A kind of synthetic method of polyolefin material with controllable degree of branching
A synthesis method and polyolefin technology, applied in the field of polyolefins, can solve the problems of difficulty in synthesizing polyolefins with a relatively high degree of branching, difficulty in controlling the branched structure of polymers, affecting material properties, and the like, achieving good fluidity, Low viscosity and controllable degree of branching
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Embodiment 1
[0036] Monomer synthesis: Take 10g of 3-bromocyclooctene, add it to 30ml of anhydrous tetrahydrofuran, slowly stir under the protection of argon and add 0.1g of cuprous iodide, and then slowly drop at a concentration of 1mol / L at 0℃ A solution of vinylmagnesium bromide in tetrahydrofuran was allowed to react for 3 hours. Slowly add saturated ammonium chloride solution to the reaction solution to terminate the reaction. The reaction solution was extracted three times with ether. The organic phase was collected and drained with saturated brine, dried by adding anhydrous magnesium sulfate, and then the reaction solution was concentrated by rotary evaporation to obtain a crude product The silica gel column is used for purification (the mobile phase is n-hexane) to obtain a pure product, the structure is shown in formula Ia, and the yield is about 40%. Proton NMR spectra such as figure 1 Shown.
[0037]
[0038] Polymerization reaction: Take 91 mg of the pure monomer obtained in the ...
Embodiment 2
[0041] Monomer synthesis: Take 10g of 3-bromocyclooctene, add it to 30ml of anhydrous tetrahydrofuran, slowly stir under the protection of argon and add 0.1g of cuprous iodide, and then slowly drop at a concentration of 1mol / L at 0℃ The allyl magnesium bromide solution in tetrahydrofuran was reacted for 3 hours. Slowly add saturated ammonium chloride solution to the reaction solution to terminate the reaction. The reaction solution was extracted three times with ether. The organic phase was collected and drained with saturated brine, dried by adding anhydrous magnesium sulfate, and then the reaction solution was concentrated by rotary evaporation to obtain a crude product The silica gel column is used for purification (the mobile phase is n-hexane) to obtain a pure product, the structure is shown in formula Ib, and the yield is about 37%. Proton NMR spectra such as figure 2 Shown.
[0042]
[0043] Polymerization reaction: Take 100 mg of the pure monomer obtained in the above s...
Embodiment 3
[0045] Monomer synthesis: Take 10g of 3-bromocyclooctene, add it to 30ml of anhydrous tetrahydrofuran, slowly stir under the protection of argon and add 0.1g of cuprous iodide, and then slowly drop at a concentration of 1mol / L at 0℃ A solution of vinylmagnesium bromide in tetrahydrofuran was allowed to react for 3 hours. Slowly add saturated ammonium chloride solution to the reaction solution to terminate the reaction. The reaction solution was extracted three times with ether. The organic phase was collected and drained with saturated brine, dried by adding anhydrous magnesium sulfate, and then concentrated by rotary evaporation to obtain the crude product. And use a silica gel column for purification (the mobile phase is n-hexane) to obtain a pure product, the structure is shown in formula Ib, and the yield is about 40%.
[0046]
[0047] Polymerization reaction: Take 100mg of the pure monomer obtained in the above steps, add anhydrous tetrahydrofuran to a constant volume of 33...
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