A kind of preparation method of bio-based epoxy resin with good deformation recovery performance
A technology based on epoxy resin and deformation recovery, applied in the field of material science, can solve the problems of poor environmental protection, low elongation at break, high brittleness, etc., and achieve the effects of low production cost, simple operation and environmental friendliness
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[0035] The preparation method of bio-based epoxy resin provided by the invention comprises the following steps:
[0036] (1) Hydroxy-terminated polysiloxane reacts with thionyl chloride to generate chloro-terminated polysiloxane;
[0037] (2) The chlorine-terminated polysiloxane and eugenol that step (1) generates are under the catalysis of NaOH and triethylamine, and heat-retaining reaction after heating up generates polysiloxane-based eugenol ether;
[0038] (3) The polysiloxane-based eugenol ether generated by step (2) is dissolved in dichloromethane, and added dropwise in the dichloromethane solution of m-chloroperoxybenzoic acid, and the insulation reaction is carried out. After filtration, the solvent was removed under reduced pressure to obtain a bio-based epoxy resin.
Embodiment 1
[0040] Put 10.0g of hydroxyl-terminated polysiloxane with a degree of polymerization of 1 (n=1) and 20.0g of thionyl chloride into the reactor of the tail gas absorption device, and keep the reaction at 60°C for 2 hours until the reaction is completed Afterwards, the excessive thionyl chloride is removed under reduced pressure under the condition that the gauge pressure is less than or equal to -0.085 MPa and the temperature is 50° C., to obtain the chloropolysiloxane.
[0041] Take 5.0 g of chloropolysiloxane and put it into a three-neck flask equipped with electric stirring, condensing reflux tube, and thermometer, and add 25.0 g of eugenol and 6.1 g of NaOH to it, then heat up to 40 ° C, and Insulate and react for 12 hours, then dissolve in 30ml of dichloromethane, wash with 3×30ml of 5% NaOH aqueous solution, take the organic phase, dry it with 2.0g of anhydrous magnesium sulfate for 12 hours, filter, and store under gauge pressure less than It is equal to -0.085MPa, and t...
Embodiment 2
[0046] Put 20.0g of hydroxyl-terminated polysiloxane with a degree of polymerization of 10 (n=10) and 45.0g of thionyl chloride into the reactor of the tail gas absorption device, and keep warm at 65°C for 2.5h. After the end, the excess thionyl chloride is removed under reduced pressure under the condition that the gauge pressure is less than or equal to -0.085 MPa and the temperature is 55° C., to obtain a chloropolysiloxane.
[0047] Take 10.0 g of chloropolysiloxane and put it into a three-neck flask equipped with electric stirring, condensing reflux tube, and thermometer, and add 50.0 g of eugenol and 14.0 g of NaOH to it, then heat up to 50 ° C, and Insulated reaction for 18h, then dissolved in 40ml of dichloromethane, washed with 3×50ml of 8% NaOH aqueous solution, took the organic phase, dried with 5.0g of anhydrous magnesium sulfate for 12h, filtered, and kept at a gauge pressure of less than It is equal to -0.085MPa, and the solvent is removed under reduced pressure ...
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