KR102511529B1 - Fire resistant silicone sealant composition for double glazing - Google Patents
Fire resistant silicone sealant composition for double glazing Download PDFInfo
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- KR102511529B1 KR102511529B1 KR1020230016497A KR20230016497A KR102511529B1 KR 102511529 B1 KR102511529 B1 KR 102511529B1 KR 1020230016497 A KR1020230016497 A KR 1020230016497A KR 20230016497 A KR20230016497 A KR 20230016497A KR 102511529 B1 KR102511529 B1 KR 102511529B1
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- 239000000203 mixture Substances 0.000 title claims abstract description 38
- 239000004590 silicone sealant Substances 0.000 title claims abstract description 16
- 230000009970 fire resistant effect Effects 0.000 title claims abstract description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000003063 flame retardant Substances 0.000 claims abstract description 28
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 26
- 239000004917 carbon fiber Substances 0.000 claims abstract description 26
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011521 glass Substances 0.000 claims abstract description 25
- -1 polysiloxane Polymers 0.000 claims abstract description 25
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- 239000000945 filler Substances 0.000 claims abstract description 19
- 239000011347 resin Substances 0.000 claims abstract description 19
- 229920005989 resin Polymers 0.000 claims abstract description 19
- 238000007789 sealing Methods 0.000 claims abstract description 16
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 13
- 229910000077 silane Inorganic materials 0.000 claims abstract description 13
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 12
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract description 12
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 12
- 239000004014 plasticizer Substances 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 239000010456 wollastonite Substances 0.000 claims abstract description 11
- 229910052882 wollastonite Inorganic materials 0.000 claims abstract description 11
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 9
- 150000002367 halogens Chemical class 0.000 claims abstract description 9
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 7
- 239000011574 phosphorus Substances 0.000 claims abstract description 7
- 238000010248 power generation Methods 0.000 claims description 19
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 12
- 229910019142 PO4 Inorganic materials 0.000 claims description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 11
- 239000010452 phosphate Substances 0.000 claims description 11
- 229920000742 Cotton Polymers 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 229910052580 B4C Inorganic materials 0.000 claims description 8
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000004697 Polyetherimide Substances 0.000 claims description 7
- 229920001601 polyetherimide Polymers 0.000 claims description 7
- 239000001569 carbon dioxide Substances 0.000 claims description 6
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 6
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 6
- 239000002121 nanofiber Substances 0.000 claims description 6
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- ZOXJGFHDIHLPTG-BJUDXGSMSA-N Boron-10 Chemical compound [10B] ZOXJGFHDIHLPTG-BJUDXGSMSA-N 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000003566 sealing material Substances 0.000 abstract description 4
- 230000002265 prevention Effects 0.000 abstract 2
- 239000000565 sealant Substances 0.000 description 28
- 239000002956 ash Substances 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 17
- 239000007864 aqueous solution Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 9
- 239000000654 additive Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 230000000704 physical effect Effects 0.000 description 7
- 239000004254 Ammonium phosphate Substances 0.000 description 5
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 5
- 235000019289 ammonium phosphates Nutrition 0.000 description 5
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 5
- 239000002318 adhesion promoter Substances 0.000 description 4
- DEIGXXQKDWULML-UHFFFAOYSA-N 1,2,5,6,9,10-hexabromocyclododecane Chemical compound BrC1CCC(Br)C(Br)CCC(Br)C(Br)CCC1Br DEIGXXQKDWULML-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000002411 thermogravimetry Methods 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 239000004114 Ammonium polyphosphate Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 235000019826 ammonium polyphosphate Nutrition 0.000 description 2
- 229920001276 ammonium polyphosphate Polymers 0.000 description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 2
- 235000011130 ammonium sulphate Nutrition 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- VNVRRNRPVIZREH-UHFFFAOYSA-N carbamoylphosphonic acid Chemical class NC(=O)P(O)(O)=O VNVRRNRPVIZREH-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- WHIVNJATOVLWBW-UHFFFAOYSA-N n-butan-2-ylidenehydroxylamine Chemical compound CCC(C)=NO WHIVNJATOVLWBW-UHFFFAOYSA-N 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 229920000388 Polyphosphate Polymers 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 229910006501 ZrSiO Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001523 electrospinning Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- 238000004079 fireproofing Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- INETXKGLHYNTHK-AQWWNALJSA-N tetrakis[(e)-butan-2-ylideneamino] silicate Chemical compound CC\C(C)=N\O[Si](O\N=C(/C)CC)(O\N=C(/C)CC)O\N=C(/C)CC INETXKGLHYNTHK-AQWWNALJSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000005341 toughened glass Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
- C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Sealing Material Composition (AREA)
Abstract
Description
본 발명은 2액형 복층유리용 2차 실링 내화 실리콘 실란트 조성물에 관한 것으로, 더욱 상세하게는 수산화마그네슘, 수산화알루미늄, 탄소섬유, 탄산화 발전회 등의 내화 첨가제를 포함하는 실란트 조성물을 조성함으로써, 내화성이 향상되어 방화성이 개선되는 2액형 복층유리용 2차 실링 내화 실리콘 실란트 조성물에 관한 것이다.The present invention relates to a secondary sealing fire-resistant silicone sealant composition for two-component double-glazed glass, and more particularly, by forming a sealant composition containing fire-resistant additives such as magnesium hydroxide, aluminum hydroxide, carbon fiber, and carbonated power generation ash, The present invention relates to a secondary sealing fire-resistant silicone sealant composition for two-component double-glazed glass having improved fire resistance.
복층유리(Double Glazing)란, 두 장의 판유리 사이에 공간을 두어 최소 두 겹으로 만들어진 판유리로 이는 일반 단판유리가 갖는 결점을 보완한 것이다. 이러한 복층유리는 단열유리(insulating glass, IG unit)라고도 한다. Double glazing is a sheet glass made of at least two layers with a space between two sheets of glass, which compensates for the shortcomings of ordinary single-pane glass. This double-glazed glass is also called insulating glass (IG unit).
상기 복층유리는 유리와 유리 사이에 마감재로 실란트 조성물이 사용되는데, 이를 복층유리 2차 실링이라고 부른다.In the double-glazed glass, a sealant composition is used as a finishing material between glass and glass, which is called double-glazed secondary sealing.
종래 이러한 실란트는 수밀, 기밀의 기능적인 목적만을 추구하였는바, 최근 이러한 실란트 역시 방화성능이 요구되며, 실링에 의한 유독가스 및 열기에 대한 확실한 차단 효과가 요구되고 있는 실정이다.Conventionally, these sealants have pursued only functional purposes of watertightness and airtightness. Recently, these sealants also require fire protection performance, and a reliable blocking effect against toxic gases and heat by sealing is required.
내화성 실란트의 선행문헌으로는 대한민국 등록특허 제10-0674035호 및 등록특허 제10-2039767호가 게시되어 있다.Korean Patent Registration No. 10-0674035 and Korean Patent Registration No. 10-2039767 have been published as prior literature on fire-resistant sealants.
상기 대한민국 등록특허 제10-0674035호는 교차결합 유기규소 화합물, 규회석 등을 포함하여 내화성을 개선하였고, 상기 대한민국 등록특허 제10-2039767호에서는 팽창 흑연, 난연제를 포함하여 방화재용 실란트 조성물을 제조하였다.Korean Patent Registration No. 10-0674035 improved fire resistance by including a cross-linked organosilicon compound, wollastonite, etc., and Korean Patent Registration No. 10-2039767 prepared a sealant composition for fire retardant materials by including expanded graphite and a flame retardant. .
그러나 선행문헌들의 어디에서도 탄소섬유, 탄산화 발전회 등을 내화 첨가제로 하는 실란트 조성물을 찾아볼 수 없었다.However, no sealant composition containing carbon fiber, carbonated power ash, etc. as a fire resistant additive was found anywhere in the prior literature.
따라서, 본 발명의 목적은 수산화마그네슘, 수산화알루미늄, 탄소섬유, 탄산화 발전회 등의 내화 첨가제를 포함함으로써, 우수한 접착성, 기밀성을 가지면서도, 내열성 및 내화성이 우수하여 방화성능이 개선된 2액형 복층유리용 2차 실링 내화 실리콘 실란트 조성물을 제공하는 데 있다. Therefore, an object of the present invention is a two-component multi-layer with excellent heat resistance and fire resistance while having excellent adhesion and airtightness by including fire resistant additives such as magnesium hydroxide, aluminum hydroxide, carbon fiber, and carbonated power generation ash, thereby improving fire protection performance. It is to provide a secondary sealing refractory silicone sealant composition for glass.
상기한 목적을 달성하기 위한 본 발명의 2액형 복층유리용 2차 실링 내화 실리콘 실란트 조성물은, 수산기말단 폴리실록산수지 100중량부, 수산화마그네슘 10~50중량부, 수산화알루미늄 10~30중량부, 할로겐계 난연제 0.01~0.1중량부, 인계 난연제 1~5중량부, 탄소섬유 10~50중량부, 탄산화 발전회 10~50중량부, 가소제 20~50중량부, 충전제 100~150중량부 및 백금 촉매 0.1~5중량부를 포함하는 주제부와; 실란 경화제를 포함하는 경화제부;의 2액형으로 구성되되, 상기 충전제는 규회석을 포함하는 것을 특징으로 한다.Secondary sealing fireproof silicone sealant composition for two-component double-glazed glass of the present invention to achieve the above object is 100 parts by weight of hydroxyl-terminated polysiloxane resin, 10 to 50 parts by weight of magnesium hydroxide, 10 to 30 parts by weight of aluminum hydroxide, halogen-based 0.01 to 0.1 parts by weight of flame retardant, 1 to 5 parts by weight of phosphorus-based flame retardant, 10 to 50 parts by weight of carbon fiber, 10 to 50 parts by weight of carbonation power ash, 20 to 50 parts by weight of plasticizer, 100 to 150 parts by weight of filler, and 0.1 to 150 parts by weight of platinum catalyst A main part containing 5 parts by weight; It is composed of a two-component type of a curing agent containing a silane curing agent; characterized in that the filler includes wollastonite.
상기 탄소섬유는, 탄소섬유를 질소분위기 하에서 600~1000℃에서 30~100분간 열처리하고, 상기 열처리된 탄소섬유를 인산염 수용액에 30~40분간 침지한 후, 건조하고 0.1~100㎛로 분쇄한 것임을 특징으로 한다. The carbon fiber is obtained by heat-treating the carbon fiber at 600-1000 ° C. for 30-100 minutes under a nitrogen atmosphere, immersing the heat-treated carbon fiber in an aqueous phosphate solution for 30-40 minutes, drying, and grinding to 0.1-100 μm. to be characterized
상기 탄산화 발전회는, 발전회에 물을 혼합하고, 이에 이산화탄소를 pH 9~10이 되도록 주입한 후, 여과, 건조하고, 상기 건조된 건조물을 인산염 수용액에 30~40분간 침지한 후, 건조하고 0.1~100㎛로 분쇄한 것임을 특징으로 한다.In the carbonation power generation ash, water is mixed with the power generation ash, carbon dioxide is injected thereto to a pH of 9 to 10, filtered and dried, and the dried product is immersed in an aqueous phosphate solution for 30 to 40 minutes, then dried It is characterized in that it is ground to 0.1 ~ 100㎛.
상기 주제부는, 보론 카바이드 10~20중량부 및 규산지르코늄 10~20중량부를 더 포함하는 것을 특징으로 한다. The main part is characterized in that it further comprises 10 to 20 parts by weight of boron carbide and 10 to 20 parts by weight of zirconium silicate.
상기 충전제는 세륨산화물을 더 포함하는 것을 특징으로 한다.The filler is characterized in that it further comprises cerium oxide.
상기 주제부는, 폴리에테르이미드 나노섬유 1~5중량부 및 난연처리된 면섬유 분말 1~5중량부를 더 포함하는 것을 특징으로 한다.The main part is characterized in that it further comprises 1 to 5 parts by weight of polyetherimide nanofibers and 1 to 5 parts by weight of flame retardant treated cotton fiber powder.
본 발명의 2액형 복층유리용 2차 실링 내화 실리콘 실란트 조성물에 의하면, 방화성능이 요구되는 복층유리의 실링재, 글레이징 등으로 사용되어 건축 구조물의 방화성능을 월등히 향상시킬 수 있다는 장점이 있다. According to the two-component double-glazed secondary sealing fire-resistant silicone sealant composition for double-glazed glass of the present invention, it is used as a sealing material, glazing, etc. of double-glazed glass requiring fire-resistance performance, and has the advantage of significantly improving the fire-resistance performance of building structures.
이하, 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail.
본 발명의 2액형 복층유리용 2차 실링 내화 실리콘 실란트 조성물은, 내화첨가제로 수산화마그네슘, 수산화알루미늄, 탄소섬유, 탄산화 발전회 등을 투입하여 실란트 조성물을 제조함으로써, 우수한 접착성 및 기밀성을 가지면서도 내화성이 향상되어, 방화성능이 요구되는 각종 건축 구조물, 특히 복층유리에 실링재로서 사용될 수 있다는 데 가장 큰 특징이 있다.The secondary sealing fireproof silicone sealant composition for two-component double-glazed glass of the present invention is prepared by preparing a sealant composition by introducing magnesium hydroxide, aluminum hydroxide, carbon fiber, carbonated power generation ash, etc. as fireproof additives, while having excellent adhesiveness and airtightness. The biggest feature is that it can be used as a sealing material for various building structures requiring fire resistance, especially double-glazed glass, because fire resistance is improved.
구체적으로 본 발명에 의한 2액형 복층유리용 2차 실링 내화 실리콘 실란트 조성물은, 수산기말단 폴리실록산수지 100중량부, 수산화마그네슘 10~50중량부, 수산화알루미늄 10~30중량부, 할로겐계 난연제 0.01~0.1중량부, 인계 난연제 1~5중량부, 탄소섬유 10~50중량부, 탄산화 발전회 10~50중량부, 가소제 20~50중량부, 충전제 100~150중량부 및 백금 촉매 0.1~5중량부를 포함하는 주제부와; 실란 경화제를 포함하는 경화제부;의 2액형으로 구성되되, 상기 충전제는 규회석을 포함하는 것을 특징으로 한다.Specifically, the secondary sealing fireproof silicone sealant composition for two-component double-glazed glass according to the present invention contains 100 parts by weight of a hydroxyl-terminated polysiloxane resin, 10 to 50 parts by weight of magnesium hydroxide, 10 to 30 parts by weight of aluminum hydroxide, and 0.01 to 0.1 parts by weight of a halogen-based flame retardant. 1 to 5 parts by weight of phosphorus flame retardant, 10 to 50 parts by weight of carbon fiber, 10 to 50 parts by weight of carbonation power ash, 20 to 50 parts by weight of plasticizer, 100 to 150 parts by weight of filler, and 0.1 to 5 parts by weight of platinum catalyst with the subject part; It is composed of a two-component type of a curing agent containing a silane curing agent; characterized in that the filler includes wollastonite.
먼저, 본 발명은 주제부와 경화제부의 2액형으로 구성되는바, 상기 주제부와 경화제부는 10:0.5~2 부피비로 혼합되어 사용됨이 바람직하다. First, the present invention is composed of a two-component type of a main part and a curing agent part, and the main part and the curing agent part are preferably mixed and used in a volume ratio of 10:0.5 to 2.
상기 주제부는 수산기말단 폴리실록산수지 100중량부, 수산화마그네슘 10~50중량부, 수산화알루미늄 10~30중량부, 할로겐계 난연제 0.01~0.1중량부, 인계 난연제 1~5중량부, 탄소섬유 10~50중량부, 탄산화 발전회 10~50중량부, 가소제 20~50중량부, 충전제 100~150중량부 및 백금 촉매 0.1~5중량부를 포함한다.The main component includes 100 parts by weight of hydroxyl-terminated polysiloxane resin, 10 to 50 parts by weight of magnesium hydroxide, 10 to 30 parts by weight of aluminum hydroxide, 0.01 to 0.1 parts by weight of halogen-based flame retardant, 1-5 parts by weight of phosphorus-based flame retardant, and 10 to 50 parts by weight of carbon fiber. 10 to 50 parts by weight of carbonation power generation ash, 20 to 50 parts by weight of a plasticizer, 100 to 150 parts by weight of a filler, and 0.1 to 5 parts by weight of a platinum catalyst.
상기 수산기말단 폴리실록산수지는 실란트 조성물을 구성하는 주성분으로, 이 기술이 속하는 분야에서 이미 공지된 성분이다. 예시적으로, 수산기말단 폴리디메틸실록산 수지(Siloxanes and Silicones, di-Me, hydroxy-terminated cas no. 70131-67-8)를 사용할 수 있다. 이하, 주제부 내 '중량부'는 상기 수산기말단 폴리실록산수지 100중량부를 기준으로 한다.The hydroxyl-terminated polysiloxane resin is a main component constituting the sealant composition and is a component already known in the field to which this technology belongs. For example, a hydroxyl-terminated polydimethylsiloxane resin (Siloxanes and Silicones, di-Me, hydroxy-terminated cas no. 70131-67-8) may be used. Hereinafter, 'parts by weight' in the main part is based on 100 parts by weight of the hydroxyl-terminated polysiloxane resin.
상기 수산화마그네슘(mignesium dihydroxide)과 수산화알루미늄(aluminium trihyroxide)은 열에 의해 분해될 때 수증기를 배출하여 일부 연소 가스를 희석하고, 열을 흡수하는 성질을 포함하고 있어 연소의 확산을 방지하는 역할을 하기 때문에 내화 첨가제로서 사용된다. The magnesium hydroxide (mignesium dihydroxide) and aluminum hydroxide (aluminum trihyroxide) emit water vapor when decomposed by heat to dilute some combustion gases and absorb heat, which serves to prevent the spread of combustion. Used as a fire retardant additive.
상기 수산화마그네슘과 수산화알루미늄은 상기 수산기말단 폴리실록산수지 100중량부에 대하여 수산화마그네슘 10~50중량부 및 수산화알루미늄 10~30중량부로 포함됨이 바람직한데, 그 함량이 상기한 범위를 벗어날 경우 충분한 내화성의 확보가 어렵거나, 실란트 조성물의 물성을 저해하기 때문이다.The magnesium hydroxide and aluminum hydroxide are preferably included in 10 to 50 parts by weight of magnesium hydroxide and 10 to 30 parts by weight of aluminum hydroxide based on 100 parts by weight of the hydroxyl-terminated polysiloxane resin. This is because it is difficult or impairs the physical properties of the sealant composition.
상기 할로겐계 난연제는 비용이 저렴한 대표적인 난연제로, 예시적으로 브롬계 난연제를 들 수 있는바, 더욱 구체적으로 hexabromocyclododecane(HBCDD), tertrabromobispheol A(TBBPA) 중 1종 이상을 사용할 수 있다. The halogen-based flame retardant is a representative low-cost flame retardant, and exemplarily brominated flame retardants may be mentioned. More specifically, at least one of hexabromocyclododecane (HBCDD) and tertrabromobispheol A (TBBPA) may be used.
다만, 이러한 할로겐계 난연제는 환경문제가 대두될 수 있으므로, 그 사용량을 상기 수산기말단 폴리실록산수지 100중량부에 대하여 0.01~0.1중량부로 함이 바람직하다. 아울러, 친환경성이 요구되는 경우 이러한 할로겐계 난연제의 사용은 생략할 수 있다.However, since such a halogen-based flame retardant may cause environmental problems, it is preferable to use 0.01 to 0.1 parts by weight based on 100 parts by weight of the hydroxyl-terminated polysiloxane resin. In addition, when eco-friendliness is required, the use of such a halogen-based flame retardant can be omitted.
상기 인계 난연제로는 암모늄 폴리포스테이트(Ammonium Polyphosphate)를 사용할 수 있는바, 이는 자체 물성에 따라 화염을 받으면 팽창되어 탄화막을 형성하는 역할을 함으로써, 방화성능을 개선해준다. Ammonium polyphosphate can be used as the phosphorus-based flame retardant, which expands upon receiving a flame according to its physical properties and serves to form a carbonized film, thereby improving fire resistance.
상기 암모늄 폴리포스테이트는 상기 수산기말단 폴리실록산수지 100중량부에 대하여 1~5중량부만큼 포함됨이 바람직하다. The ammonium polyphosphate is preferably included in an amount of 1 to 5 parts by weight based on 100 parts by weight of the hydroxyl-terminated polysiloxane resin.
상기 탄소섬유는 연기 발생을 억제하고, 절연층으로 작용하여 열의 이동을 방해하여 난연성을 확보하는 것은 물론, 실란트 조성물의 강도 및 내열성을 개선하는 역할을 한다.The carbon fiber suppresses smoke generation, acts as an insulating layer to prevent heat transfer, secures flame retardancy, and serves to improve the strength and heat resistance of the sealant composition.
이러한 탄소섬유로는 질소분위기 하에서 600~1000℃에서 30~100분간 열처리하고, 상기 열처리된 탄소섬유를 2~3부피배의 인산염 수용액에 20~30℃ 정도의 온도에서 30~40분간 침지한 후, 건조하고, 0.1~100㎛로 분쇄한 것을 사용함이 바람직하다. 이때, 상기 인산염 수용액으로는 3~10중량% 농도의 인산암모늄 수용액을 사용하면 족한바, 인산염의 종류 및 농도를 제한하지 않는다.These carbon fibers are heat treated at 600 to 1000 ° C. for 30 to 100 minutes under a nitrogen atmosphere, and the heat-treated carbon fibers are immersed in 2 to 3 times the volume of an aqueous phosphate solution at a temperature of about 20 to 30 ° C. for 30 to 40 minutes. , it is preferable to use dried and pulverized to 0.1 ~ 100㎛. At this time, as the phosphate aqueous solution, it is sufficient to use an ammonium phosphate aqueous solution having a concentration of 3 to 10% by weight, and the type and concentration of the phosphate are not limited.
통상 백금 촉매가 사용된 실란트 조성물은 인장강도가 저하되는 특징이 있는바, 본 발명은 상기 탄소섬유를 통해 이러한 단점을 개선함은 물론, 내열, 내화특성 및 전체적인 실란트 조성물의 물성을 개선하는 것이다.In general, sealant compositions using platinum catalysts have a characteristic of lowering tensile strength, and the present invention is to improve heat resistance, fire resistance, and overall physical properties of the sealant composition as well as improve these disadvantages through the carbon fiber.
상기 탄소섬유는 상기 수산기말단 폴리실록산수지 100중량부에 대하여 10~50중량부로 포함됨이 바람직하다.The carbon fiber is preferably included in an amount of 10 to 50 parts by weight based on 100 parts by weight of the hydroxyl-terminated polysiloxane resin.
상기 탄산화 발전회는 내화 및 난연성을 현저히 높여줄 뿐 아니라, 탄소섬유와의 병용시 실란트 조성물을 물성 및 내열성을 현저히 개선하는 역할을 한다.The carbonation power generation ash not only remarkably improves fire resistance and flame retardancy, but also significantly improves physical properties and heat resistance of the sealant composition when used in combination with carbon fiber.
석탄 연소 후에 남아있는 물질 중 하나인 발전회(비회, fly ash)는 SiO2, CaO, Fe2O3, Al2O3, MgO, SO3, Na2O 등을 주성분으로 하는바, 이를 탄산화할 경우 우수한 내화 특성을 발휘하는 것이다.Power ash (fly ash), one of the materials remaining after coal combustion, is mainly composed of SiO 2 , CaO, Fe 2 O 3 , Al 2 O 3 , MgO, SO 3 , Na 2 O, etc., which is carbonated If so, it exhibits excellent fire resistance properties.
이러한 탄산화 발전회를 제조하는 방법은, 발전회에 물을 1:1~2중량비로 혼합하고, 이에 이산화탄소를 pH가 9~10이 될때까지 주입한 후, 여과 및 건조하고, 상기 건조된 건조물을 2~3부피배의 인산염 수용액에 20~30℃의 온도에서 30~40분간 침지한 후, 건조하고 0.1~100㎛로 분쇄하는 것이다. 이때, 상기 인산염 수용액으로는 3~10중량% 농도의 인산암모늄 수용액을 사용하면 족한바, 인산염의 종류 및 농도를 제한하지 않는다.In the method for producing carbonation power generation ash, water is mixed with power generation ash at a weight ratio of 1:1 to 2, carbon dioxide is injected thereto until the pH is 9 to 10, followed by filtering and drying, and the dried product is It is immersed in 2 to 3 times the volume of phosphate aqueous solution at a temperature of 20 to 30 ° C for 30 to 40 minutes, dried, and pulverized to 0.1 to 100 μm. At this time, as the phosphate aqueous solution, it is sufficient to use an ammonium phosphate aqueous solution having a concentration of 3 to 10% by weight, and the type and concentration of the phosphate are not limited.
통상 탄산화 발전회의 제조시 pH가 7~8정도가 되도록 이산화탄소를 주입하는데, 이러한 경우 오히려 전체적인 실란트 조성물의 물성이 좋지 못한바, 본 발명은 pH 9~10이 되도록 이산화탄소를 주입하고, 그 내화성능을 더욱 개선하기 위하여 인산암모늄 수용액에 침지하여 사용하는 것이다. In general, carbon dioxide is injected so that the pH is about 7 to 8 during the production of carbonation power generation ash, but in this case, the physical properties of the overall sealant composition are not good. In the present invention, carbon dioxide is injected so that the pH is 9 to 10, For further improvement, it is used after being immersed in an aqueous solution of ammonium phosphate.
즉, 이러한 탄산화 발전회는 연소시 인산염에 의해 1차 적으로 탄화막을 형성하고, 발전회에 존재하는 Ca, Mg, Si 성분이 세라믹을 형성시켜 산소와 열을 차단하게 된다.That is, such carbonation power generation ash primarily forms a carbonized film by phosphate during combustion, and Ca, Mg, and Si components present in power generation ash form a ceramic to block oxygen and heat.
상기 탄산화 발전회는 상기 수산기말단 폴리실록산수지 100중량부에 대하여 10~50중량부로 포함됨이 바람직하다.The carbonation power generation ash is preferably included in an amount of 10 to 50 parts by weight based on 100 parts by weight of the hydroxyl-terminated polysiloxane resin.
상기 가소제는 실란트 조성물의 성질을 부드럽고 유동적일 수 있도록 하고, 지나치게 경직되어 굳는 것을 막아주는 역할을 하는 것으로, 폴리실록산 오일이 사용될 수 있다.The plasticizer serves to make the properties of the sealant composition soft and fluid and prevents it from being hardened due to excessive rigidity, and polysiloxane oil may be used.
상기 가소제는 상기 수산기말단 폴리실록산수지 100중량부에 대하여 20~50중량부로 포함됨이 바람직한바, 그 함량이 너무 적거나 많으면 가소제로서의 기능이 충분히 발휘될 수 없거나, 오히려 인장강도를 저하시키기 때문이다.The plasticizer is preferably included in an amount of 20 to 50 parts by weight based on 100 parts by weight of the hydroxyl-terminated polysiloxane resin, because if the content is too small or too large, the function as a plasticizer cannot be sufficiently exhibited, or rather, the tensile strength is lowered.
상기 충전제는 실란트의 강도, 경도 등을 적절하게 조절해주는 물질로서, 규회석을 사용함이 바람직하다. 상기 규회석은 실란트 조성물의 내화 특성을 개선하면서도, 결합력을 높여주는 역할을 한다.The filler is a material that appropriately adjusts the strength, hardness, etc. of the sealant, and it is preferable to use wollastonite. The wollastonite improves the fire resistance of the sealant composition and serves to increase bonding strength.
아울러, 상기 충전제는 세륨산화물(CeO2)을 더 포함하는 것이 바람직하다. 상기 세륨산화물은 내열 및 난연 특성을 개선해준다. 이때, 상기 규회석과 세륨산화물은 1:0.5~1 중량비로 사용됨이 바람직하다.In addition, the filler preferably further includes cerium oxide (CeO 2 ). The cerium oxide improves heat resistance and flame retardancy. At this time, the wollastonite and cerium oxide are preferably used in a weight ratio of 1:0.5 to 1.
상기 충전제는 상기 수산기말단 폴리실록산수지 100중량부를 기준으로 100~150중량부로 포함됨이 바람직한데, 그 함량이 너무 적으면 물성의 향상 효과가 미미하고, 과량이 되면 전체적인 접착력이 저하되는 등의 문제가 있기 때문이다. The filler is preferably included in an amount of 100 to 150 parts by weight based on 100 parts by weight of the hydroxyl-terminated polysiloxane resin. Because.
상기 백금 촉매는 경화 속도를 촉진시키는 경화촉진제로서의 역할을 하는 것이며, 최종적으로 백금은 실란트에 자기 소화성을 부여해주는 역할을 한다.The platinum catalyst serves as a curing accelerator for accelerating the curing rate, and finally, platinum serves to impart self-extinguishing properties to the sealant.
상기 백금 촉매로는 알코올, 에테르, 알데히드 등에 혼합된 염화 백금산 또는 염화 백금산 화합물 및 인산계 백금[Pt{P(OC6H5)3}4, Pt{P(C6H5)3}4, Pt{P(CH3)3}4, Pt{P(C4H9)3}4, Pt{P(OCH3)3}4, Pt{P(OC6H5)3}3, Pt{P(C6H5)3}3, Pt{P(C6H5)(C2H5)2}4, Pt{P(OC6H5)(OC2H5)2}4, Pt{P(C6H5)2(OC2H5)}4, Pt{P(CH3)2(OC4H9)}4) 등을 포함하는 것일 수 있으며, 알코올, 이소프로필 알코올, 벤젠, 자일렌 등 유기용제에 분산시켜서 사용되는 것일 수도 있음은 물론이다. The platinum catalyst includes chloroplatinic acid or a chloroplatinic acid compound mixed with alcohol, ether, aldehyde, etc., and phosphoric acid-based platinum [Pt{P(OC 6 H 5 ) 3 } 4 , Pt{P(C 6 H 5 ) 3 } 4 , Pt{P(CH 3 ) 3 } 4 , Pt{P(C 4 H 9 ) 3 } 4 , Pt{P(OCH 3 ) 3 } 4 , Pt{P(OC 6 H 5 ) 3 } 3 , Pt{ P(C 6 H 5 ) 3 } 3 , Pt{P(C 6 H 5 )(C 2 H 5 ) 2 } 4 , Pt{P(OC 6 H 5 )(OC 2 H 5 ) 2 } 4 , Pt {P(C 6 H 5 ) 2 (OC 2 H 5 )} 4 , Pt{P(CH 3 ) 2 (OC 4 H 9 )} 4 ) and the like, and alcohol, isopropyl alcohol, benzene Of course, it may be used after being dispersed in an organic solvent such as xylene.
상기 백금 촉매는 상기 수산기말단 폴리실록산수지 100중량부에 대하여 0.1~5중량부만큼 포함될 수 있는바, 그 함량이 너무 많으면 단가가 높아지고, 그 함량이 너무 적으면 경화 촉진의 효과가 미미하기 때문이다. The platinum catalyst may be included in an amount of 0.1 to 5 parts by weight based on 100 parts by weight of the hydroxyl-terminated polysiloxane resin, because if the content is too large, the unit price increases, and if the content is too small, the effect of accelerating curing is insignificant.
상기 경화제부는 실란 경화제를 포함하는 것이다.The curing agent part includes a silane curing agent.
상기 실란 경화제는 실란트 조성물의 경화를 위한 것으로, 예컨데 메틸트리(에틸메틸케톡심)실란(Methyltri(ethylmethylketoxime)silane), 테트라(메틸 에틸 케토옥심) 실란 등의 옥심계 실란 경화제, 또는 메틸 트리메톡시 실란, 비닐 트리메톡시 실란 등의 알콕시계 실란 경화제를 단독으로, 또는 이들을 2 이상 조합하여 사용할 수 있다.The silane curing agent is for curing the sealant composition, for example, an oxime-based silane curing agent such as methyltri(ethylmethylketoxime)silane, tetra(methyl ethyl ketoxime) silane, or methyl trimethoxy Alkoxy-based silane curing agents such as silane and vinyl trimethoxy silane may be used alone or in combination of two or more thereof.
아울러, 상기 경화제부는 충전제, 가소제를 소량 더 포함할 수 있는 것으로, 상기 충전제 및 가소제는 주제부와 동일한 것이 사용될 수 있다. 아울러 그 사용량은 상기 실란 경화제와 충전제가 1:0.1~1 중량비, 상기 실란 경화제와 가소제가 1:0.01~0.05 중량비 정도이면 족하다.In addition, the curing agent part may further include a small amount of a filler and a plasticizer, and the filler and plasticizer may be the same as those of the main part. In addition, the amount of the silane curing agent and the filler is 1: 0.1 to 1 weight ratio, the silane curing agent and the plasticizer is about 1: 0.01 to 0.05 weight ratio is sufficient.
한편, 본 발명의 실란트 조성물은 첨가제로, 상기 주제부 내에 접착증진제를 더 포함함이 바람직하다.Meanwhile, the sealant composition of the present invention preferably further includes an adhesion promoter in the main portion as an additive.
상기 접착증진제는 실란트 조성물의 접착성을 개선하기 위한 것으로, 아미노실란, 알콕시실란 또는 알콕시실란들, 예시적으로 n-아미노에틸-아미노프로필트리메톡시 실란을 사용할 수 있다. 이러한 접착증진제는 공지의 성분으로 상업적으로 입수 가능하다.The adhesion promoter is for improving the adhesion of the sealant composition, and aminosilane, alkoxysilane or alkoxysilanes, exemplarily n-aminoethyl-aminopropyltrimethoxy silane may be used. These adhesion promoters are commercially available as well-known components.
상기 접착증진제는 상기 수산기말단 폴리실록산수지 100중량부를 기준으로, 1~5중량부만큼 포함됨이 바람직하다.The adhesion promoter is preferably included by 1 to 5 parts by weight based on 100 parts by weight of the hydroxyl-terminated polysiloxane resin.
또한, 본 발명은 상기 주제부 내 보론 카바이드(B4C; boron carbide)를 더 포함하는 것이 바람직하다.In addition, the present invention preferably further comprises boron carbide (B 4 C; boron carbide) in the main part.
상기 보론 카바이드는 일반적으로 붕소와 탄소의 화합물을 2800℃로 가열하여 만들어지며, 경도가 높으며, 열팽창율이 적고 화학적으로 안정하다. 보론 카바이드는 산소와의 결합을 차단하여 내화성을 증진시킨다. The boron carbide is generally made by heating a compound of boron and carbon at 2800° C., has high hardness, low thermal expansion rate, and is chemically stable. Boron carbide enhances fire resistance by blocking the bond with oxygen.
이러한 보론 카바이드는 상기 상기 수산기말단 폴리실록산수지 100중량부에 대하여 10~20중량부로 포함됨이 바람직하다.The boron carbide is preferably included in an amount of 10 to 20 parts by weight based on 100 parts by weight of the hydroxyl-terminated polysiloxane resin.
또한, 본 발명은 상기 주제부 내 규산지르코늄을 더 포함하는 것이 바람직하다.In addition, the present invention preferably further comprises zirconium silicate in the main portion.
상기 규산지르코늄(ZrSiO4)은 화학조성은 ZrO2 672%, SiO2 328%이며, 소량의 Al2O3, Fe2O3, TiO2가 함유되어 있는 것이다. 또한, 내화도는 약 2500℃이며, 1800℃ 이상에서 분해되어 실리카 증기가 생성되는 것으로, 내화성이 우수하며, 실란트 조성물의 물성 역시 개선해준다.The zirconium silicate (ZrSiO 4 ) has a chemical composition of 672% ZrO 2 and 328% SiO 2 , and contains a small amount of Al 2 O 3 , Fe 2 O 3 , and TiO 2 . In addition, the fire resistance is about 2500 ° C, decomposition at 1800 ° C or higher to generate silica vapor, excellent fire resistance, and also improves the physical properties of the sealant composition.
이러한 규산지르코늄는 상기 상기 수산기말단 폴리실록산수지 100중량부에 대하여 10~20중량부로 포함됨이 바람직하다.The zirconium silicate is preferably included in an amount of 10 to 20 parts by weight based on 100 parts by weight of the hydroxyl-terminated polysiloxane resin.
한편, 상기 주제부는 내화 첨가제로 폴리에테르이미드 나노섬유 1~5중량부 및 난연처리된 면섬유 분말 1~5중량부를 더 포함하는 것이 바람직하다. On the other hand, the main component preferably further includes 1 to 5 parts by weight of polyetherimide nanofibers and 1 to 5 parts by weight of flame retardant treated cotton fiber powder as fireproof additives.
상기 폴리에테르이미드(Polyetherimide) 나노섬유는 폴리에테르이미드(Polyetherimide)를 전기방사하여 제조되는 것으로, 내화성이 우수하여 실란트 조성물의 접착성, 수밀성 등을 저해하지 않으면서도, 방화특성을 향상시킨다. 이러한 폴리에테르이미드 나노섬유는 그 입도가 50~400nm임이 바람직하다.The polyetherimide nanofibers are prepared by electrospinning polyetherimide, and have excellent fire resistance, thereby improving fire resistance without impairing adhesion and watertightness of the sealant composition. These polyetherimide nanofibers preferably have a particle size of 50 to 400 nm.
상기 난연처리된 면섬유 분말은 내화 특성이 저하되지 않도록 하면서도 인장강도를 개선해줌으로써, 백금 촉매로 인한 인장강도의 저하를 방지하는 것이다. The flame retardant treated cotton fiber powder is to prevent a decrease in tensile strength due to a platinum catalyst by improving tensile strength while not reducing fire resistance properties.
상기 난연처리된 면섬유 분말이란, 길이가 1~2mm인 면섬유를 2~3부피배의 3~10중량% 농도의 히드록시 메틸화 포스포노 카르복시 아미드 수용액에 90~100℃에서 30~40분간 침지한 후, 탈수 및 건조하고, 이를 다시 2~3부피배의 3~10중량% 농도의 황산암모늄 수용액에 20~30℃에서 30~40분간 침지한 후, 탈수 및 건조하고, 0.1~100㎛로 분쇄한 것을 의미한다. The flame retardant treated cotton fiber powder is immersed in an aqueous solution of hydroxymethylated phosphonocarboxylic amide at a concentration of 3 to 10% by weight of 2 to 3 times the length of cotton fibers having a length of 1 to 2 mm at 90 to 100 ° C. for 30 to 40 minutes. , dehydrated and dried, and immersed in an aqueous solution of ammonium sulfate at a concentration of 3 to 10% by weight by 2 to 3 times the volume at 20 to 30 ° C for 30 to 40 minutes, dehydrated and dried, and pulverized to 0.1 to 100 μm. means that
한편, 본 발명에서 별다른 설명은 생략되었다면, 각 분말 재료의 입자 크기는 0.1~500㎛ 정도임이 바람직하다.On the other hand, unless otherwise described in the present invention, it is preferable that the particle size of each powder material is about 0.1 to 500 μm.
상기와 같이 구성된 본 발명의 내화 실리콘 실란트 조성물은, 내화 특성이 우수하여, 방화성능이 요구되는 건축용 내, 외장재의 2차 실링재, 글레이징 등으로 사용되어 건축 구조물의 방화성능을 월등히 향상시킬 수 있다는 장점이 있다. The fireproof silicone sealant composition of the present invention constructed as described above has excellent fireproof properties, and is used as a secondary sealing material for building interior and exterior materials requiring fireproof performance, glazing, etc., and can significantly improve the fireproof performance of building structures. there is
이하, 본 발명을 구체적인 실시예를 통해 상세히 설명한다. Hereinafter, the present invention will be described in detail through specific examples.
(실시예 1)(Example 1)
Siloxanes and Silicones, di-Me, hydroxy-terminated(cas no. 70131-67-8) 100중량부, 수산화마그네슘 30중량부, 수산화알루미늄 20중량부, 할로겐계 난연제인 HBCDD 0.05중량부, 인계 난연제인 암모늄 폴리포스테이트 3중량부, 탄소섬유 30중량부, 탄산화 발전회 30중량부, 가소제인 Polydimethylsiloxane 40중량부, 충전제인 규회석 120중량부 및 백금 촉매(Pt{P(OC6H5)3}4) 1중량부를 혼합하여 주제부를 제조하였다.Siloxanes and Silicones, di-Me, hydroxy-terminated (cas no. 70131-67-8) 100 parts by weight, magnesium hydroxide 30 parts by weight, aluminum hydroxide 20 parts by weight, halogen-based flame retardant HBCDD 0.05 parts by weight, phosphorus-based flame retardant ammonium 3 parts by weight of polyphosphate, 30 parts by weight of carbon fiber, 30 parts by weight of carbonation power ash, 40 parts by weight of polydimethylsiloxane as a plasticizer, 120 parts by weight of wollastonite as a filler, and platinum catalyst (Pt{P(OC 6 H 5 ) 3 } 4 ) A main part was prepared by mixing 1 part by weight.
그리고 메틸트리(에틸메틸케톡심)실란과 규회석을 1:0.5 중량비로 혼합하여 경화제부를 제조하였다.Then, methyltri(ethylmethylketoxime)silane and wollastonite were mixed in a weight ratio of 1:0.5 to prepare a curing agent part.
이때, 각 분말 재료의 입도는 0.1~500㎛ 였다.At this time, the particle size of each powder material was 0.1 ~ 500㎛.
그리고 상기 탄소섬유는, 탄소섬유를 질소분위기 하에서 800℃에서 60분간 열처리하고, 상기 열처리된 탄소섬유를 3부피배의 10중량% 농도의 인산암모늄 수용액에 25℃의 온도에서 30분간 침지한 후, 실온에서 건조하고, 0.1~100㎛로 분쇄하여 제조하였다.In addition, the carbon fiber is heat treated at 800 ° C. for 60 minutes under a nitrogen atmosphere, and the heat-treated carbon fiber is immersed in an aqueous solution of ammonium phosphate at a concentration of 10% by weight at 25 ° C. for 30 minutes. It was prepared by drying at room temperature and pulverizing to 0.1 to 100 μm.
또한, 상기 탄산화 발전회는, 발전회에 물을 1:2중량비로 혼합하고, 이에 이산화탄소를 pH가 9.5가 될때까지 주입한 후, 여과한 후, 60℃에서 건조하고, 상기 건조된 건조물을 3부피배의 10중량% 농도의 인산암모늄 수용액에 25℃의 온도에서 30분간 침지한 후, 실온에서 건조하고, 0.1~100㎛로 분쇄하여 제조하였다.In addition, in the carbonation power generation ash, water is mixed with power generation ash at a weight ratio of 1:2, carbon dioxide is injected until the pH is 9.5, filtered, and dried at 60 ° C., and the dried product is 3 It was prepared by immersing in a 10% by volume aqueous solution of ammonium phosphate at a temperature of 25° C. for 30 minutes, drying at room temperature, and pulverizing to 0.1 to 100 μm.
그리고 주제부와 경화제부를 10:1부피비로 혼합하여 실란트 조성물을 제조하였다.Then, a sealant composition was prepared by mixing the main part and the curing agent part in a volume ratio of 10:1.
(실시예 2)(Example 2)
실시예 1과 동일하게 실시하되, 주제부 내 내화 첨가제로 0.1~500㎛의 보론 카바이드 15중량부 및 0.1~500㎛의 규산지르코늄 15중량부을 더 혼합하였다.It was carried out in the same manner as in Example 1, but 15 parts by weight of boron carbide of 0.1 to 500 μm and 15 parts by weight of zirconium silicate of 0.1 to 500 μm were further mixed as fireproofing additives in the main part.
(실시예 3)(Example 3)
실시예 2와 동일하게 실시하되, 상기 충전제로 규회석과 세륨산화물을 1:1 중량비로 혼합하였다. It was carried out in the same manner as in Example 2, but wollastonite and cerium oxide were mixed in a weight ratio of 1:1 as the filler.
(실시예 4)(Example 4)
실시예 3과 동일하게 실시하되, 상기 주제부 내 0.1~500㎛의 난연처리된 면섬유 분말 3중량부 및 50~400nm의 폴리에테르이미드 나노섬유 3중량부를 더 혼합하였다.It was carried out in the same manner as in Example 3, but 3 parts by weight of flame retardant treated cotton fiber powder of 0.1 to 500 μm and 3 parts by weight of polyetherimide nanofibers of 50 to 400 nm were further mixed in the main part.
이때, 상기 난연처리된 면섬유 분말은 길이가 1mm인 면섬유를 2부피배의 5중량% 농도의 히드록시 메틸화 포스포노 카르복시 아미드 수용액에 100℃에서 30분간 침지한 후, 탈수 및 함수율 5%로 건조하고, 이를 다시 2부피배의 5%농도의 황산암모늄 수용액에 25℃에서 30분간 침지한 후, 탈수 및 함수율 5%로 건조하고, 0.1~100㎛로 분쇄하여 제조하였다.At this time, the flame retardant treated cotton fiber powder is immersed in an aqueous solution of 5% by weight of hydroxymethylated phosphonocarboxamide at 100 ° C. for 30 minutes by 2 times the length of cotton fibers having a length of 1 mm, and then dehydrated and dried at a moisture content of 5% , It was again immersed in 2 volume times 5% concentration of ammonium sulfate aqueous solution at 25 ° C. for 30 minutes, dehydrated, dried to a water content of 5%, and prepared by grinding to a size of 0.1 to 100 μm.
(비교예 1)(Comparative Example 1)
실시예 1과 동일하게 실시하되, 탄소섬유 및 탄산화 발전회를 사용하지 않았다.It was carried out in the same way as in Example 1, but carbon fiber and carbonation power generation ash were not used.
(비교예 2)(Comparative Example 2)
실시예 1과 동일하게 실시하되, 탄소섬유를 사용하지 않았다.It was carried out in the same way as in Example 1, but carbon fiber was not used.
(비교예 3)(Comparative Example 3)
실시예 1과 동일하게 실시하되, 탄산화 발전회를 사용하지 않았다.It was carried out in the same manner as in Example 1, but carbonation power generation ash was not used.
(시험예 1)(Test Example 1)
3장의 5mm 유리와 2층의 공간이 있는 복층 강화유리에 실란트 조성물을 7mm의 두께로 주입하고, 실온에서 10시간 경화시켜 방화유리 조립체를 제작하였다.A sealant composition was injected to a thickness of 7 mm into three sheets of 5 mm glass and double-layered tempered glass having two layers of space, and cured at room temperature for 10 hours to prepare a fireproof glass assembly.
그리고 KS F 2845:2013에 따라 내화시험을 실시하였다. 차염성 및 차열성의 시험시간 기준은 60분이며, 60분에 시험이 자동 종료되므로 60분 미만이면 성능미달임을 의미한다. 그 결과는 하기 표 1에 나타내었다.And a fire resistance test was conducted according to KS F 2845:2013. The test time standard for flame and heat shielding properties is 60 minutes, and since the test is automatically terminated at 60 minutes, less than 60 minutes means poor performance. The results are shown in Table 1 below.
상기 표 1에서와 같이, 본 발명의 실시예 1 내지 4는 모두 차염성 및 차열성 평가기준인 60분을 초과하여 그 성능이 우수하나, 비교예 1 내지 3은 평가기준에 도달하지 못함을 확인하였다.As shown in Table 1, Examples 1 to 4 of the present invention are all excellent in performance by exceeding 60 minutes, which is the evaluation standard for flame and heat shielding properties, but Comparative Examples 1 to 3 confirm that they do not reach the evaluation criteria. did
(시험예 2)(Test Example 2)
그리고 실시예 1 내지 4 및 비교예 1 내지 3의 인장 강도, 접착성을 테스트하고, 그 결과를 하기 표 2에 나타내었다.And the tensile strength and adhesiveness of Examples 1 to 4 and Comparative Examples 1 to 3 were tested, and the results are shown in Table 2 below.
접착강도: 전착강판(폭 25 mm, 길이 150 mm) 두 장 사이에 실란트를 폭과 넓이를 각각 25mm 두께를 3mm로 하여 실온에서 7일간 경화한 후 만능인장시험기(UTM)로 접착강도를 구하였다.Bonding strength: Sealant between two electrodeposited steel plates (25 mm wide, 150 mm long) was cured at room temperature for 7 days with the width and width of 25 mm and the thickness of 3 mm, respectively, and then the adhesive strength was obtained with a universal tensile tester (UTM). .
인장강도: 실란트의 두께를 3mm로 하여 실온에서 7일간 경화한 후 아령형 3 호로 시험편을 만들고, 만능인장시험기(UTM)로 인장강도를 구하였다.Tensile strength: After curing the sealant at room temperature for 7 days with a thickness of 3 mm, a test piece was made with a dumbbell type No. 3, and the tensile strength was obtained with a universal tensile testing machine (UTM).
상기 표 2에서와 같이, 본 발명의 실시예 1 내지 4는 비교예 1 내지 3에 비해 인장강도가 우수함을 확인할 수 있었다. 다만, 접착성에 있어서는 큰 차이는 없었다.As shown in Table 2, it was confirmed that Examples 1 to 4 of the present invention had superior tensile strength compared to Comparative Examples 1 to 3. However, there was no significant difference in adhesiveness.
(시험예 3)(Test Example 3)
TGA(Thermo-Gravimetric Analysis)를 이용하여 실시예 1 내지 4 및 비교예 1 내지 3의 내열성을 평가하였다. 열분해 온도는 초기 무게의 5%가 감소되는 온도를 초기 분해온도로 하여 중량 감소율을 비교하였으며, 그 결과는 하기 표 3에 나타내었다.Heat resistance of Examples 1 to 4 and Comparative Examples 1 to 3 was evaluated using TGA (Thermo-Gravimetric Analysis). Regarding the thermal decomposition temperature, the weight loss rate was compared by setting the temperature at which 5% of the initial weight is reduced as the initial decomposition temperature, and the results are shown in Table 3 below.
상기 표 3에서와 같이, 본 발명의 실시예 1 내지 4는 비교예 1 내지 3에 비해 내열성이 우수함을 확인할 수 있었다.As shown in Table 3, it was confirmed that Examples 1 to 4 of the present invention had excellent heat resistance compared to Comparative Examples 1 to 3.
이상 설명한 내용을 통해 당업자라면 본 발명의 기술사상을 일탈하지 아니하는 범위에서 다양한 변경 및 수정 가능함을 알 수 있을 것이다. 따라서, 본 발명의 기술적 범위는 명세서의 상세한 설명에 기재된 내용으로 한정되는 것이 아니라 특허청구범위에 의해 정해져야만 할 것이다.Through the above description, those skilled in the art will know that various changes and modifications are possible without departing from the technical spirit of the present invention. Therefore, the technical scope of the present invention is not limited to the contents described in the detailed description of the specification, but should be defined by the claims.
Claims (5)
실란 경화제를 포함하는 경화제부;의 2액형으로 구성되되,
상기 충전제는 규회석을 포함하는 것을 특징으로 하는 2액형 복층유리용 2차 실링 내화 실리콘 실란트 조성물.
Hydroxyl-terminated polysiloxane resin 100 parts by weight, magnesium hydroxide 10-50 parts by weight, aluminum hydroxide 10-30 parts by weight, halogen-based flame retardant 0.01-0.1 parts by weight, phosphorus-based flame retardant 1-5 parts by weight, carbon fiber 10-50 parts by weight, carbonation A main part containing 10 to 50 parts by weight of power generation ash, 20 to 50 parts by weight of a plasticizer, 100 to 150 parts by weight of a filler, and 0.1 to 5 parts by weight of a platinum catalyst;
It is composed of a two-component type of; a curing agent part containing a silane curing agent,
The filler is a secondary sealing fire-resistant silicone sealant composition for two-component double-glazed glass, characterized in that it comprises wollastonite.
상기 탄소섬유는,
탄소섬유를 질소분위기 하에서 600~1000℃에서 30~100분간 열처리하고,
상기 열처리된 탄소섬유를 인산염 수용액에 30~40분간 침지한 후, 건조하고 0.1~100㎛로 분쇄한 것임을 특징으로 하는 2액형 복층유리용 2차 실링 내화 실리콘 실란트 조성물.
According to claim 1,
The carbon fiber,
The carbon fiber is heat treated at 600 to 1000 ° C for 30 to 100 minutes in a nitrogen atmosphere,
Secondary sealing fire-resistant silicone sealant composition for two-component double-glazed glass, characterized in that the heat-treated carbon fiber is immersed in an aqueous phosphate solution for 30 to 40 minutes, dried and pulverized to 0.1 to 100 μm.
상기 탄산화 발전회는,
발전회에 물을 혼합하고, 이에 이산화탄소를 pH 9~10이 되도록 주입한 후, 여과, 건조하고,
상기 건조된 건조물을 인산염 수용액에 30~40분간 침지한 후, 건조하고 0.1~100㎛로 분쇄한 것임을 특징으로 하는 2액형 복층유리용 2차 실링 내화 실리콘 실란트 조성물.
According to claim 1,
The carbonation development meeting,
After mixing water with the power generation ash, injecting carbon dioxide to the pH 9-10, filtering and drying,
Secondary sealing fire-resistant silicone sealant composition for two-component double-glazed glass, characterized in that the dried product is immersed in an aqueous phosphate solution for 30 to 40 minutes, dried and pulverized to 0.1 to 100 μm.
상기 주제부는,
보론 카바이드 10~20중량부 및 규산지르코늄 10~20중량부를 더 포함하는 것을 특징으로 하는 2액형 복층유리용 2차 실링 내화 실리콘 실란트 조성물.
According to any one of claims 1 to 3,
The subject part,
A secondary sealing refractory silicone sealant composition for two-component double-glazed glass, further comprising 10 to 20 parts by weight of boron carbide and 10 to 20 parts by weight of zirconium silicate.
상기 충전제는 세륨산화물을 더 포함하고,
상기 주제부는,
폴리에테르이미드 나노섬유 1~5중량부 및 난연처리된 면섬유 분말 1~5중량부를 더 포함하는 것을 특징으로 하는 2액형 복층유리용 2차 실링 내화 실리콘 실란트 조성물.According to claim 4,
The filler further includes cerium oxide,
The subject part,
A secondary sealing fireproof silicone sealant composition for two-component double-glazed glass, characterized in that it further comprises 1 to 5 parts by weight of polyetherimide nanofibers and 1 to 5 parts by weight of flame retardant treated cotton fiber powder.
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