Modified dipentaerythritol acrylate with low viscosity, high reactivity and low volume shrinkage and preparation method thereof
A dipentaerythritol and acrylate technology, which is applied in the field of modified dipentaerythritol acrylate and its preparation, can solve the problems of environmental and human health adverse effects, product volatile migration, toxicity and irritation, etc., to improve photocuring efficiency, Improve light curing rate, effect of high molecular weight
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Embodiment 1
[0050] Preparation of cyclic 1,3 propanediol carbonate-type modified dipentaerythritol from dipentaerythritol and dimethyl carbonate:
[0051] (127g, 0.5mol) dipentaerythritol, (180g, 2mol) dimethyl carbonate and (0.56g, 5mmol) 1,4-diazabicyclo[2.2.2]octane DABCO were added to a tank equipped with electric stirring and water cooling In a 2000ml reaction flask with a reflux condenser, place the flask in a sand bath in an electric heating mantle, use a temperature controller connected to a thermocouple immersed in the sand bath to control the temperature of the sand bath, use the sand bath to heat the contents of the solution in the flask with stirring To 80 ℃, by stirring, the solid component of the solution in the flask dissolves into a colorless transparent solution, the reaction temperature is maintained at 80 ℃ and continues to stir for 14 hours; the reaction product methanol is continuously distilled out during the reaction, and the excess dicarbonate The methyl ester was ...
Embodiment 2
[0053] The cyclic 1,3 propanediol carbonate type modified dipentaerythritol and the diethanolamine reaction synthesis band tertiary amine modified dipentaerythritol polyols by the gained of embodiment 1:
[0054] Before cooling the reaction product in the flask of Example 1 to room temperature, add (105g, 1mol) diethanolamine and 600ml cyclohexane, under the action of electric stirring, the solution in the flask is slowly warmed up to 70°C, and the reaction temperature is maintained at 70°C Continue to stir for 3h, cool to room temperature after the reaction is over, do multiple experiments at the same time under the same conditions for the above reactions, and one of the obtained products is subjected to purification treatments such as ethanol and water precipitation, recrystallization, etc., and is separated by silica gel chromatography (n-hexane: acetic acid Ethyl ester=4:1), all the other gained products are not processed further as next step raw material; The product after...
Embodiment 3
[0056] The cyclic 1,3 propanediol carbonate type modified dipentaerythritol and the diisopropanolamine reaction synthesis band tertiary amine modified dipentaerythritol polyol by embodiment 1 gained:
[0057] Before the reaction product in the flask of Example 1 was cooled to room temperature, (133g, 1mol) diisopropanolamine and 600ml cyclohexane were added, and under the action of electric stirring, the solution material in the flask was slowly warmed up to 70°C, and the reaction temperature was maintained Stirring was continued at 70 ° C for 3 h, and cooled to room temperature after the reaction was completed.
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