CN110975017A - Photocurable hydrophilic coating material for interventional instrument, and preparation method and application thereof - Google Patents
Photocurable hydrophilic coating material for interventional instrument, and preparation method and application thereof Download PDFInfo
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- CN110975017A CN110975017A CN201911111968.0A CN201911111968A CN110975017A CN 110975017 A CN110975017 A CN 110975017A CN 201911111968 A CN201911111968 A CN 201911111968A CN 110975017 A CN110975017 A CN 110975017A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- 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
- A61L31/08—Materials for coatings
- A61L31/10—Macromolecular materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L29/00—Materials for catheters, medical tubing, cannulae, or endoscopes or for coating catheters
- A61L29/08—Materials for coatings
- A61L29/085—Macromolecular materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- 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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- 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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/18—Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment
Abstract
The invention provides a photocuring hydrophilic coating material for an interventional instrument, and a preparation method and application thereof. The method comprises the following steps: dissolving modified acrylate resin, a polymerization monomer and a hydrophilic substance in deionized water and an organic solvent, adding a wetting agent and an adhesion promoter, uniformly stirring, carrying out light-shielding treatment on the solution, adding a photoinitiator, and stirring until the solution is uniformly clear to obtain the coating material. According to the method for preparing the coating on the surface of the interventional instrument, the used hydrophilic substance can reduce the surface friction by more than 90%, the bonding force between the base material and the coating is improved by carrying out plasma treatment on the surface of the interventional instrument, the coating can be well attached to the base material after being subjected to multiple times of friction, the hydrophilic substance is fixed in a physical and chemical double-bonding mode, and the integral wear resistance and firmness of the coating are effectively improved.
Description
Technical Field
The invention relates to the field of medical instruments, in particular to a photocuring hydrophilic coating material for an interventional instrument, and a preparation method and application thereof.
Background
With the continuous development of medical technology, interventional diagnosis and treatment technology is applied more and more widely in minimally invasive surgery, and various catheters, guide wires and balloons are continuously developed as common medical instruments in interventional surgery. The materials of these interventional instruments are usually polyurethane, silicone rubber, polyvinyl chloride, polyether amide, stainless steel and the like, and although these materials have certain blood compatibility and safety, the materials do not have lubricity, and have large friction force when being directly inserted into a human body, so that the smooth operation is difficult, and even body tissues are damaged, so that the surface lubrication treatment of the interventional instruments is very necessary.
In the published patent technology, the surface lubrication modification of the interventional device is mostly performed by a thermal curing method, which generally requires long-time heating and curing, resulting in high energy consumption and low efficiency, so that a high-efficiency photo-curing coating preparation method becomes a new research trend. In order to improve the adhesion of the coating on the surface of the interventional device, a part of patents adopt a mode of combining a bottom layer and a surface layer during the preparation of the photocuring coating, and the double-layer structure needs to carry out coating and treatment on the interventional device twice, so that the convenience of the production process is influenced. Therefore, the development of more efficient single-application, i.e., photocurable, hydrophilic coatings is urgently required.
The abrasion resistance of the coating is also a key requirement which cannot be ignored because the interventional device is not only washed by blood but also subjected to multiple rubs of the tissues in the body during the delivery process in the body. Hydrophilic substances are fixed on the surface of an interventional instrument through physical entanglement and are easy to fall off, and long-term firmness is difficult to obtain, so that a firmer chemical bond combination mode is gradually applied.
Disclosure of Invention
One object of the present invention is to provide a method for preparing a photo-curable hydrophilic coating material for an interventional instrument;
another object of the present invention is to provide a photocurable hydrophilic coating material for interventional instruments;
still another object of the present invention is to provide a method for preparing a photo-curable hydrophilic coating for an interventional device. The intervening base material is processed by plasma, and can be cured and molded by light after being coated for one time. The hydrophilic substance endows the interventional instrument with good hydrophilic lubricity and wear resistance through a chemical and physical double combination mode, and can still keep good smoothness and comprehensive performance after repeated friction.
It is a further object of the present invention to provide an interventional instrument.
In order to achieve the above object, in one aspect, the present invention provides a method for preparing a photocurable hydrophilic coating material for an interventional instrument, wherein the method comprises the following steps:
dissolving modified acrylate resin, a polymerization monomer and a hydrophilic substance in deionized water and an organic solvent, adding a wetting agent and an adhesion promoter, uniformly stirring, carrying out light-shielding treatment on the solution, adding a photoinitiator, and stirring until the solution is uniformly clear to obtain the coating material.
According to some embodiments of the present invention, after the wetting agent and the adhesion promoter are added, the mixture is stirred for 20-60min, and then the solution is protected from light.
According to some embodiments of the invention, the mass ratio of the modified acrylate resin to the polymerized monomer is 1: (0.1-1).
According to some embodiments of the present invention, wherein the polymerized monomer is selected from the group consisting of hydroxyethyl acrylate, hydroxyethyl methacrylate, glycidyl methacrylate, ethylene glycol diacrylate, trimethylolpropane triacrylate, propoxylated glycerol triacrylate, ethylene glycol dimethacrylate, and pentaerythritol triacrylate.
According to some embodiments of the present invention, the amount of the photoinitiator is 1% to 5% based on 100% by mass of the total mass of the modified polyacrylate resin and the polymerized monomer; based on the total mass of the solution system being 100%, the dosage of the hydrophilic substance is 1% -10%, the dosages of the wetting agent and the adhesion promoter are respectively and independently 0.1% -1%, the dosage of the organic solvent is 30% -80%, and the dosage of the deionized water is 10% -50%.
According to some embodiments of the invention, wherein the modified acrylate resin has a polymerizable functionality of 1 to 6.
According to some embodiments of the invention, wherein the modified acrylate resin has a polymerizable functionality of 3 to 6.
According to some embodiments of the invention, the modified acrylate resin is selected from one or more of polyester acrylate resin, polyurethane acrylate resin, epoxy acrylate resin, silicone modified acrylate resin and silicone modified polyurethane acrylate resin.
According to some embodiments of the present invention, wherein the silicone-modified acrylate resin has a viscosity of 3500-8500 mPa.s.
According to some embodiments of the present invention, wherein the hydrophilic species has a number average molecular weight of 2000-.
According to some embodiments of the invention, the hydrophilic substance is selected from one or more of polyvinylpyrrolidone, carboxymethylcellulose, polyethylene glycol, polyethylene oxide, hyaluronic acid, polyacrylic acid, and polyacrylamide.
According to some embodiments of the present invention, wherein the photoinitiator is selected from the group consisting of 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-methyl-1-phenyl-1-propanone, 2-hydroxy-4' - (2-hydroxyethoxy) -2-methyl phenyl propanone, 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide, and benzophenone in combination with one or more thereof; the adhesion promoter is selected from one or more of resin adhesion promoters and coupling agent adhesion promoters.
According to some embodiments of the invention, the resinous adhesion promoter is a mixture of one or more of acrylate and polyester resins.
According to some embodiments of the invention, the coupling agent-based adhesion promoter comprises a mixture of one or more siloxane coupling agents and phthalate coupling agents having end groups selected from epoxy, vinyl, amino, mercapto, methacryloxy.
According to some embodiments of the present invention, the coupling agent type adhesion promoter is an epoxysiloxane coupling agent or an aminosiloxane coupling agent.
According to some embodiments of the present invention, wherein the epoxysiloxane coupling agent is KH560 and/or KH 561.
According to some embodiments of the invention, wherein the aminosiloxane coupling agent is HY792 and/or KH 550.
According to some embodiments of the present invention, wherein the methacryloxysiloxane coupling agent is KH570 and/or 3- (methacryloyloxy) propyltriethoxysilane.
According to some embodiments of the invention, wherein the polyester resin is TEGO EP-DS 1300.
According to some embodiments of the invention, the organic solvent is selected from the group consisting of methanol, ethanol, isopropanol, N-dimethylformamide, N-dimethylacetamide, acetone, ethyl acetate, and tetrahydrofuran.
According to some embodiments of the invention, the wetting agent is selected from one or more of polyether modified polysiloxane, sodium dodecyl sulfate, fluorine type non-ionic wetting agent.
According to some embodiments of the invention, the polyether modified polysiloxane is BYK-333 and/or TEGO WET 260.
According to some embodiments of the invention, wherein the fluorine-based non-ionic wetting agent is FY-F6501.
On the other hand, the invention also provides the photocuring hydrophilic coating material for the interventional instrument, which is prepared by the preparation method of any one of the previous items.
On the other hand, the invention also provides a preparation method of the photocuring hydrophilic coating of the interventional instrument, wherein the method comprises the steps of coating the photocuring hydrophilic coating material on the surface of the interventional instrument in a dip-coating, spraying or brush-coating mode, and then forming under the irradiation of UV light to obtain the interventional instrument with the surface covered with the photocuring hydrophilic coating.
According to some specific embodiments of the present invention, the method comprises applying the photocurable hydrophilic coating material of the present invention on the surface of the interventional device by dip coating, wherein the dip coating comprises dipping the interventional device into the photocurable hydrophilic coating material for 1-60s before starting the pulling, and the pulling speed is controlled to be 10-40 mm/s.
According to some specific embodiments of the present invention, wherein the irradiation with UV light comprises an irradiation energy value of 100-1000mJ/cm2Is irradiated for 10-120s under UV light.
According to some embodiments of the invention, the source of UV light is an LED lamp and/or a mercury lamp.
According to some embodiments of the present invention, the method comprises drying the interventional device coated with the photo-curable hydrophilic coating material at room temperature for 1-30min, and then forming the interventional device under the irradiation of UV light to obtain the interventional device with the photo-curable hydrophilic coating covered on the surface.
According to some embodiments of the invention, the method comprises cleaning the surface of the interventional device with alcohol and then pre-treating the surface with a plasma machine.
According to some embodiments of the present invention, the gas introduced during the pre-treatment by the plasma generator is one or more selected from helium, argon, oxygen, nitrogen dioxide and nitrogen.
According to some embodiments of the invention, the time of the pretreatment is 1 to 10 min.
In another aspect, the invention also provides an interventional device prepared by the preparation method.
In conclusion, the invention provides a photocuring hydrophilic coating material for an interventional instrument, and a preparation method and application thereof. The technical scheme of the invention has the following advantages:
1. the hydrophilic substance can reduce the surface friction by more than 90 percent, and the coating uses a network structure combined by long and short molecular chains under the combined action of resin and a polymerized monomer, so that the hydrophilic substance can be embedded into the crosslinked network structure on one hand, and the coating has good flexibility under the condition of ensuring tight crosslinking on the other hand, thereby ensuring that the coating cannot be influenced by external force deformation such as bending, expansion, reciprocating friction and the like to generate obvious cracks or peeling and keeping the integrity of the coating.
2. The silanol group generated after the hydrolysis of the adhesion promoter used in the invention can form a hydrogen bond or be condensed into a covalent bond with the hydroxyl on the surface of the base material, in addition, an active group can form a chemical bond or intermolecular acting force with a hydrophilic substance wound in the coating, taking hydrophilic substance PVP as an example, PVP molecules contain lactam groups with extremely strong hydrophilicity, the lactam groups can be combined with amino and hydroxyl in the adhesion promoter, so that the hydrophilic substance is not easy to fall off in the process of rubbing with the outside, and meanwhile, the adhesion promoter of a coupling agent can be condensed into a network after the hydrolysis, thereby ensuring the lubricity and the wear resistance of the coating.
3. The single coating process adopted by the invention can be cured by light through one-time coating, thereby avoiding the complexity and inconvenience of multiple coatings and ensuring that the production process is simple, convenient and efficient.
4. The coating solution is an aqueous system, avoids the damage of excessive organic solvent to interventional instruments and body tissues, and reduces the potential damage of the solution to workers in the production process. The coating has wide application range, and is particularly suitable for common medical instruments in the technical field of cardiovascular intervention diagnosis and treatment, such as guide wires, balloon catheters, guide catheters, thrombus suction catheters, peripheral central venous catheters, microcatheters, vascular sheaths and the like.
Detailed Description
The following detailed description is provided for the purpose of illustrating the embodiments and the advantageous effects thereof, and is not intended to limit the scope of the present disclosure.
Example 1
Solution preparation: adding 2 parts of urethane acrylate resin (trifunctional, viscosity 6500mpa.s), 1 part of trimethylolpropane triacrylate and 6 parts of polyvinylpyrrolidone (K90) to a flask containing a mixed reagent of 30 parts of deionized water and 60 parts of isopropanol, and magnetically stirring until no particles are visible; adding 0.3 part of polyether modified polysiloxane (BYK-333) and 0.6 part of epoxy silane coupling agent (KH560) into the solution system, keeping stirring for 60min, adding a photoinitiator 2-hydroxy-2-methyl-1-phenyl-1-acetone accounting for 4% of the total amount of the polymerizable substances, carrying out light-resistant treatment on the flask, and then continuously stirring for 60min to obtain a coating solution.
Preparing a coating: wiping the surface of the interventional catheter with medical alcohol, placing in a plasma machine for plasma 5min, taking out the interventional catheter, immersing in coating liquid for 10s, slowly lifting at uniform speed, drying at room temperature for 10min, transferring the interventional device with the coating liquid into a photocuring machine, and irradiating with a mercury lamp light source at 400mJ/cm2The coating preparation is completed by irradiating for 30s under energy.
The lubricity test method is as follows: the preparation of the coating was carried out over half the length of the interventional catheter by the method described above, while the other half length was left untreated. One end of an intervention conduit is vertically fixed on a lower clamp of a stretcher, a self-made sliding block is clamped on the surface of the intervention conduit, the sliding block can be screwed on the intervention conduit and can provide fixed pressure for the intervention conduit through an internal rubber ring, and an interlayer in the sliding block can bear a certain volume of deionized water and can continuously infiltrate the conduit; an upper clamp connected with a mechanical sensor in a stretcher is used for clamping a sliding block, the sliding block is pulled to the upper part of the interventional catheter from the lower part of the interventional catheter at a fixed speed, the friction force of the interventional catheter on two surfaces is reflected by the stress change of the sensor, and the hydrophilic lubricity of the interventional catheter is reflected by the difference of the numerical value of the friction force. And recording the friction values corresponding to the central positions of the surfaces of the two parts, and obtaining the reduction amplitude of the friction force of the coating by the following formula:
fp-r ═ (Fpr 2-Fpr 1)/Fpr2 × 100%, where fp-r is the magnitude of the decrease in the coating friction, Fpr1 is the force value of the coated portion, and Fpr2 is the force value of the coated portion; the greater the fp-r value, the better the lubricity of the coating.
The abrasion resistance test method is as follows: the catheter coated with the above coating was loaded on the apparatus described in the lubricity test method and the slider was reciprocated vertically 30 times at a fixed moving distance and speed by program control, and initial and final values of friction were recorded, the difference in the values of friction reflecting the degree of abrasion loss of the coating and the abrasion resistance of the catheter. The magnitude of the increase in friction at the time of termination is noted as fp-i, and a smaller fp-i value indicates better abrasion resistance.
The test result shows that the friction force reduction fp-r of the surface coating of the interventional catheter in the embodiment is 92.3 percent, which indicates that the coating has excellent hydrophilic lubricity; and the coating does not have cracks and peeling phenomena in 30 test cycles, and the increase degree fp-i value of the friction force is 2.8%, which shows that the coating has good firmness and wear resistance.
Example 2
The preparation method of the solution comprises the steps of weighing 1.5 parts of organic silicon modified acrylate resin (with three functionality degrees and viscosity of 4000mPa.s), 0.5 part of hydroxyethyl methacrylate, 4 parts of polyethylene glycol (with molecular weight of 5000) and adding into a flask, adding 20 parts of deionized water, 63 parts of methanol and 10 parts of N, N-dimethylformamide, stirring and dissolving, continuously adding 0.4 part of sodium dodecyl sulfate and 0.5 part of N- β - (aminoethyl) -gamma aminopropyltrimethoxysilane (HY792) into the solution, stirring for 30min, carrying out light-shielding treatment on the flask, adding a photoinitiator 2-hydroxy-4' - (2-hydroxyethoxy) -2-methyl propiophenone with the total polymer amount of 3.5%, and keeping stirring for 30min to obtain the coating liquid for use.
Preparing a coating: wiping the surface of the interventional guide wire with medical alcohol, placing in a plasma machine for plasma 4min, taking out the interventional guide wire, immersing in the coating liquid for 20s, slowly lifting at constant speed, drying at room temperature for 20min, feeding the interventional device with the coating liquid into a photocuring machine, and irradiating with a mercury lamp light source at 500mJ/cm2The coating preparation is completed by irradiating for 40s under energy.
The test method in the embodiment 1 is used for testing, and the reduction amplitude fp-r of the friction force borne by the medium guide wire prepared coating is 91.8 percent, which shows that the hydrophilic lubricity of the coating is excellent; the coating does not crack in the 30-time period process, and the increase fp-i value of the friction force is 2.1%, which shows that the coating has good firmness and wear resistance.
Example 3
Solution preparation: 1 part of silicon modified urethane acrylate resin (six functionality, viscosity 3700mPa.s), 0.4 part of pentaerythritol triacrylate, 7 parts of hyaluronic acid (molecular weight 100 ten thousand) are added into a flask, 25 parts of deionized water, 60 parts of methanol and 6 parts of acetone are used for full dissolution, 0.3 part of fluorine non-ionic wetting agent (FY-F6501) and 0.2 part of polyester resin (TEGO EP-DS1300) are added into a solution system and stirred for 60min, the flask is subjected to light shielding treatment, 1-hydroxycyclohexyl phenyl ketone accounting for 5 percent of the total amount of the polymer is added and stirred for 60min to obtain a coating solution.
Preparing a coating: wiping the surface of the interventional balloon with medical alcohol, placing in a plasma machine for plasma 3min, taking out the interventional balloon, immersing in coating liquid for 10s, slowly lifting at uniform speed, drying at room temperature for 15min, feeding the interventional device with the coating liquid into a photocuring machine, and irradiating with a mercury lamp light source at 600mJ/cm2The coating preparation is completed by irradiating for 50s under energy.
The test method in the embodiment 1 is used for testing, and the reduction amplitude fp-r of the friction force borne by the coating prepared by inserting the medium into the saccule is 92.7 percent, which shows that the hydrophilic lubricity of the coating is excellent; the coating does not crack in the 30-time period process, and the increase fp-i value of the friction force is 2.3%, which shows that the coating has good firmness and wear resistance.
Example 4
Solution preparation: 3 parts of epoxy acrylate resin (with a bifunctional degree and a viscosity of 8500mPa.s), 0.5 part of ethylene glycol diacrylate, 10 parts of polyacrylamide (with a molecular weight of 200 ten thousand) are added into a flask, 40 parts of deionized water and 45 parts of ethanol are weighed and added into the flask to be stirred and dissolved, 0.7 part of polyether modified polysiloxane (TEGO WET 260), 0.3 part of epoxy silane coupling agent (KH560) and 0.4 part of methacryloxy coupling agent (KH570) are added into a solution system to be stirred for 30min, the flask is subjected to light shielding treatment, and benzophenone accounting for 4.5 percent of the total amount of the polymer is added into the flask to be stirred for 60min to obtain a coating liquid.
Preparing a coating: wiping the surface of the interventional vascular sheath with medical alcohol, placing in a plasma machine for plasma 3min, taking out, spraying the coating liquid on the surface of the interventional vascular sheath, drying at room temperature for 5min, sending the interventional device attached with the coating liquid into a photocuring machine, and radiating 150mJ/cm by an LED light source2The coating preparation is completed by irradiating under energy for 60 s.
The test method in the embodiment 1 is used for testing, and the friction force reduction amplitude fp-r of the coating prepared by inserting the vascular sheath in the embodiment is 92.4 percent, which shows that the hydrophilic lubricity of the coating is excellent; the coating does not crack in the 30-time period process, and the increase fp-i value of the friction force is 1.9%, which shows that the coating has good firmness and wear resistance.
Example 5
Solution preparation: 2.5 parts of urethane acrylate resin (with hexafunctionality and viscosity of 6500mPa.s), 1.9 parts of propoxylated glycerol triacrylate and 8 parts of polyvinylpyrrolidone (K90) are added into a flask, 30 parts of deionized water and 56.5 parts of N, N-dimethylformamide are weighed and added into the flask to be stirred and dissolved, 0.7 part of polyether modified polysiloxane (TEGOWET 260) and 0.3 part of KH-550 are added into a solution system to be stirred for 25min, the flask is subjected to light-shielding treatment, and then 2-hydroxy-4' - (2-hydroxyethoxy) -2-methyl propiophenone accounting for 4.0 percent of the total amount of the polymer is added into the flask to be stirred for 50min to obtain a coating solution.
Preparing a coating: wiping the surface of the interventional guide wire with medical alcohol, placing in a plasma machine for plasma 5min, taking out, dip-coating the interventional guide wire in coating liquid for 30s, slowly taking out, drying at room temperature for 15min, feeding the interventional guide wire with the coating liquid into a photocuring machine, and irradiating with a mercury lamp light source at 650mJ/cm2The coating preparation is completed by irradiating for 90s under energy.
The test method in the embodiment 1 is used for testing, and the reduction amplitude fp-r of the friction force borne by the medium guide wire prepared coating is 91.5%, which shows that the hydrophilic lubricity of the coating is excellent; the coating does not crack in the 30-time period process, and the increase fp-i value of the friction force is 2.8%, which shows that the coating has good firmness and wear resistance.
Example 6
Solution preparation: 2 parts of polyester acrylate resin (tetrafunctionality, viscosity 2000mPa. s), 1.5 parts of pentaerythritol triacrylate, 9 parts of polyethylene oxide (molecular weight 20 ten thousand) are added into a flask, 25 parts of deionized water, 40 parts of methanol and 21.5 parts of N, N-dimethylformamide are weighed and added into the flask to be stirred and dissolved, 0.4 part of sodium dodecyl sulfate and 0.5 part of 3- (2, 3-epoxypropoxy) propylmethyldiethoxysilane (KH561) are added into a solution system to be stirred for 20min, the flask is subjected to light-shielding treatment, and then 2-hydroxy-4' - (2-hydroxyethoxy) -2-methyl propiophenone accounting for 4.2 percent of the total amount of the polymer is added into the flask to be kept stirred for 30min to obtain a coating liquid.
Preparing a coating: wiping the surface of the interventional catheter with medical alcohol, placing in a plasma machine for plasma 6min, taking out, dip-coating the interventional catheter in a coating liquid for 5s, slowly taking out, drying at room temperature for 20min, sending the interventional catheter attached with the coating liquid into a photocuring machine, and irradiating with a mercury lamp light source at 450mJ/cm2The coating preparation is completed by irradiating for 80s under energy.
The test method in the embodiment 1 is used for testing, and the reduction amplitude fp-r of the friction force borne by the catheter prepared coating is 93.1%, which shows that the hydrophilic lubricity of the coating is excellent; the coating does not crack in the 30-time period process, and the increase fp-i value of the friction force is 3.6%, which shows that the coating has good firmness and wear resistance.
Example 7
Solution preparation: 4.1 parts of urethane acrylate resin (with three functionality degrees and viscosity of 3500mPa.s), 1.8 parts of ethylene glycol dimethacrylate, 6 parts of polyvinylpyrrolidone (K90) and 3 parts of polyvinylpyrrolidone (K30) are added into a flask, 30 parts of deionized water, 30 parts of isopropanol and 24 parts of N, N-dimethylformamide are weighed and added into the flask to be stirred and dissolved, 0.5 part of polyether modified polysiloxane (BYK-333) and 0.5 part of 3- (methacryloyloxy) propyltriethoxysilane are added into a solution system to be stirred continuously for 35min, 2-hydroxy-2-methyl-1-phenyl-1-acetone with the total amount of 4.5 percent of polymer is added into the flask after the flask is processed in a dark place, and the stirring is kept for 60min to obtain a coating liquid.
Preparing a coating: use medical alcohol to wipePlacing in a plasma machine for plasma 4min after wiping the surface of the interventional guide wire, taking out, brushing absorbent cotton dipped with coating liquid on the interventional guide wire, drying at room temperature for 5min, sending the interventional guide tube with the coating liquid into a light curing machine, and radiating 150mJ/cm in an LED lamp light source2The coating preparation is completed by irradiating under energy for 60 s.
The test method in the embodiment 1 is used for testing, and the reduction amplitude fp-r of the friction force borne by the medium guide wire prepared coating is 92.4 percent, which shows that the hydrophilic lubricity of the coating is excellent; the coating does not crack in the 30-time period process, and the increase fp-i value of the friction force is 3.9%, which shows that the coating has good firmness and wear resistance.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of a photo-curing hydrophilic coating material for an interventional instrument, wherein the method comprises the following steps:
dissolving modified acrylate resin, a polymerization monomer (preferably, the mass ratio of the modified acrylate resin to the polymerization monomer is 1 (0.1-1)) (preferably, the polymerization monomer is selected from one or more of hydroxyethyl acrylate, hydroxyethyl methacrylate, glycidyl methacrylate, ethylene glycol diacrylate, trimethylolpropane triacrylate, propoxylated glycerol triacrylate, ethylene glycol dimethacrylate and pentaerythritol triacrylate) and a hydrophilic substance in deionized water and an organic solvent, adding a wetting agent and an adhesion promoter, uniformly stirring (preferably, stirring for 20-60min), carrying out light-shielding treatment on the solution, adding a photoinitiator, and stirring until the solution is uniformly clarified to obtain the coating material.
2. The preparation method according to claim 1, wherein the photoinitiator is used in an amount of 1% to 5% based on 100% by mass of the total mass of the modified polyacrylate resin and the polymerized monomer; based on the total mass of the solution system being 100%, the dosage of the hydrophilic substance is 1% -10%, the dosages of the wetting agent and the adhesion promoter are respectively and independently 0.1% -1%, the dosage of the organic solvent is 30% -80%, and the dosage of the deionized water is 10% -50%.
3. The production method according to claim 1, wherein the polymerizable functionality of the modified acrylate resin is 1 to 6 (preferably, the modified acrylate resin is selected from one or more of a polyester acrylate resin, a urethane acrylate resin, an epoxy acrylate resin, a silicone modified acrylate resin, and a silicone modified urethane acrylate resin in a mixed state).
4. The preparation method according to claim 1, wherein the hydrophilic substance has a number average molecular weight of 2000-.
5. The preparation method according to claim 1, wherein the photoinitiator is selected from one or more of 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-methyl-1-phenyl-1-propanone, 2-hydroxy-4' - (2-hydroxyethoxy) -2-methyl phenyl propanone, 2,4, 6-trimethylbenzoyl-diphenyl phosphine oxide and benzophenone; the adhesion promoter is selected from one or more of resin adhesion promoters (preferably, the resin adhesion promoters are one or more of acrylate and polyester resins) and coupling agent adhesion promoters (preferably, the coupling agent comprises one or more of siloxane coupling agent with the end group selected from epoxy, vinyl, amino, sulfydryl and methacryloxy and phthalate ester coupling agent).
6. The production method according to claim 1, wherein the organic solvent is selected from a mixture of one or more of methanol, ethanol, isopropanol, N-dimethylformamide, N-dimethylacetamide, acetone, ethyl acetate, and tetrahydrofuran.
7. The method of claim 1, wherein the wetting agent is selected from the group consisting of polyether modified polysiloxane, sodium dodecyl sulfate, and a mixture of one or more of fluorine-based nonionic wetting agents.
8. The photocuring hydrophilic coating material for the interventional instrument prepared by the preparation method of any one of claims 1 to 7.
9. A method for preparing a photo-curable hydrophilic coating of an interventional device, wherein the method comprises the steps of coating the photo-curable hydrophilic coating material of claim 8 on the surface of the interventional device in a manner of dip coating, spray coating or brush coating (preferably in a manner of dip coating, wherein the dip coating comprises the steps of dipping the interventional device into the photo-curable hydrophilic coating material for 1-60s, starting to pull, controlling the pulling speed to be 10-40mm/s), and irradiating the interventional device with UV light (preferably at the light energy value of 100-1000 mJ/cm)2Irradiating the interventional device with UV light for 10-120s) to obtain an interventional device with a surface covered with a photocuring type hydrophilic coating (preferably, the interventional device coated with the photocuring type hydrophilic coating material is dried at room temperature for 1-30min and then is irradiated with UV light to obtain the interventional device with the surface covered with the photocuring type hydrophilic coating) (preferably, the method comprises the steps of wiping the surface of the interventional device with medical alcohol and then pretreating the surface of the interventional device with a plasma machine (preferably, the pretreatment time is 1-10 min)).
10. An interventional device produced by the method of claim 9.
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