CN108864922A - The preparation method of fire-retardant, waterproof, fast light aqueous polyurethane coating and adhesive - Google Patents
The preparation method of fire-retardant, waterproof, fast light aqueous polyurethane coating and adhesive Download PDFInfo
- Publication number
- CN108864922A CN108864922A CN201810625883.3A CN201810625883A CN108864922A CN 108864922 A CN108864922 A CN 108864922A CN 201810625883 A CN201810625883 A CN 201810625883A CN 108864922 A CN108864922 A CN 108864922A
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- Prior art keywords
- added
- retardant
- fire
- preparation
- coating
- Prior art date
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- 239000011527 polyurethane coating Substances 0.000 title claims abstract description 30
- 239000000853 adhesive Substances 0.000 title claims abstract description 28
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 28
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 39
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 35
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000003054 catalyst Substances 0.000 claims abstract description 33
- 238000004078 waterproofing Methods 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Substances CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000012948 isocyanate Substances 0.000 claims abstract description 18
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 14
- 229920000909 polytetrahydrofuran Polymers 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 11
- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000004945 emulsification Methods 0.000 claims abstract description 10
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 10
- 230000035484 reaction time Effects 0.000 claims abstract description 10
- RKIDDEGICSMIJA-UHFFFAOYSA-N 4-chlorobenzoyl chloride Chemical compound ClC(=O)C1=CC=C(Cl)C=C1 RKIDDEGICSMIJA-UHFFFAOYSA-N 0.000 claims abstract description 8
- -1 trimethyl hydroxyethylammonium propane Chemical compound 0.000 claims description 24
- 238000010792 warming Methods 0.000 claims description 21
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 14
- 239000003999 initiator Substances 0.000 claims description 14
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims description 14
- RDBMUARQWLPMNW-UHFFFAOYSA-N phosphanylmethanol Chemical compound OCP RDBMUARQWLPMNW-UHFFFAOYSA-N 0.000 claims description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 8
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 7
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 7
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 7
- 150000001408 amides Chemical class 0.000 claims description 7
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 7
- 229940043237 diethanolamine Drugs 0.000 claims description 7
- 150000002240 furans Chemical class 0.000 claims description 7
- QUIMTLZDMCNYGY-UHFFFAOYSA-N 2,4-dichloro-1-nitrobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C=C1Cl QUIMTLZDMCNYGY-UHFFFAOYSA-N 0.000 claims description 5
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- CZZYITDELCSZES-UHFFFAOYSA-N diphenylmethane Chemical compound C=1C=CC=CC=1CC1=CC=CC=C1 CZZYITDELCSZES-UHFFFAOYSA-N 0.000 claims description 5
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 5
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims description 4
- VHPUZTHRFWIGAW-UHFFFAOYSA-N dimethoxy-di(propan-2-yl)silane Chemical compound CO[Si](OC)(C(C)C)C(C)C VHPUZTHRFWIGAW-UHFFFAOYSA-N 0.000 claims description 4
- 238000006396 nitration reaction Methods 0.000 claims description 4
- FHHJDRFHHWUPDG-UHFFFAOYSA-N peroxysulfuric acid Chemical compound OOS(O)(=O)=O FHHJDRFHHWUPDG-UHFFFAOYSA-N 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 4
- 235000019394 potassium persulphate Nutrition 0.000 claims description 4
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 3
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 3
- 235000019864 coconut oil Nutrition 0.000 claims description 2
- 239000003240 coconut oil Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 claims 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims 1
- 235000011130 ammonium sulphate Nutrition 0.000 claims 1
- 125000005442 diisocyanate group Chemical group 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 235000019197 fats Nutrition 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000000576 coating method Methods 0.000 abstract description 67
- 239000011248 coating agent Substances 0.000 abstract description 64
- 239000003973 paint Substances 0.000 abstract description 52
- 238000005260 corrosion Methods 0.000 abstract 1
- 239000010985 leather Substances 0.000 abstract 1
- 239000002585 base Substances 0.000 description 19
- 239000000463 material Substances 0.000 description 13
- 239000003610 charcoal Substances 0.000 description 10
- 229920002635 polyurethane Polymers 0.000 description 10
- 239000004814 polyurethane Substances 0.000 description 10
- 239000003921 oil Substances 0.000 description 9
- 235000019198 oils Nutrition 0.000 description 9
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 238000002485 combustion reaction Methods 0.000 description 7
- 235000014113 dietary fatty acids Nutrition 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 239000000194 fatty acid Substances 0.000 description 7
- 229930195729 fatty acid Natural products 0.000 description 7
- 150000004665 fatty acids Chemical class 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- 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 description 5
- FLFJVPPJGJSHMF-UHFFFAOYSA-L manganese hypophosphite Chemical class [Mn+2].[O-]P=O.[O-]P=O FLFJVPPJGJSHMF-UHFFFAOYSA-L 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 4
- 238000010276 construction Methods 0.000 description 4
- 239000010426 asphalt Substances 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002966 varnish Substances 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000004922 lacquer Substances 0.000 description 2
- 239000006210 lotion Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- CCMKPCBRNXKTKV-UHFFFAOYSA-N 1-hydroxy-5-sulfanylidenepyrrolidin-2-one Chemical compound ON1C(=O)CCC1=S CCMKPCBRNXKTKV-UHFFFAOYSA-N 0.000 description 1
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 1
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 1
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- IOUVKUPGCMBWBT-DARKYYSBSA-N Phloridzin Natural products O[C@H]1[C@@H](O)[C@H](O)[C@H](CO)O[C@H]1OC1=CC(O)=CC(O)=C1C(=O)CCC1=CC=C(O)C=C1 IOUVKUPGCMBWBT-DARKYYSBSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002174 Styrene-butadiene Substances 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000004520 agglutination Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910000085 borane Inorganic materials 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000010073 coating (rubber) Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 238000005034 decoration Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- MHDVGSVTJDSBDK-UHFFFAOYSA-N dibenzyl ether Chemical compound C=1C=CC=CC=1COCC1=CC=CC=C1 MHDVGSVTJDSBDK-UHFFFAOYSA-N 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- QLBHNVFOQLIYTH-UHFFFAOYSA-L dipotassium;2-[2-[bis(carboxymethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [K+].[K+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O QLBHNVFOQLIYTH-UHFFFAOYSA-L 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 229940031098 ethanolamine Drugs 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229920000592 inorganic polymer Polymers 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000000025 natural resin Substances 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229920001558 organosilicon polymer Polymers 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- IOUVKUPGCMBWBT-UHFFFAOYSA-N phloridzosid Natural products OC1C(O)C(O)C(CO)OC1OC1=CC(O)=CC(O)=C1C(=O)CCC1=CC=C(O)C=C1 IOUVKUPGCMBWBT-UHFFFAOYSA-N 0.000 description 1
- IOUVKUPGCMBWBT-QNDFHXLGSA-N phlorizin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC(O)=CC(O)=C1C(=O)CCC1=CC=C(O)C=C1 IOUVKUPGCMBWBT-QNDFHXLGSA-N 0.000 description 1
- 235000019139 phlorizin Nutrition 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000037452 priming Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000011115 styrene butadiene Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- 229960001124 trientine Drugs 0.000 description 1
- TUUQISRYLMFKOG-UHFFFAOYSA-N trihexyl 2-acetyloxypropane-1,2,3-tricarboxylate Chemical compound CCCCCCOC(=O)CC(C(=O)OCCCCCC)(OC(C)=O)CC(=O)OCCCCCC TUUQISRYLMFKOG-UHFFFAOYSA-N 0.000 description 1
- UORVGPXVDQYIDP-UHFFFAOYSA-N trihydridoboron Substances B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- 238000009941 weaving Methods 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/08—Polyurethanes from polyethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
-
- C—CHEMISTRY; METALLURGY
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- C08G18/08—Processes
- C08G18/16—Catalysts
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- C08G18/08—Processes
- C08G18/16—Catalysts
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- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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Abstract
The invention discloses fire-retardant, waterproofs, the preparation method of fast light aqueous polyurethane coating and adhesive, it is 0.16g, polytetrahydrofuran ether glycol 76g and isocyanates 14g that catalyst B, which is added, in it in the 500ml there-necked flask for having blender, condenser pipe, thermometer, 0.5 ~ 2h is reacted at 70 ~ 80 DEG C, obtains base polyurethane prepolymer for use as A;Step is added into base polyurethane prepolymer for use as A(1)Fire retardant 0.6g, parachlorobenzoyl chloride 1.2g and the solvent DMF 11.2g reacts 2 ~ 3.5h under the conditions of 60 ~ 80 DEG C, and 4g step is added(2)Waterproofing agent and trimellitic anhydride 1.2g, 80 DEG C of reaction temperature, reaction time 1h, 6.5g triethylamine is added and carries out neutralization reaction 60min, 90 ~ 110g of water is added and is stirred emulsification 1h, fire-retardant, waterproof, fast light aqueous polyurethane coating and adhesive are obtained, which can be used for coating for internal and external wall, metallic finishes and anti-corrosion, makees the paint of timber and its as leather finishing agent.
Description
Technical field
The present invention relates to the preparation method of aqueous polyurethane coating and adhesive, particularly with regard to fire-retardant, waterproof, resistance to
The preparation method of light aqueous polyurethane coating and adhesive.
Background technique
Coating, in the entitled paint of Chinese tradition.So-called coating be coated in the body surface being protected or decorated, and
The continuous film of firm attachment can be formed with coated article, usually based on resin or oil or lotion, add or do not add face
Material, filler add corresponding additive, the thick liquid being formulated with organic solvent or water.
Founding of New is over 60 years, along with the development of national economy every profession and trade, as its matched coatings industry from one
A extremely unobtrusive small industry gradually develops into the essential important industry of all fields of national economy.By several generations
Struggle hard, pioneer and keep forging ahead, China has become second-biggest-in-the-world coating material production state and country of consumption, enters world's coating industry
The mainstream of development.
For the service life of coating depending on different products, liquid fibrous gypsum texture product uses modified organic silicone resin
Lotion is base-material, with special coating technology, assorted colored paint is coated agglutination hydrate colour particle, is uniformly and stably suspended in
In specific water-borne dispersions, various colored particles form and aspect are remained unchanged, and coloring pigment will not be precipitated in water.It is so this outer
The service life of wall coating is about 15 years.
Water paint has made good with powdery paints, and the building coating especially based on water paint is total in China's coating
About 38% is accounted in amount.Since water paint and its chemical characteristic of oil paint have difference substantially, water paint and oil paint product
Matter also has very big difference, then the outmoded understanding for big branch water paint being set to again in paint industry, is unscientific.
There are many classification method of coating, usually there is following several classification methods:
(1))Divide by the form of product, can be divided into:Liquid coating, powder-type coating, high solid coating.
(2)Decentralized medium is used by coating:Solvent based coating;Water paint(Emulsion paint, water soluble paint).
(3))Building coating, can lacquer, car paint, airplane dope, appliance finishes, woodenware can be divided by purposes to apply
Material, bridge coating, plastic paint, coating for paper, marine paint, wind-power electricity generation coating, nuclear power coating, pipeline coating, steel construction
Coating, rubber coating, aircraft coating etc..
(4)Divide by its performance, can be divided into:It is anticorrosive coating, antirusting paint, coatings, high-temperature resistant coating, ageing-resistant
Coating, acid and alkali-resistance coating, resistant to chemical media coating.
(5))By whether having color, can be divided into:Varnish, colored paint.
(6)Divide by its working procedure, can be divided into:Seal coat, putty, priming paint, base coat, finishing coat, finishing varnish.
(7)Brush coating, sprayed coating, roll coat enamel, dip-coating paint, electrophoretic coating etc. can be divided by construction method.
(8) non-viscous paint, Teflon coating, decorative paint, anticorrosive paint, conductive coating, antirust can be divided by function to apply
Material, high-temperature resistant coating, thermo-color, insulating moulding coating, fireproof coating, water-repellent paint etc..
(9) home paint can be divided into interior wall coating, exterior coating, woodcare paint, metal paint, floor paint.
(10) by paint film property point(Anti-decaying paint, insulated paint, conductive paint, Berlin black ...)
(11) by film forming matter point(Natural resin class paint, phenolic paints, alkyd paints, amino paint, nitro class paint, epoxies
It is paint, chlorinated rubber class paint, acrylic paint, polyurethanes paint, organic siliconresin class paint, fluorocarbon resin class paint, polysiloxane-based
Paint, vinyl class paint ...)
(12) type classification of base-material is pressed:Organic coating, inorganic coating, organic-inorganic composite coating can be divided into.Organic coating
Since the solvent that it is used is different, and it is divided into organic solvent type coatings and organic water borne(Including emulsion type and water-soluble)Coating two
Class.Common coating is typically all organic coating in life.Inorganic coating refers to being given birth to inorganic macromolecule material by base-material
The coating of production, including water-soluble silicate system, silica solution system, organosilicon and inorganic polymer system.Organic-inorganic composite coating
There are two types of complex form, one is coating in production using organic material and inorganic material collectively as base-material, is formed compound
Coating;Another kind is that organic coating and inorganic coating be combined with each other in decoration construction.
Classify by decorative effect:It can be divided into:1. the flat paint of smooth surface(It is commonly called as flat painting), this is most commonly seen
A kind of form of construction work;2. surface is in the sand textured coating of sand shape decorative effect, such as lacquer;3. it is three-dimensional to form ridge design
The complex layer coating of decorative effect, such as embossment.
By being classified on building using position:Be divided into interior wall coating, exterior coating, floor coating, door and window coating and
Ceiling coating.
By using function classification:Common coating and special functional building coating can be divided into(As fireproof coating, waterproof apply
Material, mildew resistant paint, road mark paint etc.).
According to using color effects to classify:Such as metallic paint, this colored paint(Or it is called:Solid color enamel), clear varnish etc..
Duan Baorong et al. is patent of invention is fire-retardant, polyurethane coating of waterproof and low VOC(201711419973.9 ), adopt
It is prepared with following step, it is characterised in that:(1), modified manganese hypophosphite preparation:With blender, thermometer
In 250ml there-necked flask be added manganese hypophosphite 11.2g, boric acid 25.6g, diethanol amine 28g, hexaphenoxycyclotriphosphazene 7.2g and
Phloridzin 2.8g and water 65g adjusts pH to 4, is heated to 80 DEG C, is stirred to react 2h, and EDTAP dipotassium ethylene diamine tetraacetate is added
1.6g, 70 DEG C are stirred to react 1h, obtain modified manganese hypophosphite;(2), with blender, condenser pipe, thermometer 250ml tri-
Azoformic acid dibenzyl ester 0.25g, polytetrahydrofuran ether glycol 72g and hexamethylene diisocyanate 18g is added in mouth bottle, in
1h is reacted at 70 DEG C, obtains base polyurethane prepolymer for use as A, the molecular weight of the polytetrahydrofuran ether glycol is 500;(3), to performed polymer
The equal three nitrogen borine of 0.68g hexahydro and 8.8g methyl ethyl ketone are added in A, 3.0h is reacted under the conditions of 70 DEG C, 1g step is added(1)Preparation
Modification manganese hypophosphite, 3.2g4- Carboxybenzeneboronic acid and N- hydroxy thiosuccinimide 3.5g, 70 DEG C of reaction temperature, when reaction
Between 1h, be added 7.8g triethylamine carry out neutralization reaction 70min, water 70g be stirred emulsification 1h, obtain fire-retardant, waterproof and low VOC
Polyurethane coating, wherein oxygen index (OI) maximum can reach 28.6, and flaming combustion time reaches 8.5, in 0.3Mpa in 30min not
Leak.
201711168086.9 invention is related to a kind of polyurethane-modified asphalt waterproofing anti-flaming dope, by following parts by weight
Raw material composition:25~30 parts of aqueous polyurethane emulsion;70-75 parts of 90# asphalt;40-60 parts of water;Styrene-butadiene latex 20-25
Part, 4-7 parts of emulsifier, 2-4 parts of polyvinyl alcohol, 1-3 parts of diethylenetriamine base propyl trimethoxy silicane;3-5 parts of fire retardant;It is poly-
1-2 parts of oxypropylene glycerin ether;3-5 parts of acetyl trihexyl citrate, 0.1-0.3 parts of hydrogenated rosin pentaerythritol ester;Carboxymethyl is fine
Tie up plain 1-3 parts of sodium;10-15 parts of modified nano calcium carbonate.The polyurethane-modified asphalt waterproofing anti-flaming dope that the present invention is prepared
Film formation compactness is good, and stability is high, the adhesion strength of waterproof layer and cement concrete basal plane for being formed in build greatly, waterproof
Effect is good, and by modification, the performances such as anti-flammability, water resistance, resistance to ag(e)ing and resistance to acid and alkali of the product are all obtained greatly
It improves, anti-flammability rank has reached that igniting is not burnt, that waterproof has reached 30min under 0.2Mpa again is water-tight.
The 201711369135.5 disclosure of the invention polyurethane coating and preparation method thereof of fire-retardant, light resistance and low VOC,
With blender, condenser pipe, thermometer 250ml there-necked flask in be added triethylene tetramine 0.22g, polytetrahydrofuran ether glycol
70g and hexamethylene diisocyanate 15g, reacts 2h at 80 DEG C, obtains base polyurethane prepolymer for use as A;It is added into performed polymer A
0.62g acetamide and 8.2g methyl ethyl ketone, react 3.5h under the conditions of 75 DEG C, be added 2g step (1) preparation modification manganese hypophosphite,
80 DEG C of reaction temperature, reaction time 2h, tri- second of 7.1g is added in 4g4- Carboxybenzeneboronic acid and diethylene triamine pentamethylene phosphonic 2.5g
Amine carries out neutralization reaction 60min, and addition vitamin C 0.9g, water 70g are stirred emulsification, obtain fire-retardant, light resistance and low VOC
Polyurethane coating, it is the polyurethane coating environmental protection of prepared fire-retardant, light resistance and low VOC, cheap, be widely used in wall
Body, furniture, ironware surface, as plastics, glass, papermaking, weaving adhesive, test find its flaming combustion time most
Low to can reach 7.2s, oxygen index (OI) can reach 27.6, show that its anti-flammability is preferable, and light resistance is lower than 0.8 in 600min.
Summary of the invention
The present invention relates to fire-retardant, waterproof, the preparation method of fast light aqueous polyurethane coating and adhesive, main thoughts
It is to synthesize a kind of fire retardant and waterproofing agent, fire retardant and waterproofing agent is reacted with base polyurethane prepolymer for use as, to improve polyurethane
The flame retardant property and waterproofness of coating, wherein the fire retardant is expansion type flame retardant, has good surplus charcoal rate and dilatancy, is come
Promote polyurethane surface have more fine and close layer of charcoal, while dilatancy have heat not heat carrier, reduce outside heat after
The tendency that afterflame is burnt, selects the waterproofness under the assistance of trimellitic anhydride, to be grafted in base polyurethane prepolymer for use as.
The preparation method of fire-retardant, waterproof, fast light aqueous polyurethane coating and adhesive, preparation method are:
(1)The preparation of fire retardant:By tetrakis hydroxymetyl phosphonium sulfuric 1mol, gamma-aminopropyl-triethoxy-silane 0.4mol and phosphoric acid
3mol is added in three-necked flask, adds triethylamine 5%(Tetrakis hydroxymetyl phosphonium sulfuric and γ-aminopropyl triethoxysilane are total
The 5% of weight)It is 4.2g, 90-120 DEG C of 3 ~ 5h of reaction with catalyst A, cools to 70 ~ 80 DEG C, 2 ~ 5h of reaction, then it is warming up to 90 ~
100 DEG C, 1 ~ 2mol diethanol amine, anesin 0.3mol and 0.1mol trimethyl hydroxyethylammonium propane diamine is added, reacts 2 ~ 6h,
Obtain the fire retardant.
(2)The preparation of waterproofing agent:By acrylic acid 10g, trimethyl hydroxyethylammonium propane diamine 1.6g and hydroxy-ethyl acrylate 0.7g
It is added in there-necked flask, adds initiator 0.6g, 70g water is then added, is gradually warming up to 85 DEG C, sequentially adds 22g cocounut oil
Fatty acid, 16g diglycollic amide and trimethylolpropane 6.9g are uniformly mixed, and are warming up to 70 DEG C, are stirred to being completely dissolved, i.e.,
Obtain the waterproofing agent.
(3)It is 0.16g, poly- tetrahydro that catalyst B is added in the 500ml there-necked flask for having blender, condenser pipe, thermometer
Furans ether glycol 76g and isocyanates 14g reacts 0.5 ~ 2h at 70 ~ 80 DEG C, obtains base polyurethane prepolymer for use as A;It is pre- to polyurethane
Step is added in aggressiveness A(1)Fire retardant 0.6g, parachlorobenzoyl chloride 1.2g and the solvent DMF 11.2g, in 60 ~ 80 DEG C of items
2 ~ 3.5h is reacted under part, and 4g step is added(2)Waterproofing agent and trimellitic anhydride 1.2g, 80 DEG C of reaction temperature, the reaction time
1h, be added 6.5g triethylamine carry out neutralization reaction 60min, be added 90 ~ 110g of water be stirred emulsification 1h, obtain fire-retardant, waterproof,
Fast light aqueous polyurethane coating and adhesive.
Catalyst A is any one of 2,4- dichloronitrobenzene, paranitroanilinum, hydroxyl sulfate, hydroxylamine chloride;
Catalyst B is para orientation nitration, benzyl benzene, diisopropyl dimethoxy silane, 3- dimethylamine propylamine
Any one;Times that the molecular weight of the polytetrahydrofuran ether glycol is 250,650,1000,1800,2000,2900
It anticipates one kind;Isocyanates is hexamethylene diisocyanate, toluene di-isocyanate(TDI), isophorone diisocyanate, 4,4'- bis-
Any one of diphenylmethane diisocyanate;Initiator is any one of ammonium persulfate, potassium peroxydisulfate.
Advantage of the invention is that:
(1)Select the catalysis of 2,4- dichloronitrobenzene, paranitroanilinum, hydroxyl sulfate, hydroxylamine chloride as expansibility flame-proof agent
Agent;Para orientation nitration, benzyl benzene, diisopropyl dimethoxy silane, 3- dimethylamine propylamine are as base polyurethane prepolymer for use as
Catalyst has nontoxic, high-efficient advantage;
(2)Synergist of the trimellitic anhydride as waterproofing agent has the effect for the combination for promoting waterproofing agent and base polyurethane prepolymer for use as
Fruit.
(3)Fire retardant is expansion type flame retardant, has good surplus charcoal rate and dilatancy, to promote polyurethane surface mask
There is more fine and close layer of charcoal, while dilatancy has the not heat carrier of heat, reduces the tendency that outside heat burns away, it is fire-retardant
Trimethyl hydroxyethylammonium propane diamine is used in agent synthesis, so that fire retardant is remained charcoal rate and improves.
(4)DMF used in the present invention is solvent(N,N-Dimethylformamide), fatty acid distribution of coconut oil purchase is in Guangzhou prestige Buddhist nun
Come Chemical Co., Ltd., above-mentioned producer can also be not limited to certainly.
Specific embodiment
Example 1
The preparation method of fire-retardant, waterproof, fast light aqueous polyurethane coating and adhesive, preparation method are:
(1)The preparation of fire retardant:By tetrakis hydroxymetyl phosphonium sulfuric 1mol, gamma-aminopropyl-triethoxy-silane 0.4mol and phosphoric acid
3mol is added in three-necked flask, adds triethylamine 5%(Tetrakis hydroxymetyl phosphonium sulfuric and γ-aminopropyl triethoxysilane are total
The 5% of weight)It is 4.2g, 90 DEG C of reaction 3h with catalyst A, cools to 70 DEG C, react 2h, then be warming up to 90 DEG C, 1mol bis- is added
Ethanol amine, anesin 0.3mol and 0.1mol trimethyl hydroxyethylammonium propane diamine react 2h, obtain the fire retardant.
(2)The preparation of waterproofing agent:By acrylic acid 10g, trimethyl hydroxyethylammonium propane diamine 1.6g and hydroxy-ethyl acrylate 0.7g
It is added in there-necked flask, adds initiator 0.6g, 70g water is then added, is gradually warming up to 85 DEG C, sequentially adds 22g cocounut oil
Fatty acid, 16g diglycollic amide and trimethylolpropane 6.9g are uniformly mixed, and are warming up to 70 DEG C, are stirred to being completely dissolved, instead
Answer 2h to get the waterproofing agent.
(3)It is 0.16g, poly- tetrahydro that catalyst B is added in the 500ml there-necked flask for having blender, condenser pipe, thermometer
Furans ether glycol 76g and isocyanates 14g, reacts 0.5h at 70 DEG C, obtains base polyurethane prepolymer for use as A;To base polyurethane prepolymer for use as A
Middle addition step(1)Fire retardant 0.6g, parachlorobenzoyl chloride 1.2g and the solvent DMF 11.2g, reacts under the conditions of 60 DEG C
4g step is added in 2h(2)Waterproofing agent and trimellitic anhydride 1.2g, 80 DEG C of reaction temperature, reaction time 1h, be added 6.5g tri-
Ethamine carries out neutralization reaction 60min, and water 90g is added and is stirred emulsification 1h, obtains fire-retardant, waterproof, fast light aqueous polyurethane applies
Material and adhesive.
Catalyst A is 2,4- dichloronitrobenzene;Catalyst B is para orientation nitration;The polytetrahydrofuran ether glycol
Molecular weight be 250;Isocyanates is hexamethylene diisocyanate;Initiator is ammonium persulfate.
Example 2
The preparation method of fire-retardant, waterproof, fast light aqueous polyurethane coating and adhesive, preparation method are:
(1)The preparation of fire retardant:By tetrakis hydroxymetyl phosphonium sulfuric 1mol, gamma-aminopropyl-triethoxy-silane 0.4mol and phosphoric acid
3mol is added in three-necked flask, adds triethylamine 5%(Tetrakis hydroxymetyl phosphonium sulfuric and γ-aminopropyl triethoxysilane are total
The 5% of weight)It is 4.2g, 120 DEG C of reaction 5h with catalyst A, cools to 80 DEG C, react 5h, then be warming up to 100 DEG C, is added
2mol diethanol amine, anesin 0.3mol and 0.1mol trimethyl hydroxyethylammonium propane diamine react 6h, obtain the fire retardant.
(2)The preparation of waterproofing agent:By acrylic acid 10g, trimethyl hydroxyethylammonium propane diamine 1.6g and hydroxy-ethyl acrylate 0.7g
It is added in there-necked flask, adds initiator 0.6g, 70g water is then added, is gradually warming up to 85 DEG C, sequentially adds 22g cocounut oil
Fatty acid, 16g diglycollic amide and trimethylolpropane 6.9g are uniformly mixed, are warming up to 70 DEG C, and stirring is stirred to being completely dissolved
It mixes, reacts 2h to get the waterproofing agent.
(3)It is 0.16g, poly- tetrahydro that catalyst B is added in the 500ml there-necked flask for having blender, condenser pipe, thermometer
Furans ether glycol 76g and isocyanates 14g, reacts 2h at 80 DEG C, obtains base polyurethane prepolymer for use as A;Into base polyurethane prepolymer for use as A
Step is added(1)Fire retardant 0.6g, parachlorobenzoyl chloride 1.2g and the solvent DMF 11.2g, reacts under the conditions of 80 DEG C
4g step is added in 3.5h(2)Waterproofing agent and trimellitic anhydride 1.2g, 80 DEG C of reaction temperature, reaction time 1h, be added 6.5g
Triethylamine carries out neutralization reaction 60min, and water 110g is added and is stirred emulsification 1h, obtains fire-retardant, waterproof, fast light aqueous polyurethane
Coating and adhesive.
Catalyst A paranitroanilinum;Catalyst B is benzyl benzene;The molecular weight of the polytetrahydrofuran ether glycol is
650;Isocyanates is toluene di-isocyanate(TDI);Initiator is potassium peroxydisulfate.
Example 3
The preparation method of fire-retardant, waterproof, fast light aqueous polyurethane coating and adhesive, preparation method are:
(1)The preparation of fire retardant:By tetrakis hydroxymetyl phosphonium sulfuric 1mol, gamma-aminopropyl-triethoxy-silane 0.4mol and phosphoric acid
3mol is added in three-necked flask, adds triethylamine 5%(For tetrakis hydroxymetyl phosphonium sulfuric and γ-aminopropyl triethoxysilane
The 5% of total weight)It is 4.2g, 105 DEG C of reaction 4h with catalyst A, cools to 75 DEG C, react 3.5h, then be warming up to 95 DEG C, is added
1.5mol diethanol amine, anesin 0.3mol and 0.1mol trimethyl hydroxyethylammonium propane diamine react 4h, it is fire-retardant to obtain this
Agent.
(2)The preparation of waterproofing agent:By acrylic acid 10g, trimethyl hydroxyethylammonium propane diamine 1.6g and hydroxy-ethyl acrylate 0.7g
It is added in there-necked flask, adds initiator 0.6g, 70g water is then added, is gradually warming up to 85 DEG C, sequentially adds 22g cocounut oil
Fatty acid, 16g diglycollic amide and trimethylolpropane 6.9g are uniformly mixed, and are warming up to 70 DEG C, are stirred to being completely dissolved, instead
Answer 2h to get the waterproofing agent.
(3)It is 0.16g, poly- tetrahydro that catalyst B is added in the 500ml there-necked flask for having blender, condenser pipe, thermometer
Furans ether glycol 76g and isocyanates 14g, reacts 1.5h at 75 DEG C, obtains base polyurethane prepolymer for use as A;To base polyurethane prepolymer for use as A
Middle addition step(1)Fire retardant 0.6g, parachlorobenzoyl chloride 1.2g and the solvent DMF 11.2g, reacts under the conditions of 70 DEG C
4g step is added in 3h(2)Waterproofing agent and trimellitic anhydride 1.2g, 80 DEG C of reaction temperature, reaction time 1h, be added 6.5g tri-
Ethamine carries out neutralization reaction 60min, and water 100g is added and is stirred emulsification 1h, obtains fire-retardant, waterproof, fast light aqueous polyurethane applies
Material and adhesive.
Catalyst A is hydroxyl sulfate;Catalyst B is diisopropyl dimethoxy silane;The polytetrahydrofuran ether two
The molecular weight of alcohol is 1000;Isocyanates is isophorone diisocyanate;Initiator is potassium peroxydisulfate.
Example 4
The preparation method of fire-retardant, waterproof, fast light aqueous polyurethane coating and adhesive, preparation method are:
(1)The preparation of fire retardant:By tetrakis hydroxymetyl phosphonium sulfuric 1mol, gamma-aminopropyl-triethoxy-silane 0.4mol and phosphoric acid
3mol is added in three-necked flask, adds triethylamine 5%(Tetrakis hydroxymetyl phosphonium sulfuric and γ-aminopropyl triethoxysilane are total
The 5% of weight)It is 4.2g, 120 DEG C of reaction 5h with catalyst A, cools to 80 DEG C, react 2h, then be warming up to 90 DEG C, 1mol is added
Diethanol amine, anesin 0.3mol and 0.1mol trimethyl hydroxyethylammonium propane diamine react 2h, obtain the fire retardant.
(2)The preparation of waterproofing agent:By acrylic acid 10g, trimethyl hydroxyethylammonium propane diamine 1.6g and hydroxy-ethyl acrylate 0.7g
It is added in there-necked flask, adds initiator 0.6g, 70g water is then added, is gradually warming up to 85 DEG C, sequentially adds 22g cocounut oil
Fatty acid, 16g diglycollic amide and trimethylolpropane 6.9g are uniformly mixed, and are warming up to 70 DEG C, are stirred to being completely dissolved, instead
Answer 2h to get the waterproofing agent.
(3)It is 0.16g, poly- tetrahydro that catalyst B is added in the 500ml there-necked flask for having blender, condenser pipe, thermometer
Furans ether glycol 76g and isocyanates 14g, reacts 0.5h at 80 DEG C, obtains base polyurethane prepolymer for use as A;To base polyurethane prepolymer for use as A
Middle addition step(1)Fire retardant 0.6g, parachlorobenzoyl chloride 1.2g and the solvent DMF 11.2g, reacts under the conditions of 60 DEG C
4g step is added in 3.5h(2)Waterproofing agent and trimellitic anhydride 1.2g, 80 DEG C of reaction temperature, reaction time 1h, be added 6.5g
Triethylamine carries out neutralization reaction 60min, and water 110g is added and is stirred emulsification 1h, obtains fire-retardant, waterproof, fast light aqueous polyurethane
Coating and adhesive.
Catalyst A is hydroxylamine chloride;Catalyst B is 3- dimethylamine propylamine;Point of the polytetrahydrofuran ether glycol
Son amount is 1800;Isocyanates is 4,4'- dicyclohexyl methyl hydride diisocyanate;Initiator is ammonium persulfate.
Example 5
The preparation method of fire-retardant, waterproof, fast light aqueous polyurethane coating and adhesive, preparation method are:
(1)The preparation of fire retardant:By tetrakis hydroxymetyl phosphonium sulfuric 1mol, gamma-aminopropyl-triethoxy-silane 0.4mol and phosphoric acid
3mol is added in three-necked flask, adds triethylamine 5%(Tetrakis hydroxymetyl phosphonium sulfuric and γ-aminopropyl triethoxysilane are total
The 5% of weight)It is 4.2g, 120 DEG C of reaction 5h with catalyst A, cools to 70 DEG C, react 2h, then be warming up to 90 DEG C, 1mol is added
Diethanol amine, anesin 0.3mol and 0.1mol trimethyl hydroxyethylammonium propane diamine react 2h, obtain the fire retardant.
(2)The preparation of waterproofing agent:By acrylic acid 10g, trimethyl hydroxyethylammonium propane diamine 1.6g and hydroxy-ethyl acrylate 0.7g
It is added in there-necked flask, adds initiator 0.6g, 70g water is then added, is gradually warming up to 85 DEG C, sequentially adds 22g cocounut oil
Fatty acid, 16g diglycollic amide and trimethylolpropane 6.9g are uniformly mixed, and are warming up to 70 DEG C, are stirred to being completely dissolved, i.e.,
Obtain the waterproofing agent.
(3)It is 0.16g, poly- tetrahydro that catalyst B is added in the 500ml there-necked flask for having blender, condenser pipe, thermometer
Furans ether glycol 76g and isocyanates 14g, reacts 2h at 70 DEG C, obtains base polyurethane prepolymer for use as A;Into base polyurethane prepolymer for use as A
Step is added(1)Fire retardant 0.6g, parachlorobenzoyl chloride 1.2g and the solvent DMF 11.2g, reacts under the conditions of 60 DEG C
4g step is added in 2h(2)Waterproofing agent and trimellitic anhydride 1.2g, 80 DEG C of reaction temperature, reaction time 1h, be added 6.5g tri-
Ethamine carries out neutralization reaction 60min, and water 90g is added and is stirred emulsification 1h, obtains fire-retardant, waterproof, fast light aqueous polyurethane applies
Material and adhesive.
Catalyst A is 2,4- dichloronitrobenzene;Catalyst B is benzyl benzene;The molecule of the polytetrahydrofuran ether glycol
Amount is 2000;Isocyanates is toluene di-isocyanate(TDI);Initiator is ammonium persulfate.
Anti-flammability is measured by oxygen index (OI), flaming combustion time, and light resistance is by measuring it in simulated solar illumination
Under ultraviolet lamp under penetrating, irradiation time 48h observes color change, and wherein anti-flammability and light resistance are and measure its polyurethane to apply
Expect that formed a film performance and dilatancy are that Muffle furnace is heated to 500 DEG C, 1g will be housed(Error is no more than 0.1g)Crucible, set
10min is heated in Muffle furnace, measures expansion rate and surplus charcoal rate(Only measure fire retardant).
1 test performance of table
Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
Oxygen index (OI)/% | 29.2 | 29.6 | 29.5 | 29.8 | 29.7 |
Flaming combustion time/s | 5.3 | 5.6 | 4.5 | 4.4 | 4.9 |
Surplus charcoal rate/% of fire retardant | 65.3 | 67.9 | 68.7 | 65.7 | 66.8 |
Fire retardant expansion rate | 69.8 | 68.9 | 68.7 | 69.2 | 69.7 |
Light resistance/grade | 3.5 | 4.0 | 4.0 | 3.5 | 3.5 |
Waterproofness(0.3Mpa)30min | It is water-tight | It is water-tight | It is water-tight | It is water-tight | It is water-tight |
As it can be seen from table 1 the polyurethane coating and adhesive are in oxygen index (OI), flaming combustion time, light resistance and waterproofness side
Face is superior to the performance of the patent of invention mentioned in background technique.
2 test performance of table(Fire retardant is not added)
Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
Oxygen index (OI)/% | 21.7 | 21.6 | 22.3 | 23.7 | 22.5 |
Flaming combustion time/s | 16.9 | 24.7 | 29.8 | 35.6 | 36.9 |
From table 2 it can be seen that not adding the flame retardant property decline of the fire retardant polyurethane coating.
3 test performance of table(Add fire retardant, but does not add catalyst A)
Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
Oxygen index (OI)/% | 25.4 | 24.8 | 25.3 | 24.9 | 25.1 |
Flaming combustion time/s | 8.9 | 12.1 | 16.5 | 21.3 | 22.3 |
Surplus charcoal rate/% of fire retardant | 52.6 | 53.9 | 57.8 | 55.2 | 51.4 |
Fire retardant expansion rate | 61.5 | 54.9 | 58.9 | 59.6 | 60.5 |
From table 3 it can be seen that fire retardant is added but catalyst A is not added getting well than table 2 in terms of anti-flammability.
4 test performance of table(Do not add fire retardant, add catalyst A, not plus trimethyl hydroxyethylammonium propane diamine)
Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
Surplus charcoal rate/% of fire retardant | 54.6 | 55.3 | 52.3 | 56.9 | 54.8 |
From table 4, it can be seen that trimethyl hydroxyethylammonium propane diamine has the effect of improving surplus charcoal rate.
5 test performance of table(Not plus waterproofing agent)
Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
Waterproofness(0.3Mpa)30min | Leak | Leak | Leak | Leak | Leak |
As can be seen from Table 5, waterproofing agent plays relatively good waterproofness.
6 test performance of table(Add waterproofing agent, non-biasing benzenetricarboxylic anhydride)
Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
Waterproofness(0.3Mpa)30min | Leak | It is water-tight | Leak | It is water-tight | Leak |
As can be seen from Table 6, add waterproofing agent and trimellitic anhydride is not added, will lead to part formulation leak.
Claims (6)
1. the preparation method of fire-retardant, waterproof, fast light aqueous polyurethane coating and adhesive, preparation method are:
(1)The preparation of fire retardant:By tetrakis hydroxymetyl phosphonium sulfuric 1mol, gamma-aminopropyl-triethoxy-silane 0.4mol and phosphoric acid
3mol is added in three-necked flask, adds triethylamine 5%(Tetrakis hydroxymetyl phosphonium sulfuric and γ-aminopropyl triethoxysilane are total
The 5% of weight)It is 4.2g, 90-120 DEG C of 3 ~ 5h of reaction with catalyst A, cools to 70 ~ 80 DEG C, 2 ~ 5h of reaction, then it is warming up to 90 ~
100 DEG C, 1 ~ 2mol diethanol amine, anesin 0.3mol and 0.1mol trimethyl hydroxyethylammonium propane diamine, reaction time 2 is added
~ 6h obtains the fire retardant;
(2)The preparation of waterproofing agent:Acrylic acid 10g, trimethyl hydroxyethylammonium propane diamine 1.6g and hydroxy-ethyl acrylate 0.7g are added
Into there-necked flask, initiator 0.6g is added, 70g water is then added, is gradually warming up to 85 DEG C, sequentially adds 22g coconut oil fat
Acid, 16g diglycollic amide and trimethylolpropane 6.9g are uniformly mixed, are warming up to 70 DEG C, and stirring is to being completely dissolved to get this
Waterproofing agent;
(3)It is 0.16g, polytetrahydrofuran that catalyst B is added in the 500ml there-necked flask for having blender, condenser pipe, thermometer
Ether glycol 76g and isocyanates 14g reacts 0.5 ~ 2h at 70 ~ 80 DEG C, obtains base polyurethane prepolymer for use as A;To base polyurethane prepolymer for use as
Step is added in A(1)Fire retardant 0.6g, parachlorobenzoyl chloride 1.2g and the solvent DMF 11.2g, under the conditions of 60 ~ 80 DEG C
2 ~ 3.5h is reacted, 4g step is added(2)Waterproofing agent and trimellitic anhydride 1.2g, 80 DEG C of reaction temperature, reaction time 1h adds
Enter 6.5g triethylamine and carry out neutralization reaction 60min, 90 ~ 110g of water is added and is stirred emulsification 1h, obtains fire-retardant, waterproof, fast light
Aqueous polyurethane coating and adhesive.
2. fire-retardant, waterproof, the preparation method of fast light aqueous polyurethane coating and adhesive as described in right 1, catalyst A are
Any one of 2,4- dichloronitrobenzene, paranitroanilinum, hydroxyl sulfate, hydroxylamine chloride.
3. such as fire-retardant, waterproof, the preparation method of fast light aqueous polyurethane coating and adhesive as described in right 1, catalyst B
For para orientation nitration, benzyl benzene, diisopropyl dimethoxy silane, 3- dimethylamine propylamine
Any one.
4. fire-retardant, waterproof, the preparation method of fast light aqueous polyurethane coating and adhesive as described in right 1, described poly- four
Any one that the molecular weight of hydrogen furans ether glycol is 250,650,1000,1800,2000,2900.
5. fire-retardant, waterproof, the preparation method of fast light aqueous polyurethane coating and adhesive as described in right 1, the isocyanide
Acid esters is hexamethylene diisocyanate, toluene di-isocyanate(TDI), isophorone diisocyanate, 4,4'- dicyclohexyl methyl hydride
Any one of diisocyanate.
6. the preparation method of fire-retardant, fast light aqueous polyurethane coating and adhesive as described in right 1, the initiator were
Any one of ammonium sulfate, potassium peroxydisulfate.
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CN113667429A (en) * | 2021-08-19 | 2021-11-19 | 矽时代材料科技股份有限公司 | Ultraviolet-curing heat-conducting adhesive tape and preparation method and application thereof |
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