Controlled radical polymerization of (meth)acrylic monomers
A free-radical, acrylic technology for use in ester copolymer adhesives, adhesive types, coatings, etc. to address undesired characteristics, poor rheological control, unpredictable properties, etc.
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[0042] Comparative Example - Using dimethyl 2,6-dibromopimelate / Cu(0) / pentamethyldiethylenetriamine in acetonitrile One-pot synthesis of polymethyl acrylate
[0043]34g acetonitrile, 0.670g dimethyl 2,6-dibromopimelate, 0.0697g pentamethyldiethylenetriamine (PMDETA) and 31.82g methyl acrylate were added with mechanical stirrer, two condensers and a rubber septum in a 250 ml four-neck round bottom flask. The mixture was stirred and cooled to -78°C, and 53 g of copper mesh treated with 0.1N hydrochloric acid was added to the mixture with continuous stirring. The flasks were then degassed using 6 freeze-pump-thaw cycles under nitrogen. Then, the reaction mixture was heated to 25°C and the polymerization was continued for 4 hours and stopped by introducing air.
[0044] The product sample was dissolved in deuterated chloroform (CDCl 3 ), and through 1 Conversion was measured by H-NMR spectroscopy. At 4 hours, the conversion of methyl acrylate was 72%. The samples were di...
Embodiment 4
[0057] Inventive Example 4 - Using PhCHBr 2 / Cu(0) / pentamethyldiethylenetriamine in acetonitrile polymethyl acrylate
[0058]
[0059] Using the method of the present invention, 34.05 g of acetonitrile, 0.530 g of a,a-dibromotoluene and 1.03 g of copper mesh treated with 0.1N hydrochloric acid were added to a 250 ml necked round bottom flask. 0.0798 g PMDETA and 31.41 g methyl acrylate were added to a 50 ml Schlenk tube. Both mixtures were degassed through 6 freeze-pump-thaw cycles under nitrogen. The methyl acrylate / PMDETA mixture was added dropwise to the flask at 45°C under nitrogen through a cannula over 30 minutes. The polymerization reaction continued for 4 hours and was stopped by introducing air.
[0060] Samples were taken at various intervals throughout the polymerization. Dissolve the sample in CDCl 3 in and through 1 Conversion was measured by H-NMR spectroscopy. At 4 hours, the conversion of methyl acrylate was 79%. The samples were dissolved i...
Embodiment 5
[0061] Inventive Example 5 - Using PhCHBr 2 / Cu(0) / pentamethyldiethylenetriamine in acetonitrile 2-ethylhexyl polyacrylate
[0062]
[0063] Using the method of the present invention, 37.60 g of acetonitrile, 1.2491 g of a,a-dibromotoluene and 0.56 g of copper mesh treated with 0.1N hydrochloric acid were added to a 250 ml necked round bottom flask. 0.0770 g PMDETA and 37.60 g 2-ethylhexyl acrylate were added to a 50 ml Schlenk tube. Both mixtures were degassed through 6 freeze-pump-thaw cycles under nitrogen. The 2-ethylhexyl acrylate / PMDETA mixture was added dropwise to the flask via cannula at 45°C under nitrogen over 60 minutes. The polymerization reaction continued for 3.5 hours and was stopped by introducing air.
[0064] Samples were taken at various intervals throughout the polymerization. Dissolve the sample in CDCl 3 in and through 1 Conversion was measured by H-NMR spectroscopy. At 4 hours, the conversion of 2-ethylhexyl acrylate was 54%. The sam...
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