Method for synthesizing ultra-high isotacticity polyl-/d-lactic acid with macromolecular initiator and condensation-ring-opening-solid-phase polymerization
A macromolecular initiator, solid-phase polymerization technology, which is applied in the field of biodegradable and environmentally friendly material synthesis, can solve the problems of low specificity such as PLLA and PDLA, and is difficult to use in the synthesis of sc-PLA, 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 materia...
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 is...
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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