CN105255433A - One-component moisture cured polyurethane sealant excellent in weather resistance and preparation method thereof - Google Patents
One-component moisture cured polyurethane sealant excellent in weather resistance and preparation method thereof Download PDFInfo
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Abstract
The invention discloses one-component moisture cured polyurethane sealant excellent in weather resistance and a preparation method thereof and relates to the field of moisture cured polyurethane sealant. The polyurethane sealant is prepared from, by mass, 20-50 parts of polyurethane prepolymers, 0.5-2 parts of water absorbing and stabilizing agents, 0.1-0.7 part of silane coupling agents, 0.1-1 part of light stabilizing agents, 0.1-1 part of antioxidant, 2-10 parts of titanium dioxide, 28-50 parts of polyurethane-used filling materials, 1-35 parts of thixotropic agents and 0.4-2 parts of first catalysts. According to the polyurethane sealant, the light stabilizing agents and the antioxidant are added, in the process of preparing the polyurethane prepolymers, alicyclic or cycloaliphatic isocyanate is used for replacing 4, 4'-diphenylmethane diisocyanate in the existing polyurethane prepolymers, and the polyurethane sealant is not prone to yellowing under ultraviolet irradiation for a long time, slow in mechanical performance degradation and suitable for being used for a long time.
Description
Technical field
The present invention relates to damp solidifying polyurethane seal gum field, specifically relate to single-component damp solidifying polyurethane seal gum had excellent weather resistance and preparation method thereof.
Background technology
From 20 century 70 mid-terms, the advantages such as single-component damp solidifying polyurethane seal gum is strong with its snappiness, shock resistance, resistance to chemical attack, quality are light, more and more widely for the outside of the industries such as automobile, building, track traffic and seal inside bonding.
Although stabilized polyurethane technology develops to some extent, the UV resistant performance of polyurethane sealant can be improved by adding auxiliary agent, still there is following shortcoming in existing single-component damp solidifying polyurethane seal gum:
(1) under the ultraviolet long-term irradiation effect of natural light, can there is xanthochromia in this polyurethane sealant, affect outward appearance;
(2) due to photoxidation catabiosis, the mechanical property of this polyurethane sealant declines, and colloid surface chaps.
Therefore, the easy xanthochromia of existing single-component damp solidifying polyurethane seal gum, weather resistance is poor, cannot life-time service.
Summary of the invention
The object of the invention is the deficiency in order to overcome above-mentioned background technology, a kind of single-component damp solidifying polyurethane seal gum had excellent weather resistance and preparation method thereof is provided, this polyurethane sealant is under long uviolizing, not easily xanthochromia, mechanical property decay slowly, weather resistance is excellent, is applicable to life-time service.
The invention provides a kind of single-component damp solidifying polyurethane seal gum had excellent weather resistance, in mass fraction, this polyurethane sealant comprises 20 ~ 50 parts of polyurethane prepolymers, 0.5 ~ 2 part of water suction stablizer, 0.1 ~ 0.7 part of silane coupling agent, 0.1 ~ 1 part of photostabilizer, 0.1 ~ 1 part of oxidation inhibitor, 2 ~ 10 parts of titanium dioxides, 28 ~ 50 parts of urethane fillers, 1 ~ 35 part of thixotropic agent, 0.4 ~ 2 part of first catalyzer, and described first catalyzer is any one in organometallics or tertiary amine compounds; Described polyurethane prepolymer comprises 20 ~ 65 parts of polyether glycols, 5 ~ 30 parts of aliphatics or alicyclic isocyanate, 0.01 ~ 0.05 part of second catalyzer, 0 ~ 7 part of thinner, described second catalyzer is dibutyl tin laurate, stannous octoate, dibutyltin diacetate, 2, any one in 2-dual-morpholinyl diethyl ether, 1,8-diazacyclo hendecene; Described water suction stablizer is tolylsulfonyl isocyanic ester; Described titanium dioxide is Rutile type Titanium Dioxide; Described silane coupling agent is any one in γ-glycidyl ether oxygen propyl trimethoxy silicane, β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane, γ-isocyanic ester propyl trimethoxy silicane, γ-isocyanic ester propyl-triethoxysilicane; Described urethane filler is any one in calcium carbonate, calcined kaolin, talcum powder, pvc resin paste grade, hollow glass microballoon, mica powder, diatomite; Described thixotropic agent is any one in hydrophobic type aerosil, organobentonite, polyureas, fibrous talc, anhydrous calcium sulfate whisker, polyamide wax.
On the basis of technique scheme, described polyether glycol is any 2 kinds in polyether Glycols and polyether-tribasic alcohol.
On the basis of technique scheme, described aliphatics or alicyclic isocyanate are any one in hexamethylene diisocyanate, isophorone diisocyanate, HMDI, xylylene diisocyanate.
On the basis of technique scheme, described thinner is any one in toluene, dimethylbenzene, dioctyl phthalate (DOP), Di Iso Decyl Phthalate.
On the basis of technique scheme, described photostabilizer is any one in benzotriazole category, Benzophenones, triazines, hindered amine light stabilizer.
On the basis of technique scheme, described oxidation inhibitor is Hinered phenols and/or phosphorous acid kind antioxidant.
On the basis of technique scheme, described first catalyzer is any one in stannous octoate, lead octoate 36, dibutyl tin laurate, tributyltin chloride, butyiin trichioride, butyltin oxide, triethylenediamine, benzyldimethylamine, pyridine.
The present invention also provides the preparation method of the above-mentioned single-component damp solidifying polyurethane seal gum had excellent weather resistance, and comprises the following steps:
The environment producing and pack this polyurethane sealant answers control temperature≤25 DEG C, relative humidity≤55%RH;
Polyurethane preformed polymer: in mass fraction, 20 ~ 65 parts of polyether glycols are added in the there-necked flask of drying, vacuumize at 120 DEG C of temperature, dehydration 0.5 ~ 1h, be cooled to about 60 DEG C, add 5 ~ 30 parts of aliphatics or alicyclic isocyanate, 0.01 ~ 0.05 part of second catalyzer, 0 ~ 7 part of thinner, described second catalyzer is dibutyl tin laurate, stannous octoate, dibutyltin diacetate, 2, any one in 2-dual-morpholinyl diethyl ether, 1,8-diazacyclo hendecene; Slowly be warming up to 80 DEG C, insulation reaction 3h under drying nitrogen protection, discharging after cooling, obtains polyurethane prepolymer, is loaded in encloses container for subsequent use;
Prepare polyurethane sealant: in mass fraction, 20 ~ 50 parts of polyurethane prepolymers are added in planet stirring still, 0.5 ~ 2 part of water suction stablizer, 0.1 ~ 0.7 part of silane coupling agent, 0.1 ~ 1 part of photostabilizer, the auxiliary agents such as 0.1 ~ 1 part of oxidation inhibitor, after stirring, add pre-dry 2 ~ 10 parts of titanium dioxides, 28 ~ 50 parts of urethane fillers, 1 ~ 35 part of thixotropic agent stirs under vacuum conditions, vacuum is removed with drying nitrogen, add 0.4 ~ 2 part of first catalyzer, described first catalyzer is any one in organometallics or tertiary amine compounds, described water suction stablizer is tolylsulfonyl isocyanic ester, described titanium dioxide is Rutile type Titanium Dioxide, described silane coupling agent is any one in γ-glycidyl ether oxygen propyl trimethoxy silicane, β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane, γ-isocyanic ester propyl trimethoxy silicane, γ-isocyanic ester propyl-triethoxysilicane, described urethane filler is any one in calcium carbonate, calcined kaolin, talcum powder, pvc resin paste grade, hollow glass microballoon, mica powder, diatomite, described thixotropic agent is any one in hydrophobic type aerosil, organobentonite, polyureas, fibrous talc, anhydrous calcium sulfate whisker, polyamide wax, vacuumize, discharging after stirring, obtain the single-component damp solidifying polyurethane seal gum had excellent weather resistance.
On the basis of technique scheme, described polyether glycol is any 2 kinds in polyether Glycols and polyether-tribasic alcohol.
On the basis of technique scheme, described aliphatics or alicyclic isocyanate are any one in hexamethylene diisocyanate, isophorone diisocyanate, HMDI, xylylene diisocyanate.
On the basis of technique scheme, described thinner is any one in toluene, dimethylbenzene, dioctyl phthalate (DOP), Di Iso Decyl Phthalate.
On the basis of technique scheme, described photostabilizer is any one in benzotriazole category, Benzophenones, triazines, hindered amine light stabilizer.
On the basis of technique scheme, described oxidation inhibitor is Hinered phenols and/or phosphorous acid kind antioxidant.
On the basis of technique scheme, described first catalyzer is any one in stannous octoate, lead octoate 36, dibutyl tin laurate, tributyltin chloride, butyiin trichioride, butyltin oxide, triethylenediamine, benzyldimethylamine, pyridine.
Compared with prior art, advantage of the present invention is as follows:
(1) photostabilizer, oxidation inhibitor is added with in the single-component damp solidifying polyurethane seal gum had excellent weather resistance of the present invention, and in the process of polyurethane preformed polymer, use aliphatics or alicyclic isocyanate to replace 4 in existing polyurethane prepolymer, 4 '-diphenylmethanediisocyanate.In ultraviolet ageing case after 3000h, there is xanthochromia in various degree in existing polyurethane sealant, and polyurethane sealant outward appearance of the present invention is without obvious xanthochromia, and therefore, polyurethane sealant of the present invention is under long uviolizing, and anti-yellowing property is excellent.
(2) in ultraviolet ageing case after 3000h, there is be full of cracks in the existing polyurethane sealant outward appearance of part, elongation at break attenuation amplitude is 23% ~ 62%; Polyurethane sealant outward appearance of the present invention is without be full of cracks, and elasticity keeps good, and elongation at break attenuation amplitude is no more than 20%.Therefore, polyurethane sealant of the present invention is under long uviolizing, and slowly, weather resistance is excellent in mechanical property decay, is applicable to life-time service.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
The content of each composition in the embodiment of the present invention, if not otherwise specified, all in mass fraction.
The embodiment of the present invention provides a kind of single-component damp solidifying polyurethane seal gum had excellent weather resistance, in mass fraction, this polyurethane sealant comprises 20 ~ 50 parts of polyurethane prepolymers, 0.5 ~ 2 part of water suction stablizer, 0.1 ~ 0.7 part of silane coupling agent, 0.1 ~ 1 part of photostabilizer, 0.1 ~ 1 part of oxidation inhibitor, 2 ~ 10 parts of titanium dioxides, 28 ~ 50 parts of urethane fillers, 1 ~ 35 part of thixotropic agent, 0.4 ~ 2 part of first catalyzer, and described first catalyzer is any one in organometallics or tertiary amine compounds; Described polyurethane prepolymer comprises 20 ~ 65 parts of polyether glycols, 5 ~ 30 parts of aliphatics or alicyclic isocyanate, 0.01 ~ 0.05 part of second catalyzer, 0 ~ 7 part of thinner, described second catalyzer is dibutyl tin laurate, stannous octoate, dibutyltin diacetate, 2, any one in 2-dual-morpholinyl diethyl ether, 1,8-diazacyclo hendecene.
The embodiment of the present invention also provides the preparation method of the above-mentioned single-component damp solidifying polyurethane seal gum had excellent weather resistance, and comprises the following steps:
The environment producing and pack this polyurethane sealant answers control temperature≤25 DEG C, relative humidity≤55%RH;
Polyurethane preformed polymer: in mass fraction, 20 ~ 65 parts of polyether glycols are added in the there-necked flask of drying, vacuumize at 120 DEG C of temperature, dehydration 0.5 ~ 1h, be cooled to about 60 DEG C, add 5 ~ 30 parts of aliphatics or alicyclic isocyanate, 0.01 ~ 0.05 part of second catalyzer, 0 ~ 7 part of thinner, described second catalyzer is dibutyl tin laurate, stannous octoate, dibutyltin diacetate, 2, any one in 2-dual-morpholinyl diethyl ether, 1,8-diazacyclo hendecene; Slowly be warming up to 80 DEG C, insulation reaction 3h under drying nitrogen protection, discharging after cooling, obtains polyurethane prepolymer, is loaded in encloses container for subsequent use;
Prepare polyurethane sealant: in mass fraction, 20 ~ 50 parts of polyurethane prepolymers are added in planet stirring still, 0.5 ~ 2 part of water suction stablizer, 0.1 ~ 0.7 part of silane coupling agent, 0.1 ~ 1 part of photostabilizer, the auxiliary agents such as 0.1 ~ 1 part of oxidation inhibitor, after stirring, add pre-dry 2 ~ 10 parts of titanium dioxides, 28 ~ 50 parts of urethane fillers, 1 ~ 35 part of thixotropic agent stirs under vacuum conditions, vacuum is removed with drying nitrogen, add 0.4 ~ 2 part of first catalyzer, described first catalyzer is any one in organometallics or tertiary amine compounds, vacuumize, discharging after stirring, obtain the single-component damp solidifying polyurethane seal gum had excellent weather resistance.
Preferably, this polyurethane sealant comprises 25 ~ 40 parts of polyurethane prepolymers, 0.8 ~ 1.1 part of water suction stablizer, 0.2 ~ 0.6 part of silane coupling agent, 0.6 ~ 0.8 part of photostabilizer, 0.3 ~ 0.6 part of oxidation inhibitor, 4 ~ 8 parts of titanium dioxides, 35 ~ 48 parts of urethane fillers, 15 ~ 30 parts of thixotropic agent, 0.5 ~ 1.5 part of first catalyzer.
Preferred, this polyurethane sealant comprises 34.5 parts of polyurethane prepolymers, 0.8 part of water suction stablizer, 0.3 part of silane coupling agent, 0.8 part of photostabilizer, 0.5 part of oxidation inhibitor, 8 parts of titanium dioxides, 43 parts of urethane fillers, 16 parts of thixotropic agent, 0.8 part of first catalyzer.
Water suction stablizer is tolylsulfonyl isocyanic ester.
Silane coupling agent is any one in γ-glycidyl ether oxygen propyl trimethoxy silicane, β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane, γ-isocyanic ester propyl trimethoxy silicane, γ-isocyanic ester propyl-triethoxysilicane.
Photostabilizer is at least one in benzotriazole category, Benzophenones, triazines, hindered amine light stabilizer.Wherein conventional benzotriazole light stabilizer has Tinuvin213, UV327, UV328, UV320, UV-P, Tinuvin571, conventional Benzophenones photostabilizer has UV-531, conventional triazines as light stabilizer has UV-1164, conventional hindered amine light stabilizer has ADEKASTABLA-52, LA-57, LA-62, LA-67, LA-63, LA-68, LA-77, LA-82, LA-87 (Japanese Ai Dike Co., Ltd.), Tinuvin622, Tinuvin770, Chisorb622LD, SanolLS-765 and SanolLS-292 (Taiwan Double Bond Chemical Ind.,Co.,Ltd.).
Oxidation inhibitor is Hinered phenols and/or phosphorous acid kind antioxidant.Such as: be any one in IrgastabPU68, Irganox245, Irganox1010, Irganox1076, Irganox1098, Irganox1135, Irganox1330 (ciba speciality chemical company of Switzerland), WestonTPP and WestonTNPP (GE speciality chemical company limited of the U.S.).
Titanium dioxide is Rutile type Titanium Dioxide.
Urethane filler is any one in calcium carbonate, calcined kaolin, talcum powder, pvc resin paste grade, hollow glass microballoon, mica powder, diatomite.
Thixotropic agent is any one in hydrophobic type aerosil, organobentonite, polyureas, fibrous talc, anhydrous calcium sulfate whisker, polyamide wax.
First catalyzer can be any one in stannous octoate, lead octoate 36, dibutyl tin laurate, tributyltin chloride, butyiin trichioride, butyltin oxide, triethylenediamine, benzyldimethylamine, pyridine.
Polyether glycol is any 2 kinds in polyether Glycols and polyether-tribasic alcohol.Such as: be Tdiol-400 (Tianjin the 3rd petroleum chemical plant, Mn=400, functionality is 2), Tdiol-700 (Tianjin the 3rd petroleum chemical plant, Mn=700, functionality is 2), Tdiol-1000 (Tianjin the 3rd petroleum chemical plant, Mn=1000, functionality is 2), Tdiol-2000 (Tianjin the 3rd petroleum chemical plant, Mn=2000, functionality is 2), TMN-700 (Tianjin the 3rd petroleum chemical plant, Mn=700, functionality is 3), TMN-1000 (Tianjin the 3rd petroleum chemical plant, Mn=1000, functionality is 3), TMN-3000 (Tianjin the 3rd petroleum chemical plant, Mn=3000, functionality is 3), TMN-4000 (Tianjin the 3rd petroleum chemical plant, Mn=4000, functionality is 3), GSE-2028 (Shanghai Gaoqiao petrochemical corporation (complex), Mn=4000, moisture≤0.05%, functionality is 2), GEP-330N (Shanghai Gaoqiao petrochemical corporation (complex), Mn=4800, moisture≤0.05%, functionality is 3), polytetrahydrofuran diol (PTMEG), DL-4000D (Shandong Lanxing Dongda Chemical Co., Ltd, Mn=4000, moisture≤0.05%) in any 2 kinds.
Aliphatics or alicyclic isocyanate are any one in hexamethylene diisocyanate, isophorone diisocyanate, HMDI, xylylene diisocyanate.
Thinner is any one in toluene, dimethylbenzene, dioctyl phthalate (DOP), Di Iso Decyl Phthalate.
The present invention will be described in detail to use 9 embodiments and 1 comparative example below.
Embodiment 1:
The present embodiment provides a kind of single-component damp solidifying polyurethane seal gum had excellent weather resistance, in mass fraction, this polyurethane sealant comprises 34.5 parts of polyurethane prepolymers, 0.8 part of tolylsulfonyl isocyanic ester, 0.3 part of γ-glycidyl ether oxygen propyl trimethoxy silicane, 0.6 part of UV327,0.3 part of Irganox1098,4 parts of titanium dioxides, 43 parts of calcium carbonate, 16 parts of polyureas, 0.8 part of lead octoate 36; Wherein, polyurethane prepolymer comprises 27 parts of polyether Glycols Tdiol-2000,13 parts of polyether-tribasic alcohol GEP-330N, 8 parts of HMDIs, 0.01 part of dibutyl tin laurate, 2 parts of toluene.
The preparation method of the above-mentioned single-component damp solidifying polyurethane seal gum had excellent weather resistance comprises the following steps:
The environment producing and pack this polyurethane sealant answers control temperature≤25 DEG C, relative humidity≤55%RH;
Polyurethane preformed polymer: add 27 parts of polyether Glycols Tdiol-2000,13 parts of polyether-tribasic alcohol GEP-330N in the there-necked flask of drying, vacuumize at 120 DEG C of temperature, dehydration 0.5h, is cooled to about 60 DEG C, add 8 part 4,4 '-dicyclohexyl methane diisocyanate, 2 parts of toluene, 0.01 part of dibutyl tin laurate, be slowly warming up to 80 DEG C, insulation reaction 3h under drying nitrogen protection, cooling discharge, obtains polyurethane prepolymer, is loaded in encloses container for subsequent use;
Prepare polyurethane sealant: in mass fraction, 34.5 parts of polyurethane prepolymers are added in planet stirring still, 0.8 part of tolylsulfonyl isocyanic ester, 0.3 part of γ-glycidyl ether oxygen propyl trimethoxy silicane, 0.3 part of Irganox1098, 0.6 part of UV327, after stirring, add pre-dry 4 parts of titanium dioxides, 43 parts of calcium carbonate, 16 parts of polyureas, stir under vacuum conditions, vacuum is removed with drying nitrogen, add 0.8 part of lead octoate 36, vacuumize, discharging after stirring, obtain the above-mentioned single-component damp solidifying polyurethane seal gum had excellent weather resistance.
Embodiment 2:
The present embodiment provides a kind of single-component damp solidifying polyurethane seal gum had excellent weather resistance, in mass fraction, this polyurethane sealant comprises 34.5 parts of polyurethane prepolymers, 0.8 part of tolylsulfonyl isocyanic ester, 0.3 part of γ-glycidyl ether oxygen propyl trimethoxy silicane, 0.8 part of LA-62,0.5 part of Irganox1098,8 parts of titanium dioxides, 43 parts of pvc resin paste grades, 16 parts of hydrophobic type aerosils, 0.8 part of dibutyl tin laurate; Wherein, polyurethane prepolymer 27 parts of polyether Glycols Tdiol-2000,13 parts of polyether-tribasic alcohol GEP-330N, 8 parts of HMDIs, 0.01 part of dibutyl tin laurate, 2 parts of toluene.
The preparation method of the above-mentioned single-component damp solidifying polyurethane seal gum had excellent weather resistance comprises the following steps:
The environment producing and pack this polyurethane sealant answers control temperature≤25 DEG C, relative humidity≤55%RH;
Polyurethane preformed polymer: preparation process is identical with embodiment 1;
Prepare polyurethane sealant: in planet stirring still, add 34.5 parts of polyurethane prepolymers, 0.8 part of tolylsulfonyl isocyanic ester, 0.3 part of γ-glycidyl ether oxygen propyl trimethoxy silicane, 0.5 part of Irganox1098, 0.8 part of LA-62, after stirring, add pre-dry 8 parts of titanium dioxides, 43 parts of pvc resin paste grades, 16 parts of hydrophobic type aerosils, stir under vacuum conditions, vacuum is removed with drying nitrogen, add 0.8 part of dibutyl tin laurate, vacuumize, discharging after stirring, obtain the above-mentioned single-component damp solidifying polyurethane seal gum had excellent weather resistance.
Embodiment 3:
The present embodiment provides a kind of single-component damp solidifying polyurethane seal gum had excellent weather resistance, in mass fraction, this polyurethane sealant comprises 20 parts of polyurethane prepolymers, 0.5 part of tolylsulfonyl isocyanic ester, 0.1 part of β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane, 0.1 part of UV-531,0.5 part of Irganox245,0.5 part of WestonTPP, 2 parts of titanium dioxides, 28 parts of calcined kaolins, 1 part of organobentonite, 0.4 part of stannous octoate; Wherein, polyurethane prepolymer comprises 10 parts of polyether Glycols Tdiol-400,10 parts of polyether-tribasic alcohol TMN-700,5 parts of hexamethylene diisocyanates, 0.01 part of dibutyltin diacetate.
The preparation method of the above-mentioned single-component damp solidifying polyurethane seal gum had excellent weather resistance comprises the following steps:
The environment producing and pack this polyurethane sealant answers control temperature≤25 DEG C, relative humidity≤55%RH;
Polyurethane preformed polymer: add 10 parts of polyether Glycols Tdiol-2000,10 parts of polyether-tribasic alcohol TMN-700 in the there-necked flask of drying, vacuumize at 120 DEG C of temperature, dehydration 0.5h, be cooled to about 60 DEG C, add 5 parts of hexamethylene diisocyanates, 0.01 part of dibutyltin diacetate, be slowly warming up to 80 DEG C, insulation reaction 3h under drying nitrogen protection, cooling discharge, obtains polyurethane prepolymer, is loaded in encloses container for subsequent use;
Prepare polyurethane sealant: in planet stirring still, add 20 parts of polyurethane prepolymers, 0.5 part of tolylsulfonyl isocyanic ester, 0.1 part of β-(3, 4-epoxycyclohexyl) ethyl trimethoxy silane, 0.1 part of UV-531, 0.5 part of Irganox245, 0.5 part of WestonTPP, after stirring, add pre-dry 8 parts of titanium dioxides, 28 parts of calcined kaolins, 1 part of organobentonite, stir under vacuum conditions, vacuum is removed with drying nitrogen, add 0.4 part of stannous octoate, vacuumize, discharging after stirring, obtain the above-mentioned single-component damp solidifying polyurethane seal gum had excellent weather resistance.
Embodiment 4:
The present embodiment provides a kind of single-component damp solidifying polyurethane seal gum had excellent weather resistance, in mass fraction, this polyurethane sealant comprises 25 parts of polyurethane prepolymers, 0.8 part of tolylsulfonyl isocyanic ester, 0.2 part of γ-isocyanic ester propyl trimethoxy silicane, 0.6 part of UV1164,0.3 part of WestonTNPP, 4 parts of titanium dioxides, 35 parts of hollow glass microballoons, 15 parts of fibrous talcs, 0.5 part of triethylenediamine; Wherein, polyurethane prepolymer comprises 30 parts of polyether Glycols GSE-2028,35 parts of polyether-tribasic alcohol TMN-4000,30 parts of isophorone diisocyanates, 0.05 part of 2,2-dual-morpholinyl diethyl ether, 7 parts of dioctyl phthalate (DOP)s.
The preparation method of the above-mentioned single-component damp solidifying polyurethane seal gum had excellent weather resistance comprises the following steps:
The environment producing and pack this polyurethane sealant answers control temperature≤25 DEG C, relative humidity≤55%RH;
Polyurethane preformed polymer: add 30 parts of polyether Glycols GSE-2028,35 parts of polyether-tribasic alcohol TMN-4000 in the there-necked flask of drying, vacuumize at 120 DEG C of temperature, dehydration 1h, be cooled to about 60 DEG C, add 30 parts of isophorone diisocyanates, 0.05 part 2,2-dual-morpholinyl diethyl ether, 7 parts of dioctyl phthalate (DOP)s, slowly be warming up to 80 DEG C, insulation reaction 3h under drying nitrogen protection, cooling discharge, obtain polyurethane prepolymer, be loaded in encloses container for subsequent use;
Prepare polyurethane sealant: in planet stirring still, add 25 parts of polyurethane prepolymers, 0.8 part of tolylsulfonyl isocyanic ester, 0.2 part of γ-isocyanic ester propyl trimethoxy silicane, 0.6 part of UV1164, 0.3 part of WestonTNPP, after stirring, add pre-dry 4 parts of titanium dioxides, 35 parts of hollow glass microballoons, 15 parts of fibrous talcs, stir under vacuum conditions, vacuum is removed with drying nitrogen, add 0.5 part of triethylenediamine, vacuumize, discharging after stirring, obtain the above-mentioned single-component damp solidifying polyurethane seal gum had excellent weather resistance.
Embodiment 5:
The present embodiment provides a kind of single-component damp solidifying polyurethane seal gum had excellent weather resistance, in mass fraction, this polyurethane sealant comprises 40 parts of polyurethane prepolymers, 1.1 parts of tolylsulfonyl isocyanic ester, 0.6 part of γ-isocyanic ester propyl-triethoxysilicane, 0.8 part of Tinuvin213,0.6 part of Irganox1330,8 parts of titanium dioxides, 48 parts of mica powders, 30 parts of polyamide waxes, 1.5 parts of tributyltin chlorides; Wherein, polyurethane prepolymer comprises 27 parts of polyether-tribasic alcohol GEP-330N, 13 parts of polyether-tribasic alcohol TMN-1000,8 parts of isophorone diisocyanates, 0.01 part of 1,8-diazacyclo hendecene, 2 parts of dimethylbenzene.
The preparation method of the above-mentioned single-component damp solidifying polyurethane seal gum had excellent weather resistance comprises the following steps:
The environment producing and pack this polyurethane sealant answers control temperature≤25 DEG C, relative humidity≤55%RH;
Polyurethane preformed polymer: add 27 parts of polyether-tribasic alcohol GEP-330N, 13 parts of polyether-tribasic alcohol TMN-1000 in the there-necked flask of drying, vacuumize at 120 DEG C of temperature, dehydration 1h, be cooled to about 60 DEG C, add 8 parts of isophorone diisocyanates, 0.01 part 1,8-diazacyclo hendecene, 2 parts of dimethylbenzene, slowly be warming up to 80 DEG C, insulation reaction 3h under drying nitrogen protection, cooling discharge, obtain polyurethane prepolymer, be loaded in encloses container for subsequent use;
Prepare polyurethane sealant: in planet stirring still, add 27 parts of polyether-tribasic alcohol GEP-330N, 13 parts of polyether-tribasic alcohol TMN-1000, 1.1 parts of tolylsulfonyl isocyanic ester, 0.6 part of γ-isocyanic ester propyl-triethoxysilicane, 0.8 part of Tinuvin213, 0.6 part of Irganox1330, after stirring, add pre-dry 8 parts of titanium dioxides, 48 parts of mica powders, 30 parts of polyamide waxes, stir under vacuum conditions, vacuum is removed with drying nitrogen, add 1.5 parts of tributyltin chlorides, vacuumize, discharging after stirring, obtain the above-mentioned single-component damp solidifying polyurethane seal gum had excellent weather resistance.
Embodiment 6:
The present embodiment provides a kind of single-component damp solidifying polyurethane seal gum had excellent weather resistance, in mass fraction, this polyurethane sealant comprises 50 parts of polyurethane prepolymers, 2 parts of tolylsulfonyl isocyanic ester, 0.7 part of γ-glycidyl ether oxygen propyl trimethoxy silicane, 1 part of Chisorb622LD, 0.1 part of IrgastabPU68,10 parts of titanium dioxides, 50 parts of diatomite, 35 parts of anhydrous calcium sulfate whiskers, 2 parts of benzyldimethylamines; Wherein, polyurethane prepolymer comprises 27 parts of polyether Glycols Tdiol-2000,13 parts of polytetrahydrofuran diols, 8 parts of xylylene diisocyanates, 0.01 part of stannous octoate, 2 parts of Di Iso Decyl Phthalates.
The preparation method of the above-mentioned single-component damp solidifying polyurethane seal gum had excellent weather resistance comprises the following steps:
The environment producing and pack this polyurethane sealant answers control temperature≤25 DEG C, relative humidity≤55%RH;
Polyurethane preformed polymer: add 27 parts of polyether Glycols Tdiol-2000,13 parts of polytetrahydrofuran diols in the there-necked flask of drying, vacuumize at 120 DEG C of temperature, dehydration 1h, be cooled to about 60 DEG C, add 8 parts of xylylene diisocyanates, 0.01 part of stannous octoate, 2 parts of Di Iso Decyl Phthalates, be slowly warming up to 80 DEG C, insulation reaction 3h under drying nitrogen protection, cooling discharge, obtains polyurethane prepolymer, is loaded in encloses container for subsequent use;
Prepare polyurethane sealant: in planet stirring still, add 50 parts of polyurethane prepolymers, 2 parts of tolylsulfonyl isocyanic ester, 0.7 part of γ-glycidyl ether oxygen propyl trimethoxy silicane, 1 part of Chisorb622LD, 0.1 part of IrgastabPU68, after stirring, add pre-dry 10 parts of titanium dioxides, 50 parts of diatomite, 35 parts of anhydrous calcium sulfate whiskers, stir under vacuum conditions, vacuum is removed with drying nitrogen, add 2 parts of benzyldimethylamines, vacuumize, discharging after stirring, obtain the above-mentioned single-component damp solidifying polyurethane seal gum had excellent weather resistance.
Embodiment 7: in the present embodiment except the first catalyzer is butyiin trichioride, urethane filler is outside talcum powder, remaining is all identical with embodiment 1.
Embodiment 8: in the present embodiment except the first catalyzer is butyltin oxide, remaining is all identical with embodiment 1.
Embodiment 9: in the present embodiment except the first catalyzer is pyridine, remaining is all identical with embodiment 1.
Comparative example 1:
Existing single-component damp solidifying polyurethane seal gum in this comparative example, in mass fraction, this polyurethane sealant comprises 34.5 parts of existing polyurethane prepolymers, 0.8 part of tolylsulfonyl isocyanic ester, 0.3 γ-glycidyl ether oxygen propyl trimethoxy silicane, 4 parts of titanium dioxides, 38 parts of calcium carbonate, 5 parts of PVC paste resins, 15 parts of polyureas, 1 part of aerosil, 0.8 part of dibutyl tin laurate; Wherein, polyurethane prepolymer comprise 27 parts of polyether Glycols Tdiol-2000,13 parts of polyether-tribasic alcohol GEP-330N, 8 part 4,4 '-diphenylmethanediisocyanate, 0.01 part of dibutyl tin laurate, 2 parts of dimethylbenzene.
Prepare existing polyurethane prepolymer: in the there-necked flask of drying, add 27 parts of polyether Glycols Tdiol-2000,13 parts of polyether-tribasic alcohol GEP-330N, vacuumize at 120 DEG C of temperature, dehydration 1h, be cooled to about 60 DEG C, add 8 part 4,4 '-diphenylmethanediisocyanate, 0.01 part of dibutyl tin laurate, 2 parts of dimethylbenzene, slowly be warming up to 80 DEG C, insulation reaction 3h under drying nitrogen protection, cooling discharge, obtain existing polyurethane prepolymer, be loaded in encloses container for subsequent use;
Prepare polyurethane sealant: in planet stirring still, add 34.5 parts of existing polyurethane prepolymers, 0.8 part of tolylsulfonyl isocyanic ester, 0.3 γ-glycidyl ether oxygen propyl trimethoxy silicane, after stirring, add pre-dry 4 parts of titanium dioxides, 38 parts of calcium carbonate, 5 parts of PVC paste resins, 15 parts of polyureas, 1 part of aerosil stir under vacuum conditions, vacuum is removed with drying nitrogen, add 0.8 part of dibutyl tin laurate, vacuumize, after stirring, discharging, obtains existing single-component damp solidifying polyurethane seal gum.
Respectively performance test is carried out to polyurethane sealant prepared by embodiment 1 ~ 9 and comparative example 1 below:
Extrude appropriate one-component polyurethane sealant on polyfluortetraethylene plate, spread to plaster trowel the glue-line that thickness is 2mm, do not make there is bubble in glue, place after 7 days under standard environment, test properties.
Anti-yellowing property: the change of naked eyes paired observation aging front and back color.
Weather resistance: the film of solidification after 7 days is put in ultraviolet (UV) aging test chamber, observes outward appearance at set intervals, use non-setting adhesive sticker face, tested for tensile strength, elongation at break;
Tensile strength, elongation at break: undertaken (adopt 1 type cut-off knife to determine test piece, draw speed is 500mm/min) by GB/T528-2009.
Thixotropy: one-component polyurethane sealant is extruded into long 70mm, the trilateral adhesive tape of wide 10mm, high 5mm, beats on the vertical plane, places 24h, the displacement of test adhesive tape.
The performance test results ginseng of embodiment 1 ~ 9 and comparative example 1 is shown in Table 1.
Interpretation of result: as can be seen from Table 1, single-component damp solidifying polyurethane seal gum of the present invention has excellent weathering resistance, wherein most preferred embodiment is embodiment 2, this polyurethane sealant is in ultraviolet ageing case after 3000h, outward appearance is without be full of cracks, and without obvious xanthochromia, elongation at break attenuation amplitude is 5.7%.
The performance test results of table 1, embodiment 1 ~ 9 and comparative example 1
Those skilled in the art can carry out various modifications and variations to the embodiment of the present invention, if these amendments and modification are within the scope of the claims in the present invention and equivalent technologies thereof, then these revise and modification also within protection scope of the present invention.
The prior art that the content do not described in detail in specification sheets is known to the skilled person.
Claims (14)
1. the single-component damp solidifying polyurethane seal gum had excellent weather resistance, it is characterized in that: in mass fraction, this polyurethane sealant comprises 20 ~ 50 parts of polyurethane prepolymers, 0.5 ~ 2 part of water suction stablizer, 0.1 ~ 0.7 part of silane coupling agent, 0.1 ~ 1 part of photostabilizer, 0.1 ~ 1 part of oxidation inhibitor, 2 ~ 10 parts of titanium dioxides, 28 ~ 50 parts of urethane fillers, 1 ~ 35 part of thixotropic agent, 0.4 ~ 2 part of first catalyzer, and described first catalyzer is any one in organometallics or tertiary amine compounds; Described polyurethane prepolymer comprises 20 ~ 65 parts of polyether glycols, 5 ~ 30 parts of aliphatics or alicyclic isocyanate, 0.01 ~ 0.05 part of second catalyzer, 0 ~ 7 part of thinner, described second catalyzer is dibutyl tin laurate, stannous octoate, dibutyltin diacetate, 2, any one in 2-dual-morpholinyl diethyl ether, 1,8-diazacyclo hendecene; Described water suction stablizer is tolylsulfonyl isocyanic ester; Described titanium dioxide is Rutile type Titanium Dioxide; Described silane coupling agent is any one in γ-glycidyl ether oxygen propyl trimethoxy silicane, β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane, γ-isocyanic ester propyl trimethoxy silicane, γ-isocyanic ester propyl-triethoxysilicane; Described urethane filler is any one in calcium carbonate, calcined kaolin, talcum powder, pvc resin paste grade, hollow glass microballoon, mica powder, diatomite; Described thixotropic agent is any one in hydrophobic type aerosil, organobentonite, polyureas, fibrous talc, anhydrous calcium sulfate whisker, polyamide wax.
2. the single-component damp solidifying polyurethane seal gum had excellent weather resistance as claimed in claim 1, is characterized in that: described polyether glycol is any 2 kinds in polyether Glycols and polyether-tribasic alcohol.
3. the single-component damp solidifying polyurethane seal gum had excellent weather resistance as claimed in claim 1, it is characterized in that: described aliphatics or alicyclic isocyanate are any one in hexamethylene diisocyanate, isophorone diisocyanate, HMDI, xylylene diisocyanate.
4. the single-component damp solidifying polyurethane seal gum had excellent weather resistance as claimed in claim 1, is characterized in that: described thinner is any one in toluene, dimethylbenzene, dioctyl phthalate (DOP), Di Iso Decyl Phthalate.
5. the single-component damp solidifying polyurethane seal gum had excellent weather resistance as claimed in claim 1, is characterized in that: described photostabilizer is any one in benzotriazole category, Benzophenones, triazines, hindered amine light stabilizer.
6. the single-component damp solidifying polyurethane seal gum had excellent weather resistance as claimed in claim 1, is characterized in that: described oxidation inhibitor is Hinered phenols and/or phosphorous acid kind antioxidant.
7. the single-component damp solidifying polyurethane seal gum had excellent weather resistance according to any one of claim 1 to 6, is characterized in that: described first catalyzer is any one in stannous octoate, lead octoate 36, dibutyl tin laurate, tributyltin chloride, butyiin trichioride, butyltin oxide, triethylenediamine, benzyldimethylamine, pyridine.
8. the preparation method of the single-component damp solidifying polyurethane seal gum had excellent weather resistance as claimed in claim 1, is characterized in that, comprise the following steps:
The environment producing and pack this polyurethane sealant answers control temperature≤25 DEG C, relative humidity≤55%RH;
Polyurethane preformed polymer: in mass fraction, 20 ~ 65 parts of polyether glycols are added in the there-necked flask of drying, vacuumize at 120 DEG C of temperature, dehydration 0.5 ~ 1h, be cooled to about 60 DEG C, add 5 ~ 30 parts of aliphatics or alicyclic isocyanate, 0.01 ~ 0.05 part of second catalyzer, 0 ~ 7 part of thinner, described second catalyzer is dibutyl tin laurate, stannous octoate, dibutyltin diacetate, 2, any one in 2-dual-morpholinyl diethyl ether, 1,8-diazacyclo hendecene; Slowly be warming up to 80 DEG C, insulation reaction 3h under drying nitrogen protection, discharging after cooling, obtains polyurethane prepolymer, is loaded in encloses container for subsequent use;
Prepare polyurethane sealant: in mass fraction, 20 ~ 50 parts of polyurethane prepolymers are added in planet stirring still, 0.5 ~ 2 part of water suction stablizer, 0.1 ~ 0.7 part of silane coupling agent, 0.1 ~ 1 part of photostabilizer, the auxiliary agents such as 0.1 ~ 1 part of oxidation inhibitor, after stirring, add pre-dry 2 ~ 10 parts of titanium dioxides, 28 ~ 50 parts of urethane fillers, 1 ~ 35 part of thixotropic agent stirs under vacuum conditions, vacuum is removed with drying nitrogen, add 0.4 ~ 2 part of first catalyzer, described first catalyzer is any one in organometallics or tertiary amine compounds, described water suction stablizer is tolylsulfonyl isocyanic ester, described titanium dioxide is Rutile type Titanium Dioxide, described silane coupling agent is any one in γ-glycidyl ether oxygen propyl trimethoxy silicane, β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane, γ-isocyanic ester propyl trimethoxy silicane, γ-isocyanic ester propyl-triethoxysilicane, described urethane filler is any one in calcium carbonate, calcined kaolin, talcum powder, pvc resin paste grade, hollow glass microballoon, mica powder, diatomite, described thixotropic agent is any one in hydrophobic type aerosil, organobentonite, polyureas, fibrous talc, anhydrous calcium sulfate whisker, polyamide wax, vacuumize, discharging after stirring, obtain the single-component damp solidifying polyurethane seal gum had excellent weather resistance.
9. the preparation method of the single-component damp solidifying polyurethane seal gum had excellent weather resistance as claimed in claim 8, is characterized in that: described polyether glycol is any 2 kinds in polyether Glycols and polyether-tribasic alcohol.
10. the preparation method of the single-component damp solidifying polyurethane seal gum had excellent weather resistance as claimed in claim 8, it is characterized in that: described aliphatics or alicyclic isocyanate are any one in hexamethylene diisocyanate, isophorone diisocyanate, HMDI, xylylene diisocyanate.
The preparation method of the 11. single-component damp solidifying polyurethane seal gums had excellent weather resistance as claimed in claim 8, is characterized in that: described thinner is any one in toluene, dimethylbenzene, dioctyl phthalate (DOP), Di Iso Decyl Phthalate.
The preparation method of the 12. single-component damp solidifying polyurethane seal gums had excellent weather resistance as claimed in claim 8, is characterized in that: described photostabilizer is any one in benzotriazole category, Benzophenones, triazines, hindered amine light stabilizer.
The preparation method of the 13. single-component damp solidifying polyurethane seal gums had excellent weather resistance as claimed in claim 8, is characterized in that: described oxidation inhibitor is Hinered phenols and/or phosphorous acid kind antioxidant.
The preparation method of 14. single-component damp solidifying polyurethane seal gums had excellent weather resistance according to any one of claim 8 to 13, is characterized in that: described first catalyzer is any one in stannous octoate, lead octoate 36, dibutyl tin laurate, tributyltin chloride, butyiin trichioride, butyltin oxide, triethylenediamine, benzyldimethylamine, pyridine.
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