EP1919829A2 - Aerogel et son procede de fabrication - Google Patents
Aerogel et son procede de fabricationInfo
- Publication number
- EP1919829A2 EP1919829A2 EP06813666A EP06813666A EP1919829A2 EP 1919829 A2 EP1919829 A2 EP 1919829A2 EP 06813666 A EP06813666 A EP 06813666A EP 06813666 A EP06813666 A EP 06813666A EP 1919829 A2 EP1919829 A2 EP 1919829A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- gel
- solution
- aerogel
- temperature
- chilled
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 239000004964 aerogel Substances 0.000 title claims abstract description 139
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 78
- 239000003054 catalyst Substances 0.000 claims abstract description 77
- 238000000034 method Methods 0.000 claims abstract description 65
- 239000000203 mixture Substances 0.000 claims abstract description 52
- 238000002156 mixing Methods 0.000 claims abstract description 28
- 239000012530 fluid Substances 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims description 187
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 98
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 81
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 claims description 76
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 57
- 239000002904 solvent Substances 0.000 claims description 53
- 238000001035 drying Methods 0.000 claims description 51
- 239000011259 mixed solution Substances 0.000 claims description 44
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 239000002245 particle Substances 0.000 claims description 32
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 30
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 29
- 150000004703 alkoxides Chemical class 0.000 claims description 27
- 239000000908 ammonium hydroxide Substances 0.000 claims description 25
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 23
- 238000009826 distribution Methods 0.000 claims description 22
- 239000011148 porous material Substances 0.000 claims description 22
- 230000005540 biological transmission Effects 0.000 claims description 20
- 238000009792 diffusion process Methods 0.000 claims description 16
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 14
- 239000004965 Silica aerogel Substances 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 12
- 230000032683 aging Effects 0.000 claims description 10
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 8
- 238000009833 condensation Methods 0.000 claims description 7
- 230000005494 condensation Effects 0.000 claims description 7
- 238000006884 silylation reaction Methods 0.000 claims description 7
- 238000013459 approach Methods 0.000 claims description 4
- 238000006136 alcoholysis reaction Methods 0.000 claims description 3
- 238000005886 esterification reaction Methods 0.000 claims description 3
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 6
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims 5
- 229940073561 hexamethyldisiloxane Drugs 0.000 claims 5
- 150000001348 alkyl chlorides Chemical class 0.000 claims 3
- 150000002576 ketones Chemical class 0.000 claims 3
- 238000007599 discharging Methods 0.000 claims 2
- 239000005055 methyl trichlorosilane Substances 0.000 claims 2
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims 2
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 28
- 230000015572 biosynthetic process Effects 0.000 abstract description 25
- 238000003786 synthesis reaction Methods 0.000 abstract description 7
- 230000002209 hydrophobic effect Effects 0.000 abstract description 3
- 229910052723 transition metal Inorganic materials 0.000 abstract 1
- 150000003624 transition metals Chemical class 0.000 abstract 1
- 239000000499 gel Substances 0.000 description 81
- 238000006243 chemical reaction Methods 0.000 description 33
- 239000000047 product Substances 0.000 description 31
- 238000002360 preparation method Methods 0.000 description 18
- 238000000149 argon plasma sintering Methods 0.000 description 13
- OZXIZRZFGJZWBF-UHFFFAOYSA-N 1,3,5-trimethyl-2-(2,4,6-trimethylphenoxy)benzene Chemical compound CC1=CC(C)=CC(C)=C1OC1=C(C)C=C(C)C=C1C OZXIZRZFGJZWBF-UHFFFAOYSA-N 0.000 description 11
- 239000006227 byproduct Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- SHOJXDKTYKFBRD-UHFFFAOYSA-N mesityl oxide Natural products CC(C)=CC(C)=O SHOJXDKTYKFBRD-UHFFFAOYSA-N 0.000 description 11
- 239000002994 raw material Substances 0.000 description 11
- 230000002829 reductive effect Effects 0.000 description 11
- 238000001338 self-assembly Methods 0.000 description 11
- 238000006460 hydrolysis reaction Methods 0.000 description 10
- 230000003287 optical effect Effects 0.000 description 10
- 238000000137 annealing Methods 0.000 description 9
- 238000003556 assay Methods 0.000 description 9
- 238000002425 crystallisation Methods 0.000 description 8
- 230000008025 crystallization Effects 0.000 description 8
- 238000007710 freezing Methods 0.000 description 8
- 230000008014 freezing Effects 0.000 description 8
- 230000007062 hydrolysis Effects 0.000 description 8
- 239000011240 wet gel Substances 0.000 description 8
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 6
- 238000009413 insulation Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 238000011049 filling Methods 0.000 description 4
- 238000001879 gelation Methods 0.000 description 4
- 239000011810 insulating material Substances 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 230000008646 thermal stress Effects 0.000 description 4
- 150000001299 aldehydes Chemical class 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000017 hydrogel Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000000741 silica gel Substances 0.000 description 3
- 229910002027 silica gel Inorganic materials 0.000 description 3
- -1 silicon alkoxide Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- 241000143637 Eleocharis confervoides Species 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910008051 Si-OH Inorganic materials 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 229910006358 Si—OH Inorganic materials 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 238000010494 dissociation reaction Methods 0.000 description 2
- 230000005593 dissociations Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 2
- 229920001903 high density polyethylene Polymers 0.000 description 2
- 239000004700 high-density polyethylene Substances 0.000 description 2
- 229940063583 high-density polyethylene Drugs 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- JTJMJGYZQZDUJJ-UHFFFAOYSA-N phencyclidine Chemical compound C1CCCCN1C1(C=2C=CC=CC=2)CCCCC1 JTJMJGYZQZDUJJ-UHFFFAOYSA-N 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 230000002441 reversible effect Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910007156 Si(OH)4 Inorganic materials 0.000 description 1
- 229910007154 Si(OH)4+4 Inorganic materials 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005882 aldol condensation reaction Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000012691 depolymerization reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 230000005237 high-frequency sound signal Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229930193185 isoxylitone Natural products 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000004531 microgranule Substances 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- 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
- C01B33/16—Preparation of silica xerogels
- C01B33/163—Preparation of silica xerogels by hydrolysis of organosilicon compounds, e.g. ethyl orthosilicate
-
- 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
-
- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04B—GENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS
- E04B1/00—Constructions in general; Structures which are not restricted either to walls, e.g. partitions, or floors or ceilings or roofs
- E04B1/62—Insulation or other protection; Elements or use of specified material therefor
- E04B1/74—Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls
- E04B1/76—Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls specifically with respect to heat only
- E04B1/78—Heat insulating elements
- E04B1/80—Heat insulating elements slab-shaped
-
- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04C—STRUCTURAL ELEMENTS; BUILDING MATERIALS
- E04C2/00—Building elements of relatively thin form for the construction of parts of buildings, e.g. sheet materials, slabs, or panels
- E04C2/54—Slab-like translucent elements
- E04C2/543—Hollow multi-walled panels with integrated webs
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
- Y02A30/24—Structural elements or technologies for improving thermal insulation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B80/00—Architectural or constructional elements improving the thermal performance of buildings
- Y02B80/10—Insulation, e.g. vacuum or aerogel insulation
Definitions
- the temperature, the pH, the induced (sonic) energy, and the ratio of carbamaldehyde, alcohol, or DAA-to-the ratio of the precursor are among the most critical parameters which determine the characteristics of the resulting aerogel, e.g., the Kalgel aerogel. Those parameters control OH dissociation, hydrolysis, and polycondensation, and thus they can control the final characteristics of the resulting aerogel product.
- the washed gel (e.g., alcogel) is then dried at a temperature of about 150 0 F (65.6 0 C) for about 6 hours, followed by drying at a temperature of about 220 0 F (104.4 0 C) for 6 hours, followed by drying (e.g., annealing of the aerogel) at a temperature of about 392 0 F (200 0 C) for up to 6 hours, e.g., typically between about 0.5-2 hours.
- the dried product is collected and screened, per the specific requirements, to obtain the final nanogel.
- one of the top, bottom and side walls 52, 54, 56, 58 is provided with an opening to facilitate filling of the internal volume of the insulating panel 50 with the aerogel and this opening is covered by a cover 66, after sufficient filling with the aerogel, to seal the aerogel therein.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Architecture (AREA)
- Organic Chemistry (AREA)
- Civil Engineering (AREA)
- Dispersion Chemistry (AREA)
- Structural Engineering (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Acoustics & Sound (AREA)
- Electromagnetism (AREA)
- Silicon Compounds (AREA)
- Silicon Polymers (AREA)
Abstract
L'invention concerne un procédé à pression ambiante et à faible durée de cycle, pour la synthèse et la fabrication d'un nanogel hydrophile et hydrophobe, à base d'un métal de transition à faible densité, hautement isolant, hautement translucide, et à faible coût. Les aspects importants portent sur le procédé de synthèse, l'étape consistant à impartir une hydrophobicité, et le procédé de fabrication. Le procédé comprend les étapes de mélange d'une solution de précurseur refroidie avec une solution de catalyseur refroidie, de façon que le mélange présente un pH compris entre 9,5 et 12,2. Le mélange est maintenu à une température de 34 °F- 55 °F pendant 1 à 120 minutes, de manière à former un gel. Le gel est silylé pendant environ 120 minutes, lavé dans un fluide de lavage, puis séché et recuit pour former l'aérogel.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US71121905P | 2005-08-25 | 2005-08-25 | |
| US11/301,724 US7618608B1 (en) | 2005-12-13 | 2005-12-13 | Aerogel and method of manufacturing same |
| PCT/US2006/032882 WO2007024925A2 (fr) | 2005-08-25 | 2006-08-22 | Aerogel et son procede de fabrication |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP1919829A2 true EP1919829A2 (fr) | 2008-05-14 |
| EP1919829A4 EP1919829A4 (fr) | 2011-03-23 |
Family
ID=37772317
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP06813666A Withdrawn EP1919829A4 (fr) | 2005-08-25 | 2006-08-22 | Aerogel et son procede de fabrication |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP1919829A4 (fr) |
| CA (1) | CA2619860A1 (fr) |
| WO (1) | WO2007024925A2 (fr) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7750056B1 (en) * | 2006-10-03 | 2010-07-06 | Sami Daoud | Low-density, high r-value translucent nanocrystallites |
| KR100868989B1 (ko) * | 2007-05-23 | 2008-11-17 | 엠파워(주) | 초소수성 실리카 에어로겔 분말의 제조방법 |
| KR20090032707A (ko) * | 2007-09-28 | 2009-04-01 | 엠파워(주) | 초소수성 실리카계 분말의 제조방법 |
| DE102008046444A1 (de) | 2008-09-09 | 2010-03-11 | Evonik Röhm Gmbh | Fassadenplatte, System und Verfahren zur Energiegewinnung |
| WO2011020671A1 (fr) | 2009-08-20 | 2011-02-24 | Evonik Röhm Gmbh | Dalle isolante en plastique, système et procédé d'isolation thermique |
| CN109851286A (zh) * | 2017-11-30 | 2019-06-07 | 湖南梨树园涂料有限公司 | 一种防脱落的保温材料及施工方法 |
| CN108479716A (zh) * | 2018-05-11 | 2018-09-04 | 广东工业大学 | 一种复合气凝胶、制备方法及其应用 |
| WO2020005965A1 (fr) * | 2018-06-25 | 2020-01-02 | The Regents Of The University Of California | Revêtements et monolithes nanoporeux optiquement transparents et thermiquement isolants |
| CN109133071B (zh) * | 2018-08-07 | 2021-10-22 | 济南大学 | 一种有机杂化二氧化硅气凝胶的制备方法 |
| CN114620736B (zh) * | 2021-12-15 | 2023-04-18 | 航天海鹰(镇江)特种材料有限公司 | 一种压缩可控的SiO2气凝胶复合材料制备方法 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1992020623A1 (fr) * | 1991-05-24 | 1992-11-26 | Sinvent A/S | Procede de preparation d'un materiau analogue a un aerogel de silice |
| US20010034375A1 (en) * | 1996-11-26 | 2001-10-25 | Fritz Schwertfeger | Organically modified aerogels, processes for their preparation by surface modification of the aqueous gel, without prior solvent exchange, and subsequent drying, and thier use |
| EP1153739A1 (fr) * | 1999-11-10 | 2001-11-14 | Matsushita Electric Works, Ltd. | Substrat d'aerogel et son procede de preparation |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5795556A (en) * | 1993-12-14 | 1998-08-18 | Hoechst Ag | Xerogels and process for their preparation |
| US6258305B1 (en) * | 1999-03-29 | 2001-07-10 | Sandia Corporation | Method for net-shaping using aerogels |
| WO2001028675A1 (fr) * | 1999-10-21 | 2001-04-26 | Aspen Systems, Inc. | Procede de production rapide d'aerogel |
-
2006
- 2006-08-22 CA CA002619860A patent/CA2619860A1/fr not_active Abandoned
- 2006-08-22 EP EP06813666A patent/EP1919829A4/fr not_active Withdrawn
- 2006-08-22 WO PCT/US2006/032882 patent/WO2007024925A2/fr active Application Filing
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1992020623A1 (fr) * | 1991-05-24 | 1992-11-26 | Sinvent A/S | Procede de preparation d'un materiau analogue a un aerogel de silice |
| US20010034375A1 (en) * | 1996-11-26 | 2001-10-25 | Fritz Schwertfeger | Organically modified aerogels, processes for their preparation by surface modification of the aqueous gel, without prior solvent exchange, and subsequent drying, and thier use |
| EP1153739A1 (fr) * | 1999-11-10 | 2001-11-14 | Matsushita Electric Works, Ltd. | Substrat d'aerogel et son procede de preparation |
Non-Patent Citations (1)
| Title |
|---|
| See also references of WO2007024925A2 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CA2619860A1 (fr) | 2007-03-01 |
| WO2007024925A3 (fr) | 2008-04-10 |
| WO2007024925A2 (fr) | 2007-03-01 |
| EP1919829A4 (fr) | 2011-03-23 |
| WO2007024925A9 (fr) | 2007-04-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US7618608B1 (en) | Aerogel and method of manufacturing same | |
| WO2007024925A2 (fr) | Aerogel et son procede de fabrication | |
| Wang et al. | Transparent thermal insulation silica aerogels | |
| US5565142A (en) | Preparation of high porosity xerogels by chemical surface modification. | |
| JP4994360B2 (ja) | アルコキシシラン基で修飾したシリカ／ラテックスハイブリッドからなるモノリシックキセロゲル及びエーロゲルの臨界未満の条件下における製造方法。 | |
| Buckley et al. | The sol-gel preparation of silica gels | |
| Shimizu et al. | Transparent, highly insulating polyethyl-and polyvinylsilsesquioxane aerogels: mechanical improvements by vulcanization for ambient pressure drying | |
| CN108609621B (zh) | 一种二氧化硅气凝胶的制备方法 | |
| Montes et al. | Aerogels and their applications | |
| US5866027A (en) | Process for producing fiber-reinforced xerogels and their use | |
| Dervin et al. | An introduction to sol-gel processing for aerogels | |
| Hæreid et al. | Properties of silica gels aged in TEOS | |
| JP2008208019A (ja) | 多孔質材及びその調製方法 | |
| US20110245359A1 (en) | Methods of preparing hybrid aerogels | |
| JP2007519780A (ja) | ケイ素結合ポリメタクリレートを含有する有機変性シリカエアロゲル | |
| CN100372765C (zh) | 一种制备憎水SiO2气凝胶的方法 | |
| JP3436037B2 (ja) | バルク状シリカ多孔体の製造方法 | |
| Rashid et al. | Silica aerogel: Synthesis, characterization, applications, and recent advancements | |
| CN115485239B (zh) | 具有增大的碱性稳定性的二氧化硅气凝胶 | |
| JP2005350519A (ja) | 多孔体およびその製造方法 | |
| KR100823072B1 (ko) | 고투명도의 에어로젤의 제조방법 및 이에 의해 제조된에어로젤 | |
| Julio et al. | Ambient pressure hybrid silica monoliths with hexamethyldisilazane: from vitreous hydrophilic xerogels to superhydrophobic aerogels | |
| Hæreid et al. | Subcritical drying of silica gels | |
| Einarsrud et al. | Preparation of transparent, monolithic silica xerogels with low density: Code: HP9 | |
| KR20090008084A (ko) | 실리카 에어로젤의 제조방법과 이에 의하여 제조된 실리카에어로젤 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
| 17P | Request for examination filed |
Effective date: 20080319 |
|
| AK | Designated contracting states |
Kind code of ref document: A2 Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IS IT LI LT LU LV MC NL PL PT RO SE SI SK TR |
|
| AX | Request for extension of the european patent |
Extension state: AL BA HR MK RS |
|
| R17D | Deferred search report published (corrected) |
Effective date: 20080410 |
|
| A4 | Supplementary search report drawn up and despatched |
Effective date: 20110221 |
|
| RIC1 | Information provided on ipc code assigned before grant |
Ipc: E04C 2/54 20060101ALI20110215BHEP Ipc: E04B 1/80 20060101ALI20110215BHEP Ipc: C01B 33/158 20060101ALI20110215BHEP Ipc: B01J 13/00 20060101ALI20110215BHEP Ipc: C01B 33/12 20060101AFI20070509BHEP |
|
| 17Q | First examination report despatched |
Effective date: 20120402 |
|
| DAX | Request for extension of the european patent (deleted) | ||
| STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN |
|
| 18D | Application deemed to be withdrawn |
Effective date: 20120814 |