Preparation method of hectorite reinforced polylactic acid-polyethylene glycol-polylactic acid triblock copolymer nano stereocomplex hydrogel
A technology of polyethylene glycol and stereocomposition, which is applied in the preparation of biomedical materials and the field of polymer composite materials
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[0017] The preparation method of polylactic acid-polyethylene glycol-polylactic acid is:
[0018] The PLLA-PEG-PLLA triblock copolymer was synthesized by PEG macromolecule-initiated lactide ring-opening polymerization, and the synthetic reaction scheme is shown below.
[0019]
[0020] Wherein, x=2000, y=800.
[0021] In the first step, a certain proportion of left-handed (L) (or right-handed D)-lactide, polyethylene glycol (PEG), stannous octoate is added in a 100mL three-necked round-bottomed flask, and N 2 After a few minutes, add a certain amount of toluene solution, stir evenly with magnetic force, and react at 120°C for 8 hours;
[0022] In the second step, the product obtained by the reaction was taken out, cooled to room temperature, and precipitated with glacial ether to obtain a white solid product;
[0023] In the third step, the white solid was dissolved with dichloromethane, stirred, dropped into glacial ether for precipitation, and suction filtered. This pro...
Embodiment 1
[0028] Preparation steps of hectorite-enhanced polylactic acid-polyethylene glycol-polylactic acid triblock copolymer stereocomposite hydrogel:
[0029] In the first step, 2g of PLLA-PEG-PLLA or PDLA-PEG-PDLA was dissolved in 4ml of tetrahydrofuran, and then added dropwise into a 15ml sample bottle filled with 8ml of deionized water. Stir evenly with a magnetic stirrer and let stand overnight at 4° C., then reduce the pressure to evaporate and remove THF in the blend to obtain a micellar solution with a concentration of 20%.
[0030] In the second step, under the condition of 4°C, first blend 20% PLLA-PEG-PLLA and PDLA-PEG-PDLA micellar solutions according to 1:1 to obtain a stereomicelle solution, and then the stereomicelle The solution and the ultrapure aqueous solution are vibrated and mixed at a ratio of 1:1 to obtain a polylactic acid-polyethylene glycol-polylactic acid triblock copolymer stereocomposite hydrogel, and then heated to obtain a structurally stable composite ...
Embodiment 2
[0032] The preparation steps of the polylactic acid-polyethylene glycol-polylactic acid triblock copolymer nano stereocomposite hydrogel reinforced by hectorite:
[0033] In the first step, 2g of PLLA-PEG-PLLA or PDLA-PEG-PDLA was dissolved in 4ml of tetrahydrofuran, and then added dropwise into a 15ml sample bottle filled with 8ml of deionized water. Stir evenly with a magnetic stirrer and let stand overnight at 4° C., then reduce the pressure to evaporate and remove THF in the blend to obtain a micellar solution with a concentration of 20%.
[0034] The second step is to weigh a certain amount of laponite powder and sodium pyrophosphate, the ratio of hectorite to sodium pyrophosphate is 10:1, and then add sodium pyrophosphate to a beaker with a certain amount of ultrapure water Then add hectorite powder slowly to the sodium pyrophosphate solution stirred with a magnetic stirrer, seal it with a plastic wrap to avoid water evaporation, and then stir overnight to obtain a conce...
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