CN101760143A - Highly-transparent polyurethane hot-melt film applicable to sandwich glass and preparation method thereof - Google Patents
Highly-transparent polyurethane hot-melt film applicable to sandwich glass and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a highly-transparent polyurethane hot-melt film applicable to sandwich glass. The hot-melt film consists of the following materials by weight percent: 40.0-86.0% of polyether polyol, 1.5-20.0% of small molecule chain extender, 10.0-33.0% of diisocyanate; 0.01%-0.50% of catalyst, 0.1-1.0% of antioxidant, 0.1-1.0% of optical stabilizer and 1.0-4.5% of coupling agent. The invention also discloses a preparation method of the highly-transparent polyurethane hot-melt film. The highly-transparent polyurethane hot-melt film prepared according to the invention performs well in terms of agglutinating glass and PC panels, has high light transmission rate and low dimness. In addition, the preparation process of the highly-transparent polyurethane hot-melt film is simple and easy to control. The highly-transparent polyurethane hot-melt film can be widely used in automobile, aviation, architecture, financial and other industries.
Description
Technical field
The present invention relates to a kind of glass, PC plate to be had the highly-transparent polyurethane hot-melt film of good adhesion, and the method for preparing this highly-transparent polyurethane hot-melt film.
Background technology
Laminated glass is a kind of ambetti of decorating with security that integrates, and has a extensive future.It not only can protect the person and property safety, but also keeps the attractive in appearance, transparent of glass, can select the pattern of decorating film simultaneously according to hobby, has application surface very widely.
At present, the widely used middle layer of China's laminated glass industry adhesives is polyvinyl butyral film (a PVB film), the PVB film can bonding effectively unorganic glass in very wide temperature range, but it is low with the bonding strength of polycarbonate (PC) plate, PET plate etc., and the easy embrittlement of PVB film at low temperatures, compound thermal expansivity differs bigger inorganic simultaneously---organic materials.
Polyurethane pellicle is a kind of novel middle layer adhesives, and it has remedied the deficiency of PVB film, from low temperature to high temperature, it can bonding unorganic glass again can bonding polycarbonate (PC) plate, transparent organic material such as PET plate.Polyurethane pellicle provides inorganic and organic compound possibility, provides light weight, product that intensity is high to market.Can be widely used in construction industry, car industry, air system, financial industry, be particularly suitable for splinter-proof glass.
Patent No. CN98110958.6 discloses a kind of film that is used for shatter proof glass, its main method is by forming heating in specific mixing equipment after urethane raw, acrylic raw material, the Resins, epoxy heat fused, stir, being mixed with respectively, it has improved the bonding of chilled glass and PC/PET plate, and keeps preferable see-through; Chinese patent CN200810079298.4 has described a kind of adhering film to glass, and this pad pasting mainly is to mix by add urethane resin in solvent-type acrylic class pressure-sensitive adhesive; But these inventions all do not relate to how preparing this kind urethane raw.In the prior art, it is a lot of to be used to prepare the urethane report with good transparency, all described as U.S. Pat 6222999, US6174984 and Chinese patent CN200580035278.1 and to be used to prepare certain methods with good clear based polyurethane, but these technology all only relate to the polyurethane elastomer that adopts the cast form to obtain the transparency, fail really to use as tackiness agent.
Summary of the invention
First purpose of the present invention is at the deficiencies in the prior art part, and a kind of laminated glass highly-transparent polyurethane hot-melt film that can be used for is provided.
Second purpose of the present invention is to provide the preparation method of above-mentioned polyurethane hot-melt film.
For reaching first purpose, the present invention adopts following technical scheme:
The highly-transparent polyurethane hot-melt film that can be used for laminated glass, form by following components in weight percentage:
Polyether glycol 40.0～86.0%
Small molecule chain extender 1.5～20.0%
Vulcabond 10.0～33.0%
Catalyzer 0.01%～0.50%
Antioxidant 0.1～1.0%
Optical stabilization agent 0.1～1.0%
Coupling agent 1.0～4.5%.
For reaching second purpose, the present invention adopts following technical scheme:
The preparation method of highly-transparent polyurethane hot-melt film may further comprise the steps successively:
1) with polyether glycol, small molecule chain extender respectively at 100-120 ℃ of following vacuum hydro-extraction 2-3h, make its moisture content less than 0.05%;
2) polyether glycol that will take off water adds in the forcing machine by weight with isocyanic ester, part catalyzer (50%-80% of total catalyst consumption), antioxidant and optical stabilization agent and mixes, reacts; Add residual catalyst, small molecule chain extender and coupling agent at the forcing machine middle part, continue reaction; The material charging region temperature of forcing machine is 90-150 ℃, reaction zone temperature 140-250 ℃, extrudes 160-210 ℃ of district's temperature, reaction times 3-8 minute; Extrude cooling granulation at last;
3) transparent particles that step 2 is obtained curtain coating on casting machine becomes transparent film.
Highly-transparent polyurethane hot-melt film by the present invention obtains has good bounding force to glass, PC plate, the transmittance height, and turbidity is low, and production technique is simple, easily control.Can be widely used in industries such as automobile, aviation, building, finance.
Embodiment
Highly-transparent polyurethane hot-melt film of the present invention is to be that 40.0～86.0% polyether glycol, 1.5～20.0% small molecule chain extender, 10.0～33.0% vulcabond, 0.01%～0.50% catalyzer, 0.1～1.0% antioxidant, 0.1～1.0%, optical stabilization agent and 1.0～4.5% coupling agents are formed by weight percent.
Wherein, described polyether glycol is to be made by the open loop of epoxy compound polymerization under as the condition of initiator and catalyzer containing active hydrogen compounds.Polyether glycol is selected from the combination that number-average molecular weight is any or at least two kinds of polyoxytrimethylene dibasic alcohol, polyoxyethylene dibasic alcohol, polytetrahydrofuran dibasic alcohol, polytetrahydrofuran-ethylene oxide copolymerization dibasic alcohol and polytetrahydrofuran-propylene oxide copolymerization dibasic alcohol of 500～6000 usually, and preferred number average molecular weight is 1000～3000 polytetrahydrofuran dibasic alcohol.
Wherein, described small molecule chain extender is selected from methyl propanediol and ethylene glycol, glycol ether, propylene glycol, 1,4-butyleneglycol, 1,6-hexylene glycol, 1,3-butyleneglycol, 1,5 pentanediols, 1, the mixture of any composition in two [2-hydroxyethyl] ethers of 4-cyclohexyl dimethanol, quinhydrones, the dipropylene glycol, or their combinations of at least two kinds.Methyl propanediol and 1 wherein, it is preferred small molecule chain extender that the 4-butyleneglycol mixes.
Wherein, described vulcabond is preferably fat (ring) adoption isocyanic ester, comprise 4,4 '-dicyclohexyl methane diisocyanate (RMDI), 1,6-hexylidene diisocyanate (HDI), isophorone diisocyanate (IPDI), 1, the mixture that in a 4-cyclohexyl diisocyanate (CHDI) and the tetramethylxylene diisocyanate (M-TMXDI) any or they are at least two kinds, further preferred HDI and IPDI, most preferably IPDI.
The production of polyurethane elastomer also needs to add catalyzer, to quicken its polyreaction.Because the property of this product needs the mixing of machine tin compound and tertiary amine and just can reach.Organo-tin compound comprises dibutyl tin laurate and stannous octoate, the preferred triethylamine of tertiary amine, triethylenediamine, trolamine etc., and the ratio of organo-tin compound and tertiary amine is 3: 1～1: 1.
The main effect of antioxidant is the thermal oxidation of retardance urethane, stops the chain-breaking reaction of the polymkeric substance that is brought out by oxygen, and decomposes the hydrogen peroxide that generates.Described antioxidant is selected from the combination of at least two kinds of any or they in 264,1010,1076,1026,245.
Wherein, described optical stabilization agent is selected from the mixture of at least two kinds of any or they among UV-9, UV-327, UV-328, UV-329, the UV-531.
Wherein, described coupling agent is selected from silane coupling agent: the combination that any in γ-An Bingjisanyiyangjiguiwan (KH-550), γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560), γ-methacryloxypropyl trimethoxy silane (KH570), vinyltriethoxysilane (A-151), vinyltrimethoxy silane (A-171), vinyl three ('beta '-methoxy oxyethyl group) silane (A-172), N-β-(the aminoethyl)-γ-An Bingjisanjiayangjiguiwan (KH-900) or they are at least two kinds.
Embodiment 1
The polyoxypropyleneglycol mixture of the polytetrahydrofuran diol of 100Kg molecular weight 2000,50Kg molecular weight 2000 at 120 ℃ of following vacuum hydro-extraction 2h, is made it moisture content less than 0.05%.
With above-mentioned polyol blends and the 0.8Kg catalyzer (mixed solution of 0.4Kg dibutyl tin laurate and 0.4Kg triethylamine) that had just taken off water, the 1Kg antioxidant 1010, after 1Kg optical stabilization agent UV328 mixes, continuously flow in the twin screw extruder in 4.5: 1 ratio with 34Kg MDI again and mix, reaction, when streams is in the middle part of forcing machine, begin to contain mixed chain extender (the 7Kg methyl propanediol of taking off water in ratios interpolations in 10: 1 of actual flow, 7Kg1, the 6-hexylene glycol), 2.4Kg coupling agent KH560,0.8Kg catalyzer (mixed solution of 0.4Kg dibutyl tin laurate and 0.4Kg triethylamine), 70 rev/mins of screw speeds, 120 ℃ of material charging region temperature, 190 ℃ of reaction zone temperatures are extruded 205 ℃ of district's temperature.It is standby to extrude cooling granulation at last, and particle obtains high transparent polyurethane hot-melt film again through the casting machine casting film-forming.Product property sees Table 1.
Embodiment 2
The polytetrahydrofuran diol of 176Kg molecular weight 2000 at 120 ℃ of following vacuum hydro-extraction 2h, is made it moisture content less than 0.05%.
With above-mentioned polyol blends and the 0.8Kg catalyzer (mixed solution of 0.4Kg dibutyl tin laurate and 0.4Kg triethylamine) that had just taken off water, 1Kg antioxidant 245, after 1Kg optical stabilization agent UV9 mixes, continuously flow in the twin screw extruder in 8.8: 1 ratio with 20Kg IPDI again and mix, reaction, when streams is in the middle part of forcing machine, begin to add and contain the mixed chain extender of taking off water (the 1Kg methyl propanediol is closed 2Kg 1 in 37.8: 1 ratios of actual flow, the 6-hexylene glycol), 2Kg coupling agent KH550,0.2Kg catalyzer (mixed solution of 0.1Kg dibutyl tin laurate and 0.1Kg triethylamine), 80 rev/mins of screw speeds, 120 ℃ of material charging region temperature, 170 ℃ of reaction zone temperatures are extruded 190 ℃ of district's temperature.It is standby to extrude cooling granulation at last, and particle obtains high transparent polyurethane hot-melt film again through the casting machine casting film-forming.Product property sees Table 1.
Embodiment 3
The polyoxypropyleneglycol of 80Kg molecular weight 1000 at 120 ℃ of following vacuum hydro-extraction 2h, is made it moisture content less than 0.05%.
With above-mentioned polyol blends and the 0.8Kg catalyzer (mixed solution of 0.4Kg dibutyl tin laurate and 0.4Kg triethylamine) that had just taken off water, the 2Kg antioxidant 1010, after 2Kg optical stabilization agent UV327 mixes, successively flow in the twin screw extruder in 1.28: 1 ratios with 66Kg HDI again and mix, reaction, when streams is in the middle part of forcing machine, begin to contain the mixed chain extender (4Kg methyl propanediol and 36Kg dipropylene glycol) of taking off water in ratios interpolations in 3.0: 1 of actual flow, 9Kg coupling agent A-172,0.2Kg catalyzer (mixed solution of 0.1Kg dibutyl tin laurate and 0.1Kg triethylamine), 80 rev/mins of screw speeds, 110 ℃ of material charging region temperature, 180 ℃ of reaction zone temperatures are extruded 190 ℃ of district's temperature.It is standby to extrude cooling granulation at last, and particle obtains high transparent polyurethane hot-melt film again through the casting machine casting film-forming.Product property sees Table 1.
Embodiment 4
The polytetrahydrofuran diol of 140Kg molecular weight 1500 at 120 ℃ of following vacuum hydro-extraction 2h, is made it moisture content less than 0.05%.
With above-mentioned polyvalent alcohol and the 0.8Kg catalyzer (mixed solution of 0.4Kg dibutyl tin laurate and 0.4Kg triethylamine) that had just taken off water, 1.0Kg antioxidant 1010, after 1.0Kg optical stabilization agent UV327 mixes, continuously flow in the twin screw extruder in 3.57: 1 ratios with 40Kg IPDI again and mix, reaction, when streams is in the middle part of forcing machine, begin to contain mixed chain extender (the 9Kg methyl propanediol of taking off water in ratios interpolations in 10.6: 1 of actual flow, 5Kg 1, the 4-butyleneglycol), 2.4Kg coupling agent KH550,0.8Kg catalyzer (mixed solution of 0.4Kg dibutyl tin laurate and 0.4Kg triethylamine), 90 rev/mins of screw speeds, 130 ℃ of material charging region temperature, 175 ℃ of reaction zone temperatures are extruded 195 ℃ of district's temperature.It is standby to extrude cooling granulation at last, and particle obtains high transparent polyurethane hot-melt film again through the casting machine casting film-forming.Product property sees Table 1.
Table 1 product physicals result
As can be seen from the table, four high transparent polyurethane hot-melt films that embodiment obtains all have the transmittance height, and turbidity is low, and is big to the bonding strength of glass, PC plate, can widely apply in industries such as automobile, aviation, building, finance.
Claims (10)
1. can be used for the highly-transparent polyurethane hot-melt film of laminated glass, it is characterized in that, form by following components in weight percentage:
Polyether glycol 40.0～86.0%
Small molecule chain extender 1.5～20.0%
Vulcabond 10.0～33.0%
Catalyzer 0.01%～0.50%
Antioxidant 0.1～1.0%
Optical stabilization agent 0.1～1.0%
Coupling agent 1.0～4.5%.
2. hot-melt film according to claim 1, it is characterized in that, it is any of polyoxytrimethylene dibasic alcohol, polyoxyethylene dibasic alcohol, polytetrahydrofuran dibasic alcohol, polytetrahydrofuran-ethylene oxide copolymerization dibasic alcohol and polytetrahydrofuran-propylene oxide copolymerization dibasic alcohol of 500～6000 that described polyether glycol is selected from number-average molecular weight, or their combinations of at least two kinds.
3. hot-melt film according to claim 2 is characterized in that, described polyether glycol is that number-average molecular weight is 1000～3000 polytetrahydrofuran dibasic alcohol.
4. hot-melt film according to claim 1, it is characterized in that, described small molecule chain extender is selected from methyl propanediol and ethylene glycol, glycol ether, propylene glycol, 1,4-butyleneglycol, 1,6-hexylene glycol, 1,3 butylene glycol, 1,5 pentanediol, 1, the mixture of any composition in two [2-hydroxyethyl] ethers of 4-cyclohexyl dimethanol, quinhydrones, the dipropylene glycol, or their combinations of at least two kinds.
5. hot-melt film according to claim 5, it is characterized in that, described vulcabond is fat [ring] adoption isocyanic ester, comprise 4,4 '-dicyclohexyl methane diisocyanate, 1,6-hexylidene diisocyanate, isophorone diisocyanate, 1, any in a 4-cyclohexyl diisocyanate and the tetramethylxylene diisocyanate, or their combinations of at least two kinds.
6. hot-melt film according to claim 1 is characterized in that, described catalyzer is the mixture of organo-tin compound and tertiary amine.
7. hot-melt film according to claim 1 is characterized in that, described antioxidant is selected from any in antioxidant 264, antioxidant 1010, antioxidant 1076, antioxidant 1026 and the antioxidant 245, or their combinations of at least two kinds.
8. hot-melt film according to claim 1, it is characterized in that, described optical stabilization agent be selected among optical stabilization agent UV-9, optical stabilization agent UV-327, optical stabilization agent UV-328, optical stabilization agent UV-329 and the optical stabilization agent UV-531 any or, their combinations of at least two kinds.
9. hot-melt film according to claim 1, it is characterized in that, described coupling agent is a silane coupling agent, comprise in γ-An Bingjisanyiyangjiguiwan, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, vinyltrimethoxy silane, vinyl three ['beta '-methoxy oxyethyl group] silane, N-β-[the aminoethyl]-γ-An Bingjisanjiayangjiguiwan any, or their combinations of at least two kinds.
10. the preparation method of highly-transparent polyurethane hot-melt film according to claim 1 is characterized in that, may further comprise the steps successively:
1) with polyether glycol, small molecule chain extender respectively at 100-120 ℃ of following vacuum hydro-extraction 2-3h, make its moisture content less than 0.05%;
2) polyether glycol that will take off water adds in the forcing machine by weight with 50%-80%, antioxidant and the optical stabilization agent of isocyanic ester, total catalyst consumption and mixes, reacts; Add residual catalyst, small molecule chain extender and coupling agent at the forcing machine middle part, continue reaction; The material charging region temperature of forcing machine is 90-150 ℃, reaction zone temperature 140-250 ℃, extrudes 160-210 ℃ of district's temperature, reaction times 3-8 minute; Extrude cooling granulation at last;
3) transparent particles that step 2 is obtained curtain coating on casting machine becomes transparent film.
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