Method for synthesizing superhigh-isotacticity poly L-/D-lactic acid through combination of macromolecular initiator and condensation-ring opening-solid phase polymerization
A macromolecular initiator, solid-phase polymerization technology, applied in the field of biodegradable and environment-friendly material synthesis, can solve the problems of PLLA, PDLA, etc., which are low in regularity, difficult to use in the synthesis of sc-PLA, etc., and achieves low energy consumption. Effect
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Embodiment 1
[0044] The operating process of the present embodiment is as described above, and the specific process parameters are as follows:
[0045] step 1:
[0046] The raw material is 90% L-lactic acid, the chiral purity of L-lactic acid is 99.5%, and the feeding amount is 100.0Kg;
[0047] The catalyst is creatinine, and the feeding amount is 0.9g;
[0048] Reaction condition parameter P 1-1 =700torr, T 1-1 =100°C, t 1-1 = 1.0h; P 1-2 =500torr, T 1-2 =120°C, t 1-2 = 1.0h; P 1-3 =100torr, T 1-3 =140°C, t 1-3 = 2.0h;
[0049] Productma-OPLLAM w 3.0×10 3 , PDI 1.2, Iso.99.0%.
[0050] Step 2:
[0051] The raw material is L-lactide, the chiral purity of L-lactide is 99.5%, and the feeding amount is 1641.6Kg;
[0052] The catalyst is creatinine acetate, and the feeding amount is 16.4g;
[0053] Reaction condition parameter P 2 = 1.0 Torr, T 2 =100°C, t 2 = 2.0h;
[0054] Producthc-MMW-PLLAM w 6.0×10 4 , PDI 1.5, Iso.99.0%.
[0055] Step 3:
[0056] The raw materi...
Embodiment 2
[0060] The operating process of the present embodiment is as described above, and the specific process parameters are as follows:
[0061] step 1:
[0062] The raw material is 90% L-lactic acid, the chiral purity of L-lactic acid is 99.8%, and the feeding amount is 50.0Kg;
[0063] Catalyst is guanidinoacetic acid, and charging amount is 2.3g;
[0064] Reaction condition parameter P 1-1 =500torr, T 1-1 =120°C, t 1-1 =2.0h;P 1-2 =100torr, T 1-2 =140°C, t 1-2 =2.0h;P 1-3 =30torr, T 1-3 =160°C, t 1-3 = 4.0h;
[0065] Productma-OPLLAM w 5.0×10 3 , PDI 1.5, Iso.99.5%.
[0066] Step 2:
[0067] The raw material is L-lactide, the chiral purity of L-lactide is 99.8%, and the feeding amount is 810.0Kg;
[0068] The catalyst is creatinine lactate, and the feeding amount is 40.5g;
[0069] Reaction condition parameter P 2 =0.1 Torr, T 2 =180°C, t 2 = 10.0h;
[0070] Producthc-MMW-PLLAM w 8.0×10 4 , PDI 1.7, Iso.99.5%.
[0071] Step 3:
[0072] The raw material i...
Embodiment 3
[0076] The operating process of the present embodiment is as described above, and the specific process parameters are as follows:
[0077] step 1:
[0078] The raw material is 90% D-lactic acid, the chiral purity of D-lactic acid is 99.5%, and the feeding amount is 100.0Kg;
[0079] The catalyst is creatine, and the feeding amount is 1.8g;
[0080] Reaction condition parameter P 1-1 =550torr, T 1-1 =108°C, t 1-1 = 1.0h; P 1-2 =350torr, T 1-2 =120°C, t 1-2 = 1.0h; P 1-3 =80torr, T 1-3 =140°C, t 1-3 = 2.0h;
[0081] Product ma-OPDLAM w 3.5×10 3 , PDI 1.5, Iso.99.2%.
[0082] Step 2:
[0083] The raw material is D-lactide, the chiral purity of D-lactide is 99.5%, and the feeding amount is 1644.7Kg;
[0084] Catalyst is bicyclic guanidine acetate, and charging amount is 32.9g;
[0085] Reaction condition parameter P 2 =0.7torr,T 2 =120°C, t 2 = 4.0h;
[0086] Producthc-MMW-PDLAM w 6.5×10 4 , PDI 1.5, Iso.99.2%.
[0087] Step 3:
[0088] The raw material i...
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