Epoxy resin toughening polymer containing spiro structure, and synthesis method and application thereof
A technology of epoxy resin and spiro ring structure is applied in the field of epoxy resin toughening agent, which can solve the problems of reducing the glass transition temperature and heat resistance of materials, and achieve the effects of improving toughness, improving compatibility and improving toughness.
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Embodiment 1
[0050] Add 0.5218g (5.54mmol) of 1,2-ethanedithiol, 0.5872g (2.77mmol) of BTU, 55.5mg of azobisisobutyronitrile, and 4.4360g of 1,4-dioxane into the sealed reactor. Stirring was started, and the air in the reactor was removed by flowing argon for 0.5h. After the aeration was completed, the reactor was sealed, and the temperature inside the reactor was adjusted to 50° C. for 48 h. After the reaction was completed, it was cooled to room temperature to obtain a mercapto-terminated intermediate solution (comprising a modified BTU polymer).
[0051] According to the molar ratio of mercapto and epoxy groups is 1.1:1, the modified BTU polymer is added to bisphenol A epoxy resin (epoxy value 0.53eq / 100g), and the modified BTU polymer and bisphenol A ring 3% triethylamine of the total mass of oxygen resin, and then adjust the concentration of the solution to 20% with 1,4-dioxane, and react at 50° C. for 144 hours. After the steps of precipitation, separation and drying, a linear poly...
Embodiment 2
[0062] Add 0.5203g (5.53mmol) of 1,2-ethanedithiol, 0.7829g (3.69mmol) of BTU, 26.1mg of azobisisobutyronitrile, and 0.5586g of 1,4-dioxane into the sealed reactor. Stirring was started, and the air in the reactor was removed by flowing argon for 0.5h. After the aeration was completed, the reactor was sealed, and the temperature inside the reactor was adjusted to 80° C. for 6 h. After the reaction was completed, it was cooled to room temperature to obtain a mercapto-terminated intermediate solution (comprising a modified BTU polymer).
[0063] According to the molar ratio of mercapto group and epoxy group is 1:1, the modified BTU polymer is added in bisphenol A epoxy resin (epoxy value 0.48eq / 100g), and the modified BTU polymer and bisphenol A ring are added 1,8-diazabicycloundec-7-ene with a total mass percentage of 3% of the oxygen resin, then adjust the solution concentration to 50% with 1,4-dioxane, and react at 80°C for 6 hours . After the steps of precipitation, separ...
Embodiment 3
[0072] Add 0.4747g (5.04mmol) of 1,2-ethanedithiol, 0.8897g (4.20mmol) of BTU, 52.20mg of azobisisobutyronitrile, and 1.5002g of 1,4-dioxane into the sealed reactor. Stirring was started, and the air in the reactor was removed by flowing argon for 0.5h. After the ventilation was completed, the reactor was sealed, and the temperature inside the reactor was adjusted to 70° C. for 24 hours. After the reaction was completed, it was cooled to room temperature to obtain a mercapto-terminated intermediate solution (comprising a modified BTU polymer).
[0073] According to the molar ratio of mercapto and epoxy groups is 1.02:1, the modified BTU polymer is added to bisphenol A epoxy resin (epoxy value 0.53eq / 100g), and the modified BTU polymer and bisphenol A ring 1,8-diazabicycloundec-7-ene with a total mass fraction of 3% of the oxygen resin, and then adjust the solution concentration to 50% with 1,4-dioxane, and react at 80°C for 6 hours . After the steps of precipitation, separa...
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