3 lines
5.0 KiB
JSON
3 lines
5.0 KiB
JSON
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"protocol": "The synthesis of hydrophilic polymers with functional groups is conducted by copolymerizing a glycidyl monomer with an N-vinyl lactam. Specific details include the use of 35-75% by weight of at least one glycidyl monomer, in combination with 10-30% by weight of the N-vinyl lactam. Additional functional groups can be introduced by including an ethylenically unsaturated carboxylic acid in percentages ranging from 0.1-10% by weight. The molecular weight of the copolymers is optimized to be within the range of 10,000-500,000. Catalysts or curing agents such as 1,3-bis(dimethylamino)-2-hydroxypropane may be utilized to facilitate the curing of the epoxy groups. The resulting polymer should demonstrate high adhesion properties and suitable mechanical characteristics under varying temperatures and humidity conditions.Copolymers are prepared by copolymerizing a mixture of 15 monomers comprising: 55 to 85% by weight of an alkyl acrylate and/or methacrylate ester containing 4 to 12 carbon atoms in the alkyl group; 0.01 to 2% by weight of a glycidyl monomer; 1 to 20% by weight of an N-vinyl lactam monomer; 0 to 15% by weight of an unsaturated carboxylic acid; 0 to 35% by weight of an alkyl acrylate and/or methacrylate ester containing less than 4 carbon atoms in the alkyl group; optionally 0 to 33% by weight of one or more other comonomers. The precise ratio of the monomers is selected to give a polymer with a glass transition temperature lower than -15° C. The weight average molecular weight of the polymers should be at least 200,000, preferably from 200,000 to 500,000, determined by size exclusion chromatography using polystyrene as the calibrator. The copolymers may be synthesized using solution, emulsion, and batch polymerization techniques.The synthesis of hydrophilic polymers is performed via solution polymerization using a mixture of solvents, preferably a blend of ethyl acetate and hexane or ethyl acetate and acetone. The solvent ratio is adjusted to achieve a reflux temperature between 68° C. and 78° C. A solids content of approximately 40% to 60% is maintained during polymerization to achieve the desired weight average molecular weight and manageable viscosities. Free-radical initiators, preferably azo-type such as 2,2'-azobis(isobutyronitrile), are used to initiate the reaction. The glycidyl monomer is limited to 2% by weight of the total monomers to avoid cross-linking. Post-polymerization cross-linking may be performed using heat, actinic or electron beam radiation. The presence of glycidyl and lactam monomers is essential for superior adhesion to high energy surfaces.A monomer mixture was prepared by mixing 423 g of 5 2-ethyl hexyl acrylate, 145 g of methyl acrylate, 3.15 g of glycidyl methacrylate, 12.6 g of N-vinyl pyrrolidone, and 44.1 g of acrylic acid. 157 g of this mixture was introduced into a 2-liter reactor equipped with a pitched turbine agitator, a reflux condenser, and a thermistor. Additionally, 73.5 g of ethyl acetate and 78.76 g of hexane were added. The reactor contents were heated to reflux, and 0.238 g of Vazo 64 was added in 5 g of ethyl acetate. The contents were held under vigorous reflux for 23 minutes. The remaining monomers, mixed with 37.2 g of ethyl acetate, 5.2 g of hexane, and 0.707 g of Vazo 64, were added as a single feed mixture over 3.5 hours, maintaining the temperature to keep the reactor contents under reflux. One hour after the end of the feed, an additional 0.17 g of Vazo 64 was added in 5 g of ethyl acetate, and the mixture was held for an additional hour. The final solids content was 46.4% and the viscosity was 23 Pa.s using #4@12 on a Brookfield viscometer.A monomer mixture was made up by mixing 453.6 g of Isooctyl acrylate, 100.8 g of methyl acrylate, 6.3 g of glycidyl methacrylate, 25.2 g of N-vinyl caprolactam, 4.1 g of acrylic acid and 0.945 g of Vazo 64. 157.5 g of this mixture was introduced to the reactor with 78.76 g of hexane, 78.76 g of ethyl acetate and heated to reflux. Once vigorous reflux initiated, the contents were held for about 12 minutes and the remaining monomers added along with 537.24 g of ethyl acetate and 75.24 g of hexane as a single feed over 3 hours. Two hours after the end of feed, the contents were cooled.To synthesize hydrophilic polymers with functional groups, combine the following monomers in specified weight percentages: For Control 1, use 65.7% 2-ethyl hexyl acrylate, 27.3% methyl acrylate, and 7% acrylic acid. For Control 2, use 67% 2-ethyl hexyl acrylate, 24% methyl acrylate, 7% acrylic acid, and 2% N-vinyl pyrrolidone. For Control 3, use 65.7% 2-ethyl hexyl acrylate, 27.2% methyl acrylate, 7% acrylic acid, and 0.1% glycidyl methacrylate. For Control 4, use 65% 2-ethyl hexyl acrylate, 27% methyl acrylate, 7% acrylic acid, and 1% glycidyl methacrylate. Add 0.2 parts by weight of aluminum acetyl acetonate as a cross-linker. The polymers are then subjected to a rivet tenting test using an adhesive transfer coating method on a cast vinyl facestock at a coat weight of 30 g/m2."
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