A kind of cross-linkable and degradable multi-block copolymer and its preparation method and application
A multi-block copolymer and reaction technology, applied in medical science, prosthesis, tissue regeneration, etc., can solve the problems of unknown impact of fillers on the biocompatibility of the main material, many factors affecting performance, and uncontrollable process
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Embodiment 1
[0061] Example 1 Preparation of Photocrosslinked Degradable Multiblock Copolymer
[0062] A kind of preparation method of photocrosslinked degradable multi-block copolymer, its synthesis process is as follows figure 1 shown, including the following steps:
[0063] 1) Synthesis of polytrimethylene carbonate (PTMC): 50 g of TMC monomer and 2.8 g of diethyleneglycol were placed in a vacuum oven for 12 h at 50 °C and vacuum degree 2 ) and 3 mL of anhydrous toluene; after sealing the polymerization bottle, vacuumize for 2 days to remove toluene and water, and then place it in an oil bath at 130 °C for 3 days. Precipitate in L petroleum ether, repeat the precipitation three times, and vacuum dry to obtain polytrimethylene carbonate (PTMC2k) with a number-average molecular weight of 2000 (Mn = 2000).
[0064] 2) Synthesis of polytrimethylene fumarate (PPF): 50 g diethyl fumarate (diethyl fumarate) and 65.97 g 1, 2-propandiol (1, 2-propandiol) were added to the three-necked flask in ...
Embodiment 2~12
[0066] Examples 2~12 Preparation of Photocrosslinked Degradable Multiblock Copolymers
[0067] The preparation method of the photocrosslinkable degradable multi-block copolymer in Examples 2~12 is the same as that in Example 1, the difference is only in the PPF synthesis reaction time (that is, the reaction time of di(hydroxypropyl) fumarate after adding vacuum and heating up. polycondensation time), the number-average molecular weight of PTMC and the PTMC feeding ratio (that is, the ratio of the mass of PTMC to the sum of the mass of PTMC and PPF), as shown in Table 1.
[0068] Table 1 The difference between the preparation method of the photocrosslinked degradable multi-block copolymer in Examples 2~12 and Example 1
[0069] PPF synthesis reaction time Number average molecular weight of PTMC PTMC feed ratio Example 2 1 h 2k 30% Example 3 1 h 2k 40% Example 4 1 h 2k 60% Example 5 1 h 2k 70% Example 6 1 h 2k 80% Exam...
Embodiment 13
[0072] Synthesis of polytrimethylene fumarate (PPF): 50 g diethyl fumarate (diethyl fumarate) and 65.97 g 1, 2-propandiol (1, 2-propandiol) were added to a three-necked flask in turn, and the flask was placed under a nitrogen atmosphere. (Flow rate: 3~5 bubbles per second) Stir at 150 rpm for 20 min, then add 0.39 g of zinc chloride (ZnCl 2 ) and 0.064 g hydroquinone; stirred at 100 °C for 30 min at 300 rpm, heated to 150 °C for 7 h, and then cooled to 100 °C (the first step) to obtain di(hydroxypropyl fumarate) ) ester (bis(hydroxypropyl) fumarate); add vacuum, react at 100 °C for 1 h, then heat up to 130 °C and react for 7 h (the second step) to obtain PPF.
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