CN114163925B - Method for modifying hydrogel lubricating coating on surface of universal equipment and universal equipment modified with hydrogel lubricating coating - Google Patents

Method for modifying hydrogel lubricating coating on surface of universal equipment and universal equipment modified with hydrogel lubricating coating Download PDF

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CN114163925B
CN114163925B CN202111477209.3A CN202111477209A CN114163925B CN 114163925 B CN114163925 B CN 114163925B CN 202111477209 A CN202111477209 A CN 202111477209A CN 114163925 B CN114163925 B CN 114163925B
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hydrogel
coating
lubricating coating
base material
polyphenol
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CN114163925A (en
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周峰
麻拴红
徐蓉年
马正峰
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Yantai Zhongke Advanced Materials And Green Chemical Industry Technology Research Institute
Lanzhou Institute of Chemical Physics LICP of CAS
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Yantai Zhongke Advanced Materials And Green Chemical Industry Technology Research Institute
Lanzhou Institute of Chemical Physics LICP of CAS
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
    • C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/28—Materials for coating prostheses
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    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/28—Materials for coating prostheses
    • A61L27/30—Inorganic materials
    • A61L27/306—Other specific inorganic materials not covered by A61L27/303 - A61L27/32
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    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
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    • A61L27/52—Hydrogels or hydrocolloids
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    • A61L29/00—Materials for catheters, medical tubing, cannulae, or endoscopes or for coating catheters
    • A61L29/14—Materials characterised by their function or physical properties, e.g. lubricating compositions
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    • A61L29/00—Materials for catheters, medical tubing, cannulae, or endoscopes or for coating catheters
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    • A61L29/145—Hydrogels or hydrocolloids
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    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
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    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
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    • A61L31/082—Inorganic materials
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    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
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    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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Abstract

The invention provides a method for modifying a hydrogel lubricating coating on the surface of a general device and the general device modified with the hydrogel lubricating coating, belonging to the technical field of material surface modification. The modification method can realize the preparation of hydrophilic hydrogel lubricating coatings on the surfaces of various materials by generating the catalyst in situ on the surface of the base material on the premise of not changing the body and the surface property of the base material, has the universality of the base material, and is suitable for the fields of surface engineering and biological medical treatment. The method has mild reaction conditions, can realize the modification of the hydrogel lubricating coating at room temperature or low temperature, and can realize the controllable coating thickness by controlling the reaction time.

Description

Method for modifying hydrogel lubricating coating on surface of universal equipment and universal equipment modified with hydrogel lubricating coating
Technical Field
The invention relates to the technical field of material surface modification, in particular to a method for modifying a hydrogel lubricating coating on the surface of a general device and the general device modified with the hydrogel lubricating coating.
Background
With the continuous development of science and technology, medical instruments are also continuously advanced. Medical devices must have good biocompatibility and low surface friction properties due to direct contact with the human body. At present, common medical instruments such as catheters, stomach tubes, syringes, guide wires, catheters, stents and the like are generally composed of inert hydrophobic materials such as polyurethane, natural rubber, polyvinyl chloride, silicon rubber or latex, the surface polarity and the surface energy of the hydrophobic materials are low, so that the compatibility of the hydrophobic materials with tissues or organs of a human body is poor, great pain is brought to patients due to large friction force of an interface in the using process, wound infection is easy to cause, and the operation is difficult. Based on this, modifying the surface of these materials and devices with hydrophilic polymer lubricating coatings is an effective way to reduce friction.
At present, aiming at the requirement of lubrication modification of the surfaces of materials and apparatuses, a common technical means in the field of medical apparatuses is to modify hydrophilic polymer coatings on the surfaces, namely, to cure single-layer or multi-layer hydrophilic polymer coatings on the surfaces of the materials and apparatuses by photopolymerization. For example, patents CN104857571A, CN104448375A and US4373009 disclose methods for modifying the outer surface of materials with a hydrophilic polymer coating. Although the hydrophilic coating modified by the method has good lubricity and biocompatibility, the formed lubricating coating is mainly made of polyvinylpyrrolidone (PVP) basically, the material type is single, and the modification method is only suitable for materials such as silica gel and PVC; in addition, considering the problem of interface combination between different base materials and the PVP coating, the transition layer material is often required to be specially designed and optimized, i.e. the base material modification universality is not possessed; moreover, the traditional forming method has strict requirements on preparation and coating processes, and the accuracy and controllability of the coating thickness are poor.
Hydrogels have been widely spotlighted in the biomedical field as three-dimensionally crosslinked hydrophilic polymer materials having excellent water-lubricating properties on their surfaces. Recently, the prior art (Yanyu, Hyundooyuk, German A.Parada, You Wu, Xinyue Liu, Christoph S.Nabzdyk, Kamal Youcef-Toumi, Jianfeng Zang, xuananhao, Multifunctional "hydrogel skins" on reverse polymers with arbitrary covers, Advanced Materials,31(7):1807101,2019) disclosed a method of modifying a hydrogel coating on the surface of a PVC catheter by photoinitiation techniques, and prepared a water lubricated catheter device therefrom, to achieve the desired effect; however, the modification method is only suitable for polymer substrates which can be expanded by organic solvents (such as acetone), and has no universality for modifying the substrates.
Chinese patent CN108117662A discloses a method for preparing a hydrophilic lubricating coating on the surface of an iron-based composite material at room temperature by adding metal catalysts such as iron powder and the like into a precursor powder of a substrate, preparing a composite substrate containing the iron catalyst after thermosetting or hot press molding, and then immersing the composite substrate into a hydrogel monomer solution; although the method has certain advancement, the inherent characteristics of the bulk material are changed by doping of the metal catalyst, so that the popularization and the application of the metal catalyst in the fields of surface engineering and medical instruments are limited. In conclusion, the versatility of the hydrogel lubricating coatings prepared by the existing methods is not solved.
Disclosure of Invention
The invention aims to provide a method for modifying a hydrogel lubricating coating on the surface of a general device and the general device modified with the hydrogel lubricating coating, which can realize the substrate modification universality of the hydrogel lubricating coating without changing the properties of the substrate.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for modifying a hydrogel lubricating coating on the surface of a general device, which comprises the following steps:
carrying out first compounding on the buffer solution of dopamine hydrochloride or dopamine analogue and the substrate to obtain the substrate deposited with the polyphenol adhesion coating; the base material is a universal device;
the substrate deposited with the polyphenol adhesion coating and polycarboxylic acid molecule-Fe3+Carrying out second compounding on the mixed aqueous solution to obtain a base material deposited with a composite adhesive coating;
carrying out ultraviolet irradiation on the base material deposited with the composite adhesion coating, carrying out third compounding on the obtained base material and a hydrogel monomer solution, and carrying out in-situ polymerization to obtain a base material modified with a hydrogel lubricating coating; the hydrogel monomer solution contains persulfate.
Preferably, the dopamine analogue comprises tannic acid or tea polyphenol; the tea polyphenols include epicatechin gallate, gallic acid or epigallocatechin.
Preferably, the universal substrate comprises a natural material or a synthetic material; the natural material comprises plant stems, plant leaves, bones, skin or hair, and the artificial material comprises an inorganic metal material, an inorganic non-metal material or an organic material.
Preferably, the concentration of the buffer solution of dopamine hydrochloride or dopamine analogue is 0.05-10 mg/mL, the temperature of the first compound is 5-40 ℃, and the time is 6-48 h.
Preferably, the polycarboxylic acid molecule is citric acid and/or oxalic acid; the polycarboxylic acid molecule-Fe3+In the mixed water solution, the mass concentration of the polycarboxylic acid molecules is 0.5-50 mg/mL, and the Fe content is3+The mass concentration of (A) is 0.5-50 mg/mL; the temperature of the second compounding is 5-40 ℃, and the time is 1-48 h.
Preferably, the irradiation intensity of the ultraviolet irradiation is 5-50 mW/cm2The irradiation time is 10 s-30 min.
Preferably, the hydrogel monomer solution comprises the following components in percentage by mass: 0.5-25% of monomer, 0.05-3% of initiator, 0.01-1% of cross-linking agent and the balance of water.
Preferably, the monomer is one or more of acrylic acid, methacrylic acid, acrylamide, hydroxyethyl acrylate, hydroxyethyl methacrylate, polyoxyethylene methacrylate, N-isopropylacrylamide, 2-acrylamido-2-methylpropanesulfonic acid, sulfonate methacrylate, chitosan acrylate, chitosan methacrylate, dimethylaminoethyl methacrylate, sodium alginate methacrylate, methacryloyl ethyl carboxybetaine, and methacryloyl ethyl sulfobetaine; the initiator is potassium persulfate and/or ammonium persulfate; the cross-linking agent is N, N' -methylene bisacrylamide and/or polyethylene glycol dimethacrylate.
Preferably, the temperature of the in-situ polymerization is-10 to 30 ℃, and the time is 0.5 to 30 min.
The invention provides a general device modified with a hydrogel lubricating coating, which is prepared by the method in the technical scheme, and comprises the general device and the hydrogel lubricating coating modified on the surface of the general device; the hydrogel lubricating coating comprises polyphenol-polycarboxylic acid molecules-Fe which are sequentially laminated on the surface of a general device3+Composite adhesive coating and hydrogel coating.
The invention provides a method for modifying the surface of a general device with water condensationA method of gluing a lubricating coating comprising the steps of: carrying out first compounding on the buffer solution of dopamine hydrochloride or dopamine analogue and the substrate to obtain the substrate deposited with the polyphenol adhesion coating; the base material is a universal device; the substrate deposited with the polyphenol adhesion coating and polycarboxylic acid molecule-Fe3+Carrying out second compounding on the mixed aqueous solution to obtain a base material deposited with a composite adhesive coating; carrying out ultraviolet irradiation on the base material deposited with the composite adhesion coating, carrying out third compounding on the obtained base material and a hydrogel monomer solution, and carrying out in-situ polymerization to obtain a base material modified with a hydrogel lubricating coating; the hydrogel monomer solution contains persulfate. According to the invention, dopamine hydrochloride or dopamine analogue is firstly used for oxidation autopolymerization, and a polyphenol adhesion coating containing catechol adhesive bonding groups is deposited on the surface of a base material to enhance the bonding force with the base material; then utilizing polyphenol to adhere phenolic hydroxyl and Fe in the coating3+Competitive complexation to form polyphenol-polycarboxylic acid molecule/Fe3+The composite adhesion coating is subjected to ultraviolet irradiation, and Fe in the composite adhesion coating is subjected to accelerated catalysis of polycarboxylic acid molecules3+In situ reduction to Fe2+Endowing the surface of the adhesive coating with in-situ catalytic initiation polymerization activity to ensure that the Fe generated by ultraviolet radiation2+And the polymer solution and persulfate in the hydrogel monomer solution generate redox reaction to generate sulfate radicals, the monomer is initiated to generate free radical crosslinking polymerization reaction at a solid-liquid interface, the hydrogel coating grows in situ on the surface of the adhesive coating, and the monomer solution far away from the surface of the base material is not polymerized, so that the influence on the self characteristics of the base material is avoided. Therefore, the modification method can realize the preparation of the hydrophilic hydrogel lubricating coating on the surfaces of various materials by generating the catalyst on the surface of the base material in situ on the premise of not changing the body and the surface property of the base material, has the universality of the base material, and is suitable for the fields of surface engineering and biological medical treatment.
The method has mild reaction conditions, can realize the modification of the hydrogel lubricating coating at room temperature or low temperature, and can realize the controllable coating thickness by controlling the reaction time; in the existing photopolymerization method, a large amount of heat energy is generated within the photopolymerization time (1 hour), the bulk solution is initiated to carry out post polymerization, and the thickness of the lubricating coating is uncontrollable.
Drawings
FIG. 1 is an optical photograph of the titanium sheet of example 1 before and after growing a lubricating coating of a poly (acrylic acid-acrylamide) hydrogel on the surface thereof;
FIG. 2 is a sectional photomicrograph of the titanium plate surface-grown poly (acrylic acid-acrylamide) hydrogel lubricant coating at various times in example 1;
FIG. 3 is a graph of thickness data for hydrogel lubricious coatings formed on the surface of various substrates in example 2;
FIG. 4 is optical photographs of the surface of various medical devices of example 3 before and after the surface is modified with a hydrogel lubricious coating;
FIG. 5 is a graph of the friction before and after growing a poly (acrylic acid-acrylamide) hydrogel lubricious coating on the surfaces of the PVC and latex catheters of example 3.
Detailed Description
The invention provides a method for modifying a hydrogel lubricating coating on the surface of a general device, which comprises the following steps:
carrying out first compounding on the buffer solution of dopamine hydrochloride or dopamine analogue and the substrate to obtain the substrate deposited with the polyphenol adhesion coating; the base material is a universal device;
the substrate deposited with the polyphenol adhesion coating and polycarboxylic acid molecule-Fe3+Carrying out second compounding on the mixed aqueous solution to obtain a base material deposited with a composite adhesive coating;
carrying out ultraviolet irradiation on the base material deposited with the composite adhesion coating, carrying out third compounding on the obtained base material and a hydrogel monomer solution, and carrying out in-situ polymerization to obtain a base material modified with a hydrogel lubricating coating; the hydrogel monomer solution contains persulfate.
In the present invention, unless otherwise specified, all the required starting materials for the preparation are commercially available products well known to those skilled in the art.
The invention carries out the first composition of the buffer solution of dopamine hydrochloride or dopamine analogue and the substrate to obtain the substrate deposited with the polyphenol adhesion coating.
In the present invention, the substrate is a general-purpose device; the universal substrate preferably comprises a natural material or a synthetic material; the natural material preferably comprises plant stems, plant leaves, bones, skin or hair, and the synthetic material preferably comprises an inorganic metal material, an inorganic non-metal material or an organic material; the inorganic metal material is preferably a titanium sheet, an aluminum sheet or a gold sheet; the inorganic non-metallic material is preferably silicon chip, glass or ceramic; the organic material is preferably polyethylene, polyurethane, polytetrafluoroethylene, polyethylene terephthalate, polypropylene, nylon or polyimide.
In the present invention, the kind of the universal base material preferably includes a catheter, a drainage tube, a throat tube, an insertion type stomach tube, a capsule type gastroscope, a biliary tract stent, an artificial joint or a blood vessel guide wire.
The source of the universal equipment is not particularly limited in the present invention, and any commercially available equipment known in the art or corresponding equipment obtained from known sources may be used.
In the present invention, the dopamine analogue preferably comprises tannic acid or tea polyphenol; the tea polyphenol comprises epicatechin gallate, gallic acid or epigallocatechin, and has the following structure:
Figure BDA0003393909370000051
Figure BDA0003393909370000061
in the invention, the buffer solution used by the dopamine hydrochloride or dopamine analogue buffer solution is preferably tris buffer solution, and the concentration of the dopamine hydrochloride or dopamine analogue buffer solution is preferably 0.05-10 mg/mL, and more preferably 1.5-2 mg/mL. The buffer solution of dopamine hydrochloride or dopamine analogue is not specially limited in dosage, and the substrate can be completely immersed.
The first compounding mode is not particularly limited in the invention, and the buffer solution can be fully contacted with the substrate according to the process well known in the art; in an embodiment of the present invention, the first compounding manner is soaking.
In the invention, the temperature of the first compounding is preferably 5-40 ℃, and the time is preferably 6-48 h, and more preferably 10-24 h. In the first compounding process, dopamine hydrochloride or dopamine analogue is oxidized and polymerized automatically, and a polyphenol adhesion coating containing catechol adhesive bonding groups is deposited on the surface of the base material.
After the first compounding is completed, the method does not need to process, and directly carries out the subsequent steps.
In the invention, the thickness of the polyphenol adhesion coating is preferably 5nm to 30nm, and more preferably 15nm to 20 nm.
After the substrate with the polyphenol adhesion coating is obtained, the substrate with the polyphenol adhesion coating is mixed with polycarboxylic acid molecule-Fe3+And carrying out second compounding on the mixed aqueous solution to obtain the substrate deposited with the composite adhesive coating. In the present invention, the polycarboxylic acid molecule is preferably citric acid and/or oxalic acid; when the polycarboxylic acid molecules are preferably citric acid and oxalic acid, the ratio of citric acid to oxalic acid is not particularly limited, and any ratio can be adopted.
In the present invention, the polycarboxylic acid molecule-Fe3+In the mixed water solution, the mass concentration of the polycarboxylic acid molecules is preferably 0.5-50 mg/mL, more preferably 25-30 mg/mL, and Fe3+The mass concentration of (b) is preferably 0.5-50 mg/mL, more preferably 10.5-21 mg/mL; in the present invention for said Fe3+The kind of the corresponding iron salt is not particularly limited, and water-soluble iron salts well known in the art can be used; in the examples of the present invention, FeCl is specifically mentioned3、Fe(NO3)3Or Fe2(SO4)3。
The invention relates to the polycarboxylic acid molecule-Fe3+The preparation process of the mixed aqueous solution is not particularly limited, and the polycarboxylic acid molecule-Fe having the above-mentioned concentration range is obtained according to a process well known in the art3+Mixing the aqueous solution.
The invention also discloses a preparation method of the polycarboxylic acid molecule-Fe3+The amount of the mixed aqueous solution is not particularly limited, and the substrate can be completely immersed. The second complexing mode is not particularly limited in the present invention, and the polycarboxylic acid molecule-Fe can be achieved according to the procedures well known in the art3+The mixed aqueous solution is fully contacted with the substrate deposited with the polyphenol adhesion coating; in an embodiment of the present invention, the second compounding manner is soaking.
In the invention, the temperature of the second compounding is preferably 5-40 ℃, and the time is preferably 1-48 h, and more preferably 3-24 h. In the second compounding process, phenolic hydroxyl and polycarboxylic acid molecule-Fe in the polyphenol adhesion coating3+Middle Fe3+Competitive complexation to form polyphenol-polycarboxylic acid molecule/Fe3+And (5) compounding an adhesion coating.
After the second compounding is completed, the present invention preferably performs the subsequent steps without post-treatment.
After the base material with the composite adhesion coating deposited is obtained, the base material with the composite adhesion coating deposited is subjected to ultraviolet irradiation, the obtained base material is subjected to third compounding with a hydrogel monomer solution, and in-situ polymerization is carried out, so that the base material modified with the hydrogel lubricating coating is obtained. In the present invention, the ultraviolet irradiation is preferably achieved by an ultraviolet lamp; the irradiation intensity of the ultraviolet irradiation is preferably 5-50 mW/cm2More preferably 15 to 30mW/cm2The irradiation time is preferably 10 s-30 min, and more preferably 2-5 min.
In the ultraviolet irradiation process, Fe in the composite adhesion coating is subjected to accelerated catalysis of polycarboxylic acid molecules3+In situ reduction to Fe2+And endowing the surface of the adhesion coating with in-situ catalytic initiation polymerization activity.
In the present invention, the hydrogel monomer solution contains persulfate; the hydrogel monomer solution preferably comprises the following components in percentage by mass: 0.5-25% of monomer, 0.05-3% of initiator, 0.01-1% of cross-linking agent and the balance of water.
In the invention, the mass percentage of the monomer is preferably 12-15%; the mass percentage content of the initiator is preferably 0.05-0.06%; the mass percentage of the cross-linking agent is preferably 0.14%.
In the present invention, the monomer is preferably one or more of acrylic acid, methacrylic acid, acrylamide, hydroxyethyl acrylate, hydroxyethyl methacrylate, polyoxyethylene methacrylate, N-isopropylacrylamide, 2-acrylamido-2-methylpropanesulfonic acid, sulfonate methacrylate, chitosan acrylate, chitosan methacrylate, dimethylaminoethyl methacrylate, sodium alginate methacrylate, methacryloethylcarboxybetaine, and methacryloethylsulfobetaine; when the monomers are more than two of the monomers, the mixture ratio of different monomers is not specially limited, and the mixture ratio can be any. The source and specific molecular weight of the monomer are not particularly limited in the present invention, and the monomer can be prepared or customized according to actual needs by a well-known preparation process.
In the present invention, the initiator is preferably potassium persulfate and/or ammonium persulfate; the cross-linking agent is preferably N, N' -methylenebisacrylamide and/or polyethylene glycol dimethacrylate. When the initiators are two of the initiators, the invention has no special limitation on the proportion of different initiators and can be used in any proportion; when the cross-linking agents are two of the cross-linking agents, the proportion of the cross-linking agents of different types is not particularly limited, and the cross-linking agents can be mixed at any proportion.
The preparation process of the hydrogel monomer solution is not particularly limited in the present invention, and the hydrogel monomer solution with the content in the above-mentioned range can be prepared according to the well-known process in the art.
The dosage of the hydrogel monomer solution is not specially limited, and the substrate can be completely immersed. The third compounding mode is not particularly limited in the invention, and the hydrogel monomer solution can be fully contacted with the substrate according to the process well known in the art; in an embodiment of the present invention, the third compounding manner is soaking.
In the present invention, theThe temperature of the in-situ polymerization is preferably-10 to 30 ℃, more preferably 25 ℃, and the time is preferably 0.5 to 30min, more preferably 5 to 20 min. In the in-situ polymerization process, Fe generated by ultraviolet irradiation2+The catalyst and persulfate in the hydrogel monomer solution generate redox reaction to generate sulfate radicals, the monomer is initiated to generate free radical crosslinking polymerization reaction at a solid-liquid interface, a hydrogel lubricating coating grows in situ on the surface of the equipment, the monomer solution far away from the base material does not polymerize, and the influence on the self characteristics of the base material is avoided.
The invention provides a general device modified with a hydrogel lubricating coating, which is prepared by the method in the technical scheme, and comprises the general device and the hydrogel lubricating coating modified on the surface of the general device; the hydrogel lubricating coating comprises polyphenol-polycarboxylic acid molecule-Fe which is sequentially laminated on the surface of a universal device3+Composite adhesive coating and hydrogel coating.
In the invention, the thickness of the hydrogel lubricating coating is preferably 100-500 μm.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparing 10mL of 2mg/mL of Tris buffer solution of dopamine hydrochloride, and soaking a titanium sheet (5.5cm x 3.0cm) in the buffer solution for 24 hours at the temperature of 20 ℃ to form a polydopamine polyphenol coating with the thickness of 20 nm;
soaking the titanium sheet modified with the polydopamine polyphenol coating in a mixed aqueous solution of ferric trichloride (21mg/mL) and citric acid (25mg/mL) for 3 hours at the temperature of 20 ℃ to form polydopamine-citric acid-Fe on the surface of the titanium sheet3+Coating;
will be modified with polydopamine-citric acid-Fe3+The coated titanium sheet is placed under an ultraviolet lamp at the concentration of 15mW/cm2Irradiating for 2min to make Fe in the coating3+Reduction to Fe2+(ii) a The obtained titanium sheet is soaked in hydrogel monomer solution (4.26g of acrylamide, 1.08g of acrylic acid, 0.05g of N, N' -methylene bisacrylamide, 0.02g of potassium persulfate and 30mL of deionized water) to carry out surface catalysis initiated free radical polymerization at room temperature, the reaction time is 5min, and a poly (acrylic acid-acrylamide) hydrogel lubricating coating grows on the surface of the titanium sheet in situ.
Example 2
Growing poly (acrylic acid-acrylamide) hydrogel lubricious coatings on various substrate surfaces: pine branches, bones, hair; titanium sheet, aluminum sheet, gold sheet; silicon wafers, glass, ceramics; polyethylene, polyurethane, polytetrafluoroethylene, polyethylene terephthalate, polypropylene, nylon, or polyimide;
preparing 100mL of 2mg/mL of Tris buffer solution of dopamine hydrochloride, and soaking different substrates in the buffer solution for 24 hours at the temperature of 20 ℃ to form a polydopamine polyphenol coating with the thickness of 20 nm;
soaking the substrate modified with the polydopamine polyphenol coating in a mixed solution of ferric trichloride (10.5mg/mL) and citric acid (25mg/mL) for 3h at 20 ℃ to form polydopamine-citric acid-Fe on the surface of the substrate3+Coating;
will be modified with polydopamine-citric acid-Fe3+The coated substrate was placed under an ultraviolet lamp at 15mW/cm2Irradiating for 5min to make Fe in the coating3+Reduction to Fe2+(ii) a And (3) soaking the different treated substrates in a monomer solution of hydrogel (12.78g of acrylamide, 3.24g of acrylic acid, 0.15g N, N' -methylene bisacrylamide, 0.06g of potassium persulfate and 90mL of deionized water) to perform surface catalysis initiated free radical polymerization at room temperature, wherein the reaction time is 3min, and growing the poly (acrylic acid-acrylamide) hydrogel lubricating coatings on the surfaces of the different substrates.
Example 3
Growing a poly (acrylic acid-acrylamide) hydrogel lubricious coating on the surface of a variety of biomedical devices: PVC catheter, latex catheter, throat tube, biliary tract bracket, titanium alloy artificial hip joint ball head, stomach tube, drainage tube and suction head;
preparing 200mL of Tris buffer solution of 1.5mg/mL dopamine hydrochloride, and soaking different types of medical instruments in the buffer solution for 10 hours at the temperature of 25 ℃ to form a polydopamine polyphenol coating with the thickness of 15 nm;
soaking different instruments modified with polydopamine polyphenol coatings in a mixed solution of ferric trichloride (21mg/mL) and citric acid (25mg/mL) for 3h at 25 ℃ to form polydopamine-citric acid-Fe on the surfaces of the different instruments3+Coating;
will be modified with polydopamine-citric acid-Fe3+Different coated instruments were placed under an ultraviolet lamp at 30mW/cm2Irradiating for 5min to make Fe in the coating3+Reduction to Fe2+(ii) a And (3) soaking the treated different instruments in a monomer solution of hydrogel (25.56g of acrylamide, 6.48g of acrylic acid, 0.30g N, N' -methylene bisacrylamide, 0.12g of potassium persulfate and 180mL of deionized water) to perform surface catalysis initiated free radical polymerization at room temperature, wherein the reaction time is 5min, and modifying the surfaces of the different instruments with poly (acrylic acid-acrylamide) hydrogel lubricating coatings.
Characterization and Performance testing
1) FIG. 1 is an optical photograph before and after the growth of the poly (acrylic acid-acrylamide) hydrogel lubricating coating on the surface of the titanium sheet in example 1, and it can be seen from FIG. 1 that the surface of the titanium sheet becomes dark in color after the modification of the hydrogel lubricating coating, and a swelling type gel small particle morphology appears, which indicates that the poly (acrylic acid-acrylamide) hydrogel lubricating coating is successfully grown on the surface of the titanium sheet, and the thickness of the hydrogel lubricating coating is 300 μm.
FIG. 2 is a morphological diagram of the lubricating coating of poly (acrylic acid-acrylamide) hydrogel on the surface of the titanium sheet in example 1, which is observed in situ by an optical microscope at 5 different time points (30s, 1min, 2min, 3min and 5min) within 5min of polymerization time; as can be seen from FIG. 2, the thickness of the hydrogel lubricant coating gradually increased with the increase of the reaction time, indicating that the modification method of the present invention has high chemical controllability.
2) The thickness of the hydrogel lubricating coating formed on the surface of various substrates in example 2 was measured by an olympus optical microscope, and the results are shown in fig. 3; as can be seen from FIG. 3, the thickness of the hydrogel lubricating coating on the surface of the hair is smaller (more than 40 μm), and the thickness of the hydrogel lubricating coating on the surface of the rest of the base materials is 100-200 μm.
3) FIG. 4 is optical photographs of the surface of various medical devices of example 3 before and after the surface is modified with a hydrogel lubricious coating; in fig. 4, the left side of a-h is a photograph of a blank medical device before the unmodified hydrogel lubricating coating, and the right side is a photograph of a modified medical device partially modified with a poly (acrylic acid-acrylamide) hydrogel lubricating coating, and as can be seen from fig. 4, the hydrogel lubricating coating is relatively uniform on the surfaces of different devices.
4) The method for testing the lubricating property of the poly (acrylic acid-acrylamide) hydrogel lubricating coating on the surface of the medical instrument by respectively taking the blank PVC catheter, the blank latex catheter, the PVC catheter modified with the poly (acrylic acid-acrylamide) hydrogel lubricating coating (PAA-PAM) and the latex catheter modified with the poly (acrylic acid-acrylamide) hydrogel lubricating coating in the embodiment 3 as samples to be tested comprises the following steps: the lubrication performance of the outer surface of the instrument was evaluated using a conventional friction tester (CSM, Switzerland). Wherein, the lubricant is water, the normal phase loading is 0.2N, the friction test couple is PDMS rubber ball (radius 6mm), the test mode is reciprocating mode (sliding distance is 5mm), the sliding frequency is 1Hz, the test cycle is 300 times, and the obtained result is shown in figure 5.
As shown in FIG. 5, after the surface of the PVC urinary catheter and the latex urinary catheter is modified with the hydrogel lubricating coating by the method, the friction coefficient of the surface of the device is remarkably reduced, and the friction coefficient is relatively stable in 300 test cycles, which indicates that the hydrogel lubricating coating formed on the surface of the device has relatively good bonding force with the surface of the device.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (9)

1. A method for modifying a hydrogel lubricating coating on the surface of a general-purpose device comprises the following steps:
carrying out first compounding on the buffer solution of dopamine hydrochloride or dopamine analogue and the substrate to obtain the substrate deposited with the polyphenol adhesion coating; the base material is a universal device;
the substrate deposited with the polyphenol adhesion coating and polycarboxylic acid molecule-Fe3+Carrying out second compounding on the mixed aqueous solution to obtain a base material deposited with a composite adhesive coating; the polycarboxylic acid molecules are citric acid and/or oxalic acid;
carrying out ultraviolet irradiation on the base material deposited with the composite adhesion coating, carrying out third compounding on the obtained base material and a hydrogel monomer solution, and carrying out in-situ polymerization to obtain a base material modified with a hydrogel lubricating coating; the hydrogel monomer solution contains persulfate;
the hydrogel monomer solution comprises the following components in percentage by mass: 0.5-25% of monomer, 0.05-3% of initiator, 0.01-1% of cross-linking agent and the balance of water;
the monomer is one or more of acrylic acid, methacrylic acid, acrylamide, hydroxyethyl acrylate, hydroxyethyl methacrylate, polyoxyethylene methacrylate, N-isopropyl acrylamide, 2-acrylamido-2-methylpropanesulfonic acid salt, sulfonic acid ester of methacrylic acid, chitosan acrylate, chitosan methacrylate, dimethylaminoethyl methacrylate, sodium alginate methacrylate, methacryloyl ethyl carboxyl betaine and methacryloyl ethyl sulfobetaine.
2. The method of claim 1, wherein said dopamine analog comprises tannic acid or tea polyphenol; the tea polyphenols include epicatechin gallate, gallic acid or epigallocatechin.
3. The method of claim 1, wherein the universal substrate comprises a natural material or a synthetic material; the natural material comprises plant stems, plant leaves, bones, skin or hair, and the artificial material comprises an inorganic metal material, an inorganic non-metal material or an organic material.
4. The method according to claim 1, wherein the concentration of the buffer solution of dopamine hydrochloride or dopamine analogue is 0.05-10 mg/mL, the temperature of the first complex is 5-40 ℃, and the time is 6-48 h.
5. The method of claim 1, wherein said polycarboxylic acid molecule is-Fe3+In the mixed water solution, the mass concentration of the polycarboxylic acid molecules is 0.5-50 mg/mL, and the Fe content is3+The mass concentration of (A) is 0.5-50 mg/mL; the temperature of the second compounding is 5-40 ℃, and the time is 1-48 h.
6. The method according to claim 1 or 5, wherein the irradiation intensity of the ultraviolet irradiation is 5-50 mW/cm2The irradiation time is 10 s-30 min.
7. The method of claim 1, wherein the initiator is potassium persulfate and/or ammonium persulfate; the cross-linking agent is N, N' -methylene bisacrylamide and/or polyethylene glycol dimethacrylate.
8. The method of claim 1, wherein the in-situ polymerization is carried out at a temperature of-10 to 30 ℃ for 0.5 to 30 min.
9. The general equipment modified with the hydrogel lubricating coating prepared by the method of any one of claims 1 to 8, which comprises the general equipment and the hydrogel lubricating coating modified on the surface of the general equipment; the hydrogel lubricating coating comprises polyphenol-polycarboxylic acid molecules-Fe which are sequentially laminated on the surface of a general device3+Composite adhesive coating and hydrogel coating.
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