Preparation method and application of a polymerizable reactive fluorocarbon-based siloxane-modified acrylate
A technology of fluorocarbon-based siloxane and polymerization reaction, which is applied in the field of functional acrylate to achieve the effect of improving hardness and scratch resistance
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Embodiment 1
[0032] (1) Synthesis of polymerizable fluorocarbon-based siloxane-modified acrylate FS-1
[0033] In a three-neck flask equipped with a thermometer, a reflux condenser, and a stirrer, add 0.03mol (16.38g) perfluorooctylethylene and 200ppm platinum catalyst KP22 in sequence, stir and heat to 80°C for 60 minutes of coordination reaction, then add 0.01mol (2.43g) Tetramethylcyclotetrasiloxane D 4 H Stir the reaction for 20 minutes, then add 0.01mol (2.26g) of 1,6-hexanediol diacrylate and control the temperature at 80°C and continue to stir the reaction for 8 hours. After the reaction is completed, decompress and remove the low boiling point to obtain a total of 21.07g, the structure of which is as follows: Shown in (1), M=H, A=-(CH 2 ) 6 OCOCH 2 CH 2 -, R f =-C 8 f 17 Polymerizable reactive fluorocarbon-based siloxane-modified acrylate (FS-1).
[0034] (2) FS-1 is used to prepare POSS / fluoro-silicon co-modified PMMA resin and molding
[0035] According to the mass rati...
Embodiment 2
[0037] (1) Synthesis of polymerizable fluorocarbon-based siloxane-modified methacrylate FS-2
[0038] In a three-neck flask equipped with a thermometer, a reflux condenser, and a stirrer, add 0.031mol (13.8g) perfluorohexylethylene and 200ppm platinum catalyst KP22 in sequence, stir and heat to 80°C and perform a coordination reaction for 60 minutes before adding 0.01mol (2.43g) Tetramethylcyclotetrasiloxane D 4 H Stir the reaction for 20min, then add 0.01mol (5.60g), M=CH 3 , b=7, the structure is CH 2 =C(CH 3 ) COO (C 3 h 6 O) 7 CO C (CH 3 )=CH 2 , Mn of about 560 polypropylene glycol dimethacrylate and temperature control 100 ℃ continuous stirring reaction 8h, the reaction is complete, reduced pressure off the low boiling, a total of 21.83g, the structure shown in formula (1), M=CH 3 , b=7, A=-(C 3 h 6 O) 7 COCH (CH 3 )CH 2 -, R f =-C 6 f 13 Polymerizable reactive fluorocarbon-based siloxane-modified methacrylate (FS-2).
[0039] (2) FS-2 is used to prepar...
Embodiment 3
[0042] (1) Synthesis of polymerizable fluorocarbon-based siloxane-modified acrylate FS-3
[0043] In a three-necked flask equipped with a thermometer, a reflux condenser, and an agitator, add 0.031mol (13.83g) of perfluorohexylethylene and 300ppm of chloroplatinic acid catalyst in sequence, stir and heat to 80°C and carry out the coordination reaction for 60min, then Add 0.01mol (2.43g) tetramethylcyclotetrasiloxane D 4 H Stir the reaction for 20min, then add 0.01mol (2.14g), M=H, a=2, structure CH 2 =CHCOO(C 2 h 4 O) 2 OCCH=CH 2 ethylene glycol diacrylate and temperature controlled 100°C for continuous stirring reaction for 10h, after the reaction was completed, decompressed and deboiled to obtain a total of 18.40g, the structure of which was shown in formula (1), M=H, A=-( C 2 h 4 O) 2 COCH 2 CH 2 -, R f =-C 6 f 13 Polymerizable reactive fluorocarbon-based siloxane-modified acrylate (FS-3).
[0044] (2) FS-3 is used to prepare POSS / fluoro-silicon co-modified P...
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