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A kind of preparation method of imitation mussel glue that can be bonded on wet surface and solidified under water

A technology of surface bonding and underwater curing, applied in the directions of adhesives, non-polymer adhesive additives, adhesive additives, etc., can solve the problems of low bonding strength of bionic mussel glue, and achieve a simple and efficient synthesis method. Compatibility and initial viscosity, the effect of breaking through technical bottlenecks

Inactive Publication Date: 2016-04-20
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a preparation method of bionic mussel glue that can be bonded on a wet surface and solidified underwater, so as to solve the problem of existing bionic mussel glue. The problem of low bonding strength in wet environment and underwater bonding

Method used

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  • A kind of preparation method of imitation mussel glue that can be bonded on wet surface and solidified under water
  • A kind of preparation method of imitation mussel glue that can be bonded on wet surface and solidified under water
  • A kind of preparation method of imitation mussel glue that can be bonded on wet surface and solidified under water

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020]

[0021] Add N-vinylpyrrolidone (NVP) (2.22g0.02mol), catechol derivative MSt (0.10g0.6mmol) and THF (5mL) into a 50ml reaction flask, add AIBN (0.04mmol6.6mg), and argon Air for 30min and react at 60℃ for 24h. Lower to room temperature, precipitate in n-hexane (100 mL), dissolve and precipitate the precipitate three times repeatedly, and dry to obtain copolymer I m (2.1g) (M n =51KDaM w / M n =1.7).

[0022] Add the prepared copolymer I to a 50ml reaction flask m , Tetrahydrofuran (6mL), boron tribromide (0.7g2.8mmol), reacted for 10 hours under the protection of argon. The concentrated reaction solution was dropped into n-hexane (50 mL) under stirring, the precipitate was repeatedly dissolved and precipitated three times, and dried to obtain polymer I' m (1.7g). Polymer I′ m Dissolve in 2mL of absolute ethanol, add 0.03g of ferric chloride, and stir evenly to obtain biomimetic mussel glue.

Embodiment 2

[0024]

[0025] Add N-vinylpyrrolidone (NVP) (2.22g0.02mol), catechol derivative BSt (3.64g0.1mol) and THF (10mL) into a 50ml reaction flask, add AIBN (0.4mmol66mg), and argon for 30min , React at 60℃ for 48h. Cool to room temperature, precipitate in n-hexane (100 mL), dissolve and precipitate the precipitate three times repeatedly, and dry to obtain copolymer I B (4.1g) (M n =4.9KDaM w / M n =2.1).

[0026] Add the prepared copolymer I to a 50ml reaction flask B , Tetrahydrofuran (15mL), concentrated hydrochloric acid (2mL), react under argon protection for 10 hours. The concentrated reaction solution was dropped into n-hexane (50 mL) under stirring, the precipitate was repeatedly dissolved and precipitated three times, and dried to obtain 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 substrate is aluminum, the wet surface is bonded under water and the bonding stren...

Embodiment 3

[0028]

[0029] Add N-vinylpyrrolidone (NVP) (2.22g0.02mol), catechol derivative ENVP (0.32g0.6mmol) and THF (10mL) into a 50ml reaction flask, add AIBN (0.5mmol82mg), and argon for 30min , React at 60℃ for 48h. Reduce to room temperature, precipitate in n-hexane (100 mL), dissolve and precipitate the precipitate three times repeatedly, and dry to obtain copolymer II E (2.0g) (M n =5.1KDaM w / M n =1.8).

[0030] Add the prepared copolymer Ⅱ into a 50ml reaction flask E , Tetrahydrofuran (15mL), concentrated hydrochloric acid (2mL), reacted for 10 hours under argon protection. The concentrated reaction solution was dropped into n-hexane (50 mL) under stirring, the precipitate was repeatedly dissolved and precipitated three times, and dried to obtain polymer II' E (1.4g). Polymer Ⅱ' E Dissolve in 10 mL of absolute ethanol, add ferric chloride at 1 / 3 (mole fraction) of the catechol group content in the polymer, stir evenly to obtain the bionic mussel glue (when the substrate is alu...

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Abstract

The invention relates to a preparation method for a biomimetic mussel adhesive used for adhesion on a wet surface and underwater curing. The method is characterized in that the biomimetic mussel adhesive is composed of two components including A and B, wherein the component A is a methanol solution of a polymer containing catechol groups; the polymer containing catechol groups is obtained in the manner that N-vinyl pyrrolidone and a polymerizable catechol derivative monomer are subjected to free radical polymerization and further subjected to deprotection; the component B is a crosslinking curing agent. The method has the advantages as follows: 1, the synthetic method is simple and efficient, raw material and reagents used in the reaction process are low in price and easy to get, and amplification in the operation process and industrial production are facilitated; 2, the biomimetic mussel adhesive has certain biocompatibility and initial adhesion performance, can be used for adhesion on the wet surface and underwater curing, and has the bonding strength being over 1 MPa, so as to be applied to adhesion of human tissue and adhesion in the wet environment of commonly-used base material as well as adhesion under the water. According to the invention, perfect combination between synthetic macromolecule and natural mussel attachment proteins is successfully realized, the technical bottleneck about the current biomimetic mussel adhesive is expected to break through, and meanwhile, a new approach for shellfish-based development of biomimetic high polymer material is provided.

Description

Technical field [0001] The invention relates to a preparation method of a bionic mussel glue that can be bonded on a wet surface and solidified under water, in particular to a polyvinylpyrrolidone-based biomimetic mussel glue with higher strength and better biocompatibility Preparation. Background technique [0002] Bonding and curing under water or in a humid environment has always been one of the difficulties in the field of adhesives. Most synthetic adhesives (such as cyanoacrylate adhesives) are difficult to achieve underwater or Strong adhesion in humid environment. Mussels have attracted much attention due to their unique physiological structure and strong adhesion under humid water environment. Studies have found that there is a large amount of 3,4-dihydroxyphenylalanine (DOPA, Dopa) in mussel silk foot adhesion-related proteins. The catechol group in DOPA has a strong coordination ability and can form a reversible organometallic complex with metal, and catechol can rea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09J125/18C09J139/04C09J11/04C08F212/14C08F226/10C08F8/12C08F226/06
Inventor 穆有炳李爱磊万晓波贾明辰王德龙
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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