Low-viscosity high-reactivity low-volume-shrinkage modified pentaerythritol acrylate and preparation method thereof
A technology of pentaerythritol acrylate and high reactivity, which is applied in the preparation of organic compounds, preparation of carbamic acid derivatives, chemical instruments and methods, etc., and can solve the adverse effects on the environment and human health, product volatile migration, toxicity and irritation and other problems, to achieve the effect of improving photocuring efficiency, increasing photocuring rate, and high molecular weight
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Embodiment 1
[0057] Preparation of cyclic 1,3 propanediol carbonate type modified pentaerythritol from pentaerythritol and dimethyl carbonate:
[0058] Add (68 g, 0.5 mol) pentaerythritol, (180 g, 2 mol) dimethyl carbonate and (0.56 g, 5 mmol) 1,4-diazabicyclo[2.2.2]octane DABCO to a device equipped with electric stirring and water-cooled reflux In the 2000ml reaction flask of the condenser, place the flask in the sand bath in the electric heating mantle, use the temperature controller connected to the thermocouple immersed in the sand bath to control the temperature of the sand bath, so that the solution substance in the flask is 80 ° C, by stirring , the solid components of the solution substance in the flask were dissolved into a colorless transparent solution, and the reaction temperature was maintained at 80°C and continued to stir for 14 hours. During the reaction, the reaction product methanol was continuously distilled out, and the excess dimethyl carbonate was distilled out after t...
Embodiment 2
[0060] The cyclic 1,3 propanediol carbonate type modified pentaerythritol and the diethanolamine are reacted to synthesize the modified pentaerythritol polyol with tertiary amine by embodiment 1 gained:
[0061] 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 heated to 70°C, and the reaction temperature is maintained at 70°C Continue to stir for 3 hours, after the reaction is over, cool to room temperature; under the same conditions as above, do multiple experiments at the same time, one of the obtained products is purified by ethanol and water precipitation, recrystallization, etc., and is separated by silica gel chromatography (n-hexane: acetic acid Ethyl ester = 4:1), the rest of the resulting product is not further processed as a raw material for the next step; the purified product is subjected to FTIR infrared ...
Embodiment 3
[0063] The cyclic 1,3 propanediol carbonate type modified pentaerythritol and diisopropanolamine reaction synthesis band tertiary amine modified pentaerythritol polyols by embodiment 1 gained:
[0064] Before cooling the reaction product in the flask of Example 1 to room temperature, (133g, 1mol) diisopropanolamine and 600ml cyclohexane were added, and under the action of electric stirring, the solution in the flask was slowly heated to 75°C, and the reaction temperature was maintained Stirring was continued at 75°C for 3h, the reaction was completed and cooled to room temperature.
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