| The alcohol-soluble epoxy-polyacrylate and amino-polyurethane was designedand synthesized, then the alcohol-soluble laminating adhesive with two-componentswas made by blending with a certain proportion. Through process optimization,product characterization, performance testing, a friendly environment, excellentadhesive properties of two-components alcohol-soluble polyacrylate-polyurethanelaminating adhesive was obtained. In this paper we studied the synthesis ofalcohol-soluble epoxy-polyacrylate and alcohol-soluble amino-polyurethane, andthe exploration of the compounding process conditions, the specific contents andresults were as follows:Firstly, synthesis of alcohol-soluble epoxy-polyacrylate through four scenarios.Scheme first, with glycidyl methacrylate (GMA) as an epoxy functional monomer,ethyl acrylate (EA),vinyl acetate (VAc) and hydroxypropyl acrylate (HPA) as themain monomer, evennitrogen-bis-isobutyronitrile (AIBN) as initiator, anhydrousethanol as solvent to obtain the GMA-epoxy modified polyacrylate solution. Theinfluence of the reaction time, temperature, the amount of initiator, functionalmonomer and the main monomer ratio was investigated. The result shows theoptimum conditions were as follows: copolymerization reaction time was5h,reaction temperature was75℃,the amount of initiator AIBN was1.0%(of totalmonomer),GMA content was13%,HPA content was14%and m(EA): m(VAC)=6:4.Scheme second, with epoxy resin E-51and methacrylate, the ethylenemethacrylic acid monoester was produced, and use this as an epoxy functionalmonomer, together with EA,VAC and HPA to obtained the ethylene methacrylicacid monoester modified polyacrylates solution. The result shows the optimumconditions were as follows: copolymerization reaction time was6h,reactiontemperature was75℃,the amount of initiator AIBN was1.6%(of totalmonomer),the ethylene methacrylic acid monoester content was13%,HPA contentwas14%and m(EA): m(VAC)=6:4.Scheme third, allyl glycidyl ether(AGE) as anepoxy functional monomer, together with EA,VAC and HPA to obtained theAGE-epoxy polyacrylate solution. The result shows the optimum conditions were asfollows: copolymerization reaction time was5h,reaction temperature was75℃,theamount of initiator AIBN was1.8%(of total monomer),the AGE content was35%,HPA content was10%and m(EA): m(VAC)=6:4.Scheme fourth, ethylenemethacrylic acid monoester and AGE)as epoxy functional monomers, together withEA,VAC and HPA to obtained the AGE-ethylene methacrylic acid monoestermodified polyacrylate solution.The result shows the optimum conditions were as follows: copolymerization reaction time was5h,reaction temperature was75℃,theamount of initiator AIBN was1.6%(of total monomer),the ethylene methacrylic acidmonoester content was15%,the AGE content was35%,HPA content was15%andm(EA): m(VAC)=6:4.By FTIR characterization, proved that the epoxygroup-containing functional groups has been in the product. By differential thermalscanning calorimetry studies showed that: only exhibit a glass transitiontemperature, respectively was4.25℃,5.16℃,-15.13℃and-0.66℃.It can provedthat the product obtained was a random copolymer.Secondly, use the method of prepolymerized body and the low-temperaturecontrol, the alcohol-soluble amino-polyurethane was synthesized. The influence ofpolyether diol (PPG) MW, the isocyanate species, the type of end-capping agentand the-NCO/-OH (R) values was investigated. The optimal synthesis conditions ofthe product was obtained. And the products were characterized by FTIR anddifferential scanning calorimeter. The result shows the optimum conditions were asfollows:PPG1000/PPG2000=2/1and the diphenylmethane diisocyanate (MDI) asthe raw material, the R value was1.4,the reaction temperature was70℃,thereaction time was2h,Diethylenetriamine as capping agent.By FTIR characterizationwe found the disappearance of characteristic peak of-NCO. And this proved in thepolyurethane prepolymer-NCO has been capped by amino group totally. Bydifferential thermal scanning calorimetry studies showed that: only exhibit a glasstransition temperature of45.83℃,this can be proved that the resulting product is arandom copolymer.Thirdly, blended alcohol-soluble epoxy-polyacrylate and the alcohol-solubleamino-polyurethane with a certain proportion to obtained the alcohol-solubletwo-component laminating adhesive. The influence of the proportion of the complex,the curing time and the curing temperature on laminating adhesive performance hasbeen discussed. The result found that when compound of the GMA-epoxy modifiedpolyacrylate and amino-polyurethane with ratio of20:14,the curing time was24h,and the curing temperature was50℃,the performance was best. Measured theBOPP lateral/MCPP peeling strength was0.138N/15mm,BOPP vertical/MCPP peelstrength was0.130N/15mm.When compound of the ethylene methacrylic acidmonoester modified polyacrylate and amino-polyurethane with ratio of20:21,thecuring time was24h,and the curing temperature was50℃,the performance was best.Measured the BOPP lateral/MCPP peeling strength was0.127N/15mm,BOPPvertical/MCPP peel strength was0.124N/15mm.When compound of the AGE-epoxypolyacrylate and amino-polyurethane with ratio of20:10,the curing time was24h,and the curing temperature was50℃,the performance was best. Measured theBOPP lateral/MCPP peeling strength was0.21N/15mm,BOPP vertical/MCPP peelstrength was0.202N/15mm.When compound of the AGE-ethylene methacrylic acid monoester modified polyacrylate and amino-polyurethane with ratio of20:6,thecuring time was24h,and the curing temperature was50℃,the performance was best.Measured the BOPP lateral/MCPP peeling strength was0.232N/15mm,BOPPvertical/MCPP peel strength was0.223N/15mm.Finally by comparison withimported lamination performance, the self-made laminating adhesive were able toreach the level of imported laminating adhesive. |
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