CN103948971A - Intervention catheter surface treatment method and intervention catheter - Google Patents
Intervention catheter surface treatment method and intervention catheter Download PDFInfo
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- CN103948971A CN103948971A CN201410104340.9A CN201410104340A CN103948971A CN 103948971 A CN103948971 A CN 103948971A CN 201410104340 A CN201410104340 A CN 201410104340A CN 103948971 A CN103948971 A CN 103948971A
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Abstract
The invention provides an intervention catheter surface treatment method and an intervention catheter. The intervention catheter surface treatment method comprises pre-treatment, modification treatment, first-coating coating, second-coating coating and aftertreatment. The intervention catheter surface treatment method effectively solves the problem that intervention catheter surface paint wetability and hydrophilic coating soundness are poor, and through combination with plasma treatment, grafting and double-layer coating system-based coating, covalent connection of the coating bottom and the intervention catheter and tight bonding of the bottom coating and the top coating are realized so that the frictional force on the treated intervention catheter in a water environment is reduced by more than 90%.
Description
Technical field
The present invention relates to medical instruments field, be specifically related to a kind of interposing catheter surface treatment method and the interposing catheter through this disposal methods.
Background technology
Endovascular Interventions technology is widely used in the aspects such as the removing of clinical angiography, angioplasty, Intravascular Thrombus or foreign body, compare with traditional medical skill, not only easy to operate, and because the wound of interventional therapy is low, can alleviate patient's misery, Operative risk is less, and medical expense is also relatively low, and therefore this technology has obtained promoting widely and using at medical domain.Endovascular Interventions technology is to arrive diseased region far away in body by means of interposing catheter by vessel lumen, and as vascular sites such as coronary artery, the diagnosis and treatment agent or insert apparatus of reinjecting, to reach the object to realize diagnosis and minimally-invasive treatment in body compared with distal part position.Research of Intravascular Catheterization is one of main apparatus of interventional technique in blood vessel, its kind can have radiography interposing catheter, drug conveying interposing catheter, angioplasty interposing catheter etc., these interposing catheters should have good operability and safety, generally need excellent blood compatibility, certain blood property of softening, ooze out, excellent antitorque knot, good mechanical performance, good machinability, have the performances such as the good compatibility with X ray opacifying agent without nuisance.
Lubricity is one of very important performance of Research of Intravascular Catheterization.In the time that conduit is entering, is exiting blood vessel and move in blood vessel, high-lubricity can suppress macromole in blood if plasma protein, platelet etc. are in the adhesion of material surface, reduce the damage to blood vessel wall and hemocyte, alleviate the disturbance to blood laminar flow, can avoid the generation of blood coagulation reaction.Therefore it is very necessary, interposing catheter being carried out to surface lubrication processing.
Summary of the invention
In view of above-mentioned deficiency, the object of this invention is to provide a kind of surface treatment method and interposing catheter of the interposing catheter that can obtain excellent Hydrophilic lubrication and wearability.
Technical scheme of the present invention is as follows:
A kind of interposing catheter surface treatment method, comprises the steps:
S100: pretreatment: interposing catheter is carried out to Cement Composite Treated by Plasma;
S200: modification: will take out and carry out carrying out washing treatment and dried after pretreated interposing catheter soaks certain hour in modified solution;
S300: apply the first coating: subbing is coated to the surface of the interposing catheter that step S200 obtains and solidifies;
S400: apply the second coating: top layer coating is coated to the interposing catheter surface that step S300 obtains and solidifies;
S500: post processing: the interposing catheter that step S400 is obtained immerses in strong aqua ammonia, carries out dried after taking-up.
Wherein, Cement Composite Treated by Plasma described in step S100 is that interposing catheter is placed in the sample room of plasma generator, carries out plasma treatment after passing into gas, and wherein discharge power is 10W to 300W, and the processing time is 1min to 5min.
Wherein, described gas is one or more in helium, argon, oxygen or nitrogen.
Wherein, in step S200, described modified solution is acrylic acid aqueous solution, and the mass percent concentration of wherein said acrylic acid aqueous solution is 5% to 95%, and temperature is 30 DEG C to 90 DEG C, and the soak time of interposing catheter is 2h to 24h.
Wherein, the baking temperature of the dried in step S200 is 75 DEG C to 85 DEG C, and be 10h to 14h drying time.
Wherein, the preparation method of described subbing is: aqueous polyurethane, polyfunctionality aziridine derivative, Siloxane-Oxyalkylene Copolymers and deionized water are added in container, at room temperature stir 25 minutes to 35 minutes, can obtain subbing, the quality of wherein said polyfunctionality aziridine derivative is 1%～10% of described aqueous polyurethane quality, the quality of described Siloxane-Oxyalkylene Copolymers is 0.05%～0.15% of described aqueous polyurethane quality, and the quality of described deionized water is 80%～99% of subbing gross mass.
Wherein, described polyfunctionality aziridine derivative is one or more in trimethylolpropane-tri-[3-(2-methylaziridine base)] propionic ester, trimethylolpropane-tri-(3-'-aziridino) propionic ester and tetramethylolmethane-tri-(3-'-aziridino) propionic ester.
Wherein, the preparation method of described top layer coating is: polymethyl vinyl ether-maleic anhydride, poly glycol monomethyl ether and organic solvent are added in container, at room temperature stir 25 minutes to 35 minutes, can obtain top layer coating, wherein the quality of poly glycol monomethyl ether is 1%～20% of polymethyl vinyl ether-maleic anhydride quality, and the quality of organic solvent is 80%～99% of top layer coating gross mass.
Wherein, described organic solvent is N, dinethylformamide, N,N-dimethylacetamide, N-Methyl pyrrolidone, N, one or more in N-dimethyl sulfoxide, ethyl acetate, butyl acetate, dichloromethane, chloroform, acetone, butanone and oxolane.
Wherein, the solidification temperature in step S300 is 55 DEG C to 65 DEG C, and be 0.8h to 1.2h hardening time; Solidification temperature in step S400 is 75 DEG C to 85 DEG C, and be 0.8h to 1.2h hardening time; The immersion time in step S500 is 0.9h to 1.3h, and baking temperature is 55 DEG C to 70 DEG C, and be 11h to 13h drying time.A kind of interposing catheter, comprises catheter main body, and the surface of described catheter main body adopts above-mentioned interposing catheter surface treatment method to process.
The invention has the beneficial effects as follows:
(1) the present invention efficiently solves the problem of interposing catheter surface coating wettability and hydrophilic coating fastness deficiency, by means such as binding plasma processing, grafting, the coatings of duplex coating system, reach that coating bottom is connected with the covalent bond of conduit and base coat and Topcoating between the object of combining closely, treated interposing catheter friction in water environment is reduced more than 90%.
(2) the present invention can be interposing catheter surface firmly hydrophilic lubrication performance is provided, especially be applicable to being applied to the macromolecular material base material that is conventionally difficult to bonding, the base materials such as such as ethylene-tetrafluoroethylene copolymer, hexafluoropropene-TFE copolymer, polypropylene, polyethylene, the scope of application is wider, the medical apparatus and instruments can be used for comprises epitheca pipe, convergent divergent channel in vagina vasorum assembly, tears sheath, and seal wire, foley's tube, guiding catheter, thrombus suction catheter, peripheral central venous catheter, angiography catheter etc.
Detailed description of the invention
In order to make object, technical scheme and the advantage of interposing catheter surface treatment method of the present invention and interposing catheter clearer, below in conjunction with specific embodiment, the present invention is further elaborated.
It should be noted that, in the situation that not conflicting, the feature in embodiment and embodiment in the application can combine mutually.
The present invention is by Cement Composite Treated by Plasma is carried out in interposing catheter surface, and graft acrylic acid, makes surface containing activated carboxyl, then by building duplex coating system, forms many components cross-linked structure in different chemical bond connection modes.Wherein, for polymethyl vinyl ether-maleic anhydride can be reacted with aziridine group, adopt poly glycol monomethyl ether and maleic anhydride group generation esterification partly, be grafted on the molecular skeleton of polymethyl vinyl ether-maleic anhydride, obtain the carboxyl that can react with aziridine group simultaneously, in addition the Oxyerhylene on poly glycol monomethyl ether can also play hydrophilic effect, polyfunctionality aziridine derivative has served as connecting duct surface carboxyl like this, polyurethane in the first coating, the cross-linking agent of hydrophilic polymer polymethyl vinyl ether-maleic anhydride, make coating outer surface both there is the effect of hydrophilic lubrication, ensure that again coating bottom is connected with the covalent bond of conduit, and first the combining closely between coating and the second coating, make crocking resistance excellence.
Interposing catheter surface treatment method of the present invention, comprises the steps:
S100: pretreatment: interposing catheter is carried out to Cement Composite Treated by Plasma.
Wherein, described Cement Composite Treated by Plasma is that interposing catheter is placed in the sample room of plasma generator, carries out plasma treatment after passing into gas, and wherein discharge power is 10W to 300W, and the processing time is 1min to 5min.The gas passing in this step is one or more in helium, argon, oxygen or nitrogen.Cement Composite Treated by Plasma is to utilize the plasma bombardment material surface of gas, makes molecular chain rupture, combination, generation free radical of material surface etc., thereby makes material surface obtain modification.
S200: modification: will take out interposing catheter after pretreated interposing catheter soaks certain hour in modified solution, with deionized water wash for several times until the pH value of wash liquid (being deionized water) do not change, afterwards this interposing catheter is placed in to vacuum drying oven, is preferably at 80 DEG C and takes out after dry 10h to 14h at 75 DEG C to 85 DEG C.Modified solution described in this step is acrylic acid aqueous solution, and in wherein said acrylic acid aqueous solution, acrylic acid mass percent concentration is 5% to 95%, and temperature is 30 DEG C to 90 DEG C, and the soak time of interposing catheter is 2h to 24h.By grafting is carried out in interposing catheter surface, make interposing catheter surface contain more pendant carboxylic group.
S300: apply the first coating: subbing is coated to the surface of the interposing catheter that step S200 obtains, and solidifies 1h at 60 DEG C;
S400: apply the second coating: top layer coating is coated to the interposing catheter surface that step S300 obtains and solidifies 1h at 80 DEG C.
When only with single polymer-coated interposing catheter surface, this coating easily comes off afterwards in water suction, and due to the restriction of interposing catheter grafting efficiency, the junction point on polymer and interposing catheter surface is limited, in the present invention, adopt double-deck coating, form multicomponent cross-linked structure by different chemical bond connection modes.
S500: post processing: the interposing catheter that step S400 is obtained immerses in strong aqua ammonia, at room temperature soaks 1h is dried 12h at 60 DEG C after taking-up, can obtain surface and have excellent hydrophilic lubrication coating and the interposing catheter of wearability.The object of this step is make in polymethyl vinyl ether-maleic anhydride remaining anhydride group open loop and form ammonium salt, and then obtains hydrophile function.
Preferably, the thickness of the first coating is 1～10 micron, and the second coating layer thickness is 1～10 micron, and the thickness ratio of the first coating layer thickness and the second coating is 1:1 to 1:1.5.The second coating is thicker can make the functional group reactions in the first coating complete.
Preferably, the preparation method of described subbing is: aqueous polyurethane, polyfunctionality aziridine derivative, Siloxane-Oxyalkylene Copolymers and deionized water are added in container, at room temperature stir 25 minutes to 35 minutes, can obtain subbing, the quality of wherein said polyfunctionality aziridine derivative is 1%～10% of described aqueous polyurethane quality, the quality of described Siloxane-Oxyalkylene Copolymers is that 0.05%～0.15%(of described aqueous polyurethane quality is preferably 0.1%), the quality of described deionized water is 80%～99% of subbing gross mass.
Further, described polyfunctionality aziridine derivative is one or more in trimethylolpropane-tri-[3-(2-methylaziridine base)] propionic ester, trimethylolpropane-tri-(3-'-aziridino) propionic ester and tetramethylolmethane-tri-(3-'-aziridino) propionic ester.
Preferably, the preparation method of described top layer coating is: polymethyl vinyl ether-maleic anhydride, poly glycol monomethyl ether and organic solvent are added in container, at room temperature stir 25 minutes to 35 minutes, can obtain top layer coating, wherein the quality of poly glycol monomethyl ether is 1%～20% of polymethyl vinyl ether-maleic anhydride quality, and the quality of organic solvent is 80%～99% of top layer coating gross mass.
Further, described organic solvent is N, dinethylformamide, N,N-dimethylacetamide, N-Methyl pyrrolidone, N, one or more in N-dimethyl sulfoxide, ethyl acetate, butyl acetate, dichloromethane, chloroform, acetone, butanone and oxolane.
Preferably, the percentage ratio that the deionized water in described subbing accounts for subbing gross mass equates with the mass percent that the organic solvent in top layer coating accounts for top layer coating gross mass.
The present invention also provides a kind of interposing catheter that adopts above-mentioned interposing catheter surface treatment method to process.This interposing catheter has good Hydrophilic lubrication and wearability.
Embodiment mono-
Preparation:
(1) prepare subbing: aqueous polyurethane, trimethylolpropane-tri-[3-(2-methylaziridine base)] propionic ester, Siloxane-Oxyalkylene Copolymers, deionized water are added in container, at room temperature stir 30 minutes, obtain subbing, wherein the quality of trimethylolpropane-tri-[3-(2-methylaziridine base)] propionic ester is 1% of aqueous polyurethane quality, the quality of Siloxane-Oxyalkylene Copolymers is 0.1% of aqueous polyurethane quality, and the quality of deionized water is 80% of subbing gross mass.
(2) prepare top layer coating: by polymethyl vinyl ether-maleic anhydride, poly glycol monomethyl ether, N, dinethylformamide adds in container, at room temperature stir 30 minutes, obtain top layer coating, wherein the quality of poly glycol monomethyl ether is 1% of polymethyl vinyl ether-maleic anhydride quality, the quality of DMF is 80% of top layer coating gross mass.
Wherein, polymethyl vinyl ether-maleic anhydride is the product that aldrich company of Sigma, number-average molecular weight are 80000, aqueous polyurethane is the Sancure777 of Lubrizol Corp. type product, poly glycol monomethyl ether is the product that aldrich company of Sigma, number-average molecular weight are 1000, Siloxane-Oxyalkylene Copolymers is the Tego Wet260 of Ying Chuan industrial group type product, and all the other are commercially available.(following examples are identical)
Preparation process:
S100: interposing catheter is positioned in the sample room of plasma generator, carries out Cement Composite Treated by Plasma after passing into argon, discharge power is 10W, and the processing time is 1min, after finishing dealing with, this interposing catheter is taken out;
S200: the interposing catheter that step S100 is obtained is soaked in the acrylic acid aqueous solution of 5wt% concentration and carries out graft modification, grafting temperature is 30 DEG C, the grafting time is 2h, react rear taking-up interposing catheter, with deionized water wash several, until the pH value of wash liquid no longer changes, afterwards conduit is positioned in vacuum drying oven to dry taking-up after 12 hours at 80 DEG C;
S300: above-mentioned subbing is coated to the surface of the interposing catheter that step S200 obtains, solidifies 0.8h to 1.2h at 55 DEG C to 65 DEG C;
S400: above-mentioned top layer coating is coated on the interposing catheter surface that step S300 obtains, solidifies 0.8h to 1.2h at 75 DEG C to 85 DEG C;
S500: the interposing catheter that step S400 is obtained is immersed in strong aqua ammonia, at room temperature soaks 0.9h to 1.3h, after taking-up at 55 DEG C to 70 DEG C dry 11h to 13h, can obtain surface and have the interposing catheter of hydrophilic lubrication coating.Strong aqua ammonia is commercial chemicals, and concentration is 22% to 30%.
Interposing catheter lubricity method of testing is as follows: to carrying out surface treatment of the present invention in the half of interposing catheter, and second half interposing catheter is not processed.Afterwards interposing catheter one end is vertically fixed in the lower clamp of stretching-machine, at self-control slide block of interposing catheter surface clamping, this slide block can be screwed on conduit and by inner rubber ring and give conduit fixing pressure, the inner interlayer of slide block can carry the deionized water of certain volume, can implement to infiltrate continuously to interposing catheter, with the upper clamp clamping slide block that is connected with mechanics sensor in stretching-machine, slide block is pulled to interposing catheter top from interposing catheter bottom according to fixed speed, the stressed variation of sensor has embodied the frictional force that interposing catheter is subject on two kinds of surfaces, the difference of friction value has reflected the Hydrophilic lubrication of conduit.(coating layer portion is stressed is Fpr1 to record the corresponding friction value in two parts centre of surface position, without coating layer portion stressed be Fpr2), can obtain the amplitude that water-wetted surface frictional force reduces, be designated as fp-r, fp-r=(Fpr2-Fpr1)/Fpr2 × 100%, fp-r value is larger, illustrates that lubricity is better.
After tested, in the present embodiment, interposing catheter friction reduces degree fp-r value higher than 90%.
Embodiment bis-
Preparation:
(1) prepare subbing: aqueous polyurethane, trimethylolpropane-tri-(3-'-aziridino) propionic ester, Siloxane-Oxyalkylene Copolymers, deionized water are added in container, at room temperature stir 30 minutes, obtain subbing, wherein the quality of trimethylolpropane-tri-(3-'-aziridino) propionic ester is 2% of aqueous polyurethane quality, the quality of Siloxane-Oxyalkylene Copolymers is 0.05% of aqueous polyurethane quality, and the quality of deionized water is 85% of subbing gross mass.
(2) prepare top layer coating: by polymethyl vinyl ether-maleic anhydride, poly glycol monomethyl ether, N, N-dimethyl acetylamide adds in container, at room temperature stir 30 minutes, obtain top layer coating, wherein the quality of poly glycol monomethyl ether is 5% of polymethyl vinyl ether-maleic anhydride quality, the quality of N,N-dimethylacetamide is 85% of top layer coating gross mass.
Preparation process:
S100: interposing catheter is positioned in the sample room of plasma generator, carries out Cement Composite Treated by Plasma after passing into helium, discharge power is 50W, and the processing time is 2min, after finishing dealing with, this interposing catheter is taken out;
S200: the interposing catheter that step S100 is obtained is soaked in the acrylic acid aqueous solution of 10wt% concentration and carries out graft modification, grafting temperature is 40 DEG C, the grafting time is 6h, react rear taking-up interposing catheter, with deionized water wash several, until the pH value of wash liquid no longer changes, afterwards conduit is positioned in vacuum drying oven to dry taking-up after 12 hours at 80 DEG C;
S300: the subbing in the present embodiment is coated to the surface of the interposing catheter that step S200 obtains, solidifies 1h at 60 DEG C;
S400: the top layer coating in the present embodiment is coated on the interposing catheter surface that step S300 obtains, solidifies 1h at 80 DEG C;
S500: the interposing catheter that step S400 is obtained is immersed in strong aqua ammonia, at room temperature soaks 1h, after taking-up at 60 DEG C dry 12h, can obtain surface and have the interposing catheter of hydrophilic lubrication coating.
Lubricity method of testing is identical with embodiment mono-.
After tested, in the present embodiment, interposing catheter friction reduction degree fp-r value is 95%.
Embodiment tri-
Preparation:
(1) prepare subbing: aqueous polyurethane, tetramethylolmethane-tri-(3-'-aziridino) propionic ester, Siloxane-Oxyalkylene Copolymers, deionized water are added in container, at room temperature stir 30 minutes, obtain subbing, wherein the quality of tetramethylolmethane-tri-(3-'-aziridino) propionic ester is 3% of aqueous polyurethane quality, the quality of Siloxane-Oxyalkylene Copolymers is 0.15% of aqueous polyurethane quality, and the quality of deionized water is 90% of subbing gross mass.
(2) prepare top layer coating: polymethyl vinyl ether-maleic anhydride, poly glycol monomethyl ether, N-Methyl pyrrolidone are added in container, at room temperature stir 30 minutes, obtain top layer coating, wherein the quality of poly glycol monomethyl ether is 10% of polymethyl vinyl ether-maleic anhydride quality, and the quality of N-Methyl pyrrolidone is 90% of top layer coating gross mass.
Preparation process:
S100: interposing catheter is positioned in the sample room of plasma generator, carries out Cement Composite Treated by Plasma after passing into oxygen, discharge power is 100W, and the processing time is 3min, after finishing dealing with, this interposing catheter is taken out;
S200: the interposing catheter that step S100 is obtained is soaked in the acrylic acid aqueous solution of 20wt% concentration and carries out graft modification, grafting temperature is 50 DEG C, the grafting time is 10h, react rear taking-up interposing catheter, with deionized water wash several, until the pH value of wash liquid no longer changes, afterwards conduit is positioned in vacuum drying oven to dry taking-up after 12 hours at 80 DEG C;
S300: above-mentioned subbing is coated to the surface of the interposing catheter that step S200 obtains, solidifies 1h at 60 DEG C;
S400: above-mentioned top layer coating is coated on the interposing catheter surface that step S300 obtains, solidifies 1h at 80 DEG C;
S500: the interposing catheter that step S400 is obtained is immersed in strong aqua ammonia, at room temperature soaks 1h, after taking-up at 60 DEG C dry 12h, can obtain surface and have the interposing catheter of hydrophilic lubrication coating.
Lubricity method of testing is identical with embodiment mono-.
After tested, in the present embodiment, interposing catheter friction reduction degree fp-r value is 94%.
Embodiment tetra-
Preparation:
(1) prepare subbing: aqueous polyurethane, trimethylolpropane-tri-[3-(2-methylaziridine base)] propionic ester, Siloxane-Oxyalkylene Copolymers, deionized water are added in container, at room temperature stir 25 minutes, obtain subbing, wherein the quality of trimethylolpropane-tri-[3-(2-methylaziridine base)] propionic ester is 4% of aqueous polyurethane quality, the quality of Siloxane-Oxyalkylene Copolymers is 0.1% of aqueous polyurethane quality, and the quality of deionized water is 95% of subbing gross mass.
(2) prepare top layer coating: by polymethyl vinyl ether-maleic anhydride, poly glycol monomethyl ether, N, N-dimethyl sulfoxide adds in container, at room temperature stir 30 minutes, obtain top layer coating, wherein the quality of poly glycol monomethyl ether is 15% of polymethyl vinyl ether-maleic anhydride quality, N, the quality of N-dimethyl sulfoxide is 95% of top layer coating gross mass.
Preparation process:
S100: interposing catheter is positioned in the sample room of plasma generator, carries out Cement Composite Treated by Plasma after passing into nitrogen, discharge power is 150W, and the processing time is 4min, after finishing dealing with, this interposing catheter is taken out;
S200: the interposing catheter that step S100 is obtained is soaked in the acrylic acid aqueous solution of 30wt% concentration and carries out graft modification, grafting temperature is 60 DEG C, the grafting time is 14h, react rear taking-up interposing catheter, with deionized water wash several, until the pH value of wash liquid no longer changes, afterwards conduit is positioned in vacuum drying oven to dry taking-up after 12 hours at 80 DEG C;
S300: above-mentioned subbing is coated to the surface of the interposing catheter that step S200 obtains, solidifies 1h at 60 DEG C;
S400: above-mentioned top layer coating is coated on the interposing catheter surface that step S300 obtains, solidifies 1h at 80 DEG C;
S500: the interposing catheter that step S400 is obtained is immersed in strong aqua ammonia, at room temperature soaks 1h, after taking-up at 60 DEG C dry 12h, can obtain surface and have the interposing catheter of hydrophilic lubrication coating.
Lubricity method of testing is identical with embodiment mono-.
After tested, in the present embodiment, interposing catheter friction reduction degree fp-r value is 95%.
Embodiment five
Preparation:
(1) prepare subbing: aqueous polyurethane, trimethylolpropane-tri-(3-'-aziridino) propionic ester, Siloxane-Oxyalkylene Copolymers, deionized water are added in container, at room temperature stir 35 minutes, obtain subbing, wherein the quality of trimethylolpropane-tri-(3-'-aziridino) propionic ester is 5% of aqueous polyurethane quality, the quality of Siloxane-Oxyalkylene Copolymers is 0.1% of aqueous polyurethane quality, and the quality of deionized water is 99% of subbing gross mass.
(2) prepare top layer coating: polymethyl vinyl ether-maleic anhydride, poly glycol monomethyl ether, ethyl acetate are added in container, at room temperature stir 25 minutes, obtain top layer coating, wherein the quality of poly glycol monomethyl ether is 20% of polymethyl vinyl ether-maleic anhydride quality, and the quality of ethyl acetate is 99% of top layer coating gross mass.
Preparation process:
S100: interposing catheter is positioned in the sample room of plasma generator, carries out Cement Composite Treated by Plasma after passing into argon and oxygen, discharge power is 200W, and the processing time is 5min, after finishing dealing with, this interposing catheter is taken out;
S200: the interposing catheter that step S100 is obtained is soaked in the acrylic acid aqueous solution of 40wt% concentration and carries out graft modification, grafting temperature is 70 DEG C, the grafting time is 18h, react rear taking-up interposing catheter, with deionized water wash several, until the pH value of wash liquid no longer changes, afterwards conduit is positioned in vacuum drying oven to dry taking-up after 14 hours at 75 DEG C;
S300: above-mentioned subbing is coated to the surface of the interposing catheter that step S200 obtains, solidifies 1h at 60 DEG C;
S400: above-mentioned top layer coating is coated on the interposing catheter surface that step S300 obtains, solidifies 1h at 80 DEG C;
S500: the interposing catheter that step S400 is obtained is immersed in strong aqua ammonia, at room temperature soaks 1h, after taking-up at 60 DEG C dry 12h, can obtain surface and have the interposing catheter of hydrophilic lubrication coating.
Lubricity method of testing is identical with embodiment mono-.
After tested, in the present embodiment, interposing catheter friction reduces degree fp-r value higher than 90%.
Embodiment six
Preparation:
(1) prepare subbing: aqueous polyurethane, tetramethylolmethane-tri-(3-'-aziridino) propionic ester, Siloxane-Oxyalkylene Copolymers, deionized water are added in container, at room temperature stir 30 minutes, obtain subbing, wherein the quality of tetramethylolmethane-tri-(3-'-aziridino) propionic ester is 6% of aqueous polyurethane quality, the quality of Siloxane-Oxyalkylene Copolymers is 0.1% of aqueous polyurethane quality, and the quality of deionized water is 83% of subbing gross mass.
(2) prepare top layer coating: polymethyl vinyl ether-maleic anhydride, poly glycol monomethyl ether, butyl acetate are added in container, at room temperature stir 35 minutes, obtain top layer coating, wherein the quality of poly glycol monomethyl ether is 3% of polymethyl vinyl ether-maleic anhydride quality, and the quality of butyl acetate is 83% of top layer coating gross mass.
Preparation process:
S100: interposing catheter is positioned in the sample room of plasma generator, carries out Cement Composite Treated by Plasma after passing into argon and oxygen, discharge power is 250W, and the processing time is 5min, after finishing dealing with, this interposing catheter is taken out;
S200: the interposing catheter that step S100 is obtained is soaked in the acrylic acid aqueous solution of 50wt% concentration and carries out graft modification, grafting temperature is 80 DEG C, the grafting time is 24h, react rear taking-up interposing catheter, with deionized water wash several, until the pH value of wash liquid no longer changes, afterwards conduit is positioned in vacuum drying oven to dry taking-up after 12 hours at 80 DEG C;
S300: above-mentioned subbing is coated to the surface of the interposing catheter that step S200 obtains, solidifies 1h at 60 DEG C;
S400: above-mentioned top layer coating is coated on the interposing catheter surface that step S300 obtains, solidifies 1h at 80 DEG C;
S500: the interposing catheter that step S400 is obtained is immersed in strong aqua ammonia, at room temperature soaks 1h, after taking-up at 60 DEG C dry 12h, can obtain surface and have the interposing catheter of hydrophilic lubrication coating.
Lubricity method of testing is identical with embodiment mono-.
After tested, in the present embodiment, interposing catheter friction reduces degree fp-r value higher than 90%.
Embodiment seven
Preparation:
(1) prepare subbing: aqueous polyurethane, trimethylolpropane-tri-[3-(2-methylaziridine base)] propionic ester, Siloxane-Oxyalkylene Copolymers, deionized water are added in container, at room temperature stir 30 minutes, obtain subbing, wherein the quality of trimethylolpropane-tri-[3-(2-methylaziridine base)] propionic ester is 7% of aqueous polyurethane quality, the quality of Siloxane-Oxyalkylene Copolymers is 0.1% of aqueous polyurethane quality, and the quality of deionized water is 87% of subbing gross mass.
(2) prepare top layer coating: polymethyl vinyl ether-maleic anhydride, poly glycol monomethyl ether, dichloromethane are added in container, at room temperature stir 30 minutes, obtain top layer coating, wherein the quality of poly glycol monomethyl ether is 7% of polymethyl vinyl ether-maleic anhydride quality, and the quality of dichloromethane is 87% of top layer coating gross mass.
Preparation process:
S100: interposing catheter is positioned in the sample room of plasma generator, carries out Cement Composite Treated by Plasma after passing into nitrogen and oxygen, discharge power is 300W, and the processing time is 5min, after finishing dealing with, this interposing catheter is taken out;
S200: the interposing catheter that step S100 is obtained is soaked in the acrylic acid aqueous solution of 60wt% concentration and carries out graft modification, grafting temperature is 90 DEG C, the grafting time is 12h, react rear taking-up interposing catheter, with deionized water wash several, until the pH value of wash liquid no longer changes, afterwards conduit is positioned in vacuum drying oven to dry taking-up after 12 hours at 80 DEG C;
S300: above-mentioned subbing is coated to the surface of the interposing catheter that step S200 obtains, solidifies 1.2h at 55 DEG C;
S400: above-mentioned top layer coating is coated on the interposing catheter surface that step S300 obtains, solidifies 1h at 80 DEG C;
S500: the interposing catheter that step S400 is obtained is immersed in strong aqua ammonia, at room temperature soaks 1h, after taking-up at 60 DEG C dry 12h, can obtain surface and have the interposing catheter of hydrophilic lubrication coating.
Lubricity method of testing is identical with embodiment mono-.
After tested, in the present embodiment, interposing catheter friction reduces degree fp-r value higher than 90%.
Embodiment eight
Preparation:
(1) prepare subbing: aqueous polyurethane, trimethylolpropane-tri-(3-'-aziridino) propionic ester, Siloxane-Oxyalkylene Copolymers, deionized water are added in container, at room temperature stir 30 minutes, obtain subbing, wherein the quality of trimethylolpropane-tri-(3-'-aziridino) propionic ester is 8% of aqueous polyurethane quality, the quality of Siloxane-Oxyalkylene Copolymers is 0.1% of aqueous polyurethane quality, and the quality of deionized water is 89% of subbing gross mass.
(2) prepare top layer coating: polymethyl vinyl ether-maleic anhydride, poly glycol monomethyl ether, chloroform are added in container, at room temperature stir 30 minutes, obtain top layer coating, wherein the quality of poly glycol monomethyl ether is 9% of polymethyl vinyl ether-maleic anhydride quality, and the quality of chloroform is 89% of top layer coating gross mass.
Preparation process:
S100: interposing catheter is positioned in the sample room of plasma generator, carries out Cement Composite Treated by Plasma after passing into argon and helium, discharge power is 30W, and the processing time is 3min, after finishing dealing with, this interposing catheter is taken out;
S200: the interposing catheter that step S100 is obtained is soaked in the acrylic acid aqueous solution of 70wt% concentration and carries out graft modification, grafting temperature is 75 DEG C, the grafting time is 8h, react rear taking-up interposing catheter, with deionized water wash several, until the pH value of wash liquid no longer changes, afterwards conduit is positioned in vacuum drying oven to dry taking-up after 10 hours at 85 DEG C;
S300: above-mentioned subbing is coated to the surface of the interposing catheter that step S200 obtains, solidifies 1h at 60 DEG C;
S400: above-mentioned top layer coating is coated on the interposing catheter surface that step S300 obtains, solidifies 0.8h at 85 DEG C;
S500: the interposing catheter that step S400 is obtained is immersed in strong aqua ammonia, at room temperature soaks 1h, after taking-up at 60 DEG C dry 12h, can obtain surface and have the interposing catheter of hydrophilic lubrication coating.
Lubricity method of testing is identical with embodiment mono-.
After tested, in the present embodiment, interposing catheter friction reduces degree fp-r value higher than 90%.
Embodiment nine
Preparation:
(1) prepare subbing: aqueous polyurethane, tetramethylolmethane-tri-(3-'-aziridino) propionic ester, Siloxane-Oxyalkylene Copolymers, deionized water are added in container, at room temperature stir 30 minutes, obtain subbing, wherein the quality of tetramethylolmethane-tri-(3-'-aziridino) propionic ester is 9% of aqueous polyurethane quality, the quality of Siloxane-Oxyalkylene Copolymers is 0.1% of aqueous polyurethane quality, and the quality of deionized water is 91% of subbing gross mass.
(2) prepare top layer coating: polymethyl vinyl ether-maleic anhydride, poly glycol monomethyl ether, acetone are added in container, at room temperature stir 30 minutes, obtain top layer coating, wherein the quality of poly glycol monomethyl ether is 11% of polymethyl vinyl ether-maleic anhydride quality, and the quality of acetone is 91% of top layer coating gross mass.
Preparation process:
S100: interposing catheter is positioned in the sample room of plasma generator, carries out Cement Composite Treated by Plasma after passing into argon and nitrogen, discharge power is 70W, and the processing time is 3min, after finishing dealing with, this interposing catheter is taken out;
S200: the interposing catheter that step S100 is obtained is soaked in the acrylic acid aqueous solution of 80wt% concentration and carries out graft modification, grafting temperature is 65 DEG C, the grafting time is 5h, react rear taking-up interposing catheter, with deionized water wash several, until the pH value of wash liquid no longer changes, afterwards conduit is positioned in vacuum drying oven to dry taking-up after 12 hours at 80 DEG C;
S300: above-mentioned subbing is coated to the surface of the interposing catheter that step S200 obtains, solidifies 0.8h at 65 DEG C;
S400: above-mentioned top layer coating is coated on the interposing catheter surface that step S300 obtains, solidifies 1h at 80 DEG C;
S500: the interposing catheter that step S400 is obtained is immersed in strong aqua ammonia, at room temperature soaks 1h, after taking-up at 60 DEG C dry 12h, can obtain surface and have the interposing catheter of hydrophilic lubrication coating.
Lubricity method of testing is identical with embodiment mono-.
After tested, in the present embodiment, interposing catheter friction reduces degree fp-r value higher than 90%.
Embodiment ten
Preparation:
(1) prepare subbing: aqueous polyurethane, trimethylolpropane-tri-[3-(2-methylaziridine base)] propionic ester, Siloxane-Oxyalkylene Copolymers, deionized water are added in container, at room temperature stir 30 minutes, obtain subbing, wherein the quality of trimethylolpropane-tri-[3-(2-methylaziridine base)] propionic ester is 10% of aqueous polyurethane quality, the quality of Siloxane-Oxyalkylene Copolymers is 0.1% of aqueous polyurethane quality, and the quality of deionized water is 93% of subbing gross mass.
(2) prepare top layer coating: polymethyl vinyl ether-maleic anhydride, poly glycol monomethyl ether, butanone are added in container, at room temperature stir 30 minutes, obtain top layer coating, wherein the quality of poly glycol monomethyl ether is 11% of polymethyl vinyl ether-maleic anhydride quality, and the quality of butanone is 93% of top layer coating gross mass.
Preparation process:
S100: interposing catheter is positioned in the sample room of plasma generator, carries out Cement Composite Treated by Plasma after passing into argon, oxygen and helium, discharge power is 90W, and the processing time is 5min, after finishing dealing with, this interposing catheter is taken out;
S200: the interposing catheter that step S100 is obtained is soaked in the acrylic acid aqueous solution of 90wt% concentration and carries out graft modification, grafting temperature is 55 DEG C, the grafting time is 15h, react rear taking-up interposing catheter, with deionized water wash several, until the pH value of wash liquid no longer changes, afterwards conduit is positioned in vacuum drying oven to dry taking-up after 12 hours at 80 DEG C;
S300: above-mentioned subbing is coated to the surface of the interposing catheter that step S200 obtains, solidifies 1h at 60 DEG C;
S400: above-mentioned top layer coating is coated on the interposing catheter surface that step S300 obtains, solidifies 1.2h at 75 DEG C;
S500: the interposing catheter that step S400 is obtained is immersed in strong aqua ammonia, at room temperature soaks 1h, after taking-up at 60 DEG C dry 12h, can obtain surface and have the interposing catheter of hydrophilic lubrication coating.
Lubricity method of testing is identical with embodiment mono-.
After tested, in the present embodiment, interposing catheter friction reduces degree fp-r value higher than 90%.
Embodiment 11
Preparation:
(1) prepare subbing: aqueous polyurethane, trimethylolpropane-tri-(3-'-aziridino) propionic ester, Siloxane-Oxyalkylene Copolymers, deionized water are added in container, at room temperature stir 30 minutes, obtain subbing, wherein the quality of trimethylolpropane-tri-(3-'-aziridino) propionic ester is 5% of aqueous polyurethane quality, the quality of Siloxane-Oxyalkylene Copolymers is 0.1% of aqueous polyurethane quality, and the quality of deionized water is 97% of subbing gross mass.
(2) prepare top layer coating: polymethyl vinyl ether-maleic anhydride, poly glycol monomethyl ether, oxolane are added in container, at room temperature stir 30 minutes, obtain top layer coating, wherein the quality of poly glycol monomethyl ether is 17% of polymethyl vinyl ether-maleic anhydride quality, and the quality of oxolane is 97% of top layer coating gross mass.
Preparation process:
S100: interposing catheter is positioned in the sample room of plasma generator, carries out Cement Composite Treated by Plasma after passing into argon, nitrogen and helium, discharge power is 110W, and the processing time is 5min, after finishing dealing with, this interposing catheter is taken out;
S200: the interposing catheter that step S100 is obtained is soaked in the acrylic acid aqueous solution of 95wt% concentration and carries out graft modification, grafting temperature is 45 DEG C, the grafting time is 17h, react rear taking-up interposing catheter, with deionized water wash several, until the pH value of wash liquid no longer changes, afterwards conduit is positioned in vacuum drying oven to dry taking-up after 12 hours at 80 DEG C;
S300: above-mentioned subbing is coated to the surface of the interposing catheter that step S200 obtains, solidifies 1h at 60 DEG C;
S400: above-mentioned top layer coating is coated on the interposing catheter surface that step S300 obtains, solidifies 1h at 80 DEG C;
S500: the interposing catheter that step S400 is obtained is immersed in strong aqua ammonia, at room temperature soaks 0.9h, after taking-up at 55 DEG C dry 13h, can obtain surface and have the interposing catheter of hydrophilic lubrication coating.
Lubricity method of testing is identical with embodiment mono-.
After tested, in the present embodiment, interposing catheter friction reduces degree fp-r value higher than 90%.
Embodiment 12
Preparation:
(1) prepare subbing: by aqueous polyurethane, trimethylolpropane-tri-(3-'-aziridino) propionic ester, tetramethylolmethane-tri-(3-'-aziridino) propionic ester, Siloxane-Oxyalkylene Copolymers, deionized water is added in container, at room temperature stir 30 minutes, obtain subbing, wherein the quality of trimethylolpropane-tri-(3-'-aziridino) propionic ester is 2% of aqueous polyurethane quality, the quality of tetramethylolmethane-tri-(3-'-aziridino) propionic ester is 2% of aqueous polyurethane quality, the quality of Siloxane-Oxyalkylene Copolymers is 0.1% of aqueous polyurethane quality, the quality of deionized water is 96% of subbing gross mass.
(2) prepare top layer coating: polymethyl vinyl ether-maleic anhydride, poly glycol monomethyl ether, ethyl acetate, dichloromethane are added in container, at room temperature stir 30 minutes, obtain top layer coating, wherein the quality of poly glycol monomethyl ether is 4% of polymethyl vinyl ether-maleic anhydride quality, the quality of ethyl acetate is 50% of top layer coating gross mass, and the quality of dichloromethane is 46% of top layer coating gross mass.
Preparation process:
S100: interposing catheter is positioned in the sample room of plasma generator, carries out Cement Composite Treated by Plasma after passing into argon, nitrogen, oxygen and helium, discharge power is 130W, and the processing time is 5min, after finishing dealing with, this interposing catheter is taken out;
S200: the interposing catheter that step S100 is obtained is soaked in the acrylic acid aqueous solution of 35wt% concentration and carries out graft modification, grafting temperature is 75 DEG C, the grafting time is 12h, react rear taking-up interposing catheter, with deionized water wash several, until the pH value of wash liquid no longer changes, afterwards conduit is positioned in vacuum drying oven to dry taking-up after 12 hours at 80 DEG C;
S300: above-mentioned subbing is coated to the surface of the interposing catheter that step S200 obtains, solidifies 1h at 60 DEG C;
S400: above-mentioned top layer coating is coated on the interposing catheter surface that step S300 obtains, solidifies 1h at 80 DEG C;
S500: the interposing catheter that step S400 is obtained is immersed in strong aqua ammonia, at room temperature soaks 1.3h, after taking-up at 70 DEG C dry 11h, can obtain surface and have the interposing catheter of hydrophilic lubrication coating.
Lubricity method of testing is identical with embodiment mono-.
After tested, in the present embodiment, interposing catheter friction reduces degree fp-r value higher than 90%.
Embodiment 13
Preparation:
(1) prepare subbing: by aqueous polyurethane, trimethylolpropane-tri-[3-(2-methylaziridine base)] propionic ester, trimethylolpropane-tri-(3-'-aziridino) propionic ester, tetramethylolmethane-tri-(3-'-aziridino) propionic ester, Siloxane-Oxyalkylene Copolymers, deionized water is added in container, at room temperature stir 30 minutes, obtain subbing, wherein the quality of trimethylolpropane-tri-[3-(2-methylaziridine base)] propionic ester is 1% of aqueous polyurethane quality, the quality of trimethylolpropane-tri-(3-'-aziridino) propionic ester is 1% of aqueous polyurethane quality, the quality of tetramethylolmethane-tri-(3-'-aziridino) propionic ester is 1% of aqueous polyurethane quality, the quality of Siloxane-Oxyalkylene Copolymers is 0.1% of aqueous polyurethane quality, the quality of deionized water is 96% of subbing gross mass.
(2) prepare top layer coating: polymethyl vinyl ether-maleic anhydride, poly glycol monomethyl ether, chloroform, acetone, oxolane are added in container, at room temperature stir 30 minutes, obtain top layer coating, wherein the quality of poly glycol monomethyl ether is 4% of polymethyl vinyl ether-maleic anhydride quality, the quality of chloroform is 30% of top layer coating gross mass, the quality of acetone is 40% of top layer coating gross mass, and the quality of oxolane is 25% of top layer coating gross mass.
Preparation process:
S100: interposing catheter is positioned in the sample room of plasma generator, carries out Cement Composite Treated by Plasma after passing into argon, discharge power is 50W, and the processing time is 3min, after finishing dealing with, this interposing catheter is taken out;
S200: the interposing catheter that step S100 is obtained is soaked in the acrylic acid aqueous solution of 25wt% concentration and carries out graft modification, grafting temperature is 60 DEG C, the grafting time is 12h, react rear taking-up interposing catheter, with deionized water wash several, until the pH value of wash liquid no longer changes, afterwards conduit is positioned in vacuum drying oven to dry taking-up after 12 hours at 80 DEG C;
S300: above-mentioned subbing is coated to the surface of the interposing catheter that step S200 obtains, solidifies 1h at 60 DEG C;
S400: above-mentioned top layer coating is coated on the interposing catheter surface that step S300 obtains, solidifies 1h at 80 DEG C;
S500: the interposing catheter that step S400 is obtained is immersed in strong aqua ammonia, at room temperature soaks 1h, after taking-up at 60 DEG C dry 12h, can obtain surface and have the interposing catheter of hydrophilic lubrication coating.
Lubricity method of testing is identical with embodiment mono-.
After tested, in the present embodiment, interposing catheter friction reduces degree fp-r value higher than 90%.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claim.
Claims (11)
1. an interposing catheter surface treatment method, is characterized in that, comprises the steps:
S100: pretreatment: interposing catheter is carried out to Cement Composite Treated by Plasma;
S200: modification: will take out and carry out carrying out washing treatment and dried after pretreated interposing catheter soaks certain hour in modified solution;
S300: apply the first coating: subbing is coated to the surface of the interposing catheter that step S200 obtains and solidifies;
S400: apply the second coating: top layer coating is coated to the interposing catheter surface that step S300 obtains and solidifies;
S500: post processing: the interposing catheter that step S400 is obtained immerses in strong aqua ammonia, carries out dried after taking-up.
2. interposing catheter surface treatment method according to claim 1, it is characterized in that, Cement Composite Treated by Plasma described in step S100 is that interposing catheter is placed in the sample room of plasma generator, after passing into gas, carry out plasma treatment, wherein discharge power is 10W to 300W, and the processing time is 1min to 5min.
3. interposing catheter surface treatment method according to claim 2, is characterized in that, described gas is one or more in helium, argon, oxygen and nitrogen.
4. interposing catheter surface treatment method according to claim 1, it is characterized in that, in step S200, described modified solution is acrylic acid aqueous solution, the mass percent concentration of wherein said acrylic acid aqueous solution is 5% to 95%, temperature is 30 DEG C to 90 DEG C, and the soak time of interposing catheter is 2h to 24h.
5. interposing catheter surface treatment method according to claim 1, is characterized in that, the baking temperature of the dried in step S200 is 75 DEG C to 85 DEG C, and be 10h to 14h drying time.
6. interposing catheter surface treatment method according to claim 1, it is characterized in that, the preparation method of described subbing is: by aqueous polyurethane, polyfunctionality aziridine derivative, Siloxane-Oxyalkylene Copolymers and deionized water are added in container, at room temperature stir 25 minutes to 35 minutes, can obtain subbing, the quality of wherein said polyfunctionality aziridine derivative is 1%～10% of described aqueous polyurethane quality, the quality of described Siloxane-Oxyalkylene Copolymers is 0.05%～0.15% of described aqueous polyurethane quality, the quality of described deionized water is 80%～99% of subbing gross mass.
7. interposing catheter surface treatment method according to claim 6, it is characterized in that, described polyfunctionality aziridine derivative is one or more in trimethylolpropane-tri-[3-(2-methylaziridine base)] propionic ester, trimethylolpropane-tri-(3-'-aziridino) propionic ester and tetramethylolmethane-tri-(3-'-aziridino) propionic ester.
8. interposing catheter surface treatment method according to claim 1, it is characterized in that, the preparation method of described top layer coating is: polymethyl vinyl ether-maleic anhydride, poly glycol monomethyl ether and organic solvent are added in container, at room temperature stir 25 minutes to 35 minutes, can obtain top layer coating, wherein the quality of poly glycol monomethyl ether is 1%～20% of polymethyl vinyl ether-maleic anhydride quality, and the quality of organic solvent is 80%～99% of top layer coating gross mass.
9. interposing catheter surface treatment method according to claim 8, it is characterized in that, described organic solvent is N, dinethylformamide, N, N-dimethyl acetylamide, N-Methyl pyrrolidone, N, one or more in N-dimethyl sulfoxide, ethyl acetate, butyl acetate, dichloromethane, chloroform, acetone, butanone and oxolane.
10. interposing catheter surface treatment method according to claim 1, is characterized in that, the solidification temperature in step S300 is 55 DEG C to 65 DEG C, and be 0.8h to 1.2h hardening time; Solidification temperature in step S400 is 75 DEG C to 85 DEG C, and be 0.8h to 1.2h hardening time; The immersion time in step S500 is 0.9h to 1.3h, and baking temperature is 55 DEG C to 70 DEG C, and be 11h to 13h drying time.
11. 1 kinds of interposing catheters, comprise catheter main body, it is characterized in that, the surface of described catheter main body adopts the interposing catheter surface treatment method described in claim 1 to 10 any one to process.
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| CN201410104340.9A CN103948971A (en) | 2014-03-20 | 2014-03-20 | Intervention catheter surface treatment method and intervention catheter |
| CN201510038107.XA CN104558666B (en) | 2014-03-20 | 2015-01-26 | Interposing catheter surface treatment method and interposing catheter |
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| JP4602556B2 (en) * | 1998-11-20 | 2010-12-22 | コロプラスト アクティーゼルスカブ | Method for sterilizing medical devices having a hydrophilic coating |
| AU2002237947B2 (en) * | 2001-01-24 | 2008-02-21 | Becton, Dickinson And Company | Lubricious coating for medical device |
| DK1809345T3 (en) * | 2004-10-07 | 2009-07-13 | Coloplast As | Medical device with a wetted hydrophilic coating |
| WO2008104572A2 (en) * | 2007-02-28 | 2008-09-04 | Dsm Ip Assets B.V. | Hydrophilic coating |
| US20100174245A1 (en) * | 2009-01-08 | 2010-07-08 | Ward Dean Halverson | System for pretreating the lumen of a catheter |
| CN101934101A (en) * | 2010-08-24 | 2011-01-05 | 北京迪玛克医药科技有限公司 | Hydrophilic coating for surface of medical apparatus and preparation method thereof |
| JP5690631B2 (en) * | 2011-03-30 | 2015-03-25 | 日本コヴィディエン株式会社 | Lubricating medical device and method for manufacturing the same |
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| CN104558666A (en) | 2015-04-29 |
| CN104558666B (en) | 2017-11-28 |
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Application publication date: 20140730 |