CN109852327B - Double-component polyurethane windshield glass adhesive with rapid curing capability and preparation method thereof - Google Patents

Double-component polyurethane windshield glass adhesive with rapid curing capability and preparation method thereof Download PDF

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CN109852327B
CN109852327B CN201910198039.1A CN201910198039A CN109852327B CN 109852327 B CN109852327 B CN 109852327B CN 201910198039 A CN201910198039 A CN 201910198039A CN 109852327 B CN109852327 B CN 109852327B
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parts
component
plasticizer
filler
carbon black
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CN109852327A (en
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孙辉
周朝栋
孟君伟
王少杰
陶小乐
何永富
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Hangzhou Zhijiang Silicone Chemicals Co Ltd
Hangzhou Zhijiang New Material Co Ltd
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Hangzhou Zhijiang Silicone Chemicals Co Ltd
Hangzhou Zhijiang New Material Co Ltd
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Abstract

The invention provides a two-component polyurethane windshield glass cement with quick curing capability and a preparation method thereof, wherein the glass cement comprises a component A and a component B: the component A comprises the following components in parts by weight: 30-50 parts of polyurethane prepolymer, 10-30 parts of plasticizer, 10-30 parts of filler, 10-30 parts of carbon black, 0.2-1 part of silane coupling agent, 0-1 part of water absorbent and 0.1-1 part of catalyst a; the component B comprises the following components: 30-50 parts of polyether polyol a, 0-10 parts of tackifying resin, 10-30 parts of plasticizer, 20-50 parts of filler, 0-20 parts of carbon black, 0-10 parts of fumed silica and 1-10 parts of distilled water. The component A and the component B are matched with each other, so that the glass cement has relatively quick curing capability. The operable time of the windshield glass cement is 16-27 min; the tensile shear strength is 0.20-0.36 MPa after 30 min.

Description

Double-component polyurethane windshield glass adhesive with rapid curing capability and preparation method thereof
Technical Field
The invention belongs to polyurethane windshield glass cement, and particularly relates to a two-component polyurethane windshield glass cement with a rapid curing capability and a preparation method thereof.
Background
The single-component polyurethane windshield glass adhesive is a moisture curing product, and the curing speed of the single-component polyurethane windshield glass adhesive is influenced by the moisture content in the air and the ambient temperature besides the performance of the single-component polyurethane windshield glass adhesive.
With the development of the modern automobile industry, the time from installation of polyurethane windshield glass glue to road test in a final assembly workshop is gradually shortened to about 2 hours, and in a low-temperature and low-humidity environment, if the polyurethane glue cannot form enough initial strength, the bonded glass, particularly front and rear windshield glass and large side window glass, can generate abnormal sound due to vehicle vibration in the road test process, so that the judgment of the quality detection link of an automobile factory is greatly influenced. Secondly, on the truck locomotive assembly production line, because the locomotive needs to be rotated when some components are installed, the curing speed of the windshield glass cement is improved, and the windshield glass cement for bonding the windshield glass and the matched components needs to be ensured to form enough bonding strength within 1 hour after construction. In addition, the after-market of automobiles also has a great demand for fast driving away when performing maintenance of windshields and other components.
Disclosure of Invention
In view of the above, the present invention is directed to a two-component polyurethane windshield glass paste with fast curing capability and a method for preparing the same, wherein the two-component polyurethane windshield glass paste has fast curing capability.
The invention provides a two-component polyurethane windshield glass adhesive with quick curing capability, which comprises a component A and a component B:
the component A comprises the following components in parts by mass:
30-50 parts of polyurethane prepolymer, 10-30 parts of plasticizer, 10-30 parts of filler, 10-30 parts of carbon black, 0.2-1 part of silane coupling agent, 0.2-1 part of water absorbent and 0.1-1 part of catalyst a;
the component B comprises the following components:
30-50 parts of polyether polyol a, 0-10 parts of tackifying resin, 10-30 parts of plasticizer, 20-50 parts of filler, 0-20 parts of carbon black, 0-10 parts of fumed silica and 1-10 parts of distilled water.
Preferably, the volume ratio of the A component to the B component is 10: 1.
Preferably, the polyether polyol a is selected from one or more of polyether diol, polyether triol and polyether tetraol.
Preferably, the tackifying resin is selected from one or more of polyethylene glycol, polyester resin diol, acrylic resin diol, polycarbonate diol, rosin resin diol, hydrogenated petroleum resin diol and terpene resin diol.
Preferably, the polyurethane prepolymer is prepared by reacting polyether polyol b, isocyanate and a catalyst b;
the mass ratio of the polyether polyol b to the isocyanate to the catalyst b is 100: 2-10: 0.01-0.05.
Preferably, the polyether polyol b is selected from polyether triols and/or polyether diols;
the isocyanate is selected from one or more of toluene diisocyanate, diphenylmethane diisocyanate, 1, 4-phenylene diisocyanate, polymethylene polyphenylene polyisocyanate, xylylene diisocyanate, tetramethylxylylene diisocyanate, tolidine diisocyanate, 1, 5-naphthalene diisocyanate, triphenylmethane triisocyanate, hexamethylene diisocyanate, trimethylhexamethylene diisocyanate, lysine diisocyanate, norbornane diisocyanate, trans cyclohexane-1, 4-diisocyanate, isophorone diisocyanate, bis (isocyanatomethyl) cyclohexane and dicyclohexylmethane diisocyanate;
the catalyst b is selected from one or more of dioctyltin dilaurate, dibutyltin dilaurate, dimethyltin dilaurate, stannous octoate, dibutyltin oxide and dioctyltin oxide.
Preferably, the filler is selected from one or more of silica, ground calcium carbonate, talc, clay, organobentonite, hydrogenated castor oil and barium sulfate;
the carbon black is selected from one or more of contact carbon black, furnace carbon black and pyrolytic carbon black;
the plasticizer is selected from one or more of alkyl sulfonate, diisooctyl phthalate, diisodecyl phthalate, diisononyl phthalate, cyclohexane 1, 2-diisononyl phthalate, diisodecyl cyclohexane 1, 2-phthalate, tricresyl phosphate and trioctyl phosphate.
The silane coupling agent is selected from one or more of beta- (3, 4-epoxycyclohexyl) ethyl trimethoxy silane, gamma-glycidyl ether propyl triethoxy silane, 3-glycidyl ether propyl methyl diethoxy silane, gamma-isocyanate propyl triethoxy silane and gamma-isocyanate propyl trimethoxy silane;
the water absorbent is selected from one or more of alkyl sulfonic acid isocyanate, calcium oxide and molecular sieve.
The invention provides a preparation method of a double-component polyurethane windshield glass adhesive, which comprises the following steps:
dehydrating polyether polyol b, mixing with isocyanate and a catalyst b, and reacting to obtain a polyurethane prepolymer;
mixing the polyurethane prepolymer, the dehydrated plasticizer, the dried filler, the dried carbon black, the silane coupling agent and the water absorbent, adding the catalyst a under the vacuum degree of not less than 980mbar, and uniformly stirring to obtain a component A;
uniformly stirring polyether polyol a, tackifying resin, a dehydrated plasticizer, dry filler, dry carbon black, dry fumed silica and distilled water to obtain a component B;
and mixing the component A and the component B to obtain the double-component polyurethane windshield glass adhesive.
The invention provides a two-component polyurethane windshield glass adhesive with quick curing capability, which comprises a component A and a component B: the component A comprises the following components in parts by mass: 30-50 parts of polyurethane prepolymer, 10-30 parts of plasticizer, 10-30 parts of filler, 10-30 parts of carbon black, 0.2-1 part of silane coupling agent, 0-1 part of water absorbent and 0.1-1 part of catalyst a; the component B comprises the following components: the adhesive comprises, by weight, 30-50 parts of polyether polyol a, 0-10 parts of tackifying resin, 10-30 parts of plasticizer, 20-50 parts of filler, 0-20 parts of carbon black, 0-10 parts of fumed silica and 1-10 parts of distilled water. The two-component polyurethane windshield glass cement provided by the invention comprises the component A and the component B which are matched with each other, so that the glass cement has relatively high curing capability. The experimental results show that: the operable time of the windshield glass cement is 16-27 min; the tensile shear strength is 0.20-0.36 MPa after 30 min; the tensile shear strength is 1.0-1.5 MPa after 60 min; the tensile shear strength is 2.0-2.5 MPa after 120 min.
Detailed Description
The invention provides a two-component polyurethane windshield glass adhesive with quick curing capability, which comprises a component A and a component B:
the component A comprises the following components in parts by mass:
30-50 parts of polyurethane prepolymer, 10-30 parts of plasticizer, 10-30 parts of filler, 10-30 parts of carbon black, 0.2-1 part of silane coupling agent, 0-1 part of water absorbent and 0.1-1 part of catalyst a;
the component B comprises the following components:
30-50 parts of polyether polyol a, 0-10 parts of tackifying resin, 10-30 parts of plasticizer, 20-50 parts of filler, 0-20 parts of carbon black, 0-10 parts of fumed silica and 1-10 parts of distilled water.
The two-component polyurethane windshield glass cement provided by the invention comprises the component A and the component B which are matched with each other, so that the glass cement has relatively high curing capability. The experimental results show that: the operable time of the windshield glass cement is 16-27 min; the tensile shear strength is 0.20-0.36 MPa after 30 min; the tensile shear strength is 1.0-1.5 MPa after 60 min; the tensile shear strength is 2.0-2.5 MPa after 120 min.
The two-component polyurethane windshield glass adhesive with the rapid curing capability provided by the invention comprises a component A; the component A comprises 30-50 parts of polyurethane prepolymer; in specific embodiments, the polyurethane prepolymer is present in an amount of 30 parts, 40 parts, or 50 parts. The polyurethane prepolymer is prepared by the reaction of polyether polyol b, isocyanate and a catalyst b;
the mass ratio of the polyether polyol b to the isocyanate to the catalyst b is 100: 2-10: 0.01-0.05.
In the invention, the polyether polyol b is preferably selected from polyether triol and/or polyether diol with the molecular weight of 3000-6000; the molecular weight of the polyether triol is preferably 3000-6000, and more preferably 4500-5000; the hydroxyl value is preferably 28 to 56mgKOH/g, more preferably 33.6 to 37.3 mgKOH/g. The molecular weight of the polyether glycol is preferably 1000-4000, and more preferably 2000-3000; the hydroxyl value is preferably 28 to 112mgKOH/g, more preferably 37.3 to 56 mgKOH/g; in a specific embodiment of the invention, the polyether triol has a molecular weight of 5000 and a hydroxyl value of 33.6 mgKOH/g; the polyether diol has a molecular weight of 2000 and a hydroxyl value of 56 mgKOH/g.
In the present invention, the isocyanate is selected from one or more of toluene diisocyanate, diphenylmethane diisocyanate, 1, 4-phenylene diisocyanate, polymethylene polyphenylene polyisocyanate, xylylene diisocyanate, tetramethylxylylene diisocyanate, tolidine diisocyanate, 1, 5-naphthalene diisocyanate, triphenylmethane triisocyanate, hexamethylene diisocyanate, trimethylhexamethylene diisocyanate, lysine diisocyanate, norbornane diisocyanate, trans-cyclohexane-1, 4-diisocyanate, isophorone diisocyanate, bis (isocyanatomethyl) cyclohexane and dicyclohexylmethane diisocyanate; wherein the toluene diisocyanate is selected from 2, 4-toluene diisocyanate and 4, 4' -toluene diisocyanate. In a particular embodiment, the isocyanate is selected from 4,4 '-toluene diisocyanate (4, 4' -MDI). In a specific example, the molar ratio of-NCO to-OH is 1.8.
In the present invention, the catalyst b is selected from one or more of dioctyltin dilaurate, dibutyltin dilaurate, dimethyltin dilaurate, stannous octoate, dibutyltin oxide and dioctyltin oxide. In a specific embodiment, the catalyst b is selected from dibutyltin dilaurate.
The reaction temperature of the polyether polyol b and the isocyanate is preferably 75-85 ℃, and the reaction time is preferably 3.5-4.5 hours; in a specific embodiment, the temperature of the reaction of the polyether polyol b and the isocyanate is 80 ℃ and the time is 4 hours. In a specific embodiment, the NCO content of the polyurethane prepolymer is 2.14%.
The component A comprises 10-30 parts of a plasticizer; in particular embodiments, the plasticizer is specifically present in an amount of 10 parts, 20 parts, or 30 parts. The plasticizer is preferably selected from one or more of alkyl sulfonate, diisooctyl phthalate, diisodecyl phthalate, diisononyl phthalate, cyclohexane 1, 2-diisononyl phthalate, diisodecyl cyclohexane 1, 2-dicarboxylate, tricresyl phosphate and trioctyl phosphate. In particular embodiments, the plasticizer is selected from one or more of diisodecyl phthalate, diisononyl phthalate, and alkyl sulfonates.
The component A comprises 10-30 parts of filler; in particular embodiments, the filler is specifically used in an amount of 10 parts, 20 parts, or 30 parts. The filler is preferably selected from one or more of silica, ground calcium carbonate, talc, clay, organobentonite, hydrogenated castor oil and barium sulphate. In particular embodiments, the filler is one or more of ground calcium carbonate, talc, and clay.
The component A comprises 10-30 parts of carbon black; in specific embodiments, the carbon black is used in an amount of 10 parts, 20 parts, or 30 parts. The carbon black is preferably selected from one or more of contact carbon black, furnace carbon black and fumed carbon black. In a specific embodiment, the carbon black is furnace carbon black.
The component A comprises 0.2-1 part of silane coupling agent; in specific embodiments, the silane coupling agent is present in an amount of 0.2 parts, 0.5 parts, or 1.0 part. The silane coupling agent is selected from one or more of beta- (3, 4-epoxycyclohexyl) ethyl trimethoxy silane, gamma-glycidyl ether propyl triethoxy silane, 3-glycidyl ether propyl methyl diethoxy silane, gamma-isocyanate propyl triethoxy silane and gamma-isocyanate propyl trimethoxy silane. In a specific embodiment, the silane coupling agent is gamma-glycidoxypropyltrimethoxysilane and/or gamma-isocyanatopropyltrimethoxysilane.
The component A comprises 0-1 part of water absorbent; in specific examples, the content of the water absorbing agent is 0 part, 0.5 part or 1.0 part. The water absorbent is preferably selected from one or more of alkyl sulphonic acid isocyanate, calcium oxide and molecular sieve. In particular embodiments of the present invention, the water-absorbing agent is selected from one or more of calcium oxide, molecular sieves, and TI water-absorbing agents.
The component A comprises 0.1-1 part of catalyst a. The catalyst a is selected from tertiary amine catalysts and/or tin catalysts; the tertiary amine catalyst is selected from one or more of N, N-dimethylcyclohexylamine, bis (2-dimethylaminoethyl) ether, bis morpholine diethyl ether, N, N, N ', N' -tetramethylalkylenediamine, triethylamine and N, N-dimethylbenzylamine; the tin catalyst is selected from one or more of dioctyltin dilaurate, dibutyltin dilaurate, dimethyltin dilaurate, stannous octoate, butyltin oxide and octyltin oxide. In a specific embodiment, the tertiary amine catalyst is dimorpholinodiethyl ether and the tin catalyst is dibutyltin dilaurate.
The two-component polyurethane windshield glass adhesive with the rapid curing capability provided by the invention comprises a component B; the component B comprises, by mass, 30-50 parts of polyether polyol a, 0-10 parts of tackifying resin, 10-30 parts of plasticizer, 20-50 parts of filler, 0-20 parts of carbon black, 0-10 parts of fumed silica and 1-10 parts of distilled water.
The component B comprises 30-50 parts of polyether polyol a. The polyether polyol a is selected from one or more of polyether diol, polyether triol and polyether tetraol; the molecular weight of the polyether glycol is preferably 1000-4000, and more preferably 2000-3000; the molecular weight of the polyether triol is preferably 3000-6000, and more preferably 4500-5000; the molecular weight of the polyether tetrahydric alcohol is preferably 1000-4000; more preferably 2000 to 3000. In a specific embodiment, the polyether polyol a is a polyether diol having a molecular weight of 2000; and or a polyether triol having a molecular weight of 5000.
The component B comprises 0-10 parts of tackifying resin. The tackifying resin is preferably selected from one or more of polyethylene glycol, polyester resin dihydric alcohol, acrylic resin dihydric alcohol, polycarbonate dihydric alcohol, rosin resin dihydric alcohol, hydrogenated petroleum resin dihydric alcohol and terpene resin dihydric alcohol. In a specific embodiment, the tackifying resin is one or more of rosin resin diol, polyester resin diol, and polycarbonate diol.
The component B comprises 10-30 parts of a plasticizer. In specific embodiments, the plasticizer is used in an amount of 20 parts, 30 parts, or 10 parts. The selection range of the plasticizer in the component B is consistent with the selection range of the plasticizer in the component A, and the specific types can be the same or different. In a specific embodiment, the plasticizer is diisodecyl phthalate.
The component B comprises 20-50 parts of filler. In particular embodiments, the filler is specifically 20 parts, 40 parts, or 50 parts. The filler is preferably selected from one or more of silica, ground calcium carbonate, talc, clay, organobentonite, hydrogenated castor oil and barium sulphate. In a particular embodiment, the filler is ground calcium carbonate.
The component B comprises 0-20 parts of carbon black. In specific examples, carbon black is used in an amount of specifically 0 part, 10 parts, or 20 parts. The carbon black is preferably selected from one or more of contact carbon black, furnace carbon black and fumed carbon black. In a specific embodiment, the carbon black is furnace carbon black.
The component B comprises 0-10 parts of fumed silica. In a specific embodiment, the content of the fumed silica is specifically 0 part, 5 parts or 10 parts.
The component B comprises 1-10 parts of distilled water. In specific embodiments, the amount of the distilled water is specifically 1 part, 5 parts, or 10 parts.
In certain embodiments of the present invention, the two-component polyurethane windshield glass paste comprises the following composition:
the component A comprises 30 parts of polyurethane prepolymer A, 30 parts of plasticizer, 10 parts of filler, 30 parts of carbon black, 0.5 part of silane coupling agent, 0.5 part of water absorbent and 0.1 part of tin catalyst; the component B comprises 30 parts of polyether polyol a, 0 part of tackifying resin, 30 parts of plasticizer, 40 parts of filler, 20 parts of carbon black, 0 part of fumed silica and 5 parts of distilled water;
or the component A comprises 30 parts of polyurethane prepolymer A, 30 parts of plasticizer, 10 parts of filler, 30 parts of carbon black, 0.5 part of silane coupling agent, 0.5 part of water absorbent, 0.2 part of tin catalyst and 0.2 part of amine catalyst; the component B comprises 30 parts of polyether polyol a, 5 parts of tackifying resin, 30 parts of plasticizer, 20 parts of filler, 20 parts of carbon black, 0 part of fumed silica and 10 parts of distilled water;
or the component A comprises 40 parts of polyurethane prepolymer A, 20 parts of plasticizer, 20 parts of filler, 20 parts of carbon black, 1.0 part of silane coupling agent, 1.0 part of water absorbent and 0.1 part of tin catalyst; the component B comprises 40 parts of polyether polyol a, 0 part of tackifying resin, 20 parts of plasticizer, 40 parts of filler, 20 parts of carbon black, 0 part of fumed silica and 5 parts of distilled water;
or the component A comprises 40 parts of polyurethane prepolymer A, 20 parts of plasticizer, 20 parts of filler, 20 parts of carbon black, 1.0 part of silane coupling agent, 1.0 part of water absorbent, 0.2 part of tin catalyst and 0.2 part of amine catalyst; the component B comprises 40 parts of polyether polyol a, 5 parts of tackifying resin, 20 parts of plasticizer, 20 parts of filler, 20 parts of carbon black, 0 part of fumed silica and 10 parts of distilled water;
or the component A comprises 50 parts of polyurethane prepolymer A, 10 parts of plasticizer, 30 parts of filler, 10 parts of carbon black, 1.0 part of silane coupling agent, 1.0 part of water absorbent, 0.2 part of tin catalyst and 0.2 part of amine catalyst; the component B comprises 50 parts of polyether polyol a, 0 part of tackifying resin, 10 parts of plasticizer, 60 parts of filler, 10 parts of carbon black, 5 parts of fumed silica and 1 part of distilled water;
or the component A comprises 50 parts of polyurethane prepolymer A, 10 parts of plasticizer, 30 parts of filler, 10 parts of carbon black, 1.0 part of silane coupling agent, 1.0 part of water absorbent and 0.1 part of tin catalyst; the component B comprises 50 parts of polyether polyol a, 0 part of tackifying resin, 10 parts of plasticizer, 40 parts of filler, 20 parts of carbon black, 0 part of fumed silica and 5 parts of distilled water;
or the component A comprises 50 parts of polyurethane prepolymer A, 10 parts of plasticizer, 30 parts of filler, 10 parts of carbon black, 0.2 part of silane coupling agent, 0.0 part of water absorbent, 0.2 part of tin catalyst and 0.2 part of amine catalyst; the component B comprises 50 parts of polyether polyol a, 5 parts of tackifying resin, 10 parts of plasticizer, 40 parts of filler, 0 part of carbon black, 10 parts of fumed silica and 5 parts of distilled water;
or the component A comprises 50 parts of polyurethane prepolymer A, 10 parts of plasticizer, 30 parts of filler, 0 part of carbon black, 1.0 part of silane coupling agent, 1.0 part of water absorbent, 0.2 part of tin catalyst and 0.2 part of amine catalyst; the component B comprises 50 parts of polyether polyol a, 5 parts of tackifying resin, 10 parts of plasticizer, 20 parts of filler, 20 parts of carbon black, 0 part of fumed silica and 10 parts of distilled water;
or the component A comprises 50 parts of polyurethane prepolymer A, 10 parts of plasticizer, 30 parts of filler, 10 parts of carbon black, 0.2 part of silane coupling agent, 0.0 part of water absorbent, 0.5 part of tin catalyst and 0.5 part of amine catalyst; the component B comprises 50 parts of polyether polyol a, 10 parts of tackifying resin, 10 parts of plasticizer, 20 parts of filler, 20 parts of carbon black, 0 part of fumed silica and 10 parts of distilled water.
The invention provides a preparation method of a double-component polyurethane windshield glass adhesive, which comprises the following steps:
dehydrating polyether polyol b, mixing with isocyanate and a catalyst b, and reacting to obtain a polyurethane prepolymer;
mixing the polyurethane prepolymer, the dehydrated plasticizer, the dried filler, the dried carbon black, the silane coupling agent and the water absorbent, adding the catalyst a under the vacuum degree of not less than 980mbar, and uniformly stirring to obtain a component A;
uniformly stirring polyether polyol a, tackifying resin, a dehydrated plasticizer, dry filler, dry carbon black, dry fumed silica and distilled water to obtain a component B;
and mixing the component A and the component B to obtain the double-component polyurethane windshield glass adhesive.
In the invention, the polyether polyol b is heated to 110-130 ℃ under stirring for dehydration for 2 hours, and then is cooled to 50 ℃ to be added with isocyanate and a catalyst b. According to the invention, the mixed polyether polyol b, isocyanate and catalyst b are preferably heated to 75-90 ℃ and then react for 2-6 hours, and the temperature is reduced to below 50 ℃ to obtain the polyurethane prepolymer.
The plasticizer is preferably dehydrated in vacuum at 110-130 ℃ for 2 hours to obtain the dehydrated plasticizer.
Preferably, the filler, the carbon black and the fumed silica are dried at 115-125 ℃ for 3-7 days until the moisture content is below 1000ppm, so as to obtain the dried filler, the dried carbon black and the dried fumed silica.
When the component B is prepared, the polyether polyol a, the tackifying resin, the dehydrated plasticizer, the dried filler, the dried carbon black and the dried fumed silica are preferably uniformly mixed, and then distilled water is added under the vacuum degree of not less than 980 mbar.
The prepared double-component polyurethane windshield glass adhesive overcomes the defect of slow curing of the single-component polyurethane windshield glass adhesive in the after-sale markets of automobile factories and automobiles, and improves the assembly effect of the windshield glass and matched components.
To further illustrate the present invention, a two-component polyurethane windshield glass paste with rapid curing capability and a method for preparing the same are described in detail below with reference to examples, but they should not be construed as limiting the scope of the invention.
Preparative example 1 preparation of polyurethane prepolymer:
1500g of polyether triol (average molecular weight of 5000, hydroxyl value of 33.6mgKOH/g) and 500g of polyether diol (average molecular weight of 2000, hydroxyl value of 56mgKOH/g) are heated to 130 ℃ for dehydration for 2 hours, then the temperature is reduced to 50 ℃, 248g of 4,4 '-diisocyanate phenyl methane (4, 4' -MDI) (NCO/OH is 1.8) and 0.15g of dibutyltin dilaurate are added, and after mixing, the temperature is raised to 90 ℃ for reaction for 6 hours, and then the polyurethane prepolymer with the NCO content of 2.14% is obtained.
Example 1
Mixing the polyurethane prepolymer in the preparation example 1, dehydrated plasticizer diisodecyl phthalate, dried heavy calcium carbonate, dried carbon black, silane coupling agent gamma-glycidyl ether propyl trimethoxy silane and TI water absorbent, adding catalyst a under the vacuum degree of not less than 980mbar, and uniformly stirring to obtain component A;
uniformly stirring polyether polyol a (polyether triol with the molecular weight of 5000), dehydrated plasticizer diisodecyl phthalate, dry heavy calcium carbonate, dry furnace carbon black, dry fumed silica and distilled water to obtain a component B;
and respectively inserting the tubes containing the component A and the component B into a high-speed mixing glue gun with a dynamic mixing head, and extruding the component A and the component B at a high speed according to the volume ratio of 10:1 by using the glue gun to obtain the double-component polyurethane windshield glass glue.
Example 2
The raw materials were the same type but in different proportions as compared with example 1.
Example 3
Compared with the example 1, the different raw materials in the component A are as follows: the filler is talcum powder; the plasticizer is diisononyl phthalate; .
The different raw materials in the component B are as follows: the filler is talcum powder; the tackifying resin is rosin resin dihydric alcohol.
Example 4
The raw materials were the same type but in different proportions as compared with example 3.
Example 5
Compared with the example 1, the different raw materials in the component A are as follows: the filler is clay; the plasticizer is alkyl sulfonate.
The different raw materials in the component B are as follows: the filler is clay; the tackifying resin is rosin resin dihydric alcohol.
Example 6
The raw materials were the same type but in different proportions as compared with example 5.
Example 7
Compared with the example 1, the different raw materials in the component A are as follows: the water absorbent is a molecular sieve; the silane coupling agent is gamma-isocyanate propyl trimethoxy silane.
The different raw materials in the component B are as follows: the tackifying resin is polyester resin dihydric alcohol.
Example 8
The raw materials were the same kind but in different proportions as compared with example 7.
Example 9
Compared with the example 3, the different raw materials in the component A are as follows: the water absorbent is a molecular sieve; the silane coupling agent is gamma-isocyanate propyl trimethoxy silane.
The different raw materials in the component B are as follows: the tackifying resin is polyester resin dihydric alcohol.
Example 10
The raw materials were the same kind but in different proportions as compared with example 9.
Example 11
Compared with the example 5, the different raw materials in the component A are as follows: the water absorbent is a molecular sieve; the silane coupling agent is gamma-isocyanate propyl trimethoxy silane.
The different raw materials in the component B are as follows: the tackifying resin is polyester resin dihydric alcohol.
Example 12
The raw materials were the same kind but in different proportions as compared with example 11.
Example 13
Compared with the example 1, the different raw materials in the component A are as follows: the water absorbent is calcium oxide; .
The different raw materials in the component B are as follows: the polyether polyol a is polyether diol (molecular weight 2000); the tackifying resin is polycarbonate dihydric alcohol.
Example 14
The raw materials were the same kind but in different proportions as compared with example 13.
Example 15
Compared with the example 3, the different raw materials in the component A are as follows: the water absorbent is calcium oxide; .
The different raw materials in the component B are as follows: the polyether polyol a is polyether diol (molecular weight 2000); the tackifying resin is polycarbonate dihydric alcohol.
Example 16
The raw materials were the same kind but in different proportions as compared with example 15.
Example 17
Compared with the example 5, the different raw materials in the component A are as follows: the water absorbent is calcium oxide; .
The different raw materials in the component B are as follows: the polyether polyol a is polyether diol (molecular weight 2000); the tackifying resin is polycarbonate dihydric alcohol.
Example 18
The raw materials were the same kind but in different proportions as compared with example 17.
The invention tests the performance of the two-component polyurethane windshield glass adhesive prepared in the embodiment 1-18, and the test method adopts GB/T7124 to respectively measure the tensile shear strength of the two-component polyurethane windshield glass adhesive after 30min, 60min and 120 min. The results are shown in tables 1 and 2 respectively, and table 1 is a tensile shear strength test result of the two-component polyurethane windshield glass cement prepared in examples 1-9 of the invention; table 2 shows the tensile shear strength test results of the two-component polyurethane windshield glass cement prepared in examples 10 to 18 of the present invention;
TABLE 1 tensile shear Strength test results for two-component polyurethane windshield glass pastes prepared in inventive examples 1-9
Figure BDA0001996453810000111
Figure BDA0001996453810000121
TABLE 2 tensile shear Strength test results for two-component polyurethane windshield glass pastes prepared in inventive examples 10-18
Figure BDA0001996453810000122
From the above examples, it can be seen that the present invention provides a two-component polyurethane windshield adhesive with fast curing capability, comprising a component a and a component B: the component A comprises the following components in parts by weight: 30-50 parts of polyurethane prepolymer, 10-30 parts of plasticizer, 10-30 parts of filler, 10-30 parts of carbon black, 0.2-1 part of silane coupling agent, 0-1 part of water absorbent and 0.1-1 part of catalyst a; the component B comprises the following components: 30-50 parts of polyether polyol a, 0-10 parts of tackifying resin, 10-30 parts of plasticizer, 20-50 parts of filler, 0-20 parts of carbon black, 0-10 parts of fumed silica and 1-10 parts of distilled water. The two-component polyurethane windshield glass cement provided by the invention comprises the component A and the component B which are matched with each other, so that the glass cement has relatively high curing capability. The experimental results show that: the operable time of the windshield glass cement is 16-27 min; the tensile shear strength is 0.20-0.36 MPa after 30 min; the tensile shear strength is 1.0-1.5 MPa after 60 min; the tensile shear strength is 2.0-2.5 MPa after 120 min.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (2)

1. A two-component polyurethane windshield glass cement with fast curing capability comprises a component A and a component B: the volume ratio of the component A to the component B is 10: 1;
the component A comprises the following components in parts by weight:
30-50 parts of polyurethane prepolymer, 10-30 parts of plasticizer, 10-30 parts of filler, 10-30 parts of carbon black, 0.2-1 part of silane coupling agent, 0-1 part of water absorbent and 0.1-1 part of catalyst a;
the silane coupling agent is selected from gamma-glycidyl ether propyl trimethoxy silane and/or gamma-isocyanate propyl trimethoxy silane; the catalyst a is selected from dimorpholinodiethyl ether and/or dibutyltin dilaurate;
the component B comprises the following components:
30-50 parts of polyether polyol a, 0-10 parts of tackifying resin, 10-30 parts of plasticizer, 20-50 parts of filler, 0-20 parts of carbon black, 0-10 parts of fumed silica and 1-10 parts of distilled water;
the polyether polyol a is selected from polyether diols with molecular weight of 2000; and/or a polyether triol having a molecular weight of 5000;
the plasticizer is diisodecyl phthalate; the filler is selected from one or more of ground calcium carbonate, talcum powder and clay;
the tackifying resin is selected from one or more of rosin resin dihydric alcohol, polyester resin dihydric alcohol and polycarbonate dihydric alcohol;
the polyurethane prepolymer is prepared by the reaction of polyether polyol b, isocyanate and a catalyst b;
the mass ratio of the polyether polyol b to the isocyanate to the catalyst b is 100: 2-10: 0.01-0.05;
the polyether polyol b is selected from polyether triol with the molecular weight of 5000 and the hydroxyl value of 33.6 mgKOH/g; and/or a polyether diol having a molecular weight of 2000 and a hydroxyl value of 56 mgKOH/g;
the isocyanate is selected from MDI;
the catalyst b is selected from one or more of dioctyltin dilaurate, dibutyltin dilaurate, dimethyltin dilaurate, stannous octoate, dibutyltin oxide and dioctyltin oxide.
2. A method of making a two-component polyurethane windshield glass paste of claim 1 comprising the steps of:
dehydrating polyether polyol b, mixing with isocyanate and a catalyst b, and reacting to obtain a polyurethane prepolymer;
mixing the polyurethane prepolymer, the dehydrated plasticizer, the dried filler, the dried carbon black, the silane coupling agent and the water absorbent, adding the catalyst a under the vacuum degree of not less than 980mbar, and uniformly stirring to obtain a component A;
uniformly stirring polyether polyol a, tackifying resin, a dehydrated plasticizer, dry filler, dry carbon black, dry fumed silica and distilled water to obtain a component B;
and mixing the component A and the component B to obtain the double-component polyurethane windshield glass adhesive.
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US6130268A (en) * 1997-06-23 2000-10-10 Polyfoam Products, Inc. Two component polyurethane construction adhesive

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US9428678B2 (en) * 2012-12-21 2016-08-30 Dow Global Technologies Llc Fast curing adhesive useful for bonding to glass
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US6130268A (en) * 1997-06-23 2000-10-10 Polyfoam Products, Inc. Two component polyurethane construction adhesive

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