Cationic end-capped siloxane prepolymer for reduced cross-link density
An alkyl and mixture technology, applied in the field of cationic monomers, can solve the problems of increasing cross-linking density and reducing cross-linking density modulus
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Embodiment 1
[0097] Example 1 Synthesis of 3-(chloroacetylamido)propyl-terminated poly(dimethylsiloxane)
[0098] Purchased from Gelest, Inc., Morrisville, PA, in dichloromethane (350 mL) and NaOH at 0°C (水溶液) (0.75 M, 150 mL), a solution of a vigorously stirred biphasic mixture of 3-aminopropyl-terminated polydimethylsiloxane (97.7, 300 g / mol) was added dropwise in dichloromethane (50 mL) Chloroacetyl chloride solution (8 mL, 0.1 mol). After reacting for one hour at ambient temperature, the organic layer was separated and separated between silica gel (25 g) and NaSO 4 (25 g) for 5 hours and filtered. The solvent was removed under reduced pressure to give the product as a colorless liquid (85 g, 83%): 1 H NMR (CDCl 3 , 400MHz) δ 6.64(br, 2H), 4.05(s, 4H), 3.29(q, J=7Hz, 4H), 1.60-1.52(m, 4H), 0.56-0.52(m, 4H), 0.06(s , about 264H); GPC: M w 3075g / mol, PD1.80. The mass spectrum of this sample showed a mass distribution of singly charged oligomers with a repeat unit mass of 74 Da. Th...
Embodiment 2
[0100] Example 2 Synthesis of cationic methacrylate-terminated poly(dimethylsiloxane)
[0101] To a solution of 3-(chloroacetylamido)propyl-terminated poly(dimethylsiloxane) (20.0 g) from Example 1 in ethyl acetate (25 mL) was added 2-(dimethicone) Methylamino)ethyl methacrylate (3.40 mL, 20.1 mmol), and the mixture was heated at 60° C. in the dark under nitrogen for 80 hours. The resulting solution was freed of solvent and / or reactants under reduced pressure to obtain a product (23.1 g) containing a residual amount (1 H NMR (CDCl 3 , 400MHz) δ 9.23(br, 2H), 6.07(s, 2H), 5.60(s, 2H), 4.71(s, 4H), 4.65-4.63(m, 4H), 4.18(br, 4H) 3.47(s , 12H), 3.19-3.13 (m, 4H), 1.88 (s, 6H), 1.59-1.49 (m, 4H), 0.51-0.47 (m, 4H), 0.01 (s, about 327H). The mass spectrum of this sample indicated a mass distribution of doubly charged oligomers with a repeating unit mass of 37 Da. When decomposed, it conforms to the repeating unit mass of 74Da (37Da×2). This is in line with the stated objective ...
Embodiment 3
[0103] Example 3 Synthesis of cationic chloride terminated poly(dimethylsiloxane) with variable terminal methacrylate
[0104] To a solution of 3-(chloroacetylamido)propyl-terminated poly(dimethylsiloxane) (50.0 g) from Example 1 in ethyl acetate (50 mL) was added 2-(dimethicone) Methylamino)ethylmethacrylate (3.03mL, 18.0mmol) and 3-(dimethylamino)propanol (0.71mL, 6.1mmol) and the mixture was heated at 60°C under nitrogen in the dark 80 hours. The resulting solution was removed of solvent and / or reactants under reduced pressure to obtain a product containing residual amounts of 2-(dimethylamino)ethyl methacrylate and 3-(dimethylamino)propanol (1 H NMR analysis readily quantified.
[0105]
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