Benzoxazine polymerization
A kind of technology of benzoxazine and polymer, applied in the field of preparing polybenzoxazine
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[0182] Differential Scanning Calorimetry
[0183] Placement in a differential scanning calorimeter (available from Seiko Instruments USA, Inc., Torrance, California, or TA Instruments, New Castle, DE) Differential scanning calorimetry ("DSC") measurements were performed on aliquots of a given reaction mixture into open DSC aluminum pans and heated from 25°C to 300°C at 10°C / min.
[0184] Materials used and abbreviations
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[0186]
preparation example 1
[0187] Preparation 1 ("PE-1"): Synthesis of Poly(acryloyl-4-oxobutyl-toluenesulfonate) :
[0188] To 9.5 g (0.05 mol) of toluenesulfonyl chloride were added 5.05 g (0.05 mol) of triethylamine, 100 mg of DMAP and 7.21 g (0.05 mol) of 4-hydroxy n-butyl acrylate. The mixture was dissolved in 50 mL of dichloromethane and allowed to stir at room temperature overnight. The precipitate was filtered to show almost quantitative yield (6.7 g precipitate, corresponding to 0.049 mol triethylamine hydrochloride), and the solution was evaporated under reduced pressure at 30° C. to remove the solvent to obtain 13.2 g (0.044 mol ; equivalent to 88% yield) acryloyl-4-oxobutyl-toluenesulfonate monomer, as obtained by 1 H-and 13 Confirmed by C-NMR.
[0189] Ultraviolet Reaction of Acryloyl-4-Oxobutyl-Tosylate Monomer
[0190] 10 mg of KB-1 photoinitiator was dissolved in 1 g of acryl-4-oxobutyl-toluenesulfonate monomer. The solution was knife-coated between two layers of silicone-coated...
example 1
[0195] Example 1 ("EX-1"): BZ-1 Catalysis Using Poly(acryloyl-4-oxobutyl-toluenesulfonate)
[0196] To poly(acryloyl-4-oxobutyl-toluenesulfonate) (0.050 g, prepared according to Preparation 1) was added 1 g of BZ-1 monomer, and the mixture was heated in an aluminum pan at 100° C. for 1 minute While stirring. The mixture was allowed to cool to room temperature, and an aliquot was subjected to thermogravimetric analysis ("TGA"). TGA showed less than 2% weight loss observed after heating at 150°C for 2 hours and less than 2.5% weight loss observed after heating at 200°C for 1 hour. Grind the rest of the mixture to a fine powder and mix well. Aliquots of the ground powder were taken to obtain DSC measurements and the results are summarized in Table 1.
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