Fluorine-containing resin conduit surface treatment method

Abstract

The invention relates to the field of fluorine-containing resin conduit surface treatment methods, and particularly discloses a fluorine-containing resin conduit surface treatment method which comprises the following steps: 1) stirring 90% or more of absolute ethyl alcohol and a silane coupling agent under a sealed condition at the stirring temperature of 15-35 DEG C; 2) adding the screened bismuth powder into a stirred mixed solution of ethanol and a silane coupling agent, and stirring; (3) standing the stirred mixed solution in a standing crushing bottle, loading a heavy object on a movable rod to compress a barrel to accelerate precipitation during the period, and after the bismuth powder is precipitated, carrying out solid-liquid separation; and injecting the separated bismuth powder into a standing crushing bottle by using absolute ethyl alcohol to wash off the silane coupling agent remaining on the bismuth powder, grinding the bismuth powder by using a pressing sheet at the bottom of a movable rod in cooperation with a grinding ball during the period, and repeatedly washing for three times during the period. According to the invention, the defect that the appearance of the pipe is rough due to the fact that the bismuth powder cannot be uniformly dispersed in the PTFE base material but is distributed on the pipe in an agglomerated form in the processing process is overcome.

Description

Technical Field

[0001] The invention relates to the field of surface treatment methods for fluorine-containing resin catheters, and in particular to a surface treatment method for fluorine-containing resin catheters. Background Art

[0002] At present, PTFE tubes used in medical devices often add some fillers to the initial base material according to different uses and performance requirements, in order to improve the hardness, development performance, wear resistance, tensile effect, etc. of the molded tubes to meet different usage requirements; in addition to the choice of fillers, the content, distribution uniformity, and dispersion of the fillers also greatly affect the effect to be achieved by the tubes.

[0003] In the process of fluororesin tube processing, bismuth powder is usually added to the PTFE base material, and the extruded tube will have a rough appearance. Because the particle size of bismuth powder is small, due to the agglomeration of molecules, the bismuth powder cannot be evenly dispersed in the PTFE base material, but is distributed on the tube in the form of agglomeration, making the tube appear rough. Summary of the invention

[0004] In view of the above problems, the present invention proposes a surface treatment method for a fluororesin catheter, which solves the defect that in the existing fluororesin catheter processing process, bismuth powder cannot be evenly dispersed in the PTFE base material, but is distributed on the tube in the form of agglomerates, thereby making the tube surface rough.

[0005] The technical solution adopted by the present invention is as follows:

[0006] A method for treating the surface of a fluorine-containing resin catheter comprises the following steps:

[0007] 1) Stir more than 90% of anhydrous ethanol and silane coupling agent under sealed conditions at a stirring temperature of 15-35° C.;

[0008] 2) adding the sieved bismuth powder to the stirred mixture of ethanol and silane coupling agent, and stirring;

[0009] 3) the stirred mixed solution is allowed to stand in a static crushing bottle, during which a heavy object is installed on the movable rod to compress the cylinder to accelerate precipitation, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the bismuth powder is ground by using the pressing tablet at the bottom of the movable rod in combination with the grinding ball, and the rinsing is repeated three times.

[0010] The product prepared by the invention has good surface quality and smooth hand feeling; the bismuth powder is evenly dispersed without agglomeration and has good development effect; and the apparent color is good and uniform; the invention solves the defect that in the processing process of the existing fluororesin catheter, the bismuth powder cannot be evenly dispersed in the PTFE base material, but is distributed on the tube in the form of agglomeration, thereby making the tube rough in appearance.

[0011] Optionally, in step 2), the stirring speed is 80-180 rpm, the stirring temperature is set to 60-80° C., and the time is 4-8 h.

[0012] Optionally, the bismuth powder treated in step 3) is placed in a vacuum drying oven for drying at a temperature of 80-140° C. for 4-8 hours.

[0013] Optionally, the dried bismuth powder is put into a blender and ground into powder.

[0014] Optionally, a propellant is added to the ground material for mixing.

[0015] Optionally, the mixed materials are sealed and left to stand at 23-27° C. for 5 to 15 hours for aging.

[0016] Optionally, the air in the powder after the extrusion auxiliary agent is added to the matured material is removed, and the paste resin is pressed into a blank corresponding to the barrel of the wire pusher, and the blank is pre-pressed, dried and sintered.

[0017] Optionally, the rotation speed in step 1) is 60-130 rpm, and the time is set to 30-60 min.

[0018] Optionally, the silane coupling agent includes one or more of KH550, KH560, and KH570.

[0019] The present invention also discloses a method for treating the surface of a fluorine-containing resin catheter, comprising the following steps:

[0020] 1) Stir more than 90% anhydrous ethanol and bismuth powder at a stirring temperature of 15-35° C., a rotation speed of 60-130 rpm, and a time setting of 30-60 min;

[0021] 2) adding a silane coupling agent to the stirred mixture of ethanol and bismuth powder, and stirring under a sealed condition; the stirring speed is 80-180 rpm, the stirring temperature is 60-80° C., and the time is 4-8 hours;

[0022] 3) the stirred mixed solution is allowed to stand in a static crushing bottle, during which a heavy object is installed on the movable rod to compress the cylinder to accelerate precipitation, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the bismuth powder is ground by using the pressing tablet at the bottom of the movable rod in combination with the grinding ball, and the rinsing is repeated three times.

[0023] Beneficial Effects

[0024] 1. The present invention uses coupling treatment of bismuth powder,

[0025] 2. The relatively sealed stirring in the present invention avoids excessive hydrolysis of the coupling agent.

[0026] 3. The product prepared by the present invention has good surface quality and smooth feel; the bismuth powder is evenly dispersed without agglomeration, and the developing effect is good; and the apparent color is good and the color is uniform.

[0027] 4. The movable rod of the present invention is provided with a weight to compress the cylinder to accelerate sedimentation, thereby utilising the separation of solid and liquid.

[0028] 5. The present invention utilizes the pressing sheet at the bottom of the movable rod in conjunction with the grinding balls and the frosted surface at the bottom of the bottle body to grind the bismuth powder. The stirring grinding of the bismuth powder can prevent the bismuth powder from agglomerating and affecting the drying efficiency, thereby reducing the time required for the subsequent grinding of the dried bismuth powder in the mixer.

[0029] 6. The present invention includes at least a plurality of grinding balls evenly distributed around the filter capsule to form an annular structure. The stirring arc plate stirs the bismuth powder to promote washing away the silane coupling agent remaining on the bismuth powder, thereby improving the cleaning efficiency. On the other hand, the stirring arc plate also loosens the bismuth powder, and the liquid flows out of the filter capsule at a rapid rate in a spiral downward direction, thereby improving the cleaning efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 It is a stereoscopic view of a stationary crushing bottle of a fluorine-containing resin catheter surface treatment method according to Example 5 of the present invention.

[0031] Figure 2 It is a stereoscopic view of the grinding balls of a stationary crushing bottle in a method for treating the surface of a fluorine-containing resin catheter according to Example 5 of the present invention.

[0032] Figure 3 It is a top view of the filter capsule of the static crushing bottle of a fluorine-containing resin catheter surface treatment method according to Example 5 of the present invention.

[0033] The reference numerals in the figures are:

[0034] 1. Spherical bottle body, 2. Tube body, 3. Cylinder body, 4. Connecting tube, 5. Filter capsule, 6. Grinding ball, 7. Movable rod, 8. Grinding sheet, 9. Sealing ring, 10. Stirring arc plate, 11. Limiting ring, 12. Limiting part. DETAILED DESCRIPTION

[0035] The specific implementation of the present invention is further described in detail below in conjunction with the accompanying drawings and examples. The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention.

[0036] The silane coupling agent of the present invention can be a product of Hangzhou Jessica Chemical Co., Ltd.

[0037] In the description of the present invention, unless otherwise specified, the terms "upper", "lower", "left", "right", "inside", "outside", "front end", "rear end", "head", "tail" and the like indicate positions or positional relationships based on the positions or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present invention. In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "connected" and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection, a direct connection, or an indirect connection through an intermediate medium. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0038] Example 1

[0039] The invention discloses a method for treating the surface of a fluorine-containing resin catheter, comprising the following steps:

[0040] 1) Stir more than 90% of anhydrous ethanol and a silane coupling agent under sealed conditions at a stirring temperature of 15° C., a rotation speed of 60 rpm, and a time setting of 30 minutes.

[0041] The silane coupling agent used in this embodiment is KH550.

[0042] 2) adding the sieved bismuth powder to the stirred mixture of ethanol and silane coupling agent, stirring at a stirring speed of 80 rpm, a stirring temperature of 60° C., and a stirring time of 4 h;

[0043] 3) the stirred mixed solution is allowed to stand in a static crushing bottle, during which a heavy object is installed on the movable rod to compress the cylinder to accelerate precipitation, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the bismuth powder is ground by using the pressing tablet at the bottom of the movable rod in combination with the grinding ball, and the rinsing is repeated three times.

[0044] 4) The treated bismuth powder is placed in a vacuum drying oven and dried at a temperature of 80° C. for 4 h.

[0045] The dried bismuth powder is put into a mixer and ground into powder.

[0046] 5) Add a propellant to the ground material for mixing. Seal the mixed material and place it at 23°C for 5 hours for aging.

[0047] 6) Remove the air from the powder after adding the extrusion auxiliary agent, and press the paste resin into a blank corresponding to the barrel of the wire pusher, pre-press the blank into shape, dry it, and sinter it.

[0048] Example 2

[0049] The invention discloses a method for treating the surface of a fluorine-containing resin catheter, comprising the following steps:

[0050] 1) Stir more than 90% of anhydrous ethanol and a silane coupling agent under sealed conditions at a stirring temperature of 35° C., a rotation speed of 130 rpm, and a time setting of 60 min.

[0051] The silane coupling agent used in this embodiment is KH560.

[0052] 2) adding the sieved bismuth powder to the stirred mixture of ethanol and silane coupling agent, stirring at a stirring speed of 180 rpm, a stirring temperature of 80° C., and a stirring time of 8 h;

[0053] 3) the stirred mixed solution is allowed to stand in a static crushing bottle, during which a heavy object is installed on the movable rod to compress the cylinder to accelerate precipitation, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the bismuth powder is ground by using the pressing tablet at the bottom of the movable rod in combination with the grinding ball, and the rinsing is repeated three times.

[0054] 4) The treated bismuth powder is placed in a vacuum drying oven for drying at a temperature of 140° C. for 8 hours. The dried bismuth powder is placed in a mixer and ground into powder.

[0055] 5) Add a propellant to the ground material for mixing. Seal the mixed material and place it at 27°C for 15 hours for aging.

[0056] 6) Remove the air from the powder after adding the extrusion auxiliary agent, and press the paste resin into a blank corresponding to the barrel of the wire pusher, pre-press the blank into shape, dry it, and sinter it.

[0057] Comparative Example 1

[0058] The invention discloses a method for treating the surface of a fluorine-containing resin catheter, comprising the following steps:

[0059] 1) Stir more than 90% of anhydrous ethanol and a silane coupling agent under sealed conditions at a stirring temperature of 25° C., a rotation speed of 100 rpm, and a time setting of 45 minutes.

[0060] The silane coupling agent used in this embodiment is KH550.

[0061] 2) adding the sieved bismuth powder to the stirred mixture of ethanol and silane coupling agent, stirring at a stirring speed of 120 rpm, a stirring temperature of 25° C., and a stirring time of 6 h;

[0062] 3) the stirred mixed solution is allowed to stand in a static crushing bottle, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the bismuth powder is ground, and the rinsing is repeated three times.

[0063] 4) The treated bismuth powder is placed in a vacuum drying oven for drying at a temperature of 80° C. for 4 hours. The dried bismuth powder is placed in a mixer and ground into powder.

[0064] 5) Add a propellant to the ground material for mixing. Seal the mixed material and place it at 23°C for 5 hours for aging.

[0065] 6) Remove the air from the powder after adding the extrusion auxiliary agent, and press the paste resin into a blank corresponding to the barrel of the wire pusher, pre-press the blank into shape, dry it, and sinter it.

[0066] Comparative Example 2

[0067] The invention discloses a method for treating the surface of a fluorine-containing resin catheter, comprising the following steps:

[0068] 1) Stir more than 90% of anhydrous ethanol and a silane coupling agent under sealed conditions at a stirring temperature of 25° C., a rotation speed of 100 rpm, and a time setting of 45 minutes.

[0069] The silane coupling agent used in this embodiment is KH550.

[0070] 2) adding the sieved bismuth powder to the stirred mixture of ethanol and silane coupling agent, stirring at a stirring speed of 120 rpm, a stirring temperature of 70° C., and a stirring time of 45 min;

[0071] 3) the stirred mixed solution is allowed to stand in a static crushing bottle, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the bismuth powder is ground, and the rinsing is repeated three times.

[0072] 4) The treated bismuth powder is placed in a vacuum drying oven for drying at a temperature of 80° C. for 4 hours. The dried bismuth powder is placed in a mixer and ground into powder.

[0073] 5) Add a propellant to the ground material for mixing. Seal the mixed material and place it at 23°C for 5 hours for aging.

[0074] 6) Remove the air from the powder after adding the extrusion auxiliary agent, and press the paste resin into a blank corresponding to the barrel of the wire pusher, pre-press the blank into shape, dry it, and sinter it.

[0075] Comparative Example 3

[0076] The invention discloses a method for treating the surface of a fluorine-containing resin catheter, comprising the following steps:

[0077] 1) Stir more than 90% of anhydrous ethanol and a silane coupling agent under sealed conditions at a stirring temperature of 25° C., a rotation speed of 100 rpm, and a time setting of 2 hours.

[0078] The silane coupling agent used in this embodiment is KH550.

[0079] 2) adding the sieved bismuth powder to the stirred mixture of ethanol and silane coupling agent, stirring at a stirring speed of 120 rpm, a stirring temperature of 70° C., and a stirring time of 45 min;

[0080] 3) the stirred mixed solution is allowed to stand in a static crushing bottle, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the bismuth powder is ground, and the rinsing is repeated three times.

[0081] 4) The treated bismuth powder is placed in a vacuum drying oven for drying at a temperature of 80° C. for 6 hours. The dried bismuth powder is placed in a mixer and ground into powder.

[0082] 5) Add a propellant to the ground material for mixing. Seal the mixed material and place it at 23°C for 5 hours for aging.

[0083] 6) Remove the air from the powder after adding the extrusion auxiliary agent, and press the paste resin into a blank corresponding to the barrel of the wire pusher, pre-press the blank into shape, dry it, and sinter it.

[0084] Comparative Example 4

[0085] The invention discloses a method for treating the surface of a fluorine-containing resin catheter, comprising the following steps:

[0086] 1) Stir more than 90% of anhydrous ethanol and a silane coupling agent under sealed conditions at a stirring temperature of 25° C., a rotation speed of 50 rpm, and a time setting of 45 minutes.

[0087] The silane coupling agent used in this embodiment is KH550.

[0088] 2) adding the sieved bismuth powder to the stirred mixture of ethanol and silane coupling agent, stirring at a stirring speed of 50 rpm, a stirring temperature of 70° C., and a stirring time of 6 h;

[0089] 3) the stirred mixed solution is allowed to stand in a static crushing bottle, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the bismuth powder is ground, and the rinsing is repeated three times.

[0090] 4) The treated bismuth powder is placed in a vacuum drying oven for drying at a temperature of 80° C. for 6 hours. The dried bismuth powder is placed in a mixer and ground into powder.

[0091] 5) Add a propellant to the ground material for mixing. Seal the mixed material and place it at 23°C for 5 hours for aging.

[0092] 6) Remove the air from the powder after adding the extrusion auxiliary agent, and press the paste resin into a blank corresponding to the barrel of the wire pusher, pre-press the blank into shape, dry it, and sinter it.

[0093] Comparative Example 5

[0094] The invention discloses a method for treating the surface of a fluorine-containing resin catheter, comprising the following steps:

[0095] 1) Stir more than 90% of anhydrous ethanol and a silane coupling agent under sealed conditions at a stirring temperature of 25° C., a rotation speed of 200 rpm, and a time setting of 45 minutes.

[0096] The silane coupling agent used in this embodiment is KH560.

[0097] 2) adding the sieved bismuth powder to the stirred mixture of ethanol and silane coupling agent, stirring at a stirring speed of 200 rpm, a stirring temperature of 70° C., and a stirring time of 6 h;

[0098] 3) the stirred mixed solution is allowed to stand in a static crushing bottle, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the bismuth powder is ground, and the rinsing is repeated three times.

[0099] 4) The treated bismuth powder is placed in a vacuum drying oven for drying at a temperature of 80° C. for 6 hours. The dried bismuth powder is placed in a mixer and ground into powder.

[0100] 5) Add a propellant to the ground material for mixing. Seal the mixed material and place it at 23°C for 5 hours for aging.

[0101] 6) Remove the air from the powder after adding the extrusion auxiliary agent, and press the paste resin into a blank corresponding to the barrel of the wire pusher, pre-press the blank into shape, dry it, and sinter it.

[0102] Comparative Example 6

[0103] The invention discloses a method for treating the surface of a fluorine-containing resin catheter, comprising the following steps:

[0104] 1) Stir more than 90% of anhydrous ethanol and a silane coupling agent under sealed conditions at a stirring temperature of 25° C., a rotation speed of 50 rpm, and a time setting of 45 minutes.

[0105] The silane coupling agent used in this embodiment is KH560.

[0106] 2) adding the sieved bismuth powder to the stirred mixture of ethanol and silane coupling agent, stirring at a stirring speed of 200 rpm, a stirring temperature of 70° C., and a stirring time of 6 h;

[0107] 3) the stirred mixed solution is allowed to stand in a static crushing bottle, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the bismuth powder is ground, and the rinsing is repeated three times.

[0108] 4) The treated bismuth powder is placed in a vacuum drying oven for drying at a temperature of 80° C. for 6 hours. The dried bismuth powder is placed in a mixer and ground into powder.

[0109] 5) Add a propellant to the ground material for mixing. Seal the mixed material and place it at 23°C for 5 hours for aging.

[0110] 6) Remove the air from the powder after adding the extrusion auxiliary agent, and press the paste resin into a blank corresponding to the barrel of the wire pusher, pre-press the blank into shape, dry it, and sinter it.

[0111] The test data of Comparative Examples 1 to 6 are as follows:

[0112] Comparative Example 1: Bismuth powder was not coupled sufficiently, and agglomerates appeared after drying, and white lumps / white lines appeared on the surface of the produced tube.

[0113] Comparative Example 2: Bismuth powder was not coupled sufficiently, and agglomerates appeared after drying, and white lumps / white lines appeared on the surface of the produced tube.

[0114] Comparative Example 3: Excessive hydrolysis, the mixed solution is too viscous and cannot be stirred by adding bismuth powder.

[0115] Comparative Example 4: Bismuth powder was not coupled sufficiently, and agglomerates appeared after drying, and white lumps / white lines appeared on the surface of the produced tube.

[0116] Comparative Example 5: Excessive hydrolysis, the mixed solution is too viscous and cannot be stirred by adding bismuth powder.

[0117] Comparative Example 6: Bismuth powder was not coupled sufficiently, and agglomerates appeared after drying, and white lumps / white lines appeared on the surface of the produced tube.

[0118] In the above comparative example, the maximum tensile strength is 33 MPa and the tensile force is 141.9 N.

[0119] In Example 1: the test tube specifications used are 2.25mm inner diameter, 3.25mm outer diameter, 2.51mm outer diameter of the core rod, 3.58mm inner diameter of the die, 50mm inner diameter of the cylinder, and F-208H as the base material. The blanks are sequentially sintered in different temperature zones, and the sintering temperatures are 180°C, 240°C, 360°C, and 390°C, respectively. The main engine speed is 11m / min, the apparent color is uniform, and there is no obvious white mass / white line. The maximum tensile force is 179N, and the tensile strength is 41.6Mpa.

[0120] In Example 2: the test tube specifications used are 2.25mm inner diameter, 3.25mm outer diameter, 2.51mm outer diameter of the core rod, 3.58mm inner diameter of the die, 50mm inner diameter of the cylinder, and F-208H as the base material. The blanks are sequentially sintered in different temperature zones, and the sintering temperatures are 180°C, 240°C, 360°C, and 390°C, respectively. The main engine speed is 11m / min, the apparent color is uniform, and there is no obvious white mass / white line. The maximum tensile force is 168.56N, and the tensile strength is 39.2Mpa.

[0121] Example 3

[0122] The present invention also discloses a method for treating the surface of a fluorine-containing resin catheter, comprising the following steps:

[0123] 1) Stir more than 90% anhydrous ethanol and bismuth powder at a stirring temperature of 15° C., a rotation speed of 60 rpm, and a time setting of 30 min;

[0124] 2) adding a silane coupling agent to the stirred mixture of ethanol and bismuth powder, and stirring under a sealed condition; the stirring speed is 80 rpm, the stirring temperature is 60° C., and the time is 4 h;

[0125] 3) the stirred mixed solution is allowed to stand in a static crushing bottle, during which a heavy object is installed on the movable rod to compress the cylinder to accelerate precipitation, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the bismuth powder is ground by using the pressing tablet at the bottom of the movable rod in combination with the grinding ball, and the rinsing is repeated three times.

[0126] 4) The treated bismuth powder is placed in a vacuum drying oven for drying at a temperature of 80° C. for 4 hours. The dried bismuth powder is placed in a mixer and ground into powder.

[0127] 5) Add a propellant to the ground material for mixing. Seal the mixed material and place it at 23°C for 5 hours for aging.

[0128] 6) Remove the air from the powder after adding the extrusion auxiliary agent, and press the paste resin into a blank corresponding to the barrel of the wire pusher, pre-press the blank into shape, dry it, and sinter it.

[0129] Example 4

[0130] The present invention also discloses a method for treating the surface of a fluorine-containing resin catheter, comprising the following steps:

[0131] 1) Stir more than 90% anhydrous ethanol and bismuth powder at a stirring temperature of 35° C., a rotation speed of 130 rpm, and a time setting of 60 min;

[0132] 2) adding a silane coupling agent to the stirred mixture of ethanol and bismuth powder, and stirring under a sealed condition; the stirring speed is 180 rpm, the stirring temperature is 80° C., and the time is 8 hours;

[0133] 3) the stirred mixed solution is allowed to stand in a static crushing bottle, during which a heavy object is installed on the movable rod to compress the cylinder to accelerate precipitation, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the bismuth powder is ground by using the pressing tablet at the bottom of the movable rod in combination with the grinding ball, and the rinsing is repeated three times.

[0134] 4) The treated bismuth powder is placed in a vacuum drying oven for drying at a temperature of 140° C. for 8 hours. The dried bismuth powder is placed in a mixer and ground into powder.

[0135] 5) Add a propellant to the ground material for mixing. Seal the mixed material and place it at 27°C for 15 hours for aging.

[0136] 6) Remove the air from the powder after adding the extrusion auxiliary agent, and press the paste resin into a blank corresponding to the barrel of the wire pusher, pre-press the blank into shape, dry it, and sinter it.

[0137] Comparative Example 7:

[0138] The present invention also discloses a method for treating the surface of a fluorine-containing resin catheter, comprising the following steps:

[0139] 1) Stir more than 90% anhydrous ethanol and bismuth powder at a stirring temperature of 25° C., a rotation speed of 100 rpm, and a time setting of 2 hours;

[0140] 2) adding a silane coupling agent to the stirred mixture of ethanol and bismuth powder, and stirring under a sealed condition; the stirring temperature is 25° C., the speed is 120 rpm, and the time is set to 6 hours;

[0141] 3) the stirred mixed solution is allowed to stand in a static crushing bottle, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the rinsing is repeated three times.

[0142] 4) The treated bismuth powder is placed in a vacuum drying oven for drying at a temperature of 140° C. for 8 hours. The dried bismuth powder is placed in a mixer and ground into powder.

[0143] 5) Add a propellant to the ground material for mixing. Seal the mixed material and place it at 27°C for 15 hours for aging.

[0144] 6) Remove the air from the powder after adding the extrusion auxiliary agent, and press the paste resin into a blank corresponding to the barrel of the wire pusher, pre-press the blank into shape, dry it, and sinter it.

[0145] Comparative Example 8:

[0146] The present invention also discloses a method for treating the surface of a fluorine-containing resin catheter, comprising the following steps:

[0147] 1) Stir more than 90% anhydrous ethanol and bismuth powder at a stirring temperature of 25° C., a rotation speed of 100 rpm, and a time setting of 2 hours;

[0148] 2) adding a silane coupling agent to the stirred mixture of ethanol and bismuth powder, and stirring under a sealed condition; the stirring temperature is 70° C., the speed is 120 rpm, and the time is set to 45 min;

[0149] 3) the stirred mixed solution is allowed to stand in a static crushing bottle, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the rinsing is repeated three times.

[0150] 4) The treated bismuth powder is placed in a vacuum drying oven for drying at a temperature of 140° C. for 8 hours. The dried bismuth powder is placed in a mixer and ground into powder.

[0151] 5) Add a propellant to the ground material for mixing. Seal the mixed material and place it at 27°C for 15 hours for aging.

[0152] 6) Remove the air from the powder after adding the extrusion auxiliary agent, and press the paste resin into a blank corresponding to the barrel of the wire pusher, pre-press the blank into shape, dry it, and sinter it.

[0153] Comparative Example 9:

[0154] The present invention also discloses a method for treating the surface of a fluorine-containing resin catheter, comprising the following steps:

[0155] 1) Stir more than 90% anhydrous ethanol and bismuth powder at a stirring temperature of 25° C., a rotation speed of 100 rpm, and a time setting of 45 minutes;

[0156] 2) adding a silane coupling agent to the stirred mixture of ethanol and bismuth powder, and stirring under a sealed condition; the stirring temperature is 25° C., the speed is 120 rpm, and the time is set to 6 hours;

[0157] 3) the stirred mixed solution is allowed to stand in a static crushing bottle, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the rinsing is repeated three times.

[0158] 4) The treated bismuth powder is placed in a vacuum drying oven for drying at a temperature of 140° C. for 8 hours. The dried bismuth powder is placed in a mixer and ground into powder.

[0159] 5) Add a propellant to the ground material for mixing. Seal the mixed material and place it at 27°C for 15 hours for aging.

[0160] 6) Remove the air from the powder after adding the extrusion auxiliary agent, and press the paste resin into a blank corresponding to the barrel of the wire pusher, pre-press the blank into shape, dry it, and sinter it.

[0161] Comparative Example 10:

[0162] The present invention also discloses a method for treating the surface of a fluorine-containing resin catheter, comprising the following steps:

[0163] 1) Stir more than 90% anhydrous ethanol and bismuth powder at a stirring temperature of 25° C., a rotation speed of 50 rpm, and a time setting of 2 h;

[0164] 2) adding a silane coupling agent to the stirred mixture of ethanol and bismuth powder, and stirring under a sealed condition; the stirring temperature is 70° C., the speed is 120 rpm, and the time is set to 6 hours;

[0165] 3) the stirred mixed solution is allowed to stand in a static crushing bottle, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the rinsing is repeated three times.

[0166] 4) The treated bismuth powder is placed in a vacuum drying oven for drying at a temperature of 140° C. for 8 hours. The dried bismuth powder is placed in a mixer and ground into powder.

[0167] 5) Add a propellant to the ground material for mixing. Seal the mixed material and place it at 27°C for 15 hours for aging.

[0168] 6) Remove the air from the powder after adding the extrusion auxiliary agent, and press the paste resin into a blank corresponding to the barrel of the wire pusher, pre-press the blank into shape, dry it, and sinter it.

[0169] Comparative Example 11:

[0170] The present invention also discloses a method for treating the surface of a fluorine-containing resin catheter, comprising the following steps:

[0171] 1) Stir more than 90% anhydrous ethanol and bismuth powder at a stirring temperature of 25° C., a rotation speed of 200 rpm, and a time setting of 2 hours;

[0172] 2) adding a silane coupling agent to the stirred mixture of ethanol and bismuth powder, and stirring under a sealed condition; the stirring temperature is 70° C., the speed is 120 rpm, and the time is set to 6 hours;

[0173] 3) the stirred mixed solution is allowed to stand in a static crushing bottle, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the rinsing is repeated three times.

[0174] 4) The treated bismuth powder is placed in a vacuum drying oven for drying at a temperature of 140° C. for 8 hours. The dried bismuth powder is placed in a mixer and ground into powder.

[0175] 5) Add a propellant to the ground material for mixing. Seal the mixed material and place it at 27°C for 15 hours for aging.

[0176] 6) Remove the air from the powder after adding the extrusion auxiliary agent, and press the paste resin into a blank corresponding to the barrel of the wire pusher, pre-press the blank into shape, dry it, and sinter it.

[0177] Comparative Example 12:

[0178] The present invention also discloses a method for treating the surface of a fluorine-containing resin catheter, comprising the following steps:

[0179] 1) Stir more than 90% anhydrous ethanol and bismuth powder at a stirring temperature of 25° C., a rotation speed of 50 rpm, and a time setting of 2 h;

[0180] 2) adding a silane coupling agent to the stirred mixture of ethanol and bismuth powder, and stirring under a sealed condition; the stirring temperature is 70° C., the speed is 200 rpm, and the time is set to 6 hours;

[0181] 3) the stirred mixed solution is allowed to stand in a static crushing bottle, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the rinsing is repeated three times.

[0182] 4) The treated bismuth powder is placed in a vacuum drying oven for drying at a temperature of 140° C. for 8 hours. The dried bismuth powder is placed in a mixer and ground into powder.

[0183] 5) Add a propellant to the ground material for mixing. Seal the mixed material and place it at 27°C for 15 hours for aging.

[0184] 6) Remove the air from the powder after adding the extrusion auxiliary agent, and press the paste resin into a blank corresponding to the barrel of the wire pusher, pre-press the blank into shape, dry it, and sinter it.

[0185] The test data of Comparative Examples 7 to 12 are as follows:

[0186] Comparative Example 1: Bismuth powder was not coupled sufficiently, and agglomerates appeared after drying, and white lumps / white lines appeared on the surface of the produced tube.

[0187] Comparative Example 2: Bismuth powder was not coupled sufficiently, and agglomerates appeared after drying, and white lumps / white lines appeared on the surface of the produced tube.

[0188] Comparative Example 3: Bismuth powder was not coupled sufficiently, and agglomerates appeared after drying, and white lumps / white lines appeared on the surface of the produced tube.

[0189] Comparative Example 4: Bismuth powder was not coupled sufficiently, and agglomerates appeared after drying, and white lumps / white lines appeared on the surface of the produced tube.

[0190] Comparative Example 5: Bismuth powder is easily splashed on the bottle wall, causing waste.

[0191] Comparative Example 6: Bismuth powder is easily splashed on the bottle wall, causing waste.

[0192] In the above comparative example, the maximum tensile strength is 32.5 MPa and the tensile force is 139.75 N.

[0193] In Example 1: the test tube specifications used are 2.25mm inner diameter, 3.25mm outer diameter, 2.51mm outer diameter of the core rod, 3.58mm inner diameter of the die, 50mm inner diameter of the cylinder, and F-208H as the base material. The blanks are sequentially sintered in different temperature zones, and the sintering temperatures are 180°C, 240°C, 360°C, and 390°C, respectively. The main engine speed is 11m / min, the apparent color is uniform, and there is no obvious white mass / white line. The maximum tensile force is 179N, and the tensile strength is 41.6Mpa.

[0194] In Example 2: the test tube specifications used are 2.25mm inner diameter, 3.25mm outer diameter, 2.51mm outer diameter of the core rod, 3.58mm inner diameter of the die, 50mm inner diameter of the cylinder, and F-208H as the base material. The blanks are sequentially sintered in different temperature zones, and the sintering temperatures are 180°C, 240°C, 360°C, and 390°C, respectively. The main engine speed is 11m / min, the apparent color is uniform, and there is no obvious white mass / white line. The maximum tensile force is 168.56N, and the tensile strength is 39.2Mpa.

[0195] Example 5

[0196] like Figure 1 , Figure 2 and Figure 3 As shown, the static crushing bottle in the present invention includes a spherical bottle body 1 with a flat bottom, a tube body 2 connected to the spherical bottle body and a cylinder body 3 inserted into the tube body of the spherical bottle body, and the flat bottom of the spherical bottle body is a frosted structure. A detachable connecting cylinder 4 is installed at the bottom of the cylinder body, and a filter capsule 5 made of flexible filter material is fixedly connected to the bottom of the connecting cylinder, and a plurality of grinding balls 6 are fixedly installed on the filter capsule; a movable rod 7 is inserted into the cylinder body, and a grinding sheet 8 is provided at the bottom of the movable rod, and the bottom surface of the grinding sheet is a frosted structure, and the periphery of the grinding sheet is an elastic sealing ring 9. The surface of the frosted ball located on the inner side of the filter capsule is provided with an arc-shaped stirring arc plate 10, and the diameter of the stirring arc plate gradually converges from the bottom to the top. A limiting ring 11 is provided at the top of the connecting cylinder, and limiting parts 12 are provided at both ends of the limiting ring.

[0197] At least a plurality of grinding balls are evenly distributed around the filter capsule to form an annular structure, and the center lines of the abdomens of the stirring arc plates in the annular structure are all arranged clockwise.

[0198] In this embodiment, the connecting cylinder can be connected to the cylinder body through a threaded structure or a snap-fit ​​structure.

[0199] In this embodiment, the spherical bottle body, the tube body and the cylinder body are all made of glass.

[0200] During the implementation of this embodiment, the stirred mixed liquid is allowed to stand still in a static crushing bottle, during which a heavy object is installed on the movable rod to compress the cylinder to accelerate precipitation. After the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle using anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, during which the pressing tablet at the bottom of the movable rod is used in conjunction with the grinding ball to grind the bismuth powder, and the rinsing is repeated three times; the pressing tablet at the bottom of the movable rod is used in conjunction with the grinding ball and the frosted surface at the bottom of the bottle body to grind the bismuth powder, which utilizes stirring to grind the bismuth powder to avoid bismuth powder agglomeration affecting the drying efficiency, thereby reducing the time for the subsequent drying of the bismuth powder in the mixer.

[0201] On the one hand, the stirring arc plate stirs the bismuth powder to promote the washing away of the silane coupling agent remaining on the bismuth powder, thereby improving the cleaning efficiency. On the other hand, the stirring arc plate also loosens the bismuth powder, and the liquid flows out of the filter capsule at a rapid speed in the spiral downward direction, thereby improving the cleaning efficiency.

[0202] The above description is only a preferred embodiment of the present invention, and does not limit the patent protection scope of the present invention. Any equivalent structural transformation made by using the contents of the present invention and the drawings, directly or indirectly used in other related technical fields, is also included in the protection scope of the present invention.

Claims

1. A method for treating the surface of a fluorine-containing resin catheter, characterized in that: The following steps are involved: 1) Stir more than 90% of anhydrous ethanol and silane coupling agent under sealed conditions at a stirring temperature of 15-35° C.; 2) adding the sieved bismuth powder to the stirred mixture of ethanol and silane coupling agent, and stirring; 3) the stirred mixed solution is allowed to stand in a static crushing bottle, during which a heavy object is installed on the movable rod to compress the cylinder to accelerate precipitation, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the bismuth powder is ground by using the pressing tablet at the bottom of the movable rod in combination with the grinding ball, and the rinsing is repeated three times.

2. A fluorine-containing resin catheter surface treatment method as claimed in claim 1, characterized in that: In step 2), the stirring speed is 80-180 rpm, the stirring temperature is set to 60-80° C., and the time is 4-8 hours.

3. A method for treating the surface of a fluorine-containing resin catheter as claimed in claim 1 or 2, characterized in that: The bismuth powder treated in step 3) is placed in a vacuum drying oven for drying at a temperature of 80-140° C. for 4-8 hours.

4. A method for treating the surface of a fluorine-containing resin catheter as claimed in claim 3, characterized in that: The dried bismuth powder is put into a mixer and ground into powder.

5. A fluorine-containing resin catheter surface treatment method as claimed in claim 4, characterized in that: A propellant is added to the ground material for mixing.

6. A method for treating the surface of a fluorine-containing resin catheter as claimed in claim 5, characterized in that: The mixed materials are sealed and left to stand at 23-27°C for 5-15 hours for aging.

7. A method for treating the surface of a fluorine-containing resin catheter as claimed in claim 6, characterized in that: The air in the powder after the extrusion auxiliary agent is added to the matured material is removed, and the paste resin is pressed into a blank corresponding to the barrel of the wire pusher, and the blank is pre-pressed, dried and sintered.

8. A method for treating the surface of a fluorine-containing resin catheter as claimed in claim 4, characterized in that: The rotation speed in step 1) is 60-130 rpm, and the time is set to 30-60 min.

9. A method for treating the surface of a fluorine-containing resin catheter as claimed in claim 1 or 2, characterized in that: The silane coupling agent includes one or more of KH550, KH560 and KH570.

10. A method for treating the surface of a fluorine-containing resin catheter, characterized in that: The following steps are involved: 1) Stir more than 90% anhydrous ethanol and bismuth powder at a stirring temperature of 15-35° C., a rotation speed of 60-130 rpm, and a time setting of 30-60 min; 2) adding a silane coupling agent to the stirred mixture of ethanol and bismuth powder, stirring under sealed conditions, with a stirring speed of 80-180 rpm, a stirring temperature of 60-80° C., and a time of 4-8 h; 3) the stirred mixed solution is allowed to stand in a static crushing bottle, during which a heavy object is installed on the movable rod to compress the cylinder to accelerate precipitation, and after the bismuth powder is precipitated, the solid and liquid are separated; the separated bismuth powder is injected into the static crushing bottle with anhydrous ethanol to rinse off the silane coupling agent remaining on the bismuth powder, and the bismuth powder is ground by using the pressing tablet at the bottom of the movable rod in combination with the grinding ball, and the rinsing is repeated three times.

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