Method for preparing polyethylene glycol network gel by using mercapto-vinyl clicking system
A technology of polyethylene glycol and olefin click, which is applied in the field of preparing polyethylene glycol network gel by using mercapto-ene click system, can solve the problems of limiting the potential application of polymer gel materials, etc. Mild conditions, efficient and fast response
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Embodiment 1
[0028] a) Synthesis of terminal mercapto compounds: 1g of dry 3-mercaptopropionic acid, 10mL of freshly steamed tetrahydrofuran were placed in a dry 100mL three-necked flask, and 0.72mL of freshly steamed SOCl was slowly added dropwise under ice-bath conditions 2 , Remove the ice bath and raise the temperature to 60°C for 4h. After the reaction was completed, excess SOCl was removed under reduced pressure 2 . N 2 Add 9.4g polyethylene glycol (M n=2000) of anhydrous THF solution 40mL, and 1.5mL of triethylamine was added dropwise, and the reaction system was carried out at 60°C for 8h. After the reaction was completed, cool to room temperature, remove salt by filtration, and remove most of THF by rotary evaporation. The residue was precipitated in a large amount of ether, and was filtered and dried to obtain the brown target product.
[0029] b) Synthesis of multi-terminal unsaturated carbon-carbon double bonds: Accurately weigh 10g polyethylene glycol (M n =2000) into a d...
Embodiment 2
[0035] The basic process is the same as in Example 1, the difference is that:
[0036] In step 1), the polyethylene glycol derivative (M n =10000) is 0.4g (0.04mmol), 0.16g (0.08mmol) end mercapto polyethylene glycol derivative (M n =2000), 5uL 1mol / L free radical initiator azobisisoheptanonitrile tetrahydrofuran solution, solvent 1mL tetrahydrofuran dissolved, under the protection of nitrogen, the reaction temperature is 70 ° C, the reaction time 1h to form a polymer gel network compound .
[0037] In step 2), the reacted polymer gel network is taken out, put into a methanol solution to remove unreacted reactants remaining in the polymer network, and a regular polymer network is obtained after drying.
[0038] The rest are completely consistent with Example 1.
Embodiment 3
[0040] The basic process is the same as in Example 1, the difference is that:
[0041] In step 1), the polyethylene glycol derivative (M n =10000) is 0.4g (0.04mmol), 0.2g (0.1mmol) terminal mercapto polyethylene glycol derivative (M n =2000), the tetrahydrofuran solution of 5uL 1mol / L free radical initiator benzoin dimethyl ether, solvent 1mL THF dissolving, under the protection of nitrogen, under the radiation of ultraviolet light, the reaction time 2min has formed polymer gel network compound.
[0042] The rest are completely consistent with Example 1.
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