CN101818040A - Fast-curing one-component polyurethane sealant and preparation method thereof - Google Patents
Fast-curing one-component polyurethane sealant and preparation method thereof Download PDFInfo
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- CN101818040A CN101818040A CN 201010154771 CN201010154771A CN101818040A CN 101818040 A CN101818040 A CN 101818040A CN 201010154771 CN201010154771 CN 201010154771 CN 201010154771 A CN201010154771 A CN 201010154771A CN 101818040 A CN101818040 A CN 101818040A
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- 239000004588 polyurethane sealant Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910000077 silane Inorganic materials 0.000 claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002318 adhesion promoter Substances 0.000 claims abstract description 9
- 239000000945 filler Substances 0.000 claims abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 8
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 7
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 5
- -1 titanic acid ester Chemical class 0.000 claims description 37
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims description 29
- 238000006243 chemical reaction Methods 0.000 claims description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 18
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 14
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 14
- 229920005862 polyol Polymers 0.000 claims description 13
- 239000004135 Bone phosphate Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 238000004448 titration Methods 0.000 claims description 10
- DXPZFIQSWQVTOO-UHFFFAOYSA-N 3-[3-aminopropyl(dimethoxy)silyl]oxy-4-phenylbutan-1-amine Chemical compound NCCC[Si](OC)(OC)OC(CCN)CC1=CC=CC=C1 DXPZFIQSWQVTOO-UHFFFAOYSA-N 0.000 claims description 9
- 239000005977 Ethylene Substances 0.000 claims description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 9
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 9
- 239000000292 calcium oxide Substances 0.000 claims description 9
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 9
- 239000006229 carbon black Substances 0.000 claims description 9
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 9
- 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 claims description 8
- 239000004902 Softening Agent Substances 0.000 claims description 8
- 239000012948 isocyanate Substances 0.000 claims description 8
- 229910002012 Aerosil® Inorganic materials 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 125000000524 functional group Chemical group 0.000 claims description 6
- 230000005587 bubbling Effects 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 230000009974 thixotropic effect Effects 0.000 claims description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 4
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 3
- 239000004800 polyvinyl chloride Substances 0.000 claims description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 2
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 2
- 239000005995 Aluminium silicate Substances 0.000 claims description 2
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 2
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 229940045714 alkyl sulfonate alkylating agent Drugs 0.000 claims description 2
- 150000008052 alkyl sulfonates Chemical class 0.000 claims description 2
- 235000012211 aluminium silicate Nutrition 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- DDSWIYVVHBOISO-UHFFFAOYSA-N ctk0i1982 Chemical compound N[SiH](N)N DDSWIYVVHBOISO-UHFFFAOYSA-N 0.000 claims description 2
- JUESRADRPFMUCL-UHFFFAOYSA-N dimethoxy-methyl-(2-methylpropyl)silane Chemical compound CO[Si](C)(OC)CC(C)C JUESRADRPFMUCL-UHFFFAOYSA-N 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 claims description 2
- DTIFFOYIBPJUET-UHFFFAOYSA-N n'-(3-trimethylsilylpropyl)ethane-1,2-diamine Chemical compound C[Si](C)(C)CCCNCCN DTIFFOYIBPJUET-UHFFFAOYSA-N 0.000 claims description 2
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 claims description 2
- 229920005906 polyester polyol Polymers 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 239000011863 silicon-based powder Substances 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 2
- QLNOVKKVHFRGMA-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical group [CH2]CC[Si](OC)(OC)OC QLNOVKKVHFRGMA-UHFFFAOYSA-N 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000004793 Polystyrene Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 238000004132 cross linking Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 229920002223 polystyrene Polymers 0.000 abstract description 2
- 239000000565 sealant Substances 0.000 abstract description 2
- 239000000377 silicon dioxide Substances 0.000 abstract description 2
- 239000000853 adhesive Substances 0.000 abstract 1
- 239000000919 ceramic Substances 0.000 abstract 1
- 230000008878 coupling Effects 0.000 abstract 1
- 238000010168 coupling process Methods 0.000 abstract 1
- 238000005859 coupling reaction Methods 0.000 abstract 1
- 239000004014 plasticizer Substances 0.000 abstract 1
- 229920000058 polyacrylate Polymers 0.000 abstract 1
- 239000004432 silane-modified polyurethane Substances 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 238000001723 curing Methods 0.000 description 17
- 238000005516 engineering process Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000013008 moisture curing Methods 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 150000003673 urethanes Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Sealing Material Composition (AREA)
Abstract
The invention relates to a sealant, in particular to a fast-curing one-component polyurethane sealant and a preparation method thereof. The fast-curing one-component polyurethane sealant is characterized by comprising 30%-60% of prepolymer containing silyl-terminated polyurethane, 0.2%-5% of silane coupling adhesion promoter, 0.301%-0.35% of catalyst, 10%-40% of plasticizer, 10%-60% of filler and 0.05-1% of antioxidant, wherein the content of each component is represented by the weight percent. The fast-curing one-component polyurethane sealant has the advantages of fast surface drying, fast curing speed, avoidance of impacts caused by the environmental temperature and the humidity, high cross-linking density, high elongation ratio, good adhesion strength, no solvent, environmental protection and excellent adhesive performance to base materials, such as metal, ceramics, glass, silica PVC, ABC, polystyrene, polyacrylate and the like.
Description
Technical field:
The present invention relates to a kind of seal gum, especially a kind of fast-curing one-component polyurethane sealant and preparation method thereof
Background technology:
In automobile and other vehicle glazing and windshield assembly technology, general edge and the car body sash frame surface that polyurethane sealant is coated in glass that adopt, then glass cementation to car body.Generally adopt at present with the single group moisture cure urethanes seal gum of polyurethane prepolymer as major ingredient, polyurethane prepolymer wherein is to be generated by polyol compound and excessive isocyanic ester polyreaction, because the polyurethane sealant that this method generates contains the NCO group of free state and the water of air reacts curing and is cured adhering glass, it is to the humidity of working-yard, temperature is extremely responsive, hot and humid degree, sealing glue solidifying is fast otherwise curing is slower, because China's four seasons are obvious, the working-yard temperature and humidity alters a great deal, and Hyundai Motor production firm is again pipelining, to temperature, the wet-solidifying single-component polyurethane elastic sealant of humidity sensitive is the requirement of incompatibility Hyundai Motor glass pipelining.
Summary of the invention:
Technical problem to be solved by this invention is the deficiency that overcomes the above-mentioned background technology, provides a kind of and is not subjected to working-yard temperature, humidity effect and speed is fast solidifies bonding fast-curing one-component polyurethane sealant
Technical scheme provided by the invention is:
Fast-curing one-component polyurethane sealant, its composition comprises and contains end-silicane-group polyurethane prepolymer 30%-60%, silane coupled adhesion promoter 0.2%-5%, catalyzer 0.301%-0.35%, softening agent 10%-40%, filler 10%-60%, antioxidant 0.05%-1%, the content of above-mentioned each component is in the quality percentage composition.
Preferably, silane coupled adhesion promoter is selected N-ethylene benzyl aminoethyl aminopropyl trimethoxysilane for use, catalyzer adopts dibutyltin diacetate, titanic acid ester composite catalyst, softening agent is selected dioctyl phthalate (DOP) for use, filler is selected talcum powder, active calcium oxide, carbon black, aerosil, light calcium carbonate for use, and antioxidant is selected Ursol D for use; The fast-curing one-component polyurethane sealant prescription is: end-silicane-group polyurethane prepolymer 42kg, talcum powder 5kg, light calcium carbonate 10kg, active calcium oxide 1kg, carbon black 18kg, aerosil 3kg, dioctyl phthalate (DOP) 19kg, N-ethylene benzyl aminoethyl aminopropyl trimethoxysilane 0.3kg, Ursol D 0.2kg, titanic acid ester 0.4kg, dibutyltin diacetate 0.08kg.
Preferably, the end-silicane-group polyurethane prepolymer is to carry out end capping and obtain with functional group's silane opposite end NCO base polyurethane prepolymer, end NCO base polyurethane prepolymer is to generate with polyol compound and isocyanate compound reaction, and functional group's silane comprises N-phenyl γ-An Bingjisanjiayangjiguiwan, γ-urea groups propyl trimethoxy silicane, two (γ-trimethoxy silyl propyl group) amine, N-β-aminoethyl-γ-aminopropyl trimethyl silane, γ-An Bingjisanjiayangjiguiwan, the γ aminopropyl triethoxysilane, γ-sulfenyl propyl trimethoxy silicane, γ-Racemic glycidol oxygen propyl trimethoxy silicane.
Preferably, polyol compound is from polyether glycol, polyester polyol, other main chains contain in the end carboxylic compound of C-C chooses any one kind of them or several combination, isocyanate compound is from tolylene diisocyanate, diphenylmethanediisocyanate, different Buddhist ketone that vulcabond, chooses any one kind of them in the 1-6-hexamethylene diisocyanate or several combination.
Preferably, silane coupled adhesion promoter is from the gamma-methyl allyl acyloxypropyl methoxy silane, triamino silane, two [3-(trimethoxy silyl) propyl group] amine of N-N-, N-β-aminoethyl-γ-An Bingjisanjiayangjiguiwan, N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane, γ-Huan Yangbingyangbingjisanjiayangjiguiwan, γ-epoxypropoxy methyl dimethoxysilane, N-phenyl-γ-An Bingjisanjiayangjiguiwan, N-phenyl-γ-ammonia isobutyl-methyl dimethoxysilane, dredge basic propyl trimethoxy silicane, the γ aminopropyl trimethoxysilane, γ-An Bingjisanyiyangjiguiwan, choose any one kind of them or several combination in the N-ethylene benzyl aminoethyl aminopropyl trimethoxysilane.
Preferably, catalyzer adopts dibutyltin diacetate, titanic acid ester composite catalyst; Wherein dibutyltin diacetate content is the 0.001%-0.5% of fast-curing one-component polyurethane sealant total mass, and titanic acid ester content is the 0.3%-3% of fast-curing one-component polyurethane sealant total mass.
Preferably, softening agent is to choose any one kind of them from phthalate, alkyl sulfonates, clorafin or several combination.
Preferably, select for use and choose any one kind of them in active calcium oxide, silicon powder, light calcium carbonate, carbon black, polyvinyl chloride resin, talcum powder, titanium dioxide, vacuum glass microballoon, the kaolin or several filler that is mixed into.
The preparation method of described fast-curing one-component polyurethane sealant comprises the steps:
1) getting polyol compound adds in the vacuum reaction still, allow polyol compound under 110 ℃ vacuum environment, dewater 2 hours, make the moisture in the polyol compound be not more than 0.01%, after then the temperature of charge in the vacuum reaction still being reduced to 50 ℃, add isocyanate compound, under nitrogen protection, stir, be heated to 82 ℃, allow polyol compound and isocyanate compound react 4 hours, obtain holding the NCO base polyurethane prepolymer;
2) will hold the NCO base polyurethane prepolymer to add vacuum reaction still internal heating to 50 ℃, under nitrogen protection, add functional group's silane stirring reaction material and slowly rise to 70 ℃, react the phenomenon that occurs appropriate bubbling and slight heat release after 1 hour, begin this moment the NCO base content of system is carried out titrimetry, be reacted to titration always and represent not exist till the free NCO base, cooling, discharging then, finish synthetic;
3) at room temperature in duplicate rows star stirring tank, add the end-silicane-group polyurethane prepolymer in proper order; silane coupled adhesion promoter; catalyzer; softening agent, filler, antioxidant; under vacuum protection, mix, be cooled to 30 ℃; add catalyzer, stir, can obtain thixotropic fast-curing one-component polyurethane sealant.
Preferably, the preparation method of fast-curing one-component polyurethane sealant comprises the steps:
1) gets in polyether-tribasic alcohol (molecular-weight average 4500) the adding vacuum reaction still of 85kg, allow polyether-tribasic alcohol 110 ℃ with under the vacuum environment dehydration 2 hours, make the moisture in the polyether-tribasic alcohol be not more than 0.01%, after then the temperature in the vacuum reaction still being reduced to 50 ℃, add the 15kg diphenylmethanediisocyanate, under nitrogen protection, stir, be heated to 82 ℃, allow polyether-tribasic alcohol and diphenylmethanediisocyanate react 4 hours, obtain holding the NCO base polyurethane prepolymer;
2) 102kg is held the NCO base polyurethane prepolymer add vacuum reaction still internal heating to 50 ℃, under nitrogen protection, add 34kg γ-An Bingjisanjiayangjiguiwan stirring reaction material and slowly rise to 70 ℃, react the phenomenon that occurs appropriate bubbling and slight heat release after 1 hour, begin this moment the NCO base content of system is carried out titrimetry, be reacted to titration always and represent not exist till the free NCO base, cooling, discharging then, finish synthetic;
3) at room temperature in duplicate rows star stirring tank, add 42kg end-silicane-group polyurethane prepolymer in proper order; the 5kg talcum powder; the 10kg light calcium carbonate; the 1kg active calcium oxide; the 18kg carbon black; the 3kg aerosil; the 19kg dioctyl phthalate (DOP); N-ethylene benzyl aminoethyl aminopropyl trimethoxysilane 0.3kg; Ursol D 0.2kg mixes, is cooled to 30 ℃ under vacuum protection, add 0.4kg titanic acid ester and dibutyltin diacetate 80g; stir, can obtain thixotropic fast-curing one-component polyurethane sealant.
Fast-curing one-component polyurethane sealant surface drying of the present invention is fast, curing speed is fast,, be not subjected to envrionment temperature, humidity effect, cross-linking density height, elongation height, bonding strength good, solvent-free, environmental protection, base materials such as metal, pottery, glass, silica PVC, ABC, polystyrene, polyacrylic ester possessed excellent adhesiveproperties, can be used for industrial circles such as automobile industry, transport trade, construction industry, equipment manufacture industry, the vehicle window of the car industry of especially suitable pipelining and the bonding assembling of windshield.
Embodiment
The preparation method of end NCO base polyurethane prepolymer:
The polyether-tribasic alcohol (molecular-weight average 4500) of getting 85kg adds in the vacuum reaction still; allow polyether-tribasic alcohol 110 ℃ with under the vacuum environment dehydration 2 hours; make the moisture in the polyether-tribasic alcohol be not more than 0.01%; after then the temperature in the vacuum reaction still being reduced to 50 ℃, add the 15kg diphenylmethanediisocyanate, under nitrogen protection; stir; be heated to 82 ℃, allow polyether-tribasic alcohol and diphenylmethanediisocyanate react 4 hours, obtain a kind of end NCO base polyurethane prepolymer.
The preparation method of end-silicane-group polyurethane prepolymer:
Hold the NCO base polyurethane prepolymer to add vacuum reaction still internal heating to 50 ℃ 102kg; under nitrogen protection, add 34kg γ-An Bingjisanjiayangjiguiwan stirring reaction material and slowly rise to 70 ℃; react the phenomenon that occurs appropriate bubbling and slight heat release after 1 hour, begin this moment the NCO base content of system is carried out titration.Be reacted to titration represents not exist till the free NCO base always.Cooling, discharging then, finish synthetic.
The fast-curing one-component polyurethane sealant preparation method:
At room temperature order adds 42kg end-silicane-group polyurethane prepolymer in duplicate rows star stirring tank; the 5kg talcum powder; the 10kg light calcium carbonate; the 1kg active calcium oxide; the 18kg carbon black; the 3kg aerosil; the 19kg dioctyl phthalate (DOP), N-ethylene benzyl aminoethyl aminopropyl trimethoxysilane 0.3kg, Ursol D 0.2kg; under vacuum protection, mix, be cooled to 30 ℃; add 0.4kg titanic acid ester and dibutyltin diacetate 80g, stir, can obtain thixotropic fast-curing one-component polyurethane sealant.
Claims (10)
1. fast-curing one-component polyurethane sealant, it is characterized in that its composition comprises contains end-silicane-group polyurethane prepolymer 30%-60%, silane coupled adhesion promoter 0.2%-5%, catalyzer 0.301%-0.35%, softening agent 10%-40%, filler 10%-60%, antioxidant 0.05%-1%, the content of above-mentioned each component is in the quality percentage composition.
2. according to the described fast-curing one-component polyurethane sealant of claim 1, it is characterized in that,
Silane coupled adhesion promoter is selected N-ethylene benzyl aminoethyl aminopropyl trimethoxysilane for use, catalyzer adopts dibutyltin diacetate, titanic acid ester composite catalyst, softening agent is selected dioctyl phthalate (DOP) for use, filler is selected talcum powder, active calcium oxide, carbon black, aerosil, light calcium carbonate for use, and antioxidant is selected Ursol D for use;
The fast-curing one-component polyurethane sealant prescription is: end-silicane-group polyurethane prepolymer 42kg, talcum powder 5kg, light calcium carbonate 10kg, active calcium oxide 1kg, carbon black 18kg, aerosil 3kg, dioctyl phthalate (DOP) 19kg, N-ethylene benzyl aminoethyl aminopropyl trimethoxysilane 0.3kg, Ursol D 0.2kg, titanic acid ester 0.4kg, dibutyltin diacetate 0.08kg.
3. according to claim 1 or 2 described fast-curing one-component polyurethane sealants, it is characterized in that, the end-silicane-group polyurethane prepolymer is to carry out end capping and obtain with functional group's silane opposite end NCO base polyurethane prepolymer, end NCO base polyurethane prepolymer is to generate with polyol compound and isocyanate compound reaction, and functional group's silane comprises N-phenyl γ-An Bingjisanjiayangjiguiwan, γ-urea groups propyl trimethoxy silicane, two (γ-trimethoxy silyl propyl group) amine, N-β-aminoethyl-γ-aminopropyl trimethyl silane, γ-An Bingjisanjiayangjiguiwan, the γ aminopropyl triethoxysilane, γ-sulfenyl propyl trimethoxy silicane, γ-Racemic glycidol oxygen propyl trimethoxy silicane.
4. according to the described fast-curing one-component polyurethane sealant of claim 3, it is characterized in that, polyol compound is from polyether glycol, polyester polyol, other main chains contain in the end carboxylic compound of C-C chooses any one kind of them or several combination, isocyanate compound is from tolylene diisocyanate, diphenylmethanediisocyanate, different Buddhist ketone that vulcabond, chooses any one kind of them in the 1-6-hexamethylene diisocyanate or several combination.
5. according to the described fast-curing one-component polyurethane sealant of claim 1, it is characterized in that silane coupled adhesion promoter is from the gamma-methyl allyl acyloxypropyl methoxy silane, triamino silane, two [3-(trimethoxy silyl) propyl group] amine of N-N-, N-β-aminoethyl-γ-An Bingjisanjiayangjiguiwan, N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane, γ-Huan Yangbingyangbingjisanjiayangjiguiwan, γ-epoxypropoxy methyl dimethoxysilane, N-phenyl-γ-An Bingjisanjiayangjiguiwan, N-phenyl-γ-ammonia isobutyl-methyl dimethoxysilane, dredge basic propyl trimethoxy silicane, the γ aminopropyl trimethoxysilane, γ-An Bingjisanyiyangjiguiwan, choose any one kind of them or several combination in the N-ethylene benzyl aminoethyl aminopropyl trimethoxysilane.
6. according to the described fast-curing one-component polyurethane sealant of claim 1, it is characterized in that catalyzer adopts dibutyltin diacetate, titanic acid ester composite catalyst; Wherein dibutyltin diacetate content is the 0.001%-0.5% of fast-curing one-component polyurethane sealant total mass, and titanic acid ester content is the 0.3%-3% of fast-curing one-component polyurethane sealant total mass.
7. according to the described fast-curing one-component polyurethane sealant of claim 1, it is characterized in that softening agent is to choose any one kind of them or several combination from phthalate, alkyl sulfonates, clorafin.
8. according to the described fast-curing one-component polyurethane sealant of claim 1, it is characterized in that, select for use and choose any one kind of them in active calcium oxide, silicon powder, light calcium carbonate, carbon black, polyvinyl chloride resin, talcum powder, titanium dioxide, vacuum glass microballoon, the kaolin or several filler that is mixed into.
9. the preparation method of fast-curing one-component polyurethane sealant according to claim 1 is characterized in that: comprise the steps:
1) getting polyol compound adds in the vacuum reaction still, allow polyol compound under 110 ℃ vacuum environment, dewater 2 hours, make the moisture in the polyol compound be not more than 0.01%, after then the temperature of charge in the vacuum reaction still being reduced to 50 ℃, add isocyanate compound, under nitrogen protection, stir, be heated to 82 ℃, allow polyol compound and isocyanate compound react 4 hours, obtain holding the NCO base polyurethane prepolymer;
2) will hold the NCO base polyurethane prepolymer to add vacuum reaction still internal heating to 50 ℃, under nitrogen protection, add functional group's silane stirring reaction material and slowly rise to 70 ℃, react the phenomenon that occurs appropriate bubbling and slight heat release after 1 hour, begin this moment the NCO base content of system is carried out titrimetry, be reacted to titration always and represent not exist till the free NCO base, cooling, discharging then, finish synthetic;
3) at room temperature in duplicate rows star stirring tank, add the end-silicane-group polyurethane prepolymer in proper order; silane coupled adhesion promoter; catalyzer; softening agent, filler, antioxidant; under vacuum protection, mix, be cooled to 30 ℃; add catalyzer, stir, can obtain thixotropic fast-curing one-component polyurethane sealant.
10. as the preparation method of fast-curing one-component polyurethane sealant as described in the claim 9, it is characterized in that: comprise the steps:
1) gets in polyether-tribasic alcohol (molecular-weight average 4500) the adding vacuum reaction still of 85kg, allow polyether-tribasic alcohol 110 ℃ with under the vacuum environment dehydration 2 hours, make the moisture in the polyether-tribasic alcohol be not more than 0.01%, after then the temperature in the vacuum reaction still being reduced to 50 ℃, add the 15kg diphenylmethanediisocyanate, under nitrogen protection, stir, be heated to 82 ℃, allow polyether-tribasic alcohol and diphenylmethanediisocyanate react 4 hours, obtain holding the NCO base polyurethane prepolymer;
2) 102kg is held the NCO base polyurethane prepolymer add vacuum reaction still internal heating to 50 ℃, under nitrogen protection, add 34kg γ-An Bingjisanjiayangjiguiwan stirring reaction material and slowly rise to 70 ℃, react the phenomenon that occurs appropriate bubbling and slight heat release after 1 hour, begin this moment the NCO base content of system is carried out titrimetry, be reacted to titration always and represent not exist till the free NCO base, cooling, discharging then, finish synthetic;
3) at room temperature in duplicate rows star stirring tank, add 42kg end-silicane-group polyurethane prepolymer in proper order; the 5kg talcum powder; the 10kg light calcium carbonate; the 1kg active calcium oxide; the 18kg carbon black; the 3kg aerosil; the 19kg dioctyl phthalate (DOP); N-ethylene benzyl aminoethyl aminopropyl trimethoxysilane 0.3kg; Ursol D 0.2kg mixes, is cooled to 30 ℃ under vacuum protection, add 0.4kg titanic acid ester and dibutyltin diacetate 80g; stir, can obtain thixotropic fast-curing one-component polyurethane sealant.
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