A kind of aliphatic polycarbonate containing amino group in side chain and preparation method thereof
A polycarbonate and aliphatic technology, applied in the field of aliphatic polycarbonate and its preparation, can solve the problems of low synthesis yield, incomplete deprotection group, low monomer polymerization activity, etc., and achieve the effect of mild conditions
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Embodiment 1
[0035] Example 1: Bulk ring-opening polymerization of AEDO.
[0036] Under the condition of nitrogen protection, 10 g of AEDO monomer (0.05 mol) was added into the polymerization bottle, and then 0.051 g of aluminum triisopropoxide (0.25 mmol) was added as an initiator, and the polymerization was carried out at 120° C. for 20 hours. After the polymerization, the polymer product was dissolved in 50 mL of chloroform, precipitated by adding 500 mL of methanol, filtered, washed, and vacuum-dried at 35° C. to constant weight to obtain 8.7 g of PAEDO with a yield of 87%.
[0037] The number average molecular weight (Mn) is 30752 and the polydispersity index (PDI) is 1.41 as measured by GPC method (tetrahydrofuran as eluent).
[0038] 1 H-NMR (CDCl 3 ,300MHz):δ0.88(t,CH 3 CH 2 ,3H),1.48(q,CH 3 CH 2 ,2H),3.33(s,CH 2 O,2H),3.93(d,CH 2 CH=CH 2 ,2H),4.11(s,CH 2 OCO,4H),5.21(m,CH=CH 2 ,2H),5.85(m,CH=CH 2 ,1H).
Embodiment 2
[0039] Example 2: Bulk ring-opening polymerization of AEDO.
[0040] Under the condition of nitrogen protection, 10 g of AEDO monomer (0.05 mol) was added into the polymerization bottle, and then 2.0 g of stannous octoate (5 mmol) was added as an initiator, and the polymerization was carried out at 150° C. for 30 hours. After the polymerization, the polymer product was dissolved in 50 mL of chloroform, precipitated by adding 500 mL of methanol, filtered, washed, and vacuum-dried at 35° C. to constant weight to obtain 8.5 g of PAEDO with a yield of 85%.
[0041] The number average molecular weight (Mn) is 637 and the polydispersity index (PDI) is 1.47 as measured by GPC method (tetrahydrofuran as eluent).
[0042] 1 The H-NMR spectrum is substantially the same as in Example 1.
Embodiment 3
[0043] Example 3: Solution ring-opening polymerization of AEDO.
[0044]Under nitrogen protection conditions, 2gAEDO monomer (0.05mol) and 0.027g benzyl alcohol (0.25mmol) are dissolved in 5mL toluene, then add the DBU toluene solution that 0.25mL concentration is 1mol / L, then react system at room temperature ( 25°C) for 20 hours of polymerization. After the polymerization, the polymer product was dissolved in 10 mL of chloroform, precipitated by adding 200 mL of methanol, filtered, washed, and vacuum-dried at 35° C. to constant weight to obtain 1.9 g of PAEDO with a yield of 95%.
[0045] The number average molecular weight is 31077 and the polydispersity index is 1.18 as measured by GPC method (tetrahydrofuran is the eluent).
[0046] 1 The H-NMR spectrum is substantially the same as in Example 1.
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