KR20170059884A - Waterproof compound contai ning carbon fiber and prepararing method thereof - Google Patents
Waterproof compound contai ning carbon fiber and prepararing method thereof Download PDFInfo
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- KR20170059884A KR20170059884A KR1020160133697A KR20160133697A KR20170059884A KR 20170059884 A KR20170059884 A KR 20170059884A KR 1020160133697 A KR1020160133697 A KR 1020160133697A KR 20160133697 A KR20160133697 A KR 20160133697A KR 20170059884 A KR20170059884 A KR 20170059884A
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- water
- bentonite
- swellable
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims description 29
- 239000004917 carbon fiber Substances 0.000 title claims description 29
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims description 23
- 238000000034 method Methods 0.000 title claims description 17
- 150000001875 compounds Chemical class 0.000 title description 2
- 239000000463 material Substances 0.000 claims abstract description 70
- 239000010426 asphalt Substances 0.000 claims abstract description 52
- 239000002775 capsule Substances 0.000 claims abstract description 44
- 229910010272 inorganic material Inorganic materials 0.000 claims abstract description 29
- 239000011147 inorganic material Substances 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011368 organic material Substances 0.000 claims abstract description 13
- 239000002131 composite material Substances 0.000 claims abstract description 8
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 75
- 239000000440 bentonite Substances 0.000 claims description 74
- 229910000278 bentonite Inorganic materials 0.000 claims description 74
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 56
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 39
- 238000004078 waterproofing Methods 0.000 claims description 38
- 239000000945 filler Substances 0.000 claims description 33
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 33
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 28
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 26
- 239000002245 particle Substances 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 23
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 22
- 235000021355 Stearic acid Nutrition 0.000 claims description 20
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 20
- 239000008117 stearic acid Substances 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000002444 silanisation Methods 0.000 claims description 14
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 12
- 239000003607 modifier Substances 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000004014 plasticizer Substances 0.000 claims description 6
- FACXGONDLDSNOE-UHFFFAOYSA-N buta-1,3-diene;styrene Chemical group C=CC=C.C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 FACXGONDLDSNOE-UHFFFAOYSA-N 0.000 claims description 5
- 229920000468 styrene butadiene styrene block copolymer Polymers 0.000 claims description 5
- 229920002125 Sokalan® Polymers 0.000 claims description 4
- 239000004433 Thermoplastic polyurethane Substances 0.000 claims description 4
- 125000003277 amino group Chemical group 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 239000004584 polyacrylic acid Substances 0.000 claims description 4
- 229920002803 thermoplastic polyurethane Polymers 0.000 claims description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 3
- 230000002776 aggregation Effects 0.000 claims description 3
- 150000001491 aromatic compounds Chemical class 0.000 claims description 3
- 238000009830 intercalation Methods 0.000 claims description 3
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- 229920000058 polyacrylate Polymers 0.000 claims description 3
- 230000000379 polymerizing effect Effects 0.000 claims description 3
- 239000002028 Biomass Substances 0.000 claims description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 238000005054 agglomeration Methods 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- KQAHMVLQCSALSX-UHFFFAOYSA-N decyl(trimethoxy)silane Chemical compound CCCCCCCCCC[Si](OC)(OC)OC KQAHMVLQCSALSX-UHFFFAOYSA-N 0.000 claims description 2
- 125000003700 epoxy group Chemical group 0.000 claims description 2
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 2
- 125000000524 functional group Chemical group 0.000 claims description 2
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 claims description 2
- KWLMIXQRALPRBC-UHFFFAOYSA-L hectorite Chemical compound [Li+].[OH-].[OH-].[Na+].[Mg+2].O1[Si]2([O-])O[Si]1([O-])O[Si]([O-])(O1)O[Si]1([O-])O2 KWLMIXQRALPRBC-UHFFFAOYSA-L 0.000 claims description 2
- 229910000271 hectorite Inorganic materials 0.000 claims description 2
- 239000000025 natural resin Substances 0.000 claims description 2
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 claims description 2
- 229920001083 polybutene Polymers 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229910000275 saponite Inorganic materials 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 229920001059 synthetic polymer Polymers 0.000 claims description 2
- RXRIEAKKQPAUKB-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1.CO[Si](OC)(OC)CCCOCC1CO1 RXRIEAKKQPAUKB-UHFFFAOYSA-N 0.000 claims description 2
- VSKJLJHPAFKHBX-UHFFFAOYSA-N 2-methylbuta-1,3-diene;styrene Chemical compound CC(=C)C=C.C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 VSKJLJHPAFKHBX-UHFFFAOYSA-N 0.000 claims 2
- IYAYDWLKTPIEDC-UHFFFAOYSA-N 2-[2-hydroxyethyl(3-triethoxysilylpropyl)amino]ethanol Chemical compound CCO[Si](OCC)(OCC)CCCN(CCO)CCO IYAYDWLKTPIEDC-UHFFFAOYSA-N 0.000 claims 1
- 150000001408 amides Chemical class 0.000 claims 1
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 claims 1
- 239000004927 clay Substances 0.000 claims 1
- 238000009396 hybridization Methods 0.000 claims 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims 1
- 230000008961 swelling Effects 0.000 abstract description 10
- 238000011049 filling Methods 0.000 abstract description 6
- 230000002522 swelling effect Effects 0.000 abstract description 4
- 239000010954 inorganic particle Substances 0.000 abstract 1
- 239000011146 organic particle Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 42
- 230000000704 physical effect Effects 0.000 description 8
- 238000010183 spectrum analysis Methods 0.000 description 8
- 238000003756 stirring Methods 0.000 description 7
- 239000013585 weight reducing agent Substances 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
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- 230000035484 reaction time Effects 0.000 description 5
- 239000010920 waste tyre Substances 0.000 description 5
- 239000000470 constituent Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229920001971 elastomer Polymers 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000011229 interlayer Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- -1 magnetic Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000005060 rubber Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229920006037 cross link polymer Polymers 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000000123 paper Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229940070721 polyacrylate Drugs 0.000 description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 2
- 239000000126 substance Chemical group 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- TUGGFUSCPLPUFY-UHFFFAOYSA-N 3-triethoxysilylpropan-1-amine Chemical compound CCO[Si](OCC)(OCC)CCCN.CCO[Si](OCC)(OCC)CCCN TUGGFUSCPLPUFY-UHFFFAOYSA-N 0.000 description 1
- 229910021532 Calcite Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- FYHXNYLLNIKZMR-UHFFFAOYSA-N calcium;carbonic acid Chemical compound [Ca].OC(O)=O FYHXNYLLNIKZMR-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000003009 desulfurizing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 229920003170 water-soluble synthetic polymer Polymers 0.000 description 1
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Classifications
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- 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
- E04B1/64—Insulation or other protection; Elements or use of specified material therefor for making damp-proof; Protection against corrosion
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D195/00—Coating compositions based on bituminous materials, e.g. asphalt, tar, pitch
-
- E—FIXED CONSTRUCTIONS
- E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
- E01D—CONSTRUCTION OF BRIDGES, ELEVATED ROADWAYS OR VIADUCTS; ASSEMBLY OF BRIDGES
- E01D19/00—Structural or constructional details of bridges
- E01D19/08—Damp-proof or other insulating layers; Drainage arrangements or devices ; Bridge deck surfacings
-
- E—FIXED CONSTRUCTIONS
- E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
- E01D—CONSTRUCTION OF BRIDGES, ELEVATED ROADWAYS OR VIADUCTS; ASSEMBLY OF BRIDGES
- E01D19/00—Structural or constructional details of bridges
- E01D19/08—Damp-proof or other insulating layers; Drainage arrangements or devices ; Bridge deck surfacings
- E01D19/083—Waterproofing of bridge decks; Other insulations for bridges, e.g. thermal ; Bridge deck surfacings
-
- E—FIXED CONSTRUCTIONS
- E02—HYDRAULIC ENGINEERING; FOUNDATIONS; SOIL SHIFTING
- E02D—FOUNDATIONS; EXCAVATIONS; EMBANKMENTS; UNDERGROUND OR UNDERWATER STRUCTURES
- E02D31/00—Protective arrangements for foundations or foundation structures; Ground foundation measures for protecting the soil or the subsoil water, e.g. preventing or counteracting oil pollution
- E02D31/02—Protective arrangements for foundations or foundation structures; Ground foundation measures for protecting the soil or the subsoil water, e.g. preventing or counteracting oil pollution against ground humidity or ground water
-
- E—FIXED CONSTRUCTIONS
- E02—HYDRAULIC ENGINEERING; FOUNDATIONS; SOIL SHIFTING
- E02D—FOUNDATIONS; EXCAVATIONS; EMBANKMENTS; UNDERGROUND OR UNDERWATER STRUCTURES
- E02D31/00—Protective arrangements for foundations or foundation structures; Ground foundation measures for protecting the soil or the subsoil water, e.g. preventing or counteracting oil pollution
- E02D31/02—Protective arrangements for foundations or foundation structures; Ground foundation measures for protecting the soil or the subsoil water, e.g. preventing or counteracting oil pollution against ground humidity or ground water
- E02D31/04—Watertight packings for use under hydraulic pressure
-
- 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
- E04B1/66—Sealings
- E04B1/665—Sheets or foils impervious to water and water vapor
-
- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04D—ROOF COVERINGS; SKY-LIGHTS; GUTTERS; ROOF-WORKING TOOLS
- E04D11/00—Roof covering, as far as not restricted to features covered by only one of groups E04D1/00 - E04D9/00; Roof covering in ways not provided for by groups E04D1/00 - E04D9/00, e.g. built-up roofs, elevated load-supporting roof coverings
- E04D11/02—Build-up roofs, i.e. consisting of two or more layers bonded together in situ, at least one of the layers being of watertight composition
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Structural Engineering (AREA)
- Civil Engineering (AREA)
- Architecture (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Materials Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Mining & Mineral Resources (AREA)
- Paleontology (AREA)
- General Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
본 발명은 방수재에 손상(잔갈림 및 찢김 등)이 발생하여 누수가 되었을 때 기능성 유/무기재료가 유실되지 않고 쪼개진 기능성 유/무기재료 캡슐(실란화 코팅) 안의 기능성 유/무기재료(벤토나이트 입자들 또는 층간에 폴리아크릴산을 삽입(intercalate)한 벤토나이트 입자들)들이 팽윤하면서 자가보수(self-repair)가 수행되어 방수재의 성능유지가 되도록 기능성 유/무기재료 캡슐을 개질아스팔트에 충진한 기능성 방수소재 및 탄소소재를 포함한 방수 개질아스팔트의 물성 제고용 하이브리드 충진재를 상기 기능성 방수소재에 충진한 고기능성 하이브리드 방수재와 그 제조방법에 관한 것이다.The present invention relates to a functional oil / inorganic material (bentonite particles) in a functional oil / inorganic material capsule (silanized coating) that does not lose functional oil / inorganic material when leakage occurs due to damage (such as grinding and tearing) (Bentonite particles intercalated with polyacrylic acid between the layers) are self-repaired while being swelled to fill the modified asphalt with a functional oil / inorganic material capsule so as to maintain the performance of the waterproofing material. And a material property of a waterproof modified asphalt including a carbon material. The present invention relates to a high performance hybrid waterproof material filled with the functional hybrid waterproof material and a method for manufacturing the same.
각종 건축 구조물 및 토목 구조물의 내구성 확보에 있어서 방수성능이 차지하는 비중은 점차로 증가하는 추세에 있다. 기존 일반적인 방수공사에 있어서 보강재가 포함된 방수시트의 주된 사용으로 방수도막 자체의 강도가 문제가 되지 않았으나 최근에 방수시트를 사용하지 않고 방수도막을 사용하는 방수공사 수요가 증가하는 추세이다. 이에 따라 새로운 방수자재 및 방수공법들이 많이 개발되고 있으나, 이러한 방수자재의 개발에 사용되는 재료적 한계로 말미암아 대부분 비슷한 재료를 활용하여 일부 기능만을 향상시킨 자재의 개발만이 이루어지고 있는 현실이다. 이러한 현(現) 방수기술의 재료적인 한계를 극복하여 방수기능의 향상 및 각종 구조물의 내구성 향상까지 기여하는 우수한 물성을 지닌 고기능성 방수재의 개발이 필요하다.The proportion of waterproof performance in the durability of various architectural structures and civil engineering structures is gradually increasing. In the conventional waterproofing work, the main use of the waterproof sheet including the reinforcing material is not the strength of the waterproof coating itself, but the demand for the waterproofing work using the waterproof coating is increasing recently. As a result, new waterproofing and waterproofing methods have been developed. However, due to the material limitations used in the development of such waterproofing materials, only materials having improved some functions have been developed using almost similar materials. It is necessary to develop a high-performance waterproofing material with excellent physical properties which contributes to improvement of waterproof function and improvement of durability of various structures by overcoming material limit of current waterproofing technology.
현재까지 개질아스팔트 요소(아스팔트, 고분자 개질제, 가소재, 점착제 등)로 구성된 방수분야의 개질아스팔트에 관한 특허 등의 명세서 및 청구항 등의 기술적 권리사항에는 방수 개질아스팔트가 파손되어 누수가 되는 경우에 파손된 틈에서 팽창하여 자가보수(self-repair)를 수행하는 방수 개질아스팔트에 첨가되는 수팽윤성 유/무기재료와 소수성인 개질아스팔트 간의 상용성에 대한 언급이 없었다. 현재까지의 방수 개질아스팔트에 첨가되는 수팽윤성 유/무기재료는 혐수성인 개질아스팔트 간에 상용성이 전혀 없으므로, 방수개질아스팔트 제조 시에 도 1과 같이 첨가되는 수팽윤성 유/무기재료 입자의 분산이 되지 않고 응집이 발생하고, 개질아스팔트 파손 및 누수 시에 누수되는 부분에 수팽윤성 유/무기재료 입자가 존재하지 않거나 유실이 되어 하자발생과 성능을 유지 못하는 치명적 결함이 있다. 도 1의 기존발명[벤토나이트가 첨가된 방수 개질아스팔트 관련 특허 제0549564호(특허문헌 1 참조)에는 폐타이어 용융액이 아스팔트 및 벤토나이트를 모두 결합한다고 기재되었으나 폐타이어 용융액과 벤토나이트는 상용성이 없으므로 폐타이어 용융액과 벤토나이트는 결합할 수 없다. 따라서 방수 개질아스팔트의 설치 후에 크L이 발생하여 누수가 되었을 때에 첨가된 벤토나이트를 아스팔트, 고분자 개질재 및 폐타이어 용융액이 물리적으로 둘러싸지(물리적 제한) 않으면 첨가된 벤토나이트는 유실되기 쉽다. 상기 기존발명은 벤토나이트가 유실되지 않도록 가황을 하여 폐타이어 용융액 및 고분자 개질재의 이중결합이 있는 탄소를 가교시키는 것을 제시하지만, 가교되는 것은 폐타이어 용융액과 고분자 개질재이므로 크L이 발생하여 누수발생 시에 벤토나이트가 외부로 노출이 되면 위와 같은 물리적 제한이 없어져서 유실되기 쉽다.To date, the technical rights of patents, claims, and claims regarding modified asphalt of waterproofing consisting of modified asphalt elements (asphalt, polymer modifier, plasticizer, adhesive, etc.) have been damaged due to breakage of waterproof modified asphalt, There has been no mention of the compatibility between the water-swellable oil / inorganic material added to the waterproof modified asphalt which expands in the gap and self-repair and the hydrophobic modified asphalt. Since the water swellable oil / inorganic material added to the waterproof modified asphalt so far does not have compatibility with the hydrophilic modified asphalt, there is no dispersion of the water swellable oil / inorganic material particles added as shown in FIG. 1 during the manufacture of the waterproof modified asphalt And there is a fatal defect which can not maintain the performance and defects due to the absence of water swelling oil / inorganic material particles in the leaking portion of the modified asphalt breakage and leakage, or the leakage. In the existing invention of FIG. 1 (patent document No. 0549564 pertaining to waterproof modified asphalt with bentonite added), it is described that the waste tire melt binds both asphalt and bentonite. However, since the waste tire melt and bentonite are incompatible with each other, The melt and bentonite can not combine. Therefore, the added bentonite is liable to be lost if the bentonite added when the leak occurs due to the occurrence of the crack after the installation of the waterproof modified asphalt is physically surrounded (physical limitation) by the asphalt, the polymer reforming material and the waste tire melt. The existing invention suggests vulcanization so as to prevent the bentonite from being lost to cross-link the double bond carbon of the waste tire melt and the polymer modifier. However, since crosslinking is a waste tire melt and a polymer modifier, When bentonite is exposed to the outside, physical limitations as described above are lost and are likely to be lost.
따라서 본 발명에서 수행하는 개질아스팔트 방수재에 첨가되는 수팽윤성 유/무기재료와 소수성인 개질아스팔트 간에 상용성을 가지게 하거나 결합하고, 동시에 상기 유/무기 재료의 수팽윤성을 유지하게 하는, 개질아스팔트 간의 상용성이 있는 기능성 유/무기 재료 캡슐을 이용한 본 발명은 방수 개질아스팔트가 하자 없이 성공적인 성능을 유지하는데 필요한, 현재까지의 기술과 차별성이 있는 공백기술이고 중요한 발명이다.Therefore, in the present invention, it is preferable that the modified asphalt waterproofing material is made to have compatibility with water-swellable organic / inorganic material and hydrophobic modified asphalt, and at the same time to maintain water swelling property of the organic / The present invention using functional organic / inorganic material capsules is a blank technology and important invention that is different from the existing technology required for waterproof modified asphalt to maintain a successful performance without defects.
또한 개질아스팔트 방수재의 인장강도 등의 물성제고 및 방수재의 경량화를 통한 건축물 경량화에 기여할 수 있는 충진재 기술개발이 필요하다. 현재 방수재에 사용되고 있는 탄산칼슘은 탈황제로 재사용되거나 건축자재, 플라스틱, 제지, 고무 등 다양한 용도의 산업재료의 충진제로 활용될 수 있으나 비중이 2.71 ∼ 2.83에 이르므로 탄소재료(탄소섬유 비중: 1.8로서 glass fiber 비중의 약 70%임)에 비해 지나치게 크다. 탄산칼슘은 주로 미립질 방해석 형태로 얻어지는데 고도 이용화를 위해서는 고기능성 물질로의 기질의 개선이 요구된다. 미립화한 탄산칼슘 분체는 매우 중요한 기능성 무기질 충진제로서 주로 플라스틱, 고무, 마그네틱, 페인트 및 제지 공업 등에 이용되고, 이러한 공업적 사용은 주로 탄산칼슘의 분산성, 점결성, 압밀성을 이용하는 것으로 탄산칼슘의 입자 형상이나 입자크기, 입자의 표면 상태에 따라 활용도가 결정된다. 그러나 이러한 미립화한 탄산칼슘 분체는 열역학적으로 높은 표면에너지와 작은 입자 크기로 인해 덩어리로 엉기는 응집현상이 일어나며 실제적인 활용에 있어서는 큰 부정적 요인이 되며, 또한 대부분의 미립 분체들의 표면은 친수성이며 큰 극성을 가지므로 대부분 비극성을 띄는 유기 매개체와의 친화력이 약하므로 고무나 페인트 등의 유기물질 제품 생산에 적용시키기에는 한계가 있다. 또한 탄산칼슘 분말을 폴리에틸렌계 및 폴리프로필렌계 탄성체에 첨가하면 용융유동성, 인장강도 및 연신율이 감소하여 오히려 시트 성형성이 저하되었다고 보고되고 있다.In addition, it is necessary to develop filler material technology that can contribute to weight reduction of buildings by improving physical properties such as tensile strength of modified asphalt waterproofing materials and lightening waterproofing materials. Currently, calcium carbonate used in waterproofing materials can be reused as a desulfurizing agent or used as a filler for various industrial materials such as building materials, plastic, paper, and rubber, but its specific gravity is 2.71 ~ 2.83. which is about 70% of the glass fiber specific gravity). Calcium carbonate is mainly obtained in the form of fine-grained calcite. In order to achieve high utilization, improvement of the substrate to a high-function material is required. The atomized calcium carbonate powder is a very important functional inorganic filler mainly used in plastics, rubber, magnetic, paint, paper industry and the like. Such industrial use mainly utilizes the dispersibility, cohesion and consolidation property of calcium carbonate, Usage is determined by shape, particle size, and particle surface state. However, since such an atomized calcium carbonate powder has a thermodynamically high surface energy and a small particle size, aggregation phenomenon occurs, which is entangled with agglomerates, which is a great negative factor in practical use. In addition, most of the fine powder particles are hydrophilic, , It has a limited affinity with an organic medium, which is mostly non-polar, and thus it is limited to be applied to the production of organic materials such as rubber and paint. Further, it has been reported that when calcium carbonate powder is added to a polyethylene-based or polypropylene-based elastomer, the melt flowability, tensile strength and elongation are decreased and the sheet formability is lowered.
본 발명은 기본적으로 단순히 성능이 좋으면서도 값이 저렴한 제품이 아니라, 소비자와 사회의 요구에 부합되는 충진재로서 물성을 제고하는 고기능성 하이브리드 소재를 제공한다.The present invention basically provides a high-performance hybrid material which improves physical properties as a filler suitable for the needs of consumers and society, not merely a low-cost product with good performance.
가장 바람직한 소재로는 탄소성형 첨단부품에 주로 투입되는 탄소섬유를 들 수 있고 상기 충진제에 용도에 따라서 적당한 비율이 적용된다.The most preferred material is carbon fiber which is mainly put into a carbon-forming advanced part, and a suitable ratio is applied to the filler depending on the use.
따라서 본 발명은 개질아스팔트와 상용성이 있도록 표면개질되거나 결합되고 동시에 캡슐 안 유/무기 재료의 수팽윤성을 유지하게 하는 수팽윤성 유/무기 캡슐이 방수재에 손상(잔갈림 및 찢김 등)이 발생 시 누수에 쓸려나가지 않고 크랙으로 갈라진 수팽윤성 유/무기 캡슐 사이 또는 수팽윤성 유/무기 캡슐 표면에 노출된 층간(inter-layer)으로 물이 침투하고 캡슐 내부의 수팽윤성 유/무기 입자가 수팽창하여 손상된 방수재가 자가보수(self-repair)가 가능한 가장 바람직한 방수소재를 제공하는 데 있다.Accordingly, the present invention relates to a water-swellable oil / inorganic capsule which is surface-modified or bonded so as to be compatible with modified asphalt and at the same time maintains the water swelling property of the encapsulated oil / inorganic material, when the waterproofing material is damaged (grinding or tearing) Water penetrates into water-swellable oil / inorganic capsules cracked into cracks without leaking into leaks or inter-layer exposed on the surface of water-swellable oil / inorganic capsules, and water swellable oil / The damaged waterproofing material is to provide the most desirable waterproofing material capable of self-repairing.
본 발명의 다른 목적은 탄소소재를 포함한 방수 개질아스팔트의 물성 제고 및 방수재의 경량화를 통한 건축물 경량화에 기여할 수 있는 하이브리드 충진재를 상기 기능성 방수소재에 충진한 우수한 고기능성 하이브리드 방수재와 그 제조방법을 제공한다.Another object of the present invention is to provide an excellent high performance hybrid waterproofing material filling a functional waterproofing material with a hybrid filler capable of contributing to weight reduction of a building by improving the physical properties of the waterproof modified asphalt containing carbon material and lightening the waterproofing material, .
본 발명의 상기 목적은 (a) 방수재의 경량화를 통한 건축물 경량화 및 인장강도 등 방수재의 물성 제고를 위하여 탄소섬유를 포함하는 하이브리드 충진재를 상기 기능성 방수소재에 충진하는 단계와;(b)상기 방수재에 크L이 발생하여 누수가 되었을 때 벤토나이트 캡슐(실란화)이 유실되지 않고 쪼개진 벤토나이트 캡슐(실란화)안의 벤토나이트 입자들 또는 벤토나이트 캡슐 표면에 노출된 벤토나이트 입자 층간(inter-layer)으로 물이 침투하고 캡슐 내부의 벤토나이트 입자가 팽윤하면서 자가보수(self-repair)가 수행되어 방수재의 성능유지가 되도록 벤토나이트 캡슐(실란화)을 개질아스팔트에 충진하여 고기능성 하이브리드 방수재를 제공함으로써 달성한다.(A) filling the functional waterproof material with a hybrid filler including carbon fibers for the purpose of improving the physical properties of the waterproof material such as weight reduction and tensile strength of the waterproof material by reducing the weight of the waterproof material; (b) Bentonite particles in cleaved bentonite capsules (silanized) or bentonite particles exposed on the surface of bentonite capsules without leakage of bentonite capsules (silanized) when leakage occurs due to large size Liquid penetration into the inter-layer And filling the modified asphalt with a bentonite capsule (silanized) so that the self-repair is performed while swelling the bentonite particles inside the capsule to maintain the performance of the waterproofing material, thereby providing a highly functional hybrid waterproofing material.
본 발명은 상기 벤토나이트 캡슐(실란화)은 본 발명의 고기능성 하이브리드 방수도막이 현장에서 도포 및 설치된 후에 크랙 발생 시 누수에 쓸려나가지 않고 크랙으로 갈라진 벤토나이트 캡슐 사이 또는 벤토나이트 캡슐 표면에 노출된 벤토나이트 입자 층간(inter-layer)으로 물이 침투하고 캡슐 내부의 벤토나이트 입자가 수팽창하여 용이하게 자가수리(self-sealing)되는 효과가 있을 뿐만 아니라 환경친화적인 하이브리드 충진재를 상기 기능성 방수소재에 충진한 고기능성 하이브리드 방수재방수재의 경량화를 통한 건축물 경량화 및 인장 및 인열강도, 신장률 등의 방수재 물성 제고에 기여하고 환경친화적인 하이브리드 충진재를 상기 기능성 방수소재에 충진한 고기능성 하이브리드 방수재를 제공하는 뛰어난 효과가 있다.In the present invention, the bentonite capsules (silanized) can be used to prevent the leakage of water when the high-performance hybrid waterproof coating film of the present invention is applied and installed in the field, and the bentonite particles interposed between cracked cracked bentonite capsules or bentonite capsules inter-layer, and the self-sealing of the bentonite particles inside the capsule can be facilitated. In addition, the functional hybrid waterproofing material filling the functional waterproofing material with the environmentally friendly hybrid filler There is an excellent effect of providing a highly functional hybrid waterproofing material which contributes to enhancement of properties of waterproofing materials such as weight reduction of buildings through lightweighting of waterproofing materials, tensile, tearing strength and elongation, and filling environmentally friendly hybrid fillers into the functional waterproofing materials.
도 1은 수팽윤성 유/무기재료가 첨가되는 방수 개질아스팔트에 관한 기존 발명의 결함을 나타낸 모식도이다.
도 2는 현장 설치된 방수재 도막의 크L과 누수 발생 시에 벤토나이트 캡슐이 유실되지 않고 수팽창하여 자가보수(self-repair)되는 과정을 나타낸 모식도이다.
도 3은 본 발명의 벤토나이트 캡슐의 제조과정을 나타낸 공정 다이어그램이다.
도 4는 본 발명에 따른 하이브리드 충전재를 첨가하여 제조한 방수소재에서 하이브리드 충전재 조성에 따른 방수소재의 인장강도 추이를 나타낸 그래프이다.
도 5는 하이브리드 충전재를 첨가하여 제조한 방수소재에서 하이브리드 충전재 조성에 따른 방수소재의 신장율 추이를 나타낸 그래프이다.
도 6은 하이브리드 충전재를 첨가하여 제조한 방수소재에서 하이브리드 충전재 조성에 따른 방수소재의 인열성능 추이를 나타낸 그래프이다.
도 7은 아미노프로필트리에톡시실란(aminopropyltriethoxysilane)을 5.0 w/ v% 농도로 60분 동안 교반 후에 섭씨 50도에서 각각 1, 2 및 5 시간 동안 실란화 반응시켜서 개질된 몬모릴로나이트(MMT)의 FT-IR 스펙트럼 분석결과를 나타낸 그래프이다.
도 8은 본 발명에 따른 아미노프로필트리에톡시실란(aminopropyltriethoxys ilane)을 5.0 w/v% 농도로 각각 20, 60 또는 100분 동안 교반 후에 섭씨 50도에서 1 시간 동안 실란화 반응시켜서 개질된 몬모릴로나이트(MMT)의 FT-IR 스펙트럼 분석결과를 나타낸 그래프이다.
도 9는 아미노프로필트리에톡시실란(aminopropyltriethoxysilane)을 각각 2.5, 5.0 및 7.5 w/v% 농도로 60분 동안 교반 후에 섭씨 50도에서 5시간 동안 실란화 반응시켜서 개질된 몬모릴로나이트(MMT)의 FT-IR 스펙트럼 분석결과를 나타낸 그래프이다.
도 10은 아미노프로필트리에톡시실란(aminopropyltriethoxysilane)을 7.5 w/ v% 농도로 60분 동안 교반 후에 각각 섭씨 50도 또는 80도에서 5시간 동안 실란화 반응시켜서 개질된 몬모릴로나이트(MMT)의 FT-IR 스펙트럼 분석결과를 나타낸 그래프이다.
도 11은 아미노프로필트리에톡시실란(aminopropyltriethoxysilane)을 5.0 w/v% 농도로 60분 동안 교반 후에 각각 섭씨 50도 또는 80도에서 5시간 동안 실란화 반응시켜서 개질된 몬모릴로나이트(MMT)의 FT-IR 스펙트럼 분석결과를 나타낸 그래프이다.
도 12는 아미노프로필트리에톡시실란(aminopropyltriethoxysilane)을 5.0 w/ v% 농도로 100분 동안 교반 후에 각각 섭씨 50도 또는 80도에서 1시간 동안 실란화 반응시켜서 개질된 몬모릴로나이트(MMT)의 FT-IR 스펙트럼 분석결과를 나타낸 그래프이다.BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a schematic diagram showing the deficiencies of the present invention relating to a waterproof modified asphalt to which a water-swellable oil / inorganic material is added.
FIG. 2 is a schematic view showing a process of self-repairing of a waterproof coating film installed on the spot and water expansion of a bentonite capsule without leakage when leakage occurs. FIG.
FIG. 3 is a process diagram showing a manufacturing process of the bentonite capsule of the present invention.
4 is a graph showing tensile strength of a waterproof material according to the composition of a hybrid filler in a waterproof material prepared by adding a hybrid filler according to the present invention.
5 is a graph showing a change in elongation percentage of a waterproof material according to a hybrid filler composition in a waterproof material prepared by adding a hybrid filler.
6 is a graph showing the tear performance of a waterproof material according to the composition of a hybrid filler in a waterproof material prepared by adding a hybrid filler.
Figure 7 shows the results of an experiment in which aminopropyltriethoxysilane was reacted at a concentration of 5.0 w / v% for 60 minutes, followed by silanization at 50 degrees Celsius for 1, 2 and 5 hours, respectively, to obtain a modified montmorillonite (MMT) IR spectral analysis results.
8 is a graph showing the results obtained by stirring the aminopropyltriethoxysilane according to the present invention at a concentration of 5.0 w / v% for 20, 60, or 100 minutes, respectively, and then silanizing the mixture at 50 degrees Celsius for 1 hour to obtain modified montmorillonite MMT) of the present invention.
9 is a graph showing the change in the activity of amorphous montmorillonite (MMT) FT-1 after aminopropyltriethoxysilane was stirred for 60 minutes at a concentration of 2.5, 5.0, and 7.5 w / v%, respectively, IR spectral analysis results.
Figure 10 shows the results of FT-IR of amorphous montmorillonite (MMT) after aminopropyltriethoxysilane was stirred at 7.5 w / v% concentration for 60 minutes and then silanized at 50 or 80 degrees Celsius for 5 hours, respectively. And Fig.
FIG. 11 shows the results of FT-IR analysis of amorphous montmorillonite (MMT) after aminopropyltriethoxysilane was stirred at a concentration of 5.0 w / v% for 60 minutes and then subjected to silanization reaction at 50 ° C. or 80 ° C. for 5 hours, And Fig.
FIG. 12 shows the results of FT-IR analysis of amorphous montmorillonite (MMT) by aminopropyltriethoxysilane at a concentration of 5.0 w / v% for 100 minutes, followed by silanation reaction at 50 ° C. or 80 ° C. for 1 hour, And Fig.
본 발명에서는 개질아스팔트와 상용성이 있도록 표면개질되거나 결합되고 동시에 캡슐 안 유/무기재료의 수팽윤성을 유지하게 하는 수팽윤성 유/무기 캡슐을 제조함으로써, 표면개질된 수팽윤성 유/무기 캡슐이 개질아스팔트와 상용성을 보유하도록 하고 동시에 수팽윤성 유/무기 캡슐 안의 수팽윤성 유/무기재료의 수팽윤성이 유지되도록 하였다. 본 발명에서 수팽윤성 유/무기재료는 수팽윤성 유기재료와 수팽윤성 무기재료 중의 어느 하나 또는 양자를 모두 포함하는 수팽윤성 재료를 의미하며, 수팽윤성 무기재료에 수팽윤성 유기재료를 결합한 복합체(composite)를 포함한다. 수팽윤성 유기재료는 카르복시메틸셀루로즈(CMC)계, 전분 및 셀루로즈와 같은 천연고분자에 석유화합물인 친수성합성고분자를 결합시킨 반합성가교고분자 및 수용성합성고분자(폴리아크릴산, 폴리비닐알콜)의 가교물을 포함한다. 수팽윤성 무기재료는 벤토나이트, 헥토라이트, 사포나이트, 몬모릴로나이트 등의 수팽윤성 점토를 포함한다. 또한 수팽윤성 유/무기재료는 벤토나이트에 아크릴아마이드(acrylamide)를 수용액에서 층간삽입(intercalate)시키고 아크릴산(acrylic acid)을 중합시켜서 제조된 폴리아클릴레이트(polyacryl ate)/벤토나이트 결합체와 같은 벤토나이트 복합체(composite)를 포함한다. 본 발명에서는 벤토나이트 또는 상기 벤토나이트 조성 중에서 몬모릴로나이트(MMT)를 취하여 수팽윤성 무기재료로서 적용하였다.In the present invention, a surface-modified water-swellable oil / inorganic capsule is modified by preparing a water-swellable oil / inorganic capsule that is surface-modified or bonded so as to be compatible with modified asphalt and at the same time maintains water- Swelling properties of the water swellable oil / inorganic material in the water swellable oil / inorganic capsules were maintained so as to have compatibility with asphalt and water swellability. In the present invention, the water-swellable organic / inorganic material means a water-swellable material including both or both of a water-swellable organic material and a water-swellable inorganic material, and a composite material obtained by bonding a water-swellable inorganic material to a water- . The water-swellable organic material is a crosslinked polymer of a semisynthetic crosslinked polymer obtained by bonding a hydrophilic synthetic polymer as a petroleum compound to a natural polymer such as carboxymethylcellulose (CMC), starch and cellulose, and a crosslinked product of a water-soluble synthetic polymer (polyacrylic acid and polyvinyl alcohol) . The water-swellable inorganic material includes water-swellable clays such as bentonite, hectorite, saponite, and montmorillonite. In addition, the water-swellable oil / inorganic material may be a bentonite composite such as a polyacryl ate / bentonite binder prepared by intercalating acrylamide into bentonite in an aqueous solution and polymerizing acrylic acid composite. In the present invention, montmorillonite (MMT) is taken out of the bentonite or the bentonite composition and applied as a water-swellable inorganic material.
본 발명에서는 (a) 방수재의 경량화를 통한 건축물 경량화 및 인장강도 등 방수재의 물성 제고를 위하여 탄소섬유를 포함하는 하이브리드 충진재를 상기 기능성 방수소재에 충진하며, 또한 (b) 방수재에 크랙이 발생하여 누수가 되었을 때 벤토나이트 캡슐(실란화)이 유실되지 않고 쪼개진 벤토나이트 캡슐(실란화)안의 벤토나이트 입자들 또는 벤토나이트 캡슐 표면에 노출된 벤토나이트 입자 층간(inter-layer )으로 물이 침투하고 캡슐 내부의 벤토나이트 입자가 팽윤하면서 자가보수(self- repair)가 수행되어 방수재의 성능유지가 되도록 벤토나이트 캡슐(실란화)을 개질아스팔트에 충진하였다.In the present invention, a hybrid filler containing carbon fibers is filled in the functional waterproofing material in order to improve the physical properties of the waterproofing material such as weight reduction and tensile strength of the building by lightening the waterproofing material, and (b) The water penetrates into the inter-layer of the bentonite particles in the split bentonite capsules (silanized) or the bentonite particles exposed on the surface of the bentonite capsules without the loss of the bentonite capsules (silanized), and the bentonite particles inside the capsules Self-repair was carried out while swelling to fill the modified asphalt with bentonite capsules (silanized) to maintain the performance of the waterproofing material.
본 발명의 벤토나이트 캡슐 제조공정은 도 3과 같으며, 첫 단계로서는 벤토나이트 입자를 원하는 크기로 응집시키는 것이다. 본 발명의 첫 단계에서는 벤토나이트를 분산시킨 극성용액(에탄올 수용액 등)에서 이온강도(예: NaClO4, 0.1 M)를 증가시키고 또한 pH를 조절하고 필요시에 교반과 응집제를 사용하여 벤토나이트를 응집시키고 건조 후에 평균입도를 측정하여 pH 및 이온강도에 따른 응집도를 측정하였다. 한편 본 발명에서는 첫 번째 벤토나이트 응집단계를 거치지 않고 다음의 두 번째 단계를 실행할 수 있다.The process for producing bentonite capsules of the present invention is shown in Fig. 3, and the first step is to coagulate the bentonite particles to a desired size. In the first step of the present invention, the ionic strength (eg, NaClO 4 , 0.1 M) is increased in a polar solution (such as an aqueous ethanol solution) in which bentonite is dispersed and the pH is adjusted, and the bentonite is agglomerated After drying, the average particle size was measured and the degree of cohesion according to pH and ionic strength was measured. In the present invention, it is possible to carry out the following second step without going through the first bentonite coagulation step.
본 발명의 두 번째 단계는 벤토나이트 표면 또는 벤토나이트 응집체 표면을 실란커플링제로써 소수성 개질하거나 결합하여 표면개질된 벤토나이트 캡슐(실란화)을 제조하는 것이다. 더 상세히 설명하면 1) 캡슐(실란화)이 되는 것이 벤토나이트 응집체이고 응집체의 평균입도가 8 ∼ 200㎛ 정도의 응집도를 보이는 pH 및 이온강도의 극성용액(에탄올 수용액 등)에서 응집된 벤토나이트의 실란화를 수행하거나; 또는 2) 첫 번째 벤토나이트 응집단계를 거치지 않고 벤토나이트 입자의 실란화를 수행하여 벤토나이트 캡슐(실란화)을 제조하는 것이다.The second step of the present invention is to hydrophobically modify or bond the bentonite surface or bentonite agglomerate surface with a silane coupling agent to produce a surface modified bentonite capsule (silanized). More specifically, 1) silanization of the bentonite agglomerated in a polar solution (such as an aqueous ethanol solution) of pH and ionic strength which exhibits cohesion of the agglomerates of bentonite and agglomerates having an average particle size of about 8 to 200 μm, ; Or 2) silanization of the bentonite particles without the first step of the bentonite agglomeration to produce bentonite capsules (silanized).
실란커플링제로서 n-옥틸트리에톡시실란(n-octyl-triethoxy-silane), 아미노프로필트리에톡시실란(aminopropyltriethoxysilane), 데실트리메톡시실란(decyltri methoxysilane), N,N-비스(2-하이드록시에틸)-3-아미노프로필트리에톡시실란(N,N-b is(2-hydroxyethyl)-3-aminopropyltriethoxy silane), 3-글라이시독시프로필트리메톡시실란(3-glycidoxypropyltrimethoxysilane) 또는 3-메타크릴록시프로필트리메톡시실란(3-metacryloxypropyl-trimethoxy-silane) 등을 사용하여 실란커플링제의 가수분해 후에 벤토나이트 표면의 OH기와 수소결합, 또는 실란커플링제의 가수분해 및 응축 후에 벤토나이트 표면과 에테르결합을 하고 그 결합체에 소수성을 부여하여 개질아스팔트와 상용성을 부여하도록 하였다. 또한 본 발명에서 실란커플링제를 이용한 벤토나이트 표면개질은 벤토나이트와 개질아스팔트간의 상용성뿐만 아니라, 상기 실란커플링제의 관능기를 아민기 또는 에폭시기를 포함한 글리시딜(glycidyl)기 등으로 설정하여, 가교된 폴리아크릴산의 -COOH기와 반응시키거나 개질아스팔트의 조성 중 극성 아로마틱 화합물에 포함된 아세트산의 -COOH기와 반응시키는 화학결합도 포함한다. 따라서 아미노프로필트리에톡시실란(aminopropyltriethoxysilan e)의 관능기인 아민기와 개질아스팔트 성분 중의 극성 아로마틱 화합물에 포함된 아세트산의 100 이상에서 아마이드 반응을 통하여, 개질아스팔트와 아미노프로필트리에톡시실란(aminopropyltriethoxysilane)으로 표면개질된 몬모릴로나이트(MMT)의 화학결합을 유도하였다. 본 발명에서 상기 벤토나이트 입자는, 벤토나이트에 아크릴아마이드(acrylamide)를 수용액에서 층간삽입(intercalate)시키고 아크릴산(acry lic acid)을 중합시켜서 제조된 폴리아크릴레이트(polyacrylate)/벤토나이트 결합체와 같은 벤토나이트 복합체(composite)를 포함한다.Examples of the silane coupling agent include n-octyl-triethoxy-silane, aminopropyltriethoxysilane, decyltri methoxysilane, N, N-bis (2- 3-aminopropyltriethoxy silane), 3-glycidoxypropyltrimethoxysilane (3-glycidoxypropyltrimethoxysilane), 3-methacryloxypropyltrimethoxysilane After the hydrolysis of the silane coupling agent using hydrolysis and condensation of the OH group on the surface of the bentonite or the silane coupling agent by using 3-methacryloxypropyl-trimethoxy-silane or the like, ether bond with the bentonite surface is performed Hydrophobicity was imparted to the combination to give compatibility with the modified asphalt. Further, in the present invention, the surface modification of the bentonite using the silane coupling agent is not limited to the compatibility between the bentonite and the modified asphalt, and the functional group of the silane coupling agent may be set to a glycidyl group containing an amine group or an epoxy group, And a chemical bond which reacts with -COOH group of polyacrylic acid or reacts with the -COOH group of acetic acid contained in the polar aromatic compound in the composition of the modified asphalt. Therefore, amines such as aminopropyltriethoxysilane (aminopropyltriethoxysilane) and amide groups in the amorphous asphalt component of amorphous aromatic compounds are reacted with amines such as aminopropyltriethoxysilane and aminopropyltriethoxysilane Chemical bond of modified montmorillonite (MMT) was induced. In the present invention, the bentonite particles may be a bentonite composite such as a polyacrylate / bentonite complex prepared by intercalating acrylamide into an aqueous solution of bentonite and polymerizing acrylic acid. ).
마지막으로 본 발명의 세 번째 단계로서는 방수재의 경량화를 통한 건축물 경량화 및 방수재의 물성 제고에 기여하고 환경친화적인 상기 벤토나이트 캡슐(실란화)을, 개질아스팔트 요소(아스팔트, 개질제, 가소재, 점착제 등)를 160 ∼ 180에서 혼합/용융한 상태에서 첨가하여 기능성 방수소재를 제조하는 것이다. 상기 개질아스팔트 요소들은 개질아스팔트 요소 합에 대하여 아스팔트 49 ∼ 90 중량%, 개질제 10 ∼ 39 중량%, 가소제 0 ∼ 12 중량%의 배합비로 고기능성 방수소재를 제조하는 것이다. 상기 개질제는 SBS(styrene-butadiene-styrene)와 SIS(styrene-isoprene-styrene) 외에 폴리부텐, 석유수지, 천연수지, 에틸렌 비닐아세테이트(ethylene vinyl acetate, EVA) 및 열가소성 폴리우레탄(Thermoplastic polyurethane) 중에서 선택되는 어느 하나 이상을 포함한다.Finally, as a third step of the present invention, the bentonite capsules (silanization), which are environmentally friendly, contribute to the improvement of the physical properties of the waterproofing material and the weight reduction of the building by reducing the weight of the waterproofing material, and the modified asphalt elements (asphalt, modifier, plasticizer, Is added at 160 to 180 in a mixed / molten state to produce a functional waterproof material. The modified asphalt elements are prepared by mixing a modified waterproof material with 49 to 90% by weight of asphalt, 10 to 39% by weight of a modifier, and 0 to 12% by weight of a plasticizer, based on the modified asphalt component sum. The modifier may be selected from polybutene, petroleum resin, natural resin, ethylene vinyl acetate (EVA) and thermoplastic polyurethane in addition to styrene-butadiene-styrene (SBS) and styrene-isoprene- Or more.
본 발명의 또 다른 세 번째 단계로서는 방수재의 경량화를 통한 건축물 경량화 및 방수재의 물성 제고에 기여하고 환경친화적인, 상기 벤토나이트 캡슐(실란화) 외에, 하이브리드 충진재를 개질아스팔트 요소(아스팔트, 고분자 개질제, 가소재, 점착제 등)를 160 ∼ 180에서 용융한 상태에서 첨가하여 고기능성 하이브리드 방수재를 제조하는 것이다. 또한 본 발명은 개질아스팔트 요소를 160-180에서 용융한 상태에서 상기 수팽윤성 유/무기 캡슐(실란화)을 제외하고 하이브리드 충전재만을 첨가하여 고기능성 하이브리드 방수재를 제조하는 것을 포함한다. 상기 하이브리드 충전재는 기존의 탄산칼슘, 탄소섬유, 탄화 바이오매스입자, 스테아린산 코팅 탄산칼슘 등을 상기 개질아스팔트 요소 총중량의 각각 0 ∼ 30, 0 ∼ 10, 0 ∼ 5, 0 ∼ 30 중량부의 비율로 혼합한 하이브리드 충진재이다. 상기 탄소섬유는 PAN( Polyacrylonitrile) 또는 피치(pitch)와 같은 전구체섬유 유래 탄소섬유를 포함한다.
Another third step of the present invention is to reduce the weight of the building through weight reduction of the waterproofing material and to contribute to the improvement of the physical properties of the waterproofing material and to improve the environmental compatibility of the bentonite capsules (silanization), as well as the hybrid filler to the modified asphalt elements (asphalt, Adhesive, etc.) at a temperature of 160 to 180 in a molten state to produce a high-performance hybrid waterproofing material. Further, the present invention includes preparing a high-performance hybrid waterproofing material by adding only a hybrid filler except for the water-swellable oil / inorganic capsules (silanized) in a state where the modified asphalt element is melted at 160-180. The hybrid filler may be prepared by mixing conventional calcium carbonate, carbon fiber, carbonized biomass particles, and stearic acid-coated calcium carbonate in a proportion of 0 to 30, 0 to 10, 0 to 5, and 0 to 30 parts by weight of the total weight of the modified asphalt component, It is a hybrid filler. The carbon fibers include precursor fiber-derived carbon fibers such as PAN (polyacrylonitrile) or pitch.
실시예Example 1. One.
하이브리드hybrid 충전재가 첨가된 방수소재 제조에서 In the manufacture of waterproof materials with added filler 하이브리드hybrid 충전재의 적정조성 Proper composition of filler
150에서 녹인 아스팔트(AP-3), 가소제(P-31), SBS(LG 501)를 개질아스팔트의 필수구성요소로 하고, 기타 개질제로서 C-5계 석유수지(A-1100)를 추가하여 본 발명의 방수소재의 기본구성요소로 하였다. 본 발명의 방수소재의 상기 기본구성요소의 조성을 각각 75.0, 6.8, 13.6, 4.6% 중량부(합 100%)로 하였다. 본 발명의 방수소재의 상기 기본구성요소(control: 테스트 1)에 하이브리드 충전재를 기본구성요소의 합(100%)에 대하여 2.5, 5.0, 7.5 및 10% 중량부를 충전하였다. 하이브리드 충전재 2.5% 중량부의 경우에는 2.5% 탄산칼슘(테스트 2), 2.5% 탄소섬유(테스트 3), 2.5% 스테아릭산코팅 탄산칼슘(테스트 4), 및 1.25% 탄소섬유와 1.25% 스테아릭산코팅 탄산칼슘(테스트 5)을 각각 투입하였다. 하이브리드 충전재 5.0% 중량부의 경우에는 5.0% 탄산칼슘(테스트 2), 5.0% 탄소섬유(테스트 3), 5.0% 스테아릭산코팅 탄산칼슘(테스트 4), 및 2.5% 탄소섬유와 2.5% 스테아릭산코팅 탄산칼슘(테스트 5)을 각각 투입하였다. 하이브리드 충전재 7.5% 중량부의 경우에는 7.5% 탄산칼슘(테스트 2), 7.5% 탄소섬유(테스트 3), 7.5% 스테아릭산코팅 탄산칼슘(테스트 4), 및 3.75% 탄소섬유와 3.75% 스테아릭산코팅 탄산칼슘(테스트 5)을 각각 투입하였다. 마지막으로 하이브리드 충전재 10% 중량부의 경우에는 10% 탄산칼슘(테스트 2), 10% 탄소섬유(테스트 3), 10% 스테아릭산코팅 탄산칼슘(테스트 4), 및 5.0% 탄소섬유와 5.0% 스테아릭산코팅 탄산칼슘(테스트 5)을 각각 투입하였다. 이러한 조성물을 180에서 2 시간 이상, 1200 rpm 이상으로 교반하여서 각각의 방수소재를 사용한 KS F 3211 규격에 따른 시편제조 및 물성실험을 수행하였다. 제조된 방수소재의 인장강도(N/mm2), 신장율(%) 및 인열성능(N/mm)에 대한 실험결과를 각각 도 4, 5 및 6에 각각 나타내었다.(A-1100) was added as an essential component of the modified asphalt and the asphalt (AP-3), plasticizer (P-31) and SBS And made the basic constituent of the waterproof material of the invention. The composition of the basic components of the waterproof material of the present invention was 75.0, 6.8, 13.6, and 4.6% by weight (total 100%). The above-mentioned basic component (control: test 1) of the waterproof material of the present invention was filled with 2.5, 5.0, 7.5 and 10% by weight of the hybrid filler relative to the sum of the basic components (100%). 2.5% carbon fiber (test 3), 2.5% stearic acid coated calcium carbonate (test 4), and 1.25% carbon fiber and 1.25% stearic acid-coated carbonic acid Calcium (Test 5) were each added. 5.0% Carbon Fiber (Test 3), 5.0% Stearic Acid Coated Carbonate (Test 4), and 2.5% Carbon Fiber and 2.5% Stearic Acid Coated Carbonate (Test 4) for 5.0% by weight of the hybrid filler, Calcium (Test 5) were each added. 7.5% carbon fiber (test 3), 7.5% stearic acid coated calcium carbonate (test 4), and 3.75% carbon fiber and 3.75% stearic acid coated carbonic acid (test 4) for 7.5% by weight of the hybrid filler, Calcium (Test 5) were each added. Finally, 10% by weight of the hybrid filler was mixed with 10% calcium carbonate (Test 2), 10% Carbon Fiber (Test 3), 10% Stearic Acid Coated Carbonate (Test 4), and 5.0% Carbon Fiber and 5.0% Stearic Acid And coated calcium carbonate (Test 5). These compositions were stirred at 180 rpm for more than 2 hours and at 1200 rpm or more, and specimens were manufactured and tested according to the KS F 3211 standard using waterproof materials. Experimental results on tensile strength (N / mm 2 ), elongation (%) and tearing performance (N / mm) of the manufactured waterproof materials are shown in FIGS. 4, 5 and 6, respectively.
도 4의 인장강도의 경우, 탄산칼슘(테스트 2) 경우는 기본구성요소(control: 테스트 1)와 별 차이가 없어서 충전재에 의한 인장강도 제고효과가 없었다. 그러나 그 외의 경우[탄소섬유(테스트 3), 스테아릭산코팅 탄산칼슘(테스트 4) 및 탄소섬유와 스테아릭산코팅 탄산칼슘의 동량 혼합물(테스트 5)]에는 스테아릭산코팅 탄산칼슘의 동량 혼합물(테스트 5)>탄소섬유((테스트3)>스테아릭산코팅 탄산칼슘(테스트4) 순으로 모두 인장강도가 제고되었는데 각각 하이브리드 충전재 조성 5.0%가 최적조성이었다. 최적조성에서 스테아릭산코팅 탄산칼슘(테스트 4) 경우보다, 탄소섬유(테스트 3) 경우가 인장강도가 약 10% 정도 더 컸고, 탄소섬유와 스테아릭산코팅 탄산칼슘의 동량 혼합물(테스트 5) 경우에는 20% 이상 제고되었다. 따라서 탄소섬유와 스테아릭산코팅 탄산칼슘의 동량 혼합물(테스트 5) 경우에서 충전재 혼합에 의한 시너지효과가 관찰되었다.In the case of the tensile strength of FIG. 4, the calcium carbonate (Test 2) was not significantly different from the basic constituent (control: Test 1) and thus had no effect of increasing the tensile strength by the filler. In other cases, however, the same amount of a mixture of stearic acid-coated calcium carbonate (Test 5) was mixed with a mixture of carbon fibers (Test 3), stearic acid-coated calcium carbonate (Test 4), and a mixture of carbon fiber and stearic acid- ) Stearic acid-coated calcium carbonate (Test 4) showed the highest tensile strength in the order of carbon fiber (Test 3) and stearic acid-coated calcium carbonate (Test 4) Tensile strength was about 10% greater for carbon fiber (Test 3), and more than 20% for the same amount of mixture of carbon fiber and stearic acid-coated calcium carbonate (Test 5) A synergistic effect by mixing the filler was observed in the case of the same amount of the mixed calcium carbonate (Test 5).
도 5와 같은 신장율의 경우에는, 하이브리드충전제가 첨가된 테스트 2, 3, 4 및 5들이 각각 기본구성요소(control: 테스트 1)와 별 차이가 없어서 충전재에 의한 신장율 제고효과가 거의 없었다. 그러나 탄산칼슘(테스트 2)과 탄소섬유(테스트 3)의 각각 10% 하이브리드 충전재의 경우에는 신장율이 각각 20% 정도 제고되었다.In the case of the elongation as shown in FIG. 5,
도 6의 인열성능의 경우에는, 인장강도와 마찬가지로 탄산칼슘(테스트 2) 경우는 기본구성요소(control: 테스트 1)와 별 차이가 없어서 충전재에 의한 인열성능 제고효과가 거의 없었다. 그러나 그 외의 경우[탄소섬유(테스트 3), 스테아릭산코팅 탄산칼슘(테스트 4) 및 탄소섬유와 스테아릭산코팅 탄산칼슘의 동량 혼합물(테스트 5)]에는 스테아릭산코팅 탄산칼슘의 동량 혼합물(테스트 5)>스테아릭산코팅 탄산칼슘(테스트4)>탄소섬유((테스트3) 순으로 모두 인열성능이 제고되었는데 각각 하이브리드 충전재 조성 5.0%가 최적조성이었다. 최적조성에서 스테아릭산코팅 탄산칼슘(테스트 4) 경우가 탄소섬유(테스트 3) 경우보다 인열성능이 약 10% 정도 더 컸고, 탄소섬유와 스테아릭산코팅 탄산칼슘의 동량 혼합물(테스트 5) 경우에는 탄소섬유(테스트 3) 경우보다 약 33% 제고되었다. 따라서 인열성능에서도 인장강도와 같이 탄소섬유와 스테아릭산코팅 탄산칼슘의 동량 혼합물(테스트 5) 경우에서 충전재 혼합에 의한 시너지효과가 관찰되었다.
In the case of the tearing performance shown in Fig. 6, the tear strength was not significantly different from that of the basic constituent (control: test 1) in the case of calcium carbonate (Test 2). In other cases, however, the same amount of a mixture of stearic acid-coated calcium carbonate (Test 5) was mixed with a mixture of carbon fibers (Test 3), stearic acid-coated calcium carbonate (Test 4), and a mixture of carbon fiber and stearic acid- ) Stearic acid-coated calcium carbonate (Test 4) and Carbon fiber (Test 3) were all in the order of tear strength, The tear performance was about 10% greater than that of the carbon fiber (Test 3), and the same amount of mixture of carbon fiber and stearic acid coated calcium carbonate (Test 5) was increased by about 33% compared to the carbon fiber (Test 3) Thus, synergistic effects of filler mixing were observed in the case of the same amount of mixture of carbon fiber and stearic acid-coated calcium carbonate (Test 5) as in tensile strength.
실시예Example 2. 2.
각 bracket 교반시간Stirring time , 각 , Angle 실란커플링제Silane coupling agent 농도 및 각 Concentration and angle 실란화Silanization 반응시간과 반응온도에 따른 아미노프로필트리에톡시실란( Aminopropyltriethoxysilane () was prepared by the reaction time and reaction temperature aminopropyltriethoxysilaneaminopropyltriethoxysilane )을 적용한 ) Applied 몬모릴로나Montmorillonas 이트(It MMT)의MMT) 개질 Modification
아미노프로필트리에톡시실란(aminopropyltriethoxysilane) 1, 2 및 3g을 80% 에탄올수용액 40ml에 각각 투입하여 2.5, 5.0 및 7.5 w/v%의 농도로 교반하였다. 20, 60 또는 100분 동안 교반 후에 각각의 농도의 아미노프로필트리에톡시실란(aminopropyltriethoxysilane) 교반액에 실란벤토나이트의 주성분인 몬모릴로나이트(MMT) 2g을 투입하였다. 투입 후에 섭씨 50도 또는 80도에서 1, 2 또는 5시간 동안 실란화 반응을 시켰다. 도 7 ∼ 12는 실란화 반응에 의하여 개질된 몬모릴로나이트(MMT)의 FT-IR 스펙트럼 분석결과이다. 1040, 1700, 2900 및 3800 ∼ 3600 cm-1에서 각각 실록산 결합(Si-O), 아민기, 메틸기 및 OH 기의 피크가 발견되었다. 실록산 결합(Si-O), 아민기, 메틸기 및 OH 기의 피크는 실란화 반응한 아미노프로필트리에톡시실란(aminopropyltriethoxysilane)에서 유래하고, 그 중에서 실록산 결합(Si-O)와 OH 기의 피크는 몬모릴로나이트(MMT)에서도 유래한다.1, 2 and 3 g of aminopropyltriethoxysilane were added to 40 ml of 80% ethanol aqueous solution, respectively, and stirred at a concentration of 2.5, 5.0 and 7.5 w / v%. After stirring for 20, 60 or 100 minutes, 2 g of montmorillonite (MMT), which is a main component of silane bentonite, was added to the aminopropyltriethoxysilane suspension of each concentration. After the addition, the silanization reaction was carried out at 50 or 80 degrees Celsius for 1, 2 or 5 hours. 7 to 12 are FT-IR spectrum analysis results of montmorillonite (MMT) modified by silanation. Peaks of siloxane bond (Si-O), amine group, methyl group and OH group were found at 1040, 1700, 2900 and 3800 ~ 3600 cm -1 , respectively. The peaks of the siloxane bond (Si-O), amine group, methyl group and OH group originate from the aminopropyltriethoxysilane obtained by the silanation reaction, and the peaks of the siloxane bond (Si-O) It is also derived from montmorillonite (MMT).
도 7은 아미노프로필트리에톡시실란(aminopropyltriethoxysilane)을 5.0 w/ v% 농도로 60분 동안 교반 후에 섭씨 50도에서 각각 1, 2 및 5 시간 동안 실란화 반응시켜서 개질된 몬모릴로나이트(MMT)의 FT-IR 스펙트럼 분석결과이다. 반응시간이 1시간에서 2시간으로 증가함에 따라서 모든 피크 세기가 급격하게 커졌으나 2시간에서 5시간이 경과하였을 때에는 모든 피크의 세기가 증가하였으나 피크세기의 증가속도는 완화되었다. 따라서 반응시간은 3시간이 적합하다고 판단되었다.Figure 7 shows the results of an experiment in which aminopropyltriethoxysilane was reacted at a concentration of 5.0 w / v% for 60 minutes, followed by silanization at 50 degrees Celsius for 1, 2 and 5 hours, respectively, to obtain a modified montmorillonite (MMT) IR spectral analysis results. As the reaction time increased from 1 hour to 2 hours, all peak intensities increased sharply. However, when 2 hours to 5 hours elapsed, all peak intensities were increased, but the increase rate of peak intensities was relaxed. Therefore, it was judged that the reaction time was suitable for 3 hours.
도 8은 아미노프로필트리에톡시실란(aminopropyltriethoxysilane)을 5.0 w/v% 농도로 각각 20, 60 또는 100분 동안 교반 후에 섭씨 50도에서 1 시간 동안 실란화 반응시켜서 개질된 몬모릴로나이트(MMT)의 FT-IR 스펙트럼 분석결과이다. 교반시간이 증가함에도 불구하고 모든 피크 세기는 거의 변화가 없었다. 따라서 교반시간은 20분이 적합하다고 판단되었다.FIG. 8 shows the results of an experiment in which aminopropyltriethoxysilane was reacted at a concentration of 5.0 w / v% for 20, 60, or 100 minutes, followed by silanization reaction at 50 degrees Celsius for 1 hour to obtain a modified montmorillonite (MMT) IR spectral analysis results. Despite the increasing agitation time, all peak intensities were almost unchanged. Therefore, it was judged that the stirring time was suitable for 20 minutes.
도 9는 아미노프로필트리에톡시실란(aminopropyltriethoxysilane)을 각각 2.5, 5.0 및 7.5 w/v% 농도로 60분 동안 교반 후에 섭씨 50℃에서 5시간 동안 실란화 반응시켜서 개질된 몬모릴로나이트(MMT)의 FT-IR 스펙트럼 분석결과이다. 아미노프로필트리에톡시실란(aminopropyltriethoxysilane) 농도가 2.5 w/v%에서 5.0 w/v%로 커질 때보다 5.0 w/v%에서 7.5 w/v%로 농도가 커짐에 따라서 모든 피크 세기 증가폭이 더 큼이 관찰되었다. 따라서 농도는 7.5 w/v%가 적합하다고 판단되었다.9 is a graph showing the effect of aminopropyltriethoxysilane on the FT-IR spectrum of modified montmorillonite (MMT) after stirring for 60 minutes at 2.5, 5.0, and 7.5 w / v% concentrations, respectively, IR spectral analysis results. As the concentration of aminopropyltriethoxysilane increased from 5.0 w / v% to 7.5 w / v% as the concentration of aminopropyltriethoxysilane increased from 2.5 w / v% to 5.0 w / v%, all peak intensity increase was larger Respectively. Therefore, it was judged that the concentration was 7.5 w / v%.
도 10은 아미노프로필트리에톡시실란(aminopropyltriethoxysilane)을 7.5 w/ v% 농도로 60분 동안 교반 후에 각각 섭씨 50℃ 또는 80℃에서 5시간 동안 실란화 반응시켜서 개질된 몬모릴로나이트(MMT)의 FT-IR 스펙트럼 분석결과이다. 반응온도가 섭씨 50℃ 또는 80℃로 증가하였을 때에 모든 피크의 세기가 매우 커졌다. 따라서 아미노프로필트리에톡시실란(aminopropyltriethoxysilane) 농도가 7.5 w/v% 일 경우에 실란화 반응온도는 섭씨 80℃가 적합하다고 판단되었다.FIG. 10 shows the results of FT-IR analysis of amorphous montmorillonite (MMT) after aminopropyltriethoxysilane was stirred at 7.5 w / v% concentration for 60 minutes and then silanized at 50 ° C. or 80 ° C. for 5 hours, Spectrum analysis results. When the reaction temperature was increased to 50 캜 or 80 캜, the intensity of all the peaks became very large. Therefore, when the aminopropyltriethoxysilane concentration was 7.5 w / v%, it was judged that the silanation temperature was 80 ℃.
도 11은 아미노프로필트리에톡시실란(aminopropyltriethoxysilane)을 5.0 w/v% 농도로 60분 동안 교반 후에 각각 섭씨 50℃ 또는 80℃에서 5시간 동안 실란화 반응시켜서 개질된 몬모릴로나이트(MMT)의 FT-IR 스펙트럼 분석결과이다. 반응온도가 섭씨 50℃ 또는 80℃로 증가하였을 때에 모든 피크의 세기는 거의 변화가 없었다. 따라서 아미노프로필트리에톡시실란(aminopropyltriethoxysilane) 농도가 5.0 w/v% 일 경우에 실란화 반응온도는 섭씨 50℃가 적합하다고 판단되었다.FIG. 11 shows the results of FT-IR analysis of amorphous montmorillonite (MMT) after aminopropyltriethoxysilane was stirred at a concentration of 5.0 w / v% for 60 minutes and then subjected to silanization reaction at 50 ° C. or 80 ° C. for 5 hours, Spectrum analysis results. When the reaction temperature was increased to 50 ° C. or 80 ° C., the intensity of all the peaks was almost unchanged. Therefore, when the aminopropyltriethoxysilane concentration was 5.0 w / v%, it was judged that the temperature of the silanation reaction was 50 ° C.
도 12는 아미노프로필트리에톡시실란(aminopropyltriethoxysilane)을 5.0 w/ v% 농도로 100분 동안 교반 후에 각각 섭씨 50℃ 또는 80℃에서 1시간 동안 실란화 반응시켜서 개질된 몬모릴로나이트(MMT)의 FT-IR 스펙트럼 분석결과이다. 반응온도가 섭씨 50℃ 또는 80℃로 증가하였을 때에 모든 피크의 세기는 거의 변화가 없었다. 따라서 아미노프로필트리에톡시실란(aminopropyltriethoxysilane) 농도가 5.0 w/v% 일 경우에 도 11과 다른 반응시간 및 다른 교반시간에도 불구하고 실란화 반응온도는 섭씨 50℃가 적합하다고 판단되었다.FIG. 12 shows the results of FT-IR analysis of amorphous montmorillonite (MMT) after aminopropyltriethoxysilane was stirred at a concentration of 5.0 w / v% for 100 minutes, followed by silanation reaction at 50 ° C. or 80 ° C. for 1 hour, Spectrum analysis results. When the reaction temperature was increased to 50 ° C. or 80 ° C., the intensity of all the peaks was almost unchanged. Therefore, in the case of aminopropyltriethoxysilane concentration of 5.0 w / v%, it was judged that the temperature of the silanization reaction was 50 ° C, even though the reaction time and the stirring time were different from those of FIG.
따라서 종합적으로 적정 반응시간, 적정교반시간, 적정농도, 적정반응온도는 각각 3시간, 20분 및 7.5 w/v% 및 섭씨 80℃가 도출되었다. 그러나 농도가 5.0 w/v% 이하일 때에는 적정반응온도는 섭씨 50℃가 도출되었다.Therefore, the optimum reaction time, the optimum stirring time, the optimum concentration, and the optimum reaction temperature were 3 hr, 20 min and 7.5 w / v% and 80 ° C, respectively. However, when the concentration was 5.0 w / v% or lower, the optimum reaction temperature was 50 ° C.
Claims (16)
수팽윤성 유/무기재료를 응집시킨 수팽윤성 유/무기재료 응집체를 제조하는 단계와;
이와 별도로 상기 응집단계를 거치지 않은 수팽윤성 유/무기재료 표면 또는 상기 수팽윤성 유/무기재료 응집체 표면을 실란커플링제로써 소수성 개질하거나 결합하여 표면개질된 수팽윤성 유/무기 캡슐(실란화)을 제조하는 단계와;
개질아스팔트 요소들을 혼합/용융한 상태에서 상기 단계에서 얻은 상기 수팽윤성 유/무기 캡슐(실란화) 또는 상기 수팽윤성 유/무기 캡슐(실란화) 외에 하이브리드 충진제를 추가로 첨가하거나, 상기 수팽윤성 유/무기 캡슐(실란화)을 제외하고 하이브리드 충전재만을 첨가하는 것을 특징으로 하는 방수소재의 제조방법.A method for manufacturing a waterproof material,
Preparing a water-swellable oil / inorganic material aggregate in which water-swellable oil / inorganic material is aggregated;
Alternatively, the surface of the water-swellable oil / inorganic material not subjected to the agglomeration step or the surface of the water-swellable oil / inorganic material agglomerate may be hydrophobically modified or bonded with a silane coupling agent to prepare a water-swellable oil / inorganic capsule (silanization) ;
(Hybridization) of the water-swellable oil / inorganic capsules (silanized) or the water-swellable oil / inorganic capsules (silanized) obtained in the above step in the state where the modified asphalt components are mixed / / ≪ / RTI > inorganic capsule (silanized).
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109650781A (en) * | 2018-12-29 | 2019-04-19 | 中设设计集团股份有限公司 | A kind of high frictional resistance thin overlay asphalt of middle low temperature warm mix and preparation method thereof |
| CN110510910A (en) * | 2019-09-26 | 2019-11-29 | 交通运输部公路科学研究所 | A kind of thin micro crack microcapsules self-repair material of the concrete that cyst wall is degradable |
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2016
- 2016-10-14 KR KR1020160133697A patent/KR20170059884A/en active Search and Examination
- 2016-11-03 KR KR1020160145760A patent/KR101837014B1/en active IP Right Grant
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109650781A (en) * | 2018-12-29 | 2019-04-19 | 中设设计集团股份有限公司 | A kind of high frictional resistance thin overlay asphalt of middle low temperature warm mix and preparation method thereof |
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| CN112745048A (en) * | 2019-10-30 | 2021-05-04 | 中国石油化工股份有限公司 | Biomass additive for asphalt and preparation method and application thereof |
| CN112745048B (en) * | 2019-10-30 | 2022-03-08 | 中国石油化工股份有限公司 | Biomass additive for asphalt and preparation method and application thereof |
| CN111171671A (en) * | 2019-12-26 | 2020-05-19 | 中南林业科技大学 | Fireproof super-hydrophobic coating, super-hydrophobic material and preparation method thereof |
| CN111423818A (en) * | 2020-04-13 | 2020-07-17 | 广州大学 | Modified asphalt and preparation method thereof |
| CN111909611A (en) * | 2020-08-19 | 2020-11-10 | 成都新柯力化工科技有限公司 | High-elongation anti-sagging polyurethane waterproof coating and preparation method thereof |
| CN112375322A (en) * | 2020-11-26 | 2021-02-19 | 丽天防水科技有限公司 | Waterproof coiled material sizing material with high peel strength, preparation method and waterproof coiled material |
| CN112375322B (en) * | 2020-11-26 | 2021-07-23 | 丽天防水科技有限公司 | Waterproof coiled material sizing material with high peel strength, preparation method and waterproof coiled material |
| CN115869919A (en) * | 2022-11-30 | 2023-03-31 | 南昌大学 | Method for improving carboxymethylation efficiency of cellulose and promoting insertion of cellulose into clay mineral layer, product and application of product |
| CN115869919B (en) * | 2022-11-30 | 2024-05-03 | 南昌大学 | Method for improving cellulose carboxymethylation efficiency and promoting intercalation of cellulose into clay mineral layers, product and application of product |
| CN116677018A (en) * | 2023-07-31 | 2023-09-01 | 上海勘测设计研究院有限公司 | Self-repairing capsule for refuse landfill impervious layer and anti-seepage method |
| CN116677018B (en) * | 2023-07-31 | 2023-10-10 | 上海勘测设计研究院有限公司 | Self-repairing capsule for refuse landfill impervious layer and anti-seepage method |
Also Published As
| Publication number | Publication date |
|---|---|
| KR20170059888A (en) | 2017-05-31 |
| KR101837014B1 (en) | 2018-04-20 |
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