A kind of preparation method of polylactide
A technology of polylactide and lactide, which is applied in the direction of lithium organic compounds, etc., can solve the problems of difficult degradation of polymeric materials, aggravated pollution, and constraints on the rapid development of polymeric materials, and achieves controllable molecular weight, less metal residues, Various effects of catalyst structure changes
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Embodiment 1
[0043] The structural formula of the ligand used is the above formula (A), where Ar is 4-methylphenyl, and the reaction process is as follows: under a nitrogen atmosphere, dissolve 0.51 g of the ligand in 10 mL of dry n-hexane, and add equimolar A certain amount of n-butyllithium was slowly raised to room temperature for 3 hours, filtered and washed with dry n-hexane, collected and dried to weigh 0.49g solid, yield 94%.
[0044] The NMR information of the obtained product is as follows. It can be seen from the NMR information that the lithium compound whose Ar is 4-methylphenyl was successfully synthesized.
[0045] 1 HNMR (400MHz, CDCl 3 ) δ 7.40(d, J =7.5Hz,2H,Ph- H ), 7.24–6.91 (m, 10H, Ph- H ),6.62(d, J =7.6Hz,2H,Ph- H ),4.40(s,4H,C H 2 N),2.72(s,12H,NC H 3 ),2.20(s,6H,C H 3 ).
[0046] 13 CNMR (100MHz, CDCl 3 ) δ152.45, 146.61, 134.27, 129.81, 128.23, 127.98, 126.66, 124.17, 116.34, 114.34, 48.86, 45.46, 20.40.
Embodiment 2
[0048] The structural formula of the ligand used is the above formula (A), where Ar is 2,6-dimethylphenyl, and the reaction process is as follows: under a nitrogen atmosphere, dissolve 0.47g of the ligand in 10mL of dry cyclohexane, and at 0°C Add 1.05 times the molar amount of n-butyllithium, slowly rise to room temperature and react for 6 hours, filter and wash the filter cake with dry n-hexane, collect and dry and weigh to obtain 0.46g solid, yield 95%.
[0049] The NMR information of the obtained product is as follows. It can be seen from the NMR information that the lithium compound whose Ar is 2,6-dimethylphenyl was successfully synthesized.
[0050] 1 HNMR (400MHz, CDCl 3 ) δ 7.42 (dd, J =6.2,1.3Hz,2H,Ph- H ),7.28-7.25(m,2H,Ph- H ),7.17(dd, J =7.0,1.0Hz,2H,Ph- H ),7.06(td, J =7.4,1.2Hz,2H),7.00(d, J =7.4Hz,4H),6.83(t, J =7.5Hz,2H),4.17(s,4H,NC H 2 Ph),2.73(s,12H,NC H 3 ),2.31(s,12H,PhC H 3 ).
[0051] 13 CNMR (100MHz, CDCl 3 ) δ 152.80, 146.54, 135...
Embodiment 3
[0053] The structural formula of the ligand used is the above formula (A), where Ar is 2,6-diethylphenyl, and the reaction process is as follows: under a nitrogen atmosphere, dissolve 0.34 g of the ligand in 5 mL of dry toluene, and add 1.1 times the molar amount of methyllithium was raised to room temperature and reacted for 1 hour, filtered and washed with dry n-hexane, collected, dried and weighed to obtain 0.32g, with a yield of 91%.
[0054] The crystal structure of the obtained product is shown in figure 1 As shown, the NMR information is as follows, it can be seen that the lithium compound whose Ar is 2,6-diethylphenyl was successfully synthesized.
[0055] 1 HNMR (400MHz, CDCl 3 ) δ 7.48–7.45 (m,2H,Ph- H ),7.29(dd, J =7.8,1.5Hz,2H,Ph- H ),7.19(dd, J =8.0,1.1Hz,2H,Ph- H ),7.13(d, J =7.9Hz,2H,Ph- H ),7.09(m,4H,Ph- H ),6.97(dd, J =8.1,6.9Hz,2H,Ph- H ),4.12(s,4H,NC H 2 Ph),2.73(s,12H,NC H 3 ),2.52(q, J =7.5Hz,8H,C H 2 CH 3 ),1.15(t, J =7.5Hz,12H,CH ...
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