A kind of macromolecular photoinitiator and its application and preparation method
A photoinitiator and macromolecular technology, applied in the field of photocuring, can solve the problems of affecting the quality of color glue, difficult to dissolve, low solubility, etc., and achieve the effect of improving the initiation efficiency, increasing the resin content and the appropriate molecular weight
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Embodiment 1
[0049] Example 1. Poly(4-(2-Acrylomethyl)benzophenone Synthesis
[0050]
[0051] Add 48g methanol (1.5mol) to the 250mL three-necked flask and stir, heat up to reflux, slowly add 42g diketene (0.5mol), continue to react at reflux temperature for 5h, and distill under reduced pressure to obtain methyl acetoacetate 89.4g (0.77mol) .
[0052] Add 200mL of THF and 15.6g of stirred and dispersed NaH (60% dispersed in mineral oil, 0.39mol) to a 500mL there-neck flask under argon protection, and 34.8g of methyl acetoacetate (0.3mol) was added dropwise to the flask at room temperature medium and stir well. When the liquid in the flask became clear, 46.8 g of methyl iodide (0.33 mmol) was added dropwise, the mixture was stirred at 40 °C for 10 h, the reaction solution was quenched with saturated aqueous ammonium chloride and extracted with ethyl acetate three times. The combined organic layers were dried over anhydrous sodium sulfate, and the solvent was spin-dried, and separat...
Embodiment 2
[0069] Example 2. Poly 4-(2-ethyl acrylate) benzophenone F-2 Synthesis
[0070]
[0071] The synthesis process of F-2 is referred to the synthesis of F-1, the difference is that the methanol used in A-1 is replaced by ethanol.
[0072] NMR data of E-2: 1 HNMR (300 Hz) in DMSO: δ 1.07 ppm (t, 3H), 4.00 ppm (q, 2H), 6.19, 6.37 ppm (d, J=58.3, 2H), 7.41-7.84 ppm (m, 9H).
[0073] F-2 molecular weight data: M w = 8500, PDI = 1.49.
Embodiment 3
[0074] Example 3. Poly4'-methoxy, 4-(2-ethyl acrylate) benzophenone F-3 Synthesis
[0075] The synthesis process of F-3 refers to the synthesis of F-1, the difference is that the raw material E-3 for synthesizing F-3 is to use the 4-bromobenzophenone used in E-1 with 4-bromo, 4'-methoxy The base benzophenone C-1 is replaced, and the synthetic method of C-1 is as follows:
[0076]
[0077] Into a 500mL three-necked flask, add 21.95g 4-bromobenzoyl chloride (0.1mol) and 17.3g anhydrous aluminum trichloride (0.13mol), and add 100mL CH 2 Cl 2 The solids were dissolved and placed in a low temperature reaction bath at 10°C with stirring. Mix 140.6 g of anisole (0.13 mol) with 50 ml of CH 2 Cl 2 Mix well, add to constant pressure dropping funnel and start dripping. After the dropwise addition, add 20mL CH2 Cl 2 Rinse the constant-pressure dropping funnel, slowly raise the temperature of the cooling bath to 20°C, and continue stirring. At the end of the reaction, the react...
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