sheet having excellent heat insulation and durability and uniform thickness.
  • aerogel sheet is a highly porous material having a high porosity of 90% or more and up to 99% of the solids known to date.
  • the gel is prepared by sol-gel polymerization of a silica precursor solution and then under supercritical or atmospheric pressure conditions. Obtained by drying. That is, the airgel sheet has a pore structure filled with air.
  • Such airgel sheet has lightness and heat insulation, sound absorption, etc. due to its unique pore structure in which 90-99% of the interior space is empty, and the biggest advantage is 36mW / mk, which is the thermal conductivity of organic insulation materials such as styrofoam. It is a high thermal insulation with a thermal conductivity of less than 30mW / mk significantly lower.
  • the airgel sheet according to the prior art has a high raw material cost and manufacturing cost in spite of excellent thermal conductivity, and in particular, there is a limit to increasing the thickness due to the limitation of the manufacturing method.
  • an air layer is formed due to incomplete bonding between the airgel sheets, and thus there is a problem in that thermal conductivity and durability are reduced.
  • an object of the present invention is to laminate the airgel sheet and fiber sheet to increase the bonding and durability, in particular, a composite sheet manufacturing method comprising an airgel sheet that can significantly reduce the manufacturing cost And to provide a manufacturing apparatus.
  • Step S30 may be included.
  • step S10 may be further included a step (S15) for drying the airgel sheet 30.
  • step S20 and step S30 may be a step (S25) of temporarily fixing the need for the laminated airgel sheet 30 and the fiber sheet (10).
  • step S30 by cutting the composite sheet 40 to a predetermined size may further comprise the step (S40) of manufacturing a composite pad (50).
  • the step S20 (a) preparing a silica sol (2); (b) preparing a gel catalyst (3); (c) spraying and impregnating the silica sol (2) prepared in step (a) on the surface of the fiber sheet (1); (d) spraying the gelling catalyst (3) prepared in step (b) on the surface of the fiber sheet (1) impregnated with the silica sol (2) to prepare a gel sheet (20) gelled silica sol ; (e) aging the gel sheet 20 in which the silica sol is gelled; (f) adding a coating solution to the aged gel sheet 20 to modify the surface; (g) drying the gel sheet 20 having the surface modified to prepare an airgel sheet 30.
  • the silica sol 2 may be prepared by mixing TEOS (tetraethly orthosilicate) with ethanol.
  • TEOS tetraethly orthosilicate
  • the gelation catalyst 3 may be prepared by mixing ethanol and aqueous ammonia (NH 4 OH).
  • Step (c) and step (d) may be made in the conveyor belt for transporting the fiber sheet 1 from one side to the other side.
  • the gelling catalyst 3 may be injected onto the surface of the fiber sheet 1 at a rate of 0.035 to 0.012 L / min, and left for 8 to 12 minutes to gel the silica sol.
  • the silica sol gelled gel sheet 20 may be aged at a high temperature of 70 ° C. for 50 minutes.
  • the coating solution in step (f) may be prepared by mixing ethanol and ammonia water (NH 4 OH).
  • step (f) 1.6 times of the silica sol (2) impregnated with the coating solution on the surface of the fiber sheet (1) is added, and the surface is modified by aging and HMDS (Hexamethyldisilazane) for 1 hour at a high temperature of 70 °C. can do.
  • HMDS Hexamethyldisilazane
  • the surface-modified gel sheet 20 is dried by injecting carbon dioxide at a rate of 70 L / min for 10 minutes at a temperature of 28 ° C. and 70 bar, and drying by heating up to 50 ° C. for 1 minute 20 minutes.
  • the second drying step and then injecting carbon dioxide at a rate of 0.7L / min for 20 minutes in the environment of 50 °C and 150bar
  • the third drying step to dry, and injecting carbon dioxide at a rate of 0.7L / min 20 minutes after 20 minutes It may include a fourth drying step of drying.
  • the third drying step may recover ethanol generated from the gel sheet 20 as the surface is modified while injecting carbon dioxide.
  • the step (g) may further include a discharge step of discharging carbon dioxide for 2 hours after the fourth drying step.
  • Steps (e), (f) and (g) can be made in a reaction vessel containing a gel sheet.
  • a manufacturing apparatus for performing the composite sheet manufacturing method including the airgel sheet according to the first embodiment of the present invention includes a gel sheet maker 100 for manufacturing a gel sheet 20; A reaction vessel 200 for aging, surface modifying, and drying the gel sheet 20 manufactured by the gel sheet maker 100 to produce an airgel sheet 30; It comprises a composite sheet maker 300 for manufacturing a composite sheet 40 by bonding the airgel sheet 30 and the fiber sheet 10 produced by the reaction vessel 200, the composite sheet maker 300 An airgel sheet feed roller 310 for supplying the airgel sheet 30, a plurality of fiber sheet feed rollers 320 for supplying the fiber sheet 10 so as to be laminated on both sides of the airgel sheet 30, and the airgel It may include a heat presser 330 for pressing the heat and pressure in the state in which the fiber sheet 10 is interposed between the sheet 30 to produce a composite sheet 40.
  • the composite sheet maker 300 is a drying member 340 for drying the airgel sheet 30 supplied from the airgel sheet supply roller 310 and the airgel sheet 30 is interposed with the fiber sheet 10
  • a needling member 350 may be further included by needling to temporarily join.
  • the gel sheet manufacturing machine 100 is a winding roller 110 in which the fiber sheet 1 is wound, a conveyor belt 120 for transferring the fiber sheet 1 wound in the winding roller 110 from one side to the other side, and the Silica sol supply member 130 for impregnating by spraying the silica sol (2) on the surface of the fiber sheet (1) located on the conveyor belt 120, the surface of the fiber sheet (1) located on the conveyor belt 120
  • Composite sheet manufacturing method comprises the steps of preparing an airgel sheet 30 (S10); Stacking the fiber sheets 10 on both sides of the airgel sheet 30 (S20); And bonding the laminated airgel sheet 30 and the fiber sheet 10 with heat and pressure to produce a composite sheet 40 laminated with the fiber sheet 10, the airgel sheet 30, and the fiber sheet 10.
  • the airgel sheet 30 is made of a composite comprising an airgel matrix and the reinforcing structure, the airgel matrix is continuous (continuous) through the reinforcing structure
  • the reinforcing structure is a lofty fibrous batt, wherein the fibers are oriented along all three axes, and the bet is in the form of a sheet such that the composite is a lightweight, insulating product that is elastic and durable, and the lofty fibrous batt is thick Compressible to at least 50% of and recover to at least 70% of the original thickness after 5 seconds of compression, the density of the Lofty fibrous bets is between 0.001 and 0.26 g / cm3,
  • the cross sectional area of the discernible fibers in the cross section of the composite may be less than 10% of the total cross sectional area.
  • the lofty fibrous batting may maintain at least 50% of the original thickness after addition of a gel forming liquid to form the airgel matrix.
  • the lofty fibrous bets may have elasticity that is compressible to at least 65% of the original thickness and that recovers to at least 75% of the original thickness after compression for 5 seconds.
  • the cross sectional area of the fibers of the Lofty fibrous bet identifiable in the cross section of the composite may be less than 8% of the total area of the cross section.
  • the present invention has the following effects.
  • the composite sheet manufacturing method comprising an airgel sheet according to the present invention can increase the bonding and durability by manufacturing a composite sheet by laminating the airgel sheet and fiber sheet, can significantly reduce the manufacturing cost, in particular to increase the thickness stably You can.
  • the present invention can increase the thickness while maintaining the luxury of the outer shell by laminating the airgel sheet and the fiber sheet.
  • the present invention can produce an airgel sheet having excellent heat insulation and durability, in particular, a uniform thickness by using a method for producing an airgel sheet.
  • high quality silica sol can be obtained by mixing TEOS (tetraethly orthosilicate) with ethanol.
  • a high quality gelling catalyst can be obtained by mixing ethanol and ammonia water (NH 4 OH).
  • FIG. 1 is a flow chart showing a manufacturing method of a composite sheet including an airgel sheet according to a first embodiment of the present invention.
  • Figure 2 is a flow chart showing a method of manufacturing an airgel sheet according to a first embodiment of the present invention.
  • FIG 3 is a view showing an apparatus for producing an airgel sheet according to a first embodiment of the present invention.
  • FIG 4 is a view showing an aging step using a reaction vessel according to a first embodiment of the present invention.
  • FIG 5 is a view showing a surface modification step using the reaction vessel according to the first embodiment of the present invention.
  • FIG. 6 is a view showing a drying step using a reaction vessel according to the first embodiment of the present invention.
  • FIG. 7 is a view showing an apparatus for manufacturing a composite sheet including an airgel sheet according to the first embodiment of the present invention.
  • FIG. 8 is a view showing an airgel composite in a composite sheet including an airgel sheet according to a second embodiment of the present invention.
  • Composite sheet manufacturing method comprising an airgel sheet according to the first embodiment of the present invention, as shown in Figure 1, a composite sheet laminated with a fiber sheet 10, an airgel sheet 30 and a fiber sheet 10
  • the airgel sheet preparation step (S10) including a fiber sheet lamination step (S20), and a composite sheet manufacturing step (S30).
  • Airgel sheet preparation step (S10) is to prepare the airgel sheet 30. First, the method of manufacturing an airgel sheet is demonstrated.
  • a method of manufacturing an airgel sheet is to produce an airgel sheet having excellent heat insulation and durability, particularly uniform thickness, as shown in Figure 2, (a) preparing a silica sol (2) (b) preparing a gelation catalyst (3), (c) impregnating the surface of the fiber sheet (1) by impregnating the silica sol (2) prepared in the step (a), (d) silica Spraying the gelling catalyst (3) prepared in the step (b) on the surface of the sol-impregnated fiber sheet (1) to produce a gel sol gelled gel sheet 20, (e) the silica sol Aging the gelled gel sheet 20, (f) adding a coating solution to the aged gel sheet 20 to modify the surface, and (g) the gel sheet 20 having the surface modified. Drying to prepare the airgel sheet 30.
  • silica sol manufacturing step is to obtain a silica sol
  • a silica sol (2) is prepared by mixing TEOS (tetraethly orthosilicate) and ethanol. That is, silica sol 2 is prepared by including 1.2 kg of TEOS and 2.7 kg of ethanol in a reactor (not shown).
  • TEOS is a solvent having excellent reactivity with water, using a hydrolyzed, it can further increase the reactivity. That is, by mixing the hydrolyzed TEOS and ethanol can be obtained a silica sol excellent in reactivity.
  • the gelation catalyst preparation step is to obtain a gelation catalyst, to prepare a gelation catalyst (3) by mixing ethanol and ammonia water (NH 4 OH). That is, 0.5 kg of ethanol and 30 ml of ammonia water (NH 4 OH) are mixed in a reaction tank (not shown) to prepare a gel catalyst 3.
  • the composite sheet manufacturing apparatus is a gel sheet maker 100 for producing a gel sheet 20, a reaction vessel 200 for producing an airgel sheet through the gel sheet 20 and It includes a composite sheet maker 300 for manufacturing a composite sheet 40 through the airgel sheet 30.
  • (c) the silica sol injection step and (d) gelling catalyst injection step is performed by the gel sheet maker 100, which will be described in detail for the gel sheet maker 100.
  • the gel sheet manufacturing machine 100 is, as shown in FIG. 3, the fiber sheet 1 is wound in a roll shape, the winding roller 110, the fiber sheet 1 wound on the winding roller 110 at one side.
  • Silica sol supply member 130 for impregnating by spraying the silica sol (2) prepared in step (a) on the surface of the conveyor belt 120, the fiber sheet 1 located on the conveyor belt 120 to the other side,
  • Catalyst supply member 140 for producing a gel sol gelled gel sheet 20 by injecting the gel catalyst (3) prepared in step (b) on the surface of the fiber sheet (1) located on the conveyor belt 120
  • a recovery roller 150 which winds and recovers the gel sheet 20 transferred to the other side by the conveyor belt 120 in a roll form.
  • the conveyor belt 120 transfers the fiber sheet 1 wound on the winding roller 110 from one side to the other side.
  • the silica sol supply member 130 on the surface of the fiber sheet 1 conveyed by the conveyor belt 120 is impregnated silica sol by spraying the silica sol (2) prepared in step (a), and the catalyst supply
  • the member 140 sprays the gelation catalyst 3 on the surface of the fiber sheet 1 impregnated with silica sol to produce a gel sheet 20 in which silica sol is gelled.
  • the gel sheet 20 transferred to the other side of the conveyor belt 120 is recovered while being wound again by the recovery roller 150.
  • the conveyor belt 120 includes a scraper 160 for uniformly controlling the thickness of the silica sol 2 and the gelling catalyst 3 sprayed on the fiber sheet 1. That is, the scraper 160 includes a first scraper 161 for adjusting the thickness of the silica sol 2 sprayed on the surface of the fiber sheet 1, and a gelation catalyst 3 sprayed on the surface of the fiber sheet 1. And a second scraper 162 for adjusting the thickness of the substrate.
  • the first scraper 161 and the second scraper 162 have the same shape and are installed on the upper surface of the conveyor belt 120 so as to be height-adjustable in the vertical direction, such as the silica sol 2 and the catalyst for gelation 3. ) To uniformly adjust the thickness, thereby obtaining a gel sheet 20 of uniform quality.
  • the silica sol spraying step is impregnated by spraying the silica sol (2) prepared in step (a) on the surface of the fiber sheet. That is, the silica sol (2) prepared in step (a) is injected into the silica sol supply member 130 and stored. Then, when the fiber sheet 1 is transferred to the lower portion of the silica sol supply member 130 by the conveyor belt 120, the silica sol 2 is sprayed through the silica sol supply member 130 to form the fiber sheet 1. Impregnate the surface.
  • the silica sol 2 sprayed on the fiber sheet 1 has a uniform thickness while passing through the first scraper 161 installed on the conveyor belt 120. That is, the first scraper 161 may uniformly control the thickness of the silica sol 2 by blocking the silica sol 2 having a predetermined thickness or more from passing therethrough.
  • the gel catalyst catalyst spraying step may inject gelation catalyst 3 onto the surface of the fiber sheet 1 impregnated with silica sol by step (c) to gel the silica sol. That is, the gel catalyst 3 prepared in step (b) is injected into the catalyst supply member 140 and stored. Then, when the fiber sheet 1 impregnated with silica sol is transferred to the lower portion of the catalyst supply member 140 by the conveyor belt 120, the gelling catalyst 3 is transferred to the fiber sheet through the catalyst supply member 140. By spraying on the surface of 1) to gel the silica sol, a gel sheet 20 in which the silica sol is gelled can be obtained.
  • the catalyst supply member 140 is sprayed at a set speed of the stored gelling catalyst 3, and left for a set time to stably gel the silica sol. That is, the catalyst supply member 140 sprays the gelling catalyst 3 on the surface of the fiber sheet 1 at a rate of 0.035 to 0.012 L / min, and is allowed to stand for 8 to 12 minutes to gradually gel the silica sol.
  • the catalyst supply member 140 may uniformly control the gelling of the silica sol by varying the injection speed of the gelling catalyst 3 in accordance with the density of the silica sol (2) impregnated in the fiber sheet (1).
  • the silicasol density is 40 kg / m 3
  • the injection speed of the gelling catalyst 3 is adjusted to 0.035 L / min.
  • the silica sol 2 impregnated in the fiber sheet 1 has a content of 30wt% and a thermal conductivity of 14.9mW / mK.
  • the injection speed of the gelling catalyst (3) is adjusted to 0.017 L / min.
  • the silica sol 2 impregnated in the fiber sheet 1 has a content of 38 wt% and a thermal conductivity of 14.1 mW / mK.
  • the injection speed of the gelling catalyst (3) is adjusted to 0.014 L / min.
  • the silica sol 2 impregnated in the fiber sheet 1 has a content of 38 wt% and a thermal conductivity of 13.6 mW / mK.
  • the injection speed of the gelling catalyst (3) is adjusted to 0.012 L / min.
  • the silica sol 2 impregnated in the fiber sheet 1 has a content of 55wt% and a thermal conductivity of 13.0mW / mK.
  • the injection speed of the gelling catalyst decreases, thereby inducing stable gelation of the silica sol.
  • the gel sheet 20 manufactured as described above is recovered while being wound in a roll form by the recovery roller 150, the recovered gel sheet 20 by using the reaction vessel 200 (e) gel sheet aging
  • the airgel sheet 30 may be prepared by performing the step, (f) gel sheet surface modification, and (g) gel sheet drying.
  • the reaction vessel 200 has an accommodation space 210 for hermetically receiving the gel sheet 20 recovered in the form of a roll, as shown in FIGS. 4 to 6, and is connected to the accommodation space at one end.
  • An injection port 220 and an outlet 230 connected to the accommodation space 210 is formed at the other end.
  • Step (e) Gel sheet aging step ages the gel sheet 20, as shown in FIG. That is, the gel sheet 20 recovered in step (d) is accommodated in the accommodation space 210 of the reaction vessel 2000. Next, the accommodating space 210 of the reaction vessel 200 is heated to 70 ° C. for 50 minutes to uniformize the tissue of the gel sheet 20.
  • the (e) gel sheet aging step is left for 10 minutes at room temperature (or 25 °C) before aging in the reaction vessel 200, the aging proceeds. That is, by inducing stable gelation of the silica sol 2 and then aging, the structure of the gel sheet 20 can be made more uniform.
  • (F) gel sheet surface modification step is to modify the surface by spraying the coating liquid on the aged gel sheet 20, as shown in FIG. That is, (f) gel sheet surface modification step to prepare a coating solution by mixing ethanol and ammonia water (NH 4 OH). Then, the coating liquid is injected into the accommodation space 210 through the injection port 220 of the reaction vessel 200 into which the gel sheet 20 is inserted to modify the surface of the gel sheet 20. At this time, the coating solution is sprayed 1.6 times the silica sol impregnated on the surface of the fiber sheet in the step (c), the reaction vessel 200 is aged by aging and HMDS (Hxamethyldisilazane) for 1 hour at a high temperature of 70 °C gel sheet (20) Modify the surface of the.
  • HMDS Hexamethyldisilazane
  • HMDS Hexamethyldisilazane
  • (g) Gel sheet drying step as shown in Figure 6, to dry the gel sheet 20, the surface is modified to complete the airgel sheet 30.
  • (g) gel sheet drying step is a supercritical drying is carried out in a state that the gel sheet 20 is accommodated in the reaction vessel (200). That is, (g) gel sheet drying step is the first drying step of drying the surface-modified gel sheet 20 by injecting carbon dioxide at a rate of 70L / min for 10 minutes at 28 °C and 70 bar environment, 50 °C for 1 minute 20 minutes The secondary drying step of heating and drying to a furnace, and the third drying step of drying by injecting carbon dioxide at a rate of 0.7 L / min for 20 minutes at 50 ° C. and 150 bar, and 0.7 L / min for 20 minutes after 20 minutes of rest. And a fourth drying step of drying by injecting at a speed. As the drying step is performed, the drying rate of the gel sheet 20 may be increased.
  • the third drying of the gel sheet drying step is ethanol is generated in the reaction vessel 200 by the chemical reaction of carbon dioxide and the gel sheet 20, the ethanol generated in the reaction vessel 200 is discharge port 230 Discharge through and recover.
  • the gel sheet drying step includes a discharge step of discharging carbon dioxide for 2 hours after the fourth drying, thereby inducing a gentle environmental change in the gel sheet 20 to uniformize the tissue of the gel sheet 20. do.
  • the airgel sheet 30 is manufactured.
  • the step of laminating the fiber sheet 10 on both sides of the airgel sheet 30 is performed.
  • a fiber sheet 10 such as a blanket (blanket).
  • Composite sheet manufacturing method (S30) is a composite sheet 40 by manufacturing the laminated fiber sheet 10, the airgel sheet 30, and the fiber sheet 10 by heat and pressure. In this case, a composite sheet maker is used.
  • the composite sheet maker 300 according to the first embodiment of the present invention, as shown in Figure 7, the airgel sheet feed roller 310 for supplying the airgel sheet 30, the fiber on both sides of the airgel sheet 30 A plurality of fiber sheet supply roller 320 for supplying the sheet 10, respectively, the airgel sheet 30 and the heat-compressor 330 for pressing the fiber sheet 10 with heat and pressure to produce a composite sheet 40
  • the composite sheet 40 may be obtained while passing through the heat presser 330.
  • the composite sheet maker 300 further includes a drying member 340 for drying the airgel sheet 30 supplied from the airgel sheet supply roller 310, and the drying member 340. Increases the drying rate of the airgel sheet 30 further improves the bonding to the fiber sheet 10.
  • the composite sheet manufacturing apparatus 300 further includes a needling member 350 for needlessly bonding the airgel sheet 30 having the fiber sheet 10 interposed therebetween, and the needle
  • the ring member 350 prevents irregular bonding from occurring as a result of temporarily bonding the airgel sheet 30 and the fiber sheet 10.
  • the composite sheet maker 300 further includes a cutting member 360 for cutting the composite sheet 40 to a predetermined size to process the composite pad 50, the cutting member ( 360 is processed to the composite pad 50 by cutting the composite sheet 40 to increase the efficiency of use and storage.
  • the laminated fiber sheet 10, airgel sheet 30 and the fiber sheet 10 are bonded by heat and pressure to produce a composite sheet 40.
  • step S10 and step S20 further comprises the step of drying the prepared airgel sheet 30 (S15).
  • the airgel sheet 30 is dried by high temperature heat through the drying member 340 to evaporate moisture, thereby increasing the drying rate of the airgel sheet 30.
  • step S20 and step S30 includes the step of temporarily fixing the laminated airgel sheet 30 and the fiber sheet 10 by needling (S25).
  • the temporary fixing step (S25) is temporarily fixed by needling the airgel sheet 30 and the fiber sheet 10 in order to prevent movement when the laminated airgel sheet 30 and the fiber sheet 10 is compressed.
  • the composite sheet 40 of uniform quality can be obtained.
  • the composite sheet 40 laminated with the airgel sheet 30, the fiber sheet 10, and the airgel sheet 30 has been described as one embodiment.
  • a composite sheet 40 in which 30 and one or more fiber sheets 10 are laminated may also be manufactured.
  • the composite sheet 40 prepared as described above can be cut to a predetermined size to obtain a composite pad 50. That is, the composite pad 40 may be cut to a predetermined size through the cutting member 360 to obtain the composite pad 50.
  • the composite sheet manufacturing method and apparatus including an airgel having such a configuration and method it is possible to obtain a composite sheet and a composite pad having high adhesion and durability, low manufacturing cost, and particularly stable thickness.
  • Composite sheet manufacturing method shows another embodiment of the airgel sheet preparation step (S10) in the composite sheet manufacturing method according to the first embodiment described above.
  • the fiber sheet 10 is formed on both sides of the airgel sheet 30.
  • the airgel sheet preparation step (S10) prepares the airgel sheet 30 from the composite 20 including the airgel matrix and the reinforcing structure 21.
  • the airgel composite 20 is composed of two phases.
  • the first phase is a low density airgel matrix and the second phase is a reinforcing phase.
  • the reinforcing phase is primarily composed of a lofty fibrous material, preferably a lofty batting and a mixture of one or more fibrous materials of significantly different thickness, length or aspect ratio. Suitable mixtures of the two fibrous material systems are such that when short, high aspect ratio microfibers (one fibrous material) are dispersed throughout a continuous aerogel matrix that penetrates lofty fiber batting (other fibrous materials). Is made.
  • the airgel matrix is continuous through the reinforcing structure 21, the reinforcing structure 21 is a ropety fibrous bet, wherein the fibers are oriented along all three axes, and the Lofty fibrous bet is
  • the composite 20 is a resilient, durable lightweight insulation product, and the lofty fibrous bet is compressible to at least 50% of the thickness and recovers to at least 70% of the original thickness after 5 seconds of compression, and the lofty
  • the density of the fibrous batting is between 0.001 and 0.26 g / cm 3 and the cross sectional area of the discernible fibers in the cross section of the composite 20 may be less than 10% of the total cross sectional area.
  • the airgel matrix may be an organic airgel, an inorganic airgel or a mixture thereof.
  • the organic airgel is polyacrylate, polystyrene, polyacrylonitrile, polyurethane, polyimide, polyfurfural alcohol, phenyl furfuryl alcohol, melamine formaldehyde, resorcinol formaldehyde, cresol formaldehyde, phenol formaldehyde , Polyvinyl alcohol dialdehyde, polycyanurate, polyacrylamide, various epoxy, agar, agarose, or a mixture of two or more of them (CS Ashley, CJ Brinker and DM Smith, Journal of Non Crystalline Solid, Volume 285, 2001).
  • suitable metal alkoxides are those having 1 to 6 carbon atoms, preferably 1 to 4 carbon atoms in each alkyl group.
  • suitable metal alkoxides include tetraethoxysilane (TEOS), tetramethoxysilane (TMOS), tetra-n-propoxysilane, aluminum isopropoxide, aluminum sec-butoxide, cerium isopropoxide, Hafnium tert-butoxide, magnesium aluminum isopropoxide, yttrium isopropoxide, titanium isopropoxide, zirconium isopropoxide and the like.
  • TEOS tetraethoxysilane
  • TMOS tetramethoxysilane
  • tetra-n-propoxysilane aluminum isopropoxide, aluminum sec-butoxide, cerium isopropoxide, Hafnium tert-butoxide, magnesium aluminum isopropoxide, yttrium isopropoxide
  • silica precursors these materials can be partially hydrolyzed and stabilized at low pH with polymers of polysilic acid esters, for example polydiethoxysiloxanes. These materials are commercially available as alcohol solutions (eg Silbond®40, 40% silica content, Silbond Corporation). Pre-polymerized silica precursors are particularly suitable for the airgel composite 20 of the present invention.
  • Suitable materials for producing airgels used at low temperatures are non-refractory metal alkoxides based on oxide-forming metals. Suitable such metals are silicon, magnesium, mixtures thereof. Suitable alkoxides for high temperatures are generally refractory metal alkoxides capable of forming oxides, for example zirconia, yttria, hafnia, alumina, titania, ceria and the like and mixtures thereof such as zirconia and yttria. It is also possible to use non-refractory metals and refractory metals such as silicon and / or mixtures of magnesium and aluminum.
  • An advantage of using one or more metal oxide matrix materials in an airgel structure is the enhancement of IR clouding achieved by providing chemical functionalities that absorb radiation at a wide range of wavelengths.
  • Finely dispersed dopants such as carbon black, titania, iron oxides, silicon, carbides, molybdenum, silicides, manganese oxides, polydialkylsiloxanes, where the alkyl groups have from 1 to 4 carbon atoms Can be added to improve thermal performance at high temperatures by increasing the opacity of the airgel to IR transmission. Suitable amounts of such dopants are generally from 1 to 20 wt%, preferably from 2 to 10% of the weight of the final composite.
  • Lofty fibrous bets are defined as fibrous materials that exhibit bulk properties and significant elasticity (complete bulk recovery zones).
  • a suitable form is a soft web.
  • the use of Lofty batting reinforcements avoids substantial deterioration of the thermal performance of the airgel while minimizing the volume of the unsupported airgel.
  • batting means a layer or sheet of fibrous material that is used as a lining cover, cotton or container, or a blanket for thermal insulation.
  • the reinforcing fibrous material used in the second embodiment of the present invention is one or a plurality of lofty fibrous batting layers.
  • the use of lofty batting reinforcements avoids substantial deterioration of the thermal performance of the airgel while minimizing the volume of the unsupported airgel.
  • batting is a product made from carding or Garnetting fibers that form a smooth web of fibers in the form of a sheet, but in the present invention a "batting” is a non-sheet that is sufficiently open to "rope". Web in the form of, for example, Primaloft® products from Albany International. Generally, batting refers to a layer or sheet of fibrous material used as a lining cover, cotton or container, or a blanket for thermal insulation. Fibers suitable for producing batting are relatively thin and have deniers of 15 or less, preferably 10 or less. The softness of the web is a by-product of the relatively thin and oriented fibers that are used to make the fibrous web.
  • the batting retains a small number of individual threads (or fibers) so as not to significantly alter the thermal properties of the reinforced composite 20 compared to non-reinforced aerogels of the same material.
  • it is called "lofty”.
  • the cross section of the fiber in the cross section of the final airgel composite 20 is less than 10%, preferably less than 8%, most preferably less than 5% of the total cross section of the cross section.
  • the lofty bets have a thermal conductivity of 50 mW / m-K or less at room temperature and pressure to promote the formation of low thermal conductivity airgel composite 20.
  • the Lofty bet is (i) compressible to at least 50%, preferably at least 65%, most preferably at least 80% of the intrinsic thickness and at least 70%, preferably at least at least after a few seconds of compression 75%, most preferably at least 80%.
  • lofty bets can be substantially restored to their original size and shape by removing air (bulk) in the case of compression. For example, a HolofilTM bet can be compressed to a minimum of 0.2 "from the original 1.5" thickness and will return to the original thickness when the load is removed.
  • the bet may be considered to have 1.3 "air (bulk) and 0.2" fibers. It is compressible up to 87% and recovers to almost 100% of its original thickness. Glass fiber batting used for home insulation can be recovered to approximately 80% of its original thickness, although compressed and slowed to a similar degree.
  • the batting used in the second embodiment of the present invention is substantially different from the fibrous mat.
  • a fibrous mat is a "tightly woven or tangle of lumps", that is, a dense and relatively rigid fibrous structure that retains minimal open space between adjacent fibers.
  • the mat has a density of 2.5 lbs / ft3 (0.41 g / cc), while the ropet bets used herein have a much smaller density, i.e. 0.1-16 lbs / ft3 (0.001-0.26 g / cc), preferably 2.4 To 6.1 lbs / ft 3 (0.04-0.1 g / cc).
  • the mat is compressible to less than 20% and shows little elasticity.
  • the cross section of the mat fiber accounts for up to 30-50% of the total cross section.
  • the bet maintains at least 50% thickness after the gel forming liquid is poured.
  • the fiber composite material traveling in the z-axis acts as a heat conduit to produce To significantly increase the thermal conductivity of
  • bets that retain almost straight (non-curly) fibers in the x-y horizontal plane are more rigid than typical lofty bets of equal density where the bent or curly fibers run in all three axes.
  • the bet should show less heat flow in the z axis (heat flow direction).
  • the fibers in the z axis can be composed of a material different from that in the x and y axes (preferably, a material having a lower thermal conductivity).
  • the z-axis fibers may be made more pliable than the fibers in the x-y direction to provide a more twisted path for heat conduction.
  • the same fiber materials and methods can be used throughout the batting to minimize thermal conduction on all axes, but using many of these materials and methods will reduce the elasticity of the resulting composites, since in many insulating products the heat flow is treated in a particular direction. Can be.
  • An ideal lofty bet has fine, curly fibers evenly distributed throughout the composite 20.

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  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Laminated Bodies (AREA)

Abstract

La présente invention concerne un procédé de fabrication d'une feuille composite comprenant une feuille d'aérogel. Le procédé peut comprendre les étapes consistant : à préparer une feuille d'aérogel (30) (S10) ; à stratifier des feuilles de fibre (10) sur les deux côtés de la feuille d'aérogel (30), respectivement (S20) ; et à coller la feuille d'aérogel (30) et les feuilles de fibre (10) stratifiées par chaleur et pression pour fabriquer une feuille composite (40) ayant la feuille de fibre (10), la feuille d'aérosol (30) et la feuille de fibre (10) stratifiées en séquence (S30).
PCT/KR2017/001327 2016-02-19 2017-02-07 Procédé et appareil de fabrication de feuille composite comprenant une feuille d'aérogel Ceased WO2017142244A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
EP17753405.4A EP3326810B1 (fr) 2016-02-19 2017-02-07 Procédé et appareil de fabrication de feuille composite comprenant une feuille d'aérogel
JP2018520558A JP6612443B2 (ja) 2016-02-19 2017-02-07 エアロゲルシートを含む複合シートの製造方法及び製造装置
US15/755,500 US10682839B2 (en) 2016-02-19 2017-02-07 Apparatus and method for manufacturing composite sheet comprising aerogel sheet
CN201780003197.6A CN108136749B (zh) 2016-02-19 2017-02-07 包含气凝胶片的复合片材的制备方法和制备装置

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KR10-2016-0019833 2016-02-19
KR20160019833 2016-02-19
KR1020160095254A KR101962206B1 (ko) 2016-02-19 2016-07-27 에어로겔 시트를 포함하는 복합시트 제조방법 및 제조장치
KR10-2016-0095254 2016-07-27

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3536494A1 (fr) * 2018-03-09 2019-09-11 Deutsches Zentrum für Luft- und Raumfahrt e.V. Procédé d'assemblage en une seule étape pour corps composites de composant renforcé par des fibres et d'aérogel
CN113478930A (zh) * 2021-07-22 2021-10-08 浙江圣润纳米科技有限公司 一种高抗拉拔气凝胶复合材料及其制备方法
CN114682177A (zh) * 2022-03-22 2022-07-01 张成群 一种通用型复合气凝胶材料的生产系统
EP4282798A4 (fr) * 2021-08-20 2025-01-15 Gong Yi Van-research Innovation Composite Material Co., Ltd Dispositif de préparation de feutre d'aérogel et procédé associé

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR19990009158A (ko) * 1997-07-08 1999-02-05 최세영 실리카 에어로겔의 제조방법
KR100909732B1 (ko) * 2000-12-22 2009-07-29 아스펜 에어로겔, 인코퍼레이티드 섬유성 배팅을 보유하는 에어로겔 복합물
US20140287641A1 (en) * 2013-03-15 2014-09-25 Aerogel Technologies, Llc Layered aerogel composites, related aerogel materials, and methods of manufacture
KR101506096B1 (ko) * 2013-11-08 2015-03-25 지오스 에어로겔 리미티드 적층방식을 이용한 에어로겔이 함침된 단열원단의 제조장치 및 제조방법
KR20150093122A (ko) * 2014-02-06 2015-08-17 주식회사 엘지화학 소수성 실리카 에어로겔의 제조방법

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR19990009158A (ko) * 1997-07-08 1999-02-05 최세영 실리카 에어로겔의 제조방법
KR100909732B1 (ko) * 2000-12-22 2009-07-29 아스펜 에어로겔, 인코퍼레이티드 섬유성 배팅을 보유하는 에어로겔 복합물
US20140287641A1 (en) * 2013-03-15 2014-09-25 Aerogel Technologies, Llc Layered aerogel composites, related aerogel materials, and methods of manufacture
KR101506096B1 (ko) * 2013-11-08 2015-03-25 지오스 에어로겔 리미티드 적층방식을 이용한 에어로겔이 함침된 단열원단의 제조장치 및 제조방법
KR20150093122A (ko) * 2014-02-06 2015-08-17 주식회사 엘지화학 소수성 실리카 에어로겔의 제조방법

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3536494A1 (fr) * 2018-03-09 2019-09-11 Deutsches Zentrum für Luft- und Raumfahrt e.V. Procédé d'assemblage en une seule étape pour corps composites de composant renforcé par des fibres et d'aérogel
CN113478930A (zh) * 2021-07-22 2021-10-08 浙江圣润纳米科技有限公司 一种高抗拉拔气凝胶复合材料及其制备方法
EP4282798A4 (fr) * 2021-08-20 2025-01-15 Gong Yi Van-research Innovation Composite Material Co., Ltd Dispositif de préparation de feutre d'aérogel et procédé associé
CN114682177A (zh) * 2022-03-22 2022-07-01 张成群 一种通用型复合气凝胶材料的生产系统

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