KR102658779B1 - Flame retardant paint and waterproof paint composition and method for producing the same - Google Patents
Flame retardant paint and waterproof paint composition and method for producing the same Download PDFInfo
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- KR102658779B1 KR102658779B1 KR1020240010842A KR20240010842A KR102658779B1 KR 102658779 B1 KR102658779 B1 KR 102658779B1 KR 1020240010842 A KR1020240010842 A KR 1020240010842A KR 20240010842 A KR20240010842 A KR 20240010842A KR 102658779 B1 KR102658779 B1 KR 102658779B1
- Authority
- KR
- South Korea
- Prior art keywords
- weight
- parts
- monomer units
- flame retardant
- melamine
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- 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 title claims abstract description 51
- 239000003063 flame retardant Substances 0.000 title claims abstract description 46
- 239000003973 paint Substances 0.000 title claims abstract description 41
- 239000000203 mixture Substances 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 65
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229920002050 silicone resin Polymers 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 23
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 23
- 239000010439 graphite Substances 0.000 claims abstract description 23
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229920005989 resin Polymers 0.000 claims abstract description 21
- 239000011347 resin Substances 0.000 claims abstract description 21
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 20
- 239000004114 Ammonium polyphosphate Substances 0.000 claims abstract description 19
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims abstract description 19
- 229920001276 ammonium polyphosphate Polymers 0.000 claims abstract description 19
- 239000005038 ethylene vinyl acetate Substances 0.000 claims abstract description 18
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims abstract description 18
- 239000008213 purified water Substances 0.000 claims abstract description 18
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 17
- 239000000178 monomer Substances 0.000 claims description 60
- 229910021389 graphene Inorganic materials 0.000 claims description 42
- 239000000835 fiber Substances 0.000 claims description 40
- 239000008199 coating composition Substances 0.000 claims description 23
- 239000002131 composite material Substances 0.000 claims description 19
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 16
- 239000011248 coating agent Substances 0.000 claims description 16
- 238000000576 coating method Methods 0.000 claims description 16
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- -1 polydimethylsiloxane Polymers 0.000 claims description 13
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 10
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 10
- RGAHQVPQZZNNOV-UHFFFAOYSA-N 2-diethoxyphosphorylethyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCP(=O)(OCC)OCC RGAHQVPQZZNNOV-UHFFFAOYSA-N 0.000 claims description 9
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 9
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 9
- RZMWTGFSAMRLQH-UHFFFAOYSA-L disodium;2,2-dihexyl-3-sulfobutanedioate Chemical compound [Na+].[Na+].CCCCCCC(C([O-])=O)(C(C([O-])=O)S(O)(=O)=O)CCCCCC RZMWTGFSAMRLQH-UHFFFAOYSA-L 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 8
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 8
- 239000002105 nanoparticle Substances 0.000 claims description 8
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 8
- 239000011787 zinc oxide Substances 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 7
- UOKUUKOEIMCYAI-UHFFFAOYSA-N trimethoxysilylmethyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)COC(=O)C(C)=C UOKUUKOEIMCYAI-UHFFFAOYSA-N 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 4
- 238000003763 carbonization Methods 0.000 description 4
- 230000001112 coagulating effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000000704 physical effect Effects 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 238000004078 waterproofing Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003929 acidic solution Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002341 toxic gas Substances 0.000 description 2
- IHCCLXNEEPMSIO-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperidin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 IHCCLXNEEPMSIO-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- 206010003497 Asphyxia Diseases 0.000 description 1
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- 230000004308 accommodation Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 239000003864 humus Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- 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
- C09D123/00—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers
- C09D123/02—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D123/04—Homopolymers or copolymers of ethene
- C09D123/08—Copolymers of ethene
- C09D123/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
- C09D123/0853—Vinylacetate
-
- 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
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with 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
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
-
- 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
- C09D143/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing boron, silicon, phosphorus, selenium, tellurium, or a metal; Coating compositions based on derivatives of such polymers
- C09D143/04—Homopolymers or copolymers of monomers containing silicon
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/80—Processes for incorporating ingredients
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
본 발명은 에틸렌비닐아세테이트 공중합체 수지, 실리콘 수지, 팽창흑연, 멜라민, 멜라민시아누레이트, 수산화알루미늄, 펜타에리트리톨, 암모늄폴리인산염, 이산화티타늄 및 정제수를 포함하는 방염 및 방수 도료 조성물을 제공한다.The present invention provides a flame retardant and waterproof paint composition containing ethylene vinyl acetate copolymer resin, silicone resin, expanded graphite, melamine, melamine cyanurate, aluminum hydroxide, pentaerythritol, ammonium polyphosphate, titanium dioxide, and purified water.
Description
본 발명은 방염도료 및 방수도료 조성물 및 이의 제조방법에 관한 것이다.The present invention relates to flame retardant paint and waterproof paint compositions and methods for producing the same.
일반적으로, 방염처리는 건물 및 지하시설물의 내부, 외부 재질에 화재의 발생과 확산을 원천적으로 봉쇄하는 물질로 표면을 처리하는 것으로, 화재의 발생과 확산을 저지하여 안전을 도모하도록 한다.In general, flame retardant treatment refers to surface treatment of the interior and exterior materials of buildings and underground facilities with materials that fundamentally block the occurrence and spread of fire, thereby promoting safety by preventing the occurrence and spread of fire.
현대와 같이, 고층빌딩의 증가, 지하철과 같은 지하시설물의 확충 및 주택의 밀집 등에 의해 화재가 발생하면 대형으로 확산되기 쉽고, 화재 발생장소의 접근이 어려워 화재진압에 어려움이 있으며, 화재발생 지역에서 대피하기도 어려워 인명피해가 많이 발생되는 문제점이 있었다.In modern times, when a fire breaks out due to the increase in high-rise buildings, the expansion of underground facilities such as subways, and the density of houses, it is easy to spread to a large scale, and it is difficult to extinguish the fire due to the difficult access to the place where the fire occurred. There was a problem that it was difficult to evacuate and many casualties occurred.
이에, 화재를 관리하는 소방법은 화재의 발생과 확산을 저지하도록 방염처리대상을 법으로 지정하여 방염 선처리 대상품인 각종 설치 막, 신내 장시물 및 카펫트 등은 제조 또는 생산과정에서 방염처리를 하거나, 난연성 소재로 제조 또는 생산하도록 규정하고 있다Accordingly, the Fire Protection Act that manages fires legally designates flame retardant treatment targets to prevent the occurrence and spread of fire, and various installation membranes, new interior decorations, and carpets, which are subject to flame retardant treatment, must be flame retardant treated during the manufacturing or production process. It is stipulated that it must be manufactured or produced with flame retardant materials.
이러한 정책적 노력에도 불구하고 많은 건물들은 아직 고온의 열과 화염에 약하며, 특히 냉동 창고, 휘발성 물질을 다루는 곳, 또는 전력구와 같은 화재 발생시 진압이 거의 불가능한 곳은 일반적인 방염도료나 방염페인트로는 화재의 정도를 줄이지 못한다.Despite these policy efforts, many buildings are still vulnerable to high-temperature heat and flames, especially in places where it is almost impossible to extinguish a fire in the event of a fire, such as a refrigerated warehouse, a place where volatile substances are handled, or a power outlet. cannot be reduced.
방염이 잘되는 도료는 화염과 고온의 열을 막을 수 있지만 방염 성분의 연소로 유독가스가 방출되어 인명 구조 시 더 어려운 상황을 만들게 된다. 즉, 화재 시 화염으로 인한 인명사고보다 유독가스로 인한 질식사고가 더 많음으로 방염도료 선택시 이를 고려해야 한다. 또한 방염이 잘되는 물질이 있어도 근본 열을 차단하지 못함으로 전도된 열은 피도포면 물체의 변형을 일으키고 내부화재를 발생하게 한다.Paints that are highly flame retardant can block flames and high temperatures, but combustion of flame retardant components releases toxic gases, creating a more difficult situation when rescuing people. In other words, since there are more suffocation accidents caused by toxic gases than fatal accidents caused by flames during a fire, this must be taken into consideration when selecting a flame retardant paint. In addition, even if there is a material that is good at flame retardancy, it does not block the fundamental heat, so the conducted heat causes deformation of the coated object and causes internal fire.
또한, 내부로 전달된 열은 쉽게 방출되지 않으므로 건축물의 골격의 근간이 되는 H빔을 녹게 하여 건물의 붕괴를 일으키게 한다.Additionally, since the heat transferred inside is not easily released, it melts the H-beams that form the basis of the building's skeleton, causing the building to collapse.
특히 다양한 생활의 변화로 숙박시설과 공공시설이 늘어나면서 화재 발생 시 유기 방염물질이 오히려 더 많은 인명피해를 일으키는 것으로 밝혀짐에 따라 근래에는 무기 또는 수성으로 방염물질을 연구하는 추세이다.In particular, as the number of accommodations and public facilities increases due to various changes in life, organic flame retardants have been found to cause more casualties in the event of a fire, so in recent years, there has been a trend to research inorganic or water-based flame retardants.
본 발명은 상기와 같은 문제점을 해결하기 위해 안출된 것으로서, 본 발명의 목적은 방염 및 방수 기능성 도료 조성물을 제공하는 것이다.The present invention was devised to solve the above problems, and the purpose of the present invention is to provide a flame retardant and waterproof functional paint composition.
본 발명의 과제는 이상에서 언급한 과제들로 제한되지 않으며, 언급되지 않은 또 다른 과제들은 아래의 기재로부터 당업자에게 명확하게 이해될 수 있을 것이다.The object of the present invention is not limited to the problems mentioned above, and other problems not mentioned will be clearly understood by those skilled in the art from the description below.
상기 목적을 달성하기 위하여 본 발명은In order to achieve the above object, the present invention
에틸렌비닐아세테이트 공중합체 수지, 실리콘 수지, 팽창흑연, 멜라민, 멜라민시아누레이트, 수산화알루미늄, 펜타에리트리톨, 암모늄폴리인산염, 이산화티타늄 및 정제수를 포함하는 방염 및 방수 도료 조성물을 제공한다.Provided is a flame retardant and waterproof paint composition containing ethylene vinyl acetate copolymer resin, silicone resin, expanded graphite, melamine, melamine cyanurate, aluminum hydroxide, pentaerythritol, ammonium polyphosphate, titanium dioxide, and purified water.
또한, 상기 방염 및 방수 도료 조성물은 에틸렌비닐아세테이트 공중합체 수지 39-41 중량부, 실리콘 수지 10-12 중량부, 팽창흑연 11-13 중량부, 그래핀 복합섬유 3-5 중량부, 멜라민 2-3 중량부, 멜라민시아누레이트 2-4 중량부, 수산화알루미늄 1-3 중량부, 펜타에리트리톨 2-3 중량부, 암모늄폴리인산염 4-6 중량부, 이산화티타늄 0.8-1.2 중량부 및 정제수 17-19 중량부를 포함하고,In addition, the flame retardant and waterproof paint composition includes 39-41 parts by weight of ethylene vinyl acetate copolymer resin, 10-12 parts by weight of silicone resin, 11-13 parts by weight of expanded graphite, 3-5 parts by weight of graphene composite fiber, and 2-500 parts by weight of melamine. 3 parts by weight, melamine cyanurate 2-4 parts by weight, aluminum hydroxide 1-3 parts by weight, pentaerythritol 2-3 parts by weight, ammonium polyphosphate 4-6 parts by weight, titanium dioxide 0.8-1.2 parts by weight and purified water 17 Contains -19 parts by weight,
상기 실리콘 수지는 메틸트리메톡시실란 단량체 단위 38-42 중량부, 비닐트리메톡시실란 단량체 단위 38-42 중량부 및 (트리메톡시실릴)메틸 메타크릴레이트((trimethoxysilyl)methyl methacrylate) 단량체 단위 28-32 중량부를 포함하고,The silicone resin contains 38-42 parts by weight of methyltrimethoxysilane monomer units, 38-42 parts by weight of vinyltrimethoxysilane monomer units, and 28 parts by weight of (trimethoxysilyl)methyl methacrylate monomer units. Contains -32 parts by weight,
상기 그래핀 복합섬유는,The graphene composite fiber,
메틸트리에톡시실란 단량체 단위 48-52 중량부, 비닐트리에톡시실란 단량체 단위 23-27 중량부 및 (2-디에틸포스페이토에틸)트리에톡시실란((2-Diethylphosphatoethyl)triethoxysilane) 단량체 단위 23-27 중량부를 포함하는 실리콘 수지 68-72 중량부, 폴리디메틸실록산 15-19 중량부, 소듐디헥실술포숙시네이트 3-7 중량부, 산화아연 나노입자 3-7 중량부, 트리스(2,4-디-터트-부틸페닐) 포스파이트(Tris(2,4-di-tert-butylphenyl) phosphite) 0.8-1.2 중량부, 에틸렌비스(스테아르산 아미드)(Ethylenebis(stearamide)) 0.8-1.2 중량부 및 백금계 촉매 0.8-1.2 중량부를 혼합하고, 38-42℃의 온도에서 400-600 rpm의 회전속도로 교반하여 코팅조성물을 제조하는 단계; 그래핀섬유에 상기 코팅조성물을 코팅하는 단계; 및 코팅조성물이 코팅된 그래핀섬유를 160-180℃의 온도에서 건조 및 경화시키는 단계;를 수행하여 제조되는 것을 특징으로 한다.48-52 parts by weight of methyltriethoxysilane monomer units, 23-27 parts by weight of vinyltriethoxysilane monomer units and (2-Diethylphosphatoethyl)triethoxysilane monomer units 68-72 parts by weight of silicone resin containing 23-27 parts by weight, 15-19 parts by weight of polydimethylsiloxane, 3-7 parts by weight of sodium dihexyl sulfosuccinate, 3-7 parts by weight of zinc oxide nanoparticles, Tris (2, 4-di-tert-butylphenyl) phosphite (Tris(2,4-di-tert-butylphenyl) phosphite) 0.8-1.2 parts by weight, ethylenebis(stearamide) 0.8-1.2 parts by weight and 0.8-1.2 parts by weight of a platinum-based catalyst, and stirring at a rotation speed of 400-600 rpm at a temperature of 38-42° C. to prepare a coating composition; Coating the coating composition on graphene fibers; And drying and curing the graphene fiber coated with the coating composition at a temperature of 160-180°C.
또한, 본 발명은In addition, the present invention
메틸트리에톡시실란 단량체 단위 48-52 중량부, 비닐트리에톡시실란 단량체 단위 23-27 중량부 및 (2-디에틸포스페이토에틸)트리에톡시실란((2-Diethylphosphatoethyl)triethoxysilane) 단량체 단위 23-27 중량부를 포함하는 실리콘 수지 68-72 중량부, 폴리디메틸실록산 15-19 중량부, 소듐디헥실술포숙시네이트 3-7 중량부, 산화아연 나노입자 3-7 중량부, 트리스(2,4-디-터트-부틸페닐) 포스파이트(Tris(2,4-di-tert-butylphenyl) phosphite) 0.8-1.2 중량부, 에틸렌비스(스테아르산 아미드)(Ethylenebis(stearamide)) 0.8-1.2 중량부 및 백금계 촉매 0.8-1.2 중량부를 혼합하고, 38-42℃의 온도에서 400-600 rpm의 회전속도로 교반하여 코팅조성물을 제조하는 단계; 그래핀섬유에 상기 코팅조성물을 코팅하는 단계; 및 코팅조성물이 코팅된 그래핀섬유를 160-180℃의 온도에서 건조 및 경화시키는 단계;를 포함하는 그래핀 복합섬유를 제조하는 단계; 및48-52 parts by weight of methyltriethoxysilane monomer units, 23-27 parts by weight of vinyltriethoxysilane monomer units and (2-Diethylphosphatoethyl)triethoxysilane monomer units 68-72 parts by weight of silicone resin containing 23-27 parts by weight, 15-19 parts by weight of polydimethylsiloxane, 3-7 parts by weight of sodium dihexyl sulfosuccinate, 3-7 parts by weight of zinc oxide nanoparticles, Tris (2, 4-di-tert-butylphenyl) phosphite (Tris(2,4-di-tert-butylphenyl) phosphite) 0.8-1.2 parts by weight, ethylenebis(stearamide) 0.8-1.2 parts by weight and 0.8-1.2 parts by weight of a platinum-based catalyst, and stirring at a rotation speed of 400-600 rpm at a temperature of 38-42° C. to prepare a coating composition; Coating the coating composition on graphene fibers; And drying and curing the graphene fiber coated with the coating composition at a temperature of 160-180°C; manufacturing a graphene composite fiber including; and
에틸렌비닐아세테이트 공중합체 수지 39-41 중량부, 메틸트리메톡시실란 단량체 단위 38-42 중량부, 비닐트리메톡시실란 단량체 단위 38-42 중량부 및 (트리메톡시실릴)메틸 메타크릴레이트((trimethoxysilyl)methyl methacrylate) 단량체 단위 28-32 중량부를 포함하는 실리콘 수지 10-12 중량부, 팽창흑연 11-13 중량부, 상기 그래핀 복합섬유 3-5 중량부, 멜라민 2-3 중량부, 멜라민시아누레이트 2-4 중량부, 수산화알루미늄 1-3 중량부, 펜타에리트리톨 2-3 중량부, 암모늄폴리인산염 4-6 중량부, 이산화티타늄 0.8-1.2 중량부 및 정제수 17-19 중량부를 혼합하고, 5℃ 이상의 온도에서 800-1200 rpm의 회전속도로 교반하는 단계;를 포함하는 방염 및 방수 도료 조성물의 제조방법을 제공한다.39-41 parts by weight of ethylene vinyl acetate copolymer resin, 38-42 parts by weight of methyltrimethoxysilane monomer units, 38-42 parts by weight of vinyltrimethoxysilane monomer units, and (trimethoxysilyl)methyl methacrylate (( trimethoxysilyl)methyl methacrylate) 10-12 parts by weight of silicone resin containing 28-32 parts by weight of monomer units, 11-13 parts by weight of expanded graphite, 3-5 parts by weight of the graphene composite fiber, 2-3 parts by weight of melamine, melamine city Mix 2-4 parts by weight of anurate, 1-3 parts by weight of aluminum hydroxide, 2-3 parts by weight of pentaerythritol, 4-6 parts by weight of ammonium polyphosphate, 0.8-1.2 parts by weight of titanium dioxide, and 17-19 parts by weight of purified water. It provides a method for producing a flame retardant and waterproof paint composition comprising: stirring at a rotation speed of 800-1200 rpm at a temperature of 5°C or higher.
본 발명에 따른 방염 및 방수 도료 조성물은 방염 기능성과 방수 기능성을 동시에 가지며, 우수한 특성을 가진다.The flame retardant and waterproof paint composition according to the present invention has both flame retardant functionality and waterproof functionality and has excellent properties.
또한, 본 발명에 따른 방염 및 방수 도료 조성물은 내수성, 내마모성, 인장강도, 신장률 및 인열강도가 우수하다.In addition, the flame retardant and waterproof paint composition according to the present invention has excellent water resistance, abrasion resistance, tensile strength, elongation, and tear strength.
이하에서는 다양한 실시예를 보다 상세하게 설명한다. 본 명세서에 기재된 실시예는 다양하게 변형될 수 있다. 특정한 실시예가 상세한 설명에서 자세하게 설명될 수 있다. 그러나 개시된 특정한 실시 예는 다양한 실시예를 쉽게 이해하도록 하기 위한 것일 뿐이다. 따라서 개시된 특정 실시예에 의해 기술적 사상이 제한되는 것은 아니며, 발명의 사상 및 기술 범위에 포함되는 모든 균등물 또는 대체물을 포함하는 것으로 이해되어야 한다.Hereinafter, various embodiments will be described in more detail. The embodiments described herein may be modified in various ways. Specific embodiments may be described in detail in the detailed description. However, the specific embodiments disclosed are only intended to facilitate understanding of the various embodiments. Accordingly, the technical idea is not limited to the specific embodiments disclosed, and should be understood to include all equivalents or substitutes included in the spirit and technical scope of the invention.
1차, 2차, 제1, 제2 등과 같이 서수를 포함하는 용어는 다양한 구성요소들을 설명하는데 사용될 수 있지만, 이러한 구성요소들은 상술한 용어에 의해 한정되지는 않는다. 상술한 용어는 하나의 구성요소를 다른 구성요소로부터 구별하는 목적으로만 사용된다.Terms containing ordinal numbers, such as primary, secondary, first, second, etc., may be used to describe various components, but these components are not limited by the above-mentioned terms. The above-mentioned terms are used only for the purpose of distinguishing one component from another.
본 명세서에서, '포함한다' 또는 '가지다' 등의 용어는 명세서상에 기재된 특징, 숫자, 단계, 동작, 구성요소, 부품 또는 이들을 조합한 것이 존재함을 지정하려는 것이지, 하나 또는 그 이상의 다른 특징들이나 숫자, 단계, 동작, 구성요소, 부품 또는 이들을 조합한 것들의 존재 또는 부가 가능성을 미리 배제하지 않는 것으로 이해되어야 한다. 어떤 구성요소가 다른 구성요소에 '연결되어' 있다거나 '접속되어' 있다고 언급된 때에는, 그 다른 구성요소에 직접적으로 연결되어 있거나 또는 접속되어 있을 수도 있지만, 중간에 다른 구성요소가 존재할 수도 있다고 이해되어야 할 것이다. 반면에, 어떤 구성요소가 다른 구성요소에 '직접 연결되어' 있다거나 '직접 접속되어' 있다고 언급된 때에는, 중간에 다른 구성요소가 존재하지 않는 것으로 이해되어야 할 것이다.In this specification, terms such as 'include' or 'have' are intended to designate the presence of features, numbers, steps, operations, components, parts, or combinations thereof described in the specification, but are not intended to indicate the presence of one or more other features. It should be understood that this does not exclude in advance the possibility of the existence or addition of elements, numbers, steps, operations, components, parts, or combinations thereof. When a component is said to be 'connected' or 'connected' to another component, it is understood that it may be directly connected or connected to the other component, but that other components may exist in between. It should be. On the other hand, when a component is mentioned as being 'directly connected' or 'directly connected' to another component, it should be understood that there are no other components in between.
그 밖에도, 본 발명을 설명함에 있어서, 관련된 공지 기능 혹은 구성에 대한 구체적인 설명이 본 발명의 요지를 불필요하게 흐릴 수 있다고 판단되는 경우, 그에 대한 상세한 설명은 축약하거나 생략한다.In addition, when describing the present invention, if it is determined that a detailed description of a related known function or configuration may unnecessarily obscure the gist of the present invention, the detailed description thereof is abbreviated or omitted.
본 발명은This invention
에틸렌비닐아세테이트 공중합체 수지, 실리콘 수지, 팽창흑연, 멜라민, 멜라민시아누레이트, 수산화알루미늄, 펜타에리트리톨, 암모늄폴리인산염, 이산화티타늄 및 정제수를 포함하는 방염 및 방수 도료 조성물을 제공한다.Provided is a flame retardant and waterproof paint composition containing ethylene vinyl acetate copolymer resin, silicone resin, expanded graphite, melamine, melamine cyanurate, aluminum hydroxide, pentaerythritol, ammonium polyphosphate, titanium dioxide, and purified water.
이하, 본 발명에 따른 방염 및 방수 도료 조성물에 대하여 상세히 설명한다.Hereinafter, the flame retardant and waterproof paint composition according to the present invention will be described in detail.
상기 방염 및 방수 도료 조성물은 에틸렌비닐아세테이트 공중합체 수지 39-41 중량부, 실리콘 수지 10-12 중량부, 팽창흑연 15-17 중량부, 멜라민 2-3 중량부, 멜라민시아누레이트 2-4 중량부, 수산화알루미늄 1-3 중량부, 펜타에리트리톨 2-3 중량부, 암모늄폴리인산염 4-6 중량부, 이산화티타늄 0.8-1.2 중량부 및 정제수 17-19 중량부를 포함하는 것이 바람직하고, 에틸렌비닐아세테이트 공중합체 수지 39.5-40.5 중량부, 실리콘 수지 10.5-11.5 중량부, 팽창흑연 15.5-16.5 중량부, 멜라민 2.3-2.7 중량부, 멜라민시아누레이트 2.5-3.5 중량부, 수산화알루미늄 1.5-2.5 중량부, 펜타에리트리톨 2.3-2.7 중량부, 암모늄폴리인산염 4.5-5.5 중량부, 이산화티타늄 0.9-1.1 중량부 및 정제수 17.5-18.5 중량부를 포함하는 것이 더욱 바람직하다.The flame retardant and waterproof paint composition includes 39-41 parts by weight of ethylene vinyl acetate copolymer resin, 10-12 parts by weight of silicone resin, 15-17 parts by weight of expanded graphite, 2-3 parts by weight of melamine, and 2-4 parts by weight of melamine cyanurate. parts by weight, 1-3 parts by weight of aluminum hydroxide, 2-3 parts by weight of pentaerythritol, 4-6 parts by weight of ammonium polyphosphate, 0.8-1.2 parts by weight of titanium dioxide, and 17-19 parts by weight of purified water, and ethylene vinyl Acetate copolymer resin 39.5-40.5 parts by weight, silicone resin 10.5-11.5 parts by weight, expanded graphite 15.5-16.5 parts by weight, melamine 2.3-2.7 parts by weight, melamine cyanurate 2.5-3.5 parts by weight, aluminum hydroxide 1.5-2.5 parts by weight , 2.3-2.7 parts by weight of pentaerythritol, 4.5-5.5 parts by weight of ammonium polyphosphate, 0.9-1.1 parts by weight of titanium dioxide, and 17.5-18.5 parts by weight of purified water.
상기 에틸렌비닐아세테이트 공중합체 수지는 부착성, 내구성, 방수성이 우수한 수지로 메인 수지로 적용된다.The ethylene vinyl acetate copolymer resin is a resin with excellent adhesion, durability, and waterproofing properties and is applied as the main resin.
상기 실리콘 수지는 접착성, 내구성, 방수성을 보조하여 주는 보조 수지로 적용된다. The silicone resin is applied as an auxiliary resin that assists in adhesion, durability, and waterproofing.
상기 실리콘 수지는 메틸트리메톡시실란 단량체 단위 38-42 중량부, 비닐트리메톡시실란 단량체 단위 38-42 중량부 및 (트리메톡시실릴)메틸 메타크릴레이트((trimethoxysilyl)methyl methacrylate) 단량체 단위 28-32 중량부를 포함하는 것이 바람직하다. 상기 실리콘 수지는 메틸트리메톡시실란 단량체 단위, 비닐트리메톡시실란 단량체 단위 및 (트리메톡시실릴)메틸 메타크릴레이트((trimethoxysilyl)methyl methacrylate) 단량체 단위를 포함하여 방염 기능성, 난연성을 보조하여 주며, 우수한 접착성, 내구성, 방수성을 확보할 수 있다.The silicone resin contains 38-42 parts by weight of methyltrimethoxysilane monomer units, 38-42 parts by weight of vinyltrimethoxysilane monomer units, and 28 parts by weight of (trimethoxysilyl)methyl methacrylate monomer units. It is preferable to include -32 parts by weight. The silicone resin includes methyltrimethoxysilane monomer units, vinyltrimethoxysilane monomer units, and (trimethoxysilyl)methyl methacrylate monomer units to provide flame retardant functionality and flame retardancy. , excellent adhesion, durability, and waterproofing can be secured.
상기 실리콘 수지는 다음과 같은 방법으로 제조되는 것을 사용한다. 구체적으로, 각 단량체 단위를 제공하기 위한 단량체를 반응기에 첨가하고, 단량체 총 중량의 0.5-1.5배의 유기용제를 첨가한 후, 적정량의 산성 용액을 드로핑하여 pH를 1.0-5.0으로 조절하고, 균일하게 충분히 교반한다. 상기 유기용제는 에탄올, 메탄올, 부탄올, 크실렌, 부틸 아세테이트 또는 아세톤이다. 또한 상기 산성용액은 염산, 황산, 질산, 인산(Phosphoric Acid) 또는 초산용액이다. 다음, 단량체 총 중량의 0.1-1.0배의 물을 첨가하고, 가열하여 60-80℃에서 회류시킨다. 반응하여 단상으로 변하여 완전히 투명하게 되면, 그 상태에서 2-5시간 동안 보온한다. 이후, pH를 5.5-6.5 사이로 조절하고, 고형분 함량의 20 중량%에 해당하는 유기용제를 보충 첨가하고, 냉각시킨 후 여과하여 실리콘 수지를 완성한다.The silicone resin is manufactured using the following method. Specifically, monomers to provide each monomer unit are added to the reactor, 0.5-1.5 times the total weight of the monomer organic solvent is added, and then an appropriate amount of acidic solution is dropped to adjust the pH to 1.0-5.0, Stir thoroughly and uniformly. The organic solvent is ethanol, methanol, butanol, xylene, butyl acetate or acetone. Additionally, the acidic solution is hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, or acetic acid. Next, 0.1-1.0 times the total weight of the monomer was added, heated, and refluxed at 60-80°C. When it reacts and changes into a single phase and becomes completely transparent, keep it warm for 2-5 hours. Afterwards, the pH is adjusted to between 5.5-6.5, an organic solvent equivalent to 20% by weight of the solid content is added, cooled, and filtered to complete the silicone resin.
상기 팽창흑연은 평균입경이 18-25 ㎛이고, 400-500배의 팽창율을 가지며, 밀도가 2.5-3.2 g/cm3인 것을 사용할 수 있다. 상기 팽창흑연은 방염 기능성을 부여하기 위한 난연제로 적용된다.The expanded graphite may have an average particle diameter of 18-25 ㎛, an expansion rate of 400-500 times, and a density of 2.5-3.2 g/cm 3 . The expanded graphite is applied as a flame retardant to provide flame retardant functionality.
상기 멜라민, 멜라민시아누레이트 및 수산화알루미늄은 팽창흑연과 함께 방염 기능성을 부여하기 위한 난연제로 적용된다.The melamine, melamine cyanurate, and aluminum hydroxide are used together with expanded graphite as a flame retardant to provide flame retardant functionality.
상기 팽창흑연, 멜라민, 멜라민시아누레이트, 수산화알루미늄 및 암모늄폴리인산염을 난연제로 적용하되, 15-17:2-3:2-4:1-3:4-6의 중량비율로 적용함으로써 우수한 방염 기능성과 함께 내구성을 확보할 수 있다.The expanded graphite, melamine, melamine cyanurate, aluminum hydroxide, and ammonium polyphosphate are applied as flame retardants, and are applied at a weight ratio of 15-17:2-3:2-4:1-3:4-6 to provide excellent flame retardancy. Durability can be secured along with functionality.
상기 펜타에리트리톨(Pentaerythritol)은 무취, 백색의 결정형 분말로써 윤활유로 활용되어 팽창흑연, 멜라민, 멜라민시아누레이트, 수산화알루미늄 및 암모늄폴리인산염의 분산을 용이하게 하여 우수한 방염 기능성을 확보할 수 있다.Pentaerythritol is an odorless, white crystalline powder that is used as a lubricant to facilitate dispersion of expanded graphite, melamine, melamine cyanurate, aluminum hydroxide, and ammonium polyphosphate, thereby ensuring excellent flame retardant functionality.
또한, 상기 방염 및 방수 도료 조성물은 에틸렌비닐아세테이트 공중합체 수지 39-41 중량부, 실리콘 수지 10-12 중량부, 팽창흑연 11-13 중량부, 그래핀 복합섬유 3-5 중량부, 멜라민 2-3 중량부, 멜라민시아누레이트 2-4 중량부, 수산화알루미늄 1-3 중량부, 펜타에리트리톨 2-3 중량부, 암모늄폴리인산염 4-6 중량부, 이산화티타늄 0.8-1.2 중량부 및 정제수 17-19 중량부를 포함하는 것이 더욱 바람직하고, 에틸렌비닐아세테이트 공중합체 수지 39.5-40.5 중량부, 실리콘 수지 10.5-11.5 중량부, 팽창흑연 11.5-12.5 중량부, 그래핀 복합섬유 3.5-4.5 중량부, 멜라민 2.3-2.7 중량부, 멜라민시아누레이트 2.5-3.5 중량부, 수산화알루미늄 1.5-2.5 중량부, 펜타에리트리톨 2.3-2.7 중량부, 암모늄폴리인산염 4.5-5.5 중량부, 이산화티타늄 0.9-1.1 중량부 및 정제수 17.5-18.5 중량부를 포함하는 것이 가장 바람직하다.In addition, the flame retardant and waterproof paint composition includes 39-41 parts by weight of ethylene vinyl acetate copolymer resin, 10-12 parts by weight of silicone resin, 11-13 parts by weight of expanded graphite, 3-5 parts by weight of graphene composite fiber, and 2-500 parts by weight of melamine. 3 parts by weight, melamine cyanurate 2-4 parts by weight, aluminum hydroxide 1-3 parts by weight, pentaerythritol 2-3 parts by weight, ammonium polyphosphate 4-6 parts by weight, titanium dioxide 0.8-1.2 parts by weight and purified water 17 It is more preferable to include -19 parts by weight, 39.5-40.5 parts by weight of ethylene vinyl acetate copolymer resin, 10.5-11.5 parts by weight of silicone resin, 11.5-12.5 parts by weight of expanded graphite, 3.5-4.5 parts by weight of graphene composite fiber, and melamine. 2.3-2.7 parts by weight, melamine cyanurate 2.5-3.5 parts by weight, aluminum hydroxide 1.5-2.5 parts by weight, pentaerythritol 2.3-2.7 parts by weight, ammonium polyphosphate 4.5-5.5 parts by weight, titanium dioxide 0.9-1.1 parts by weight, and It is most preferable to include 17.5-18.5 parts by weight of purified water.
상기 그래핀 복합섬유는,The graphene composite fiber,
메틸트리에톡시실란 단량체 단위 48-52 중량부, 비닐트리에톡시실란 단량체 단위 23-27 중량부 및 (2-디에틸포스페이토에틸)트리에톡시실란((2-Diethylphosphatoethyl)triethoxysilane) 단량체 단위 23-27 중량부를 포함하는 실리콘 수지 68-72 중량부, 폴리디메틸실록산 15-19 중량부, 소듐디헥실술포숙시네이트 3-7 중량부, 산화아연 나노입자 3-7 중량부, 트리스(2,4-디-터트-부틸페닐) 포스파이트(Tris(2,4-di-tert-butylphenyl) phosphite) 0.8-1.2 중량부, 에틸렌비스(스테아르산 아미드)(Ethylenebis(stearamide)) 0.8-1.2 중량부 및 백금계 촉매 0.8-1.2 중량부를 혼합하고, 38-42℃의 온도에서 400-600 rpm의 회전속도로 교반하여 코팅조성물을 제조하는 단계; 그래핀섬유에 상기 코팅조성물을 코팅하는 단계; 및 코팅조성물이 코팅된 그래핀섬유를 160-180℃의 온도에서 건조 및 경화시키는 단계;를 수행하여 제조되는 것을 사용한다.48-52 parts by weight of methyltriethoxysilane monomer units, 23-27 parts by weight of vinyltriethoxysilane monomer units and (2-Diethylphosphatoethyl)triethoxysilane monomer units 68-72 parts by weight of silicone resin containing 23-27 parts by weight, 15-19 parts by weight of polydimethylsiloxane, 3-7 parts by weight of sodium dihexyl sulfosuccinate, 3-7 parts by weight of zinc oxide nanoparticles, Tris (2, 4-di-tert-butylphenyl) phosphite (Tris(2,4-di-tert-butylphenyl) phosphite) 0.8-1.2 parts by weight, ethylenebis(stearamide) 0.8-1.2 parts by weight and 0.8-1.2 parts by weight of a platinum-based catalyst, and stirring at a rotation speed of 400-600 rpm at a temperature of 38-42° C. to prepare a coating composition; Coating the coating composition on graphene fibers; and drying and curing the graphene fiber coated with the coating composition at a temperature of 160-180°C.
상기 그래핀섬유는, 그래핀 분산액을 제조하는 단계; 및 상기 그래핀 분산액을 그래핀 섬유 형태로 습식 방사하고, 응고액에서 응고하는 단계;를 수행하여 제조되는 것을 사용한다. 또한, 상기 응고액에서 응고하여 형성된 그래핀섬유를 환원처리하는 단계; 및 상기 환원처리된 그래핀섬유를 열처리하는 단계;를 더 수행하여 제조될 수 있다. 상기 환원처리는 히드라진을 첨가하고, 70-80℃의 온도에서 5-7시간 동안 처리하는 것일 수 있다. 상기 열처리는 900-1100℃의 온도에서 1-3시간 동안 수행하는 것일 수 있다.The graphene fibers include preparing a graphene dispersion; and wet spinning the graphene dispersion in the form of graphene fibers and coagulating it in a coagulating liquid. In addition, reducing the graphene fibers formed by solidifying in the coagulating liquid; and heat-treating the reduced graphene fiber. The reduction treatment may include adding hydrazine and treating at a temperature of 70-80°C for 5-7 hours. The heat treatment may be performed at a temperature of 900-1100°C for 1-3 hours.
상기 그래핀 복합섬유는 상기 그래핀섬유를 코팅조성물로 코팅하는 것이 바람직하다.The graphene composite fiber is preferably coated with a coating composition.
상기 코팅조성물은 메틸트리에톡시실란 단량체 단위 48-52 중량부, 비닐트리에톡시실란 단량체 단위 23-27 중량부 및 (2-디에틸포스페이토에틸)트리에톡시실란((2-Diethylphosphatoethyl)triethoxysilane) 단량체 단위 23-27 중량부를 포함하는 실리콘 수지를 포함한다. 상기 실리콘 수지는 상기 단량체 단위를 포함하여 그래핀 복합섬유를 도료 조성물에 적용하는 경우 혼화성이 우수하여 고르게 분산될 수 있어 성능을 향상시킬 수 있고, 특히 (2-디에틸포스페이토에틸)트리에톡시실란 단량체 단위를 포함하여 난연성이 우수하다.The coating composition includes 48-52 parts by weight of methyltriethoxysilane monomer units, 23-27 parts by weight of vinyltriethoxysilane monomer units, and (2-diethylphosphatoethyl)triethoxysilane ((2-Diethylphosphatoethyl) triethoxysilane) and a silicone resin containing 23-27 parts by weight of monomer units. When applying graphene composite fibers containing the monomer units to a paint composition, the silicone resin has excellent miscibility and can be evenly dispersed to improve performance, especially (2-diethylphosphate ethyl)tri. It has excellent flame retardancy due to the inclusion of ethoxysilane monomer units.
상기 코팅조성물은 폴리디메틸실록산을 포함하여 내구성이 우수한 첨가제를 제조할 수 있다.The coating composition can produce an additive with excellent durability by including polydimethylsiloxane.
상기 소듐디헥실술포숙시네이트는 섬유의 인장신도, 열안정성을 개선하여 준다.The sodium dihexyl sulfosuccinate improves the tensile elongation and thermal stability of the fiber.
상기 산화아연 나노입자는 섬유의 내구성을 향상시켜 준다.The zinc oxide nanoparticles improve the durability of the fiber.
상기 트리스(2,4-디-터트-부틸페닐) 포스파이트(Tris(2,4-di-tert-butylphenyl) phosphite)는 산화방지제로 적용된다.The tris(2,4-di-tert-butylphenyl) phosphite is applied as an antioxidant.
상기 에틸렌비스(스테아르산 아미드)(Ethylenebis(stearamide))는 분산제로 적용된다.The ethylenebis(stearamide) is applied as a dispersant.
또한, 본 발명은In addition, the present invention
메틸트리에톡시실란 단량체 단위 48-52 중량부, 비닐트리에톡시실란 단량체 단위 23-27 중량부 및 (2-디에틸포스페이토에틸)트리에톡시실란((2-Diethylphosphatoethyl)triethoxysilane) 단량체 단위 23-27 중량부를 포함하는 실리콘 수지 68-72 중량부, 폴리디메틸실록산 15-19 중량부, 소듐디헥실술포숙시네이트 3-7 중량부, 산화아연 나노입자 3-7 중량부, 트리스(2,4-디-터트-부틸페닐) 포스파이트(Tris(2,4-di-tert-butylphenyl) phosphite) 0.8-1.2 중량부, 에틸렌비스(스테아르산 아미드)(Ethylenebis(stearamide)) 0.8-1.2 중량부 및 백금계 촉매 0.8-1.2 중량부를 혼합하고, 38-42℃의 온도에서 400-600 rpm의 회전속도로 교반하여 코팅조성물을 제조하는 단계; 그래핀섬유에 상기 코팅조성물을 코팅하는 단계; 및 코팅조성물이 코팅된 그래핀섬유를 160-180℃의 온도에서 건조 및 경화시키는 단계;를 포함하는 그래핀 복합섬유를 제조하는 단계; 및48-52 parts by weight of methyltriethoxysilane monomer units, 23-27 parts by weight of vinyltriethoxysilane monomer units and (2-Diethylphosphatoethyl)triethoxysilane monomer units 68-72 parts by weight of silicone resin containing 23-27 parts by weight, 15-19 parts by weight of polydimethylsiloxane, 3-7 parts by weight of sodium dihexyl sulfosuccinate, 3-7 parts by weight of zinc oxide nanoparticles, Tris (2, 4-di-tert-butylphenyl) phosphite (Tris(2,4-di-tert-butylphenyl) phosphite) 0.8-1.2 parts by weight, ethylenebis(stearamide) 0.8-1.2 parts by weight and 0.8-1.2 parts by weight of a platinum-based catalyst, and stirring at a rotation speed of 400-600 rpm at a temperature of 38-42° C. to prepare a coating composition; Coating the coating composition on graphene fibers; And drying and curing the graphene fiber coated with the coating composition at a temperature of 160-180°C; manufacturing a graphene composite fiber including; and
에틸렌비닐아세테이트 공중합체 수지 39-41 중량부, 메틸트리메톡시실란 단량체 단위 38-42 중량부, 비닐트리메톡시실란 단량체 단위 38-42 중량부 및 (트리메톡시실릴)메틸 메타크릴레이트((trimethoxysilyl)methyl methacrylate) 단량체 단위 28-32 중량부를 포함하는 실리콘 수지 10-12 중량부, 팽창흑연 11-13 중량부, 상기 그래핀 복합섬유 3-5 중량부, 멜라민 2-3 중량부, 멜라민시아누레이트 2-4 중량부, 수산화알루미늄 1-3 중량부, 펜타에리트리톨 2-3 중량부, 암모늄폴리인산염 4-6 중량부, 이산화티타늄 0.8-1.2 중량부 및 정제수 17-19 중량부를 혼합하고, 5℃ 이상의 온도에서 800-1200 rpm의 회전속도로 교반하는 단계;를 포함하는 방염 및 방수 도료 조성물의 제조방법을 제공한다. 상기 교반하는 단계에서 온도는 5℃ 이상의 온도인 것이 바람직하고, 5-15℃인 것이 더욱 바람직하다.39-41 parts by weight of ethylene vinyl acetate copolymer resin, 38-42 parts by weight of methyltrimethoxysilane monomer units, 38-42 parts by weight of vinyltrimethoxysilane monomer units, and (trimethoxysilyl)methyl methacrylate (( trimethoxysilyl)methyl methacrylate) 10-12 parts by weight of silicone resin containing 28-32 parts by weight of monomer units, 11-13 parts by weight of expanded graphite, 3-5 parts by weight of the graphene composite fiber, 2-3 parts by weight of melamine, melamine city Mix 2-4 parts by weight of anurate, 1-3 parts by weight of aluminum hydroxide, 2-3 parts by weight of pentaerythritol, 4-6 parts by weight of ammonium polyphosphate, 0.8-1.2 parts by weight of titanium dioxide, and 17-19 parts by weight of purified water. It provides a method for producing a flame retardant and waterproof paint composition comprising: stirring at a rotation speed of 800-1200 rpm at a temperature of 5°C or higher. In the stirring step, the temperature is preferably 5°C or higher, and more preferably 5-15°C.
이하, 본 발명을 하기의 실시예에 의해 보다 상세하게 설명한다.Hereinafter, the present invention will be explained in more detail by the following examples.
단, 하기 실시예는 본 발명의 내용을 예시하는 것일 뿐 발명의 범위가 실시예 및 실험예에 의해 한정되는 것은 아니다.However, the following examples only illustrate the content of the present invention and the scope of the invention is not limited by the examples and experimental examples.
<제조예 1> 그래핀 복합섬유의 제조<Preparation Example 1> Preparation of graphene composite fiber
흑연을 강산처리하는 휴머스 방법에 의해 제조한 산화그래핀을 15 mg/ml로 정제수에 분산시켜 그래핀 분산액을 제조하였다. 상기 그래핀 분산액을 이용해 습식 방사하여 에탄올과 물이 1:3의 중량비율로 혼합된 응고액에서 응고하였다. 응고한 섬유를 건조시킨 후, 히드라진으로 75℃의 온도에서 6시간 동안 처리한 후, 1000℃의 온도에서 2시간 동안 열처리하여 그래핀섬유를 제조하였다.Graphene oxide prepared by the Humus method of treating graphite with strong acid was dispersed in purified water at 15 mg/ml to prepare a graphene dispersion. The graphene dispersion was wet-spun and solidified in a coagulating solution containing ethanol and water mixed at a weight ratio of 1:3. After drying the coagulated fiber, it was treated with hydrazine at a temperature of 75°C for 6 hours and then heat treated at a temperature of 1000°C for 2 hours to produce graphene fiber.
메틸트리에톡시실란 단량체 단위 50 중량부, 비닐트리에톡시실란 단량체 단위 25 중량부 및 (2-디에틸포스페이토에틸)트리에톡시실란((2-Diethylphosphatoethyl)triethoxysilane) 단량체 단위 25 중량부를 포함하는 실리콘 수지 70 중량부, 폴리디메틸실록산 17 중량부, 소듐디헥실술포숙시네이트 5 중량부, 산화아연 나노입자 5 중량부, 트리스(2,4-디-터트-부틸페닐) 포스파이트(Tris(2,4-di-tert-butylphenyl) phosphite) 1 중량부, 에틸렌비스(스테아르산 아미드)(Ethylenebis(stearamide)) 1 중량부 및 백금계 촉매 1 중량부를 혼합하고, 40℃의 온도에서 500 rpm의 회전속도로 교반하여 코팅조성물을 제조하였다.Contains 50 parts by weight of methyltriethoxysilane monomer units, 25 parts by weight of vinyltriethoxysilane monomer units, and 25 parts by weight of (2-Diethylphosphatoethyl)triethoxysilane monomer units. 70 parts by weight of silicone resin, 17 parts by weight of polydimethylsiloxane, 5 parts by weight of sodium dihexyl sulfosuccinate, 5 parts by weight of zinc oxide nanoparticles, tris (2,4-di-tert-butylphenyl) phosphite (Tris ( Mix 1 part by weight of 2,4-di-tert-butylphenyl) phosphite, 1 part by weight of ethylenebis(stearamide), and 1 part by weight of a platinum-based catalyst, and stir at 500 rpm at a temperature of 40°C. A coating composition was prepared by stirring at a rotating speed.
상기 그래핀섬유에 코팅조성물을 코팅하고, 170℃의 온도에서 건조 및 경화하여 그래핀 복합섬유를 제조하였다.The graphene composite fiber was prepared by coating the graphene fiber with a coating composition and drying and curing it at a temperature of 170°C.
<실시예 1> 방염 및 방수 도료 조성물의 제조-1<Example 1> Preparation of flame retardant and waterproof paint composition-1
에틸렌비닐아세테이트 공중합체 수지 40 중량부, 실리콘 수지로 폴리디메틸실록산 11 중량부, 팽창흑연 16 중량부, 멜라민 2.5 중량부, 멜라민시아누레이트 3 중량부, 수산화알루미늄 2 중량부, 펜타에리트리톨 2.5 중량부, 암모늄폴리인산염 5 중량부, 이산화티타늄 1 중량부 및 정제수 18 중량부를 혼합하고, 5℃의 온도에서 1000 rpm의 회전속도로 교반하여 방염 및 방수 도료 조성물을 제조하였다.40 parts by weight of ethylene vinyl acetate copolymer resin, 11 parts by weight of polydimethylsiloxane as a silicone resin, 16 parts by weight of expanded graphite, 2.5 parts by weight of melamine, 3 parts by weight of melamine cyanurate, 2 parts by weight of aluminum hydroxide, 2.5 parts by weight of pentaerythritol A flame retardant and waterproof paint composition was prepared by mixing 5 parts by weight of ammonium polyphosphate, 1 part by weight of titanium dioxide, and 18 parts by weight of purified water, and stirring at a rotation speed of 1000 rpm at a temperature of 5°C.
<실시예 2> 방염 및 방수 도료 조성물의 제조-2<Example 2> Preparation of flame retardant and waterproof paint composition-2
에틸렌비닐아세테이트 공중합체 수지 40 중량부, 메틸트리메톡시실란 단량체 단위 40 중량부, 비닐트리메톡시실란 단량체 단위 40 중량부 및 (트리메톡시실릴)메틸 메타크릴레이트((trimethoxysilyl)methyl methacrylate) 단량체 단위 30 중량부를 포함하는 실리콘 수지 11 중량부, 팽창흑연 16 중량부, 멜라민 2.5 중량부, 멜라민시아누레이트 3 중량부, 수산화알루미늄 2 중량부, 펜타에리트리톨 2.5 중량부, 암모늄폴리인산염 5 중량부, 이산화티타늄 1 중량부 및 정제수 18 중량부를 혼합하고, 5℃의 온도에서 1000 rpm의 회전속도로 교반하여 방염 및 방수 도료 조성물을 제조하였다.40 parts by weight of ethylene vinyl acetate copolymer resin, 40 parts by weight of methyltrimethoxysilane monomer units, 40 parts by weight of vinyltrimethoxysilane monomer units, and (trimethoxysilyl)methyl methacrylate monomer 11 parts by weight of silicone resin containing 30 parts by weight, 16 parts by weight of expanded graphite, 2.5 parts by weight of melamine, 3 parts by weight of melamine cyanurate, 2 parts by weight of aluminum hydroxide, 2.5 parts by weight of pentaerythritol, 5 parts by weight of ammonium polyphosphate , 1 part by weight of titanium dioxide and 18 parts by weight of purified water were mixed and stirred at a rotation speed of 1000 rpm at a temperature of 5°C to prepare a flame retardant and waterproof paint composition.
<실시예 3> 방염 및 방수 도료 조성물의 제조-3<Example 3> Preparation of flame retardant and waterproof paint composition-3
에틸렌비닐아세테이트 공중합체 수지 40 중량부, 메틸트리메톡시실란 단량체 단위 40 중량부, 비닐트리메톡시실란 단량체 단위 40 중량부 및 (트리메톡시실릴)메틸 메타크릴레이트((trimethoxysilyl)methyl methacrylate) 단량체 단위 30 중량부를 포함하는 실리콘 수지 11 중량부, 팽창흑연 12 중량부, 상기 제조예 1에서 제조한 그래핀 복합섬유 4 중량부, 멜라민 2.5 중량부, 멜라민시아누레이트 3 중량부, 수산화알루미늄 2 중량부, 펜타에리트리톨 2.5 중량부, 암모늄폴리인산염 5 중량부, 이산화티타늄 1 중량부 및 정제수 18 중량부를 혼합하고, 5℃의 온도에서 1000 rpm의 회전속도로 교반하여 방염 및 방수 도료 조성물을 제조하였다.40 parts by weight of ethylene vinyl acetate copolymer resin, 40 parts by weight of methyltrimethoxysilane monomer units, 40 parts by weight of vinyltrimethoxysilane monomer units, and (trimethoxysilyl)methyl methacrylate monomer 11 parts by weight of silicone resin containing 30 parts by weight of the unit, 12 parts by weight of expanded graphite, 4 parts by weight of the graphene composite fiber prepared in Preparation Example 1, 2.5 parts by weight of melamine, 3 parts by weight of melamine cyanurate, 2 parts by weight of aluminum hydroxide 2.5 parts by weight of pentaerythritol, 5 parts by weight of ammonium polyphosphate, 1 part by weight of titanium dioxide, and 18 parts by weight of purified water were mixed and stirred at a rotation speed of 1000 rpm at a temperature of 5°C to prepare a flame retardant and waterproof paint composition. .
<실시예 4> 방염 및 방수 도료 조성물의 제조-4<Example 4> Preparation of flame retardant and waterproof paint composition-4
에틸렌비닐아세테이트 공중합체 수지 40 중량부, 메틸트리메톡시실란 단량체 단위 40 중량부, 비닐트리메톡시실란 단량체 단위 40 중량부 및 (트리메톡시실릴)메틸 메타크릴레이트((trimethoxysilyl)methyl methacrylate) 단량체 단위 30 중량부를 포함하는 실리콘 수지 11 중량부, 팽창흑연 8 중량부, 상기 제조예 1에서 제조한 그래핀 복합섬유 8 중량부, 멜라민 2.5 중량부, 멜라민시아누레이트 3 중량부, 수산화알루미늄 2 중량부, 펜타에리트리톨 2.5 중량부, 암모늄폴리인산염 5 중량부, 이산화티타늄 1 중량부 및 정제수 18 중량부를 혼합하고, 5℃의 온도에서 1000 rpm의 회전속도로 교반하여 방염 및 방수 도료 조성물을 제조하였다.40 parts by weight of ethylene vinyl acetate copolymer resin, 40 parts by weight of methyltrimethoxysilane monomer units, 40 parts by weight of vinyltrimethoxysilane monomer units, and (trimethoxysilyl)methyl methacrylate monomer 11 parts by weight of silicone resin containing 30 parts by weight of the unit, 8 parts by weight of expanded graphite, 8 parts by weight of the graphene composite fiber prepared in Preparation Example 1, 2.5 parts by weight of melamine, 3 parts by weight of melamine cyanurate, 2 parts by weight of aluminum hydroxide 2.5 parts by weight of pentaerythritol, 5 parts by weight of ammonium polyphosphate, 1 part by weight of titanium dioxide, and 18 parts by weight of purified water were mixed and stirred at a rotation speed of 1000 rpm at a temperature of 5°C to prepare a flame retardant and waterproof paint composition. .
<실험예 1> 내수성, 내마모성, 방염 기능성 분석<Experimental Example 1> Water resistance, abrasion resistance, and flame retardant functionality analysis
1. 내수성1. Water resistance
상기 실시예 1-4에서 제조한 방염 및 방수 도료 조성물을 스테인레스 PNL에 Bar coater #14(32 ㎛)로 도포하여 140℃에서 2시간 경화시켜 도막을 형성한 뒤 24시간 동안 상온에서 건조하였다. 이후, 표면에 도막이 형성된 스테인레스 PNL을 24시간 동안 물에 침지시켜 손으로 문질렀을 때 도막의 벗겨짐 여부를 육안으로 관찰하였으며, 그 결과를 하기 표 1에 나타내었다.The flame retardant and waterproof paint composition prepared in Examples 1-4 was applied to stainless steel PNL using Bar coater #14 (32 ㎛), cured at 140°C for 2 hours to form a coating film, and dried at room temperature for 24 hours. Thereafter, the stainless steel PNL with the coating film formed on the surface was immersed in water for 24 hours and rubbed by hand to visually observe whether the coating film was peeled off. The results are shown in Table 1 below.
<평가기준><Evaluation criteria>
◎ : 표면의 도막이 거의 벗겨지지 않음 (약 90% 이상 잔존)◎: The coating film on the surface is almost not peeled off (approximately 90% or more remains).
○ : 표면의 도막이 벗겨지지 않음 (약 70-90% 잔존)○: Surface coating does not peel off (approximately 70-90% remaining)
△ : 표면의 도막이 약간 벗겨짐 (약 40-70% 잔존)△: The surface coating film is slightly peeled off (approximately 40-70% remaining).
× : 표면의 도막이 벗겨짐 (약 10-40% 잔존)×: Surface coating peeling off (approximately 10-40% remaining)
상기 표 1에 나타낸 바와 같이, 본 발명에 따른 방염 및 방수 도료 조성물은 내수성이 우수한 것을 확인할 수 있었다.As shown in Table 1, it was confirmed that the flame retardant and waterproof paint composition according to the present invention had excellent water resistance.
2. 내마모성2. Wear resistance
상기 실시예 1-4에서 제조한 방염 및 방수 도료 조성물을 스테인레스 PNL에 Bar coater #14(32 ㎛)로 도포하여 140℃에서 2시간 경화시켜 도막을 형성한 뒤 24시간 동안 상온에서 건조하였다. 이후, 표면에 도막이 형성된 스테인레스 PNL 표면을 못으로 긁은 후 긁힌 흔적을 육안으로 관찰하였으며, 그 결과를 하기 표 2에 나타내었다.The flame retardant and waterproof paint composition prepared in Examples 1-4 was applied to stainless steel PNL using Bar coater #14 (32 ㎛), cured at 140°C for 2 hours to form a coating film, and dried at room temperature for 24 hours. Afterwards, the surface of the stainless steel PNL with a coating film formed on the surface was scratched with a nail and the scratch marks were observed with the naked eye, and the results are shown in Table 2 below.
<평가기준><Evaluation criteria>
◎ : 표면에 스크래치가 전혀 발생하지 않음 (약 90% 이상 잔존)◎: No scratches on the surface (approximately 90% or more remaining)
○ : 표면에 스크래치가 발생하지 않음 (약 70-90% 잔존)○: No scratches on the surface (approximately 70-90% remaining)
△ : 표면에 스크래치가 약간 발생함 (약 40-70% 잔존)△: Slight scratches on the surface (approximately 40-70% remaining)
× : 표면에 스크래치가 크게 발생함 (약 10-40% 잔존)×: Large scratches appear on the surface (approximately 10-40% remain)
상기 표 2에 나타낸 바와 같이, 본 발명에 따른 방염 및 방수 도료 조성물은 내마모성이 우수한 것을 확인할 수 있었다.As shown in Table 2, it was confirmed that the flame retardant and waterproof paint composition according to the present invention had excellent abrasion resistance.
3. 방염 기능성3. Flame retardant functionality
상기 실시예 1-4에서 제조한 방염 및 방수 도료 조성물을 실험시료인 MDF목재 시료에 도포하여 45°연소시험기 내의 시험체 받침틀에 실험시료를 고정시킨 후, 버너의 불꽃 길이가 65 mm가 되도록 하여 불꽃 끝이 실험시료 중앙 하단에 접하도록 하였다. 각 실험시료에 대해 1분 동안 가열을 진행하였으며, 가열시간 중에 착염되는 실험시료에 대해서는 착염 후 2초 후에 버너를 제거하였으며, 그 결과를하기 표 3에 나타내었다. 이때, 잔염시간은 연소하는 상태가 그칠 때까지의 시간을 의미하며, 잔신시간은 버너의 불꽃을 제거한 때부터 불꽃을 올리지 아니하고 연소하는 상태가 그칠 때까지의 잔염시간(잔염이 생기는 동안의 시간 제외)을 의미한다. 또한, 탄화면적 및 탄화길이는 불꽃에 의해 탄화된 면적과 길이를 측정한 것이다.The flame retardant and waterproof paint composition prepared in Example 1-4 was applied to the MDF wood sample as the test sample, the test sample was fixed to the test specimen support frame in the 45° combustion tester, and the flame length of the burner was set to 65 mm. The end was placed in contact with the bottom center of the test sample. Heating was performed for 1 minute for each experimental sample, and for the experimental samples that were complexed during the heating time, the burner was removed 2 seconds after complexing. The results are shown in Table 3 below. At this time, afterflame time means the time until the burning state ceases, and afterflame time refers to the time from when the flame of the burner is removed until the burning state ceases without raising the flame (excluding the time while afterflame occurs). ) means. In addition, the carbonization area and carbonization length are measurements of the area and length carbonized by the flame.
상기 표 3에 나타낸 바와 같이, 본 발명에 따른 방염 및 방수 도료 조성물은 방염 기능성이 우수한 것을 확인할 수 있었다.As shown in Table 3, it was confirmed that the flame retardant and waterproof paint composition according to the present invention had excellent flame retardant functionality.
<실험예 2> 물성 분석<Experimental Example 2> Physical property analysis
상기 실시예 1-4에서 제조한 방염 및 방수 도료 조성물을 도포한 후 건조하여 도료층을 제조하고, 상기 도료층의 물성을 평가하기 위하여 KSF 4922에 의거하여 각 도료층의 물성을 측정하였으며, 그 결과를 하기 표 4에 나타내었다.The flame retardant and waterproof paint composition prepared in Example 1-4 was applied and then dried to prepare a paint layer. In order to evaluate the physical properties of the paint layer, the physical properties of each paint layer were measured according to KSF 4922. The results are shown in Table 4 below.
상기 표 4에 나타낸 바와 같이, 본 발명에 따른 방염 및 방수 도료 조성물은 우수한 물성을 가지는 것을 확인할 수 있었다.As shown in Table 4, it was confirmed that the flame retardant and waterproof paint composition according to the present invention had excellent physical properties.
Claims (3)
상기 방염 및 방수 도료 조성물은 에틸렌비닐아세테이트 공중합체 수지 39-41 중량부, 실리콘 수지 10-12 중량부, 팽창흑연 11-13 중량부, 그래핀 복합섬유 3-5 중량부, 멜라민 2-3 중량부, 멜라민시아누레이트 2-4 중량부, 수산화알루미늄 1-3 중량부, 펜타에리트리톨 2-3 중량부, 암모늄폴리인산염 4-6 중량부, 이산화티타늄 0.8-1.2 중량부 및 정제수 17-19 중량부를 포함하고,
상기 실리콘 수지는 메틸트리메톡시실란 단량체 단위 38-42 중량부, 비닐트리메톡시실란 단량체 단위 38-42 중량부 및 (트리메톡시실릴)메틸 메타크릴레이트((trimethoxysilyl)methyl methacrylate) 단량체 단위 28-32 중량부를 포함하고,
상기 그래핀 복합섬유는,
메틸트리에톡시실란 단량체 단위 48-52 중량부, 비닐트리에톡시실란 단량체 단위 23-27 중량부 및 (2-디에틸포스페이토에틸)트리에톡시실란((2-Diethylphosphatoethyl)triethoxysilane) 단량체 단위 23-27 중량부를 포함하는 실리콘 수지 68-72 중량부, 폴리디메틸실록산 15-19 중량부, 소듐디헥실술포숙시네이트 3-7 중량부, 산화아연 나노입자 3-7 중량부, 트리스(2,4-디-터트-부틸페닐) 포스파이트(Tris(2,4-di-tert-butylphenyl) phosphite) 0.8-1.2 중량부, 에틸렌비스(스테아르산 아미드)(Ethylenebis(stearamide)) 0.8-1.2 중량부 및 백금계 촉매 0.8-1.2 중량부를 혼합하고, 38-42℃의 온도에서 400-600 rpm의 회전속도로 교반하여 코팅조성물을 제조하는 단계; 그래핀섬유에 상기 코팅조성물을 코팅하는 단계; 및 코팅조성물이 코팅된 그래핀섬유를 160-180℃의 온도에서 건조 및 경화시키는 단계;를 수행하여 제조되는 것을 특징으로 하는 방염 및 방수 도료 조성물.According to paragraph 1,
The flame retardant and waterproof paint composition includes 39-41 parts by weight of ethylene vinyl acetate copolymer resin, 10-12 parts by weight of silicone resin, 11-13 parts by weight of expanded graphite, 3-5 parts by weight of graphene composite fiber, and 2-3 parts by weight of melamine. parts, 2-4 parts by weight of melamine cyanurate, 1-3 parts by weight of aluminum hydroxide, 2-3 parts by weight of pentaerythritol, 4-6 parts by weight of ammonium polyphosphate, 0.8-1.2 parts by weight of titanium dioxide, and 17-19 parts by weight of purified water. Contains a weight part,
The silicone resin contains 38-42 parts by weight of methyltrimethoxysilane monomer units, 38-42 parts by weight of vinyltrimethoxysilane monomer units, and 28 parts by weight of (trimethoxysilyl)methyl methacrylate monomer units. Contains -32 parts by weight,
The graphene composite fiber,
48-52 parts by weight of methyltriethoxysilane monomer units, 23-27 parts by weight of vinyltriethoxysilane monomer units and (2-Diethylphosphatoethyl)triethoxysilane monomer units 68-72 parts by weight of silicone resin containing 23-27 parts by weight, 15-19 parts by weight of polydimethylsiloxane, 3-7 parts by weight of sodium dihexyl sulfosuccinate, 3-7 parts by weight of zinc oxide nanoparticles, Tris (2, 4-di-tert-butylphenyl) phosphite (Tris(2,4-di-tert-butylphenyl) phosphite) 0.8-1.2 parts by weight, ethylenebis(stearamide) 0.8-1.2 parts by weight and 0.8-1.2 parts by weight of a platinum-based catalyst, and stirring at a rotation speed of 400-600 rpm at a temperature of 38-42° C. to prepare a coating composition; Coating the coating composition on graphene fibers; and drying and curing the graphene fiber coated with the coating composition at a temperature of 160-180°C.
에틸렌비닐아세테이트 공중합체 수지 39-41 중량부, 메틸트리메톡시실란 단량체 단위 38-42 중량부, 비닐트리메톡시실란 단량체 단위 38-42 중량부 및 (트리메톡시실릴)메틸 메타크릴레이트((trimethoxysilyl)methyl methacrylate) 단량체 단위 28-32 중량부를 포함하는 실리콘 수지 10-12 중량부, 팽창흑연 11-13 중량부, 상기 그래핀 복합섬유 3-5 중량부, 멜라민 2-3 중량부, 멜라민시아누레이트 2-4 중량부, 수산화알루미늄 1-3 중량부, 펜타에리트리톨 2-3 중량부, 암모늄폴리인산염 4-6 중량부, 이산화티타늄 0.8-1.2 중량부 및 정제수 17-19 중량부를 혼합하고, 5℃ 이상의 온도에서 800-1200 rpm의 회전속도로 교반하는 단계;를 포함하는 방염 및 방수 도료 조성물의 제조방법.48-52 parts by weight of methyltriethoxysilane monomer units, 23-27 parts by weight of vinyltriethoxysilane monomer units and (2-Diethylphosphatoethyl)triethoxysilane monomer units 68-72 parts by weight of silicone resin containing 23-27 parts by weight, 15-19 parts by weight of polydimethylsiloxane, 3-7 parts by weight of sodium dihexyl sulfosuccinate, 3-7 parts by weight of zinc oxide nanoparticles, Tris (2, 4-di-tert-butylphenyl) phosphite (Tris(2,4-di-tert-butylphenyl) phosphite) 0.8-1.2 parts by weight, ethylenebis(stearamide) 0.8-1.2 parts by weight and 0.8-1.2 parts by weight of a platinum-based catalyst, and stirring at a rotation speed of 400-600 rpm at a temperature of 38-42° C. to prepare a coating composition; Coating the coating composition on graphene fibers; And drying and curing the graphene fiber coated with the coating composition at a temperature of 160-180°C; manufacturing a graphene composite fiber including; and
39-41 parts by weight of ethylene vinyl acetate copolymer resin, 38-42 parts by weight of methyltrimethoxysilane monomer units, 38-42 parts by weight of vinyltrimethoxysilane monomer units, and (trimethoxysilyl)methyl methacrylate (( trimethoxysilyl)methyl methacrylate) 10-12 parts by weight of silicone resin containing 28-32 parts by weight of monomer units, 11-13 parts by weight of expanded graphite, 3-5 parts by weight of the graphene composite fiber, 2-3 parts by weight of melamine, melamine city Mix 2-4 parts by weight of anurate, 1-3 parts by weight of aluminum hydroxide, 2-3 parts by weight of pentaerythritol, 4-6 parts by weight of ammonium polyphosphate, 0.8-1.2 parts by weight of titanium dioxide, and 17-19 parts by weight of purified water. A method for producing a flame retardant and waterproof paint composition comprising: stirring at a rotation speed of 800-1200 rpm at a temperature of 5°C or higher.
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| KR20070090029A (en) * | 2005-03-28 | 2007-09-04 | 제너럴 일렉트릭 캄파니 | Flame retardant thermoplastic composition and articles comprising the same |
| KR20070109267A (en) | 2006-05-10 | 2007-11-15 | 우성테크 주식회사 | Fireproof paint composition and manufacturing method of using thereof for fireproof paint |
| KR20180120258A (en) * | 2016-03-10 | 2018-11-05 | 클라리언트 플라스틱스 앤드 코팅즈 리미티드 | Halogen-free, foamable refractory coatings and their uses |
| KR102545123B1 (en) * | 2023-01-26 | 2023-06-19 | 유태진 | Waterproofing agent and waterproofing construction method using the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20070090029A (en) * | 2005-03-28 | 2007-09-04 | 제너럴 일렉트릭 캄파니 | Flame retardant thermoplastic composition and articles comprising the same |
| KR20070109267A (en) | 2006-05-10 | 2007-11-15 | 우성테크 주식회사 | Fireproof paint composition and manufacturing method of using thereof for fireproof paint |
| KR20180120258A (en) * | 2016-03-10 | 2018-11-05 | 클라리언트 플라스틱스 앤드 코팅즈 리미티드 | Halogen-free, foamable refractory coatings and their uses |
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