Method for grafting polymer in double bond position of natural rubber by adopting atom transfer radical polymerization (ATRP)
A technology for grafting polymer and natural rubber, which is applied in the field of grafting polymers at the double bond position of natural rubber, can solve the problems of branching, uncontrollable molecular weight, inability to control the length of the grafted chain and the uniformity of length, etc. The effect of simplicity, improved performance and product consistency
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Embodiment 1
[0028] (1) Take 1g38.6% ENR (degree of epoxidation = 38.6%) and fully dissolve it in 10mL of dichloromethane, mix with 0.869g 2-bromoisobutyric acid (BIBA) and 0.0437g 2-bromoisobutyric acid tetra Methylammonium salts were added together into a Schlenk flask equipped with magnetic stirring, and placed in an oil bath at 60°C for 24 h under nitrogen protection. After the reaction, the product was precipitated with excess methanol, and the Methanol was repeatedly dissolved-precipitated, and the precipitate was vacuum-dried at 35°C to constant weight. The resulting macromolecular initiator BIBA-NR was 1 H-NMR analysis, measured halogen atom loading T t = 20.3%.
[0029](2) Add 1gBIBA-NR together with 0.269gCuBr, 0.325gN, N, N', N", N"-pentamethyldiethylenetriamine (PMDETA) into a Schlenk flask equipped with magnetic stirring, and use The reaction flask was tightly sealed with a rubber septum, degassed under vacuum and filled with argon. Then 20 ml of toluene and 10 g of methyl...
Embodiment 2
[0031] (1) Dilute 38.6% ENR latex to a dry content of 5%, and 2 CO 3 Adjust the pH to 8. Add 20g of ENR latex, 2.296g of p-carboxybenzenesulfonyl chloride (CSBA) and 0.0437g of NaOH into a Schlenk flask equipped with magnetic stirring, and react in an oil bath at 30°C under nitrogen protection After 24 hours of reaction, the product was precipitated with excess methanol, washed repeatedly with distilled water and methanol, and the residue was vacuum-dried at 35°C until constant weight. Gained macromolecular initiator CSBA-NR via 1 H-NMR analysis, measured halogen atom loading T t = 27.2%.
[0032] (2) Add 1gCSBA-NR together with 0.201gCuCl, 0.351gN, N, N', N", N"-pentamethyldiethylenetriamine (PMDETA) into a Schlenk flask equipped with magnetic stirring, and use The reaction flask was tightly sealed with a rubber septum, degassed under vacuum and filled with argon. Then 20 ml of toluene and 10 g of methyl methacrylate (MMA) were introduced through a syringe, and placed in...
Embodiment 3
[0034] (1) Dilute 38.6% ENR latex to a dry content of 5%, and 2 CO 3 Adjust the pH to 8. Add 20 g of ENR latex together with 2.238 g of p-bromomethylbenzoic acid (BPTA) and 0.0437 g of NaOH into a Schlenk flask equipped with magnetic stirring, and place it in an oil bath at 30 °C under nitrogen protection After 48 hours of reaction, the macroinitiator BPTA-NR emulsion was obtained after the reaction. Part of the product was precipitated with excess methanol, and washed repeatedly with distilled water and methanol, and the residue was vacuum-dried at 35°C to constant weight. The obtained BPTA-NR was used for 1 H-NMR analysis, measured halogen atom loading T t = 23.9%.
[0035] (2) Inject 10 g of styrene (St) directly into the obtained BPTA-NR emulsion, tightly seal the Schlenk flask with a rubber septum, degas and fill it with argon under vacuum, then add 0.178 g CuBr, 0.508 g 4,4 '-bis(penta-nonyl)-2,2'-bipyridine (dNbpy), placed in an oil bath at 60°C for reaction. After...
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