Preparation method for biomimetic mussel adhesive used for adhesion on wet surface and underwater curing
A technology of surface bonding and underwater curing, used in adhesives, non-polymer adhesive additives, adhesive additives, etc.
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Embodiment 1
[0022]
[0023] Add N-vinylpyrrolidone ( NVP )( 2.22g 0.02mol), catechol derivatives MSt (0.10g 0.6mmol) and THF (5mL), AIBN (0.04mmol 6.6mg) was added, argon flowed for 30min, and the reaction was carried out at 60°C for 24h. Cool down to room temperature, precipitate in normal hexane (100mL), dissolve and precipitate the precipitate three times, and dry to obtain the copolymer I m (2.1g) (M n =51KDa M w / M n =1.7).
[0024] Add the prepared copolymer in the 50ml reaction bottle I m , tetrahydrofuran (6mL), boron tribromide (0.7g 2.8mmol), and react under the protection of argon for 10 hours. The concentrated reaction solution was dropped into n-hexane (50mL) under stirring, and the precipitate was dissolved and precipitated three times, and dried to obtain the polymer I′ m (1.7g). polymer I′ m Dissolve in 2mL of absolute ethanol, add 0.03g of ferric chloride, stir evenly to obtain bionic mussel glue.
Embodiment 2
[0026]
[0027] Add N-vinylpyrrolidone ( NVP )( 2.22g 0.02mol), catechol derivatives BSt (3.64g 0.1mol) and THF (10mL), add AIBN (0.4mmol 66mg), flow argon for 30min, and react at 60°C for 48h. Cool down to room temperature, precipitate in normal hexane (100mL), dissolve and precipitate the precipitate three times, and dry to obtain the copolymer I B (4.1g) (M n =4.9KDa M w / M n =2.1).
[0028] Add the prepared copolymer in the 50ml reaction bottle I B , tetrahydrofuran (15mL), concentrated hydrochloric acid (2mL), and reacted for 10 hours under the protection of argon. The concentrated reaction solution was dropped into n-hexane (50mL) under stirring, and the precipitate was dissolved and precipitated three times, and dried to obtain the polymer I′ B (3.1g). polymer I′ B Dissolve in 35mL of absolute ethanol, add 0.57g of ferric chloride, and stir evenly to obtain biomimetic mussel glue (when the base material is aluminum, the bonding strength is 1.2MPa aft...
Embodiment 3
[0030]
[0031] Add N-vinylpyrrolidone ( NVP )( 2.22g 0.02mol), catechol derivatives ENVP (0.32g 0.6mmol) and THF (10mL), add AIBN (0.5mmol 82mg), flow argon for 30min, and react at 60°C for 48h. Cool down to room temperature, precipitate in normal hexane (100mL), dissolve and precipitate the precipitate three times, and dry to obtain the copolymer Ⅱ E (2.0g) (M n =5.1KDa M w / M n =1.8).
[0032] Add the prepared copolymer in the 50ml reaction bottle Ⅱ E , tetrahydrofuran (15mL), concentrated hydrochloric acid (2mL), and reacted for 10 hours under the protection of argon. The concentrated reaction solution was dropped into n-hexane (50mL) under stirring, and the precipitate was dissolved and precipitated three times, and dried to obtain the polymer Ⅱ′ E (1.4g). polymer Ⅱ′ EDissolve in 10mL of absolute ethanol, add ferric chloride according to 1 / 3 (mol fraction) of the catechol group content in the polymer, and stir evenly to obtain bionic mussel glue (when t...
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