Preparation method of medical PTFE etched tube

Through the preparation method of PTFE etching tubes using ultrasonic cleaning and plasma surface activation treatment in medical device manufacturing, the problem of insufficient surface adhesion performance of PTFE materials is solved, and the effect of improving the surface adhesion performance and interface properties of PTFE pipes is achieved, and the medical device is satisfied High precision and biocompatibility requirements.

CN119408001APending Publication Date: 2025-02-11XIANJU ECO ADVANCED MATERIAL TECHNOLOGY CO LTD +2
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Patent Information

Application Number
CN202411397837.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-09
Publication Date
2025-02-11

AI Technical Summary

Technical Problem

In medical device manufacturing, the low surface energy of PTFE materials makes it difficult for its surface to form effective adhesion to other materials, limiting its application in coating, bonding or coating processes.

Method used

Using a preparation method of medical PTFE etching tube, ultrasonic cleaning and plasma surface activation treatment, followed by etching using sodium naphthalene etching solution in the etching tank, etching stabilizer is added during the etching process to improve stability, and through multi-stage Pure water rinsing and clean hot air drying ensure surface cleanliness.

Benefits of technology

It significantly improves the surface adhesion performance of PTFE pipes, enhances the interface properties with other materials, reduces surface tension, improves the corrosion resistance and oxidation resistance of the materials, and meets the high precision, cleanliness and biological phase of medical devices. Capacitive requirements.

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Abstract

The invention discloses a preparation method of a medical PTFE etched tube, and relates to the technical field of medical apparatus and instrument manufacturing. The method comprises the following steps: firstly, drying a pipe through an ultrasonic cleaning and drying machine; then plasma surface activation treatment is carried out to enhance the surface performance, and then etching is carried out under the assistance of a rotary conveying device to ensure uniformity; and finally, through multi-stage pure water rinsing and clean hot air drying, it is ensured that the surface of the pipe is clean and free of impurities. According to the method, the interface property of the material is improved, the surface tension is reduced, and the corrosion resistance and oxidation resistance of the material are improved.
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Description

Technical Field

[0001] The invention relates to the technical field of medical device manufacturing, in particular to a method for preparing a medical PTFE etching tube. Background Art

[0002] As a high-performance engineering plastic, polytetrafluoroethylene (PTFE) is widely used in various industrial and medical fields due to its excellent chemical inertness, excellent electrical insulation performance, low friction coefficient, high temperature resistance and excellent biocompatibility. In the field of medical devices, PTFE materials have become an important material for manufacturing medical devices such as catheters, endoscope insertion tubes, cardiovascular devices, and surgical suture coverings due to their biocompatibility and chemical corrosion resistance.

[0003] During the application process, PTFE material exhibits extremely low surface energy, which makes it difficult for its surface to form effective adhesion with other materials. Although this characteristic can avoid friction and adhesion problems between materials in some application scenarios, in other application scenarios, especially when the PTFE surface needs to be coated, bonded or painted, low surface energy becomes a significant technical obstacle. In the manufacturing process of medical devices, the surface of the device usually needs to be combined with other biocompatible materials. For example, when coating a drug coating on the surface of a catheter or bonding components of different materials in a medical device, it is necessary to ensure that the adhesion of the PTFE surface is strong enough.

[0004] In order to solve the above problems, etching the surface of PTFE has become a common and effective means. Through etching, the surface structure of PTFE can be changed, the surface roughness and chemical activity can be increased, thereby significantly improving its adhesion to other materials. At present, the commonly used PTFE etching methods in industry mainly include chemical etching, plasma etching and laser etching. For example, the patent document: polytetrafluoroethylene tube and medical tube using the polytetrafluoroethylene tube (application number: JP2022081112) provides a thin-walled PTFE tube with moderate stretchability and sufficient strength, and good uniformity during stretching, and provides a medical tube with excellent softness and dimensional accuracy. These methods have a wide range of applications in the industrial field and can achieve mass production. However, in the manufacture of medical devices, these industrial-grade etching methods often face the following problems: accuracy requirements, cleanliness requirements, biocompatibility requirements, and consistency and repeatability.

[0005] Therefore, in view of the special requirements in the field of medical devices, it is urgent to develop a method for preparing PTFE etching tubes specifically for medical use. The method should meet medical standards in terms of etching accuracy, surface cleanliness, biocompatibility and production consistency, ensure that no harmful substances are introduced during the preparation process, and the etching effect is uniform and consistent. In addition, in order to adapt to the increasingly stringent regulations and standards in the medical device industry, the method should also have a high degree of controllability and repeatability to ensure the safety and reliability of the final product. Through such a preparation method, the application value of PTFE etching tubes in medical devices can be greatly improved, providing technical support for the development of safer and more efficient medical devices. Summary of the invention

[0006] The present invention provides a method for preparing a medical PTFE etching tube to solve at least one technical problem in the above-mentioned background technology.

[0007] In order to solve the above technical problems, the embodiments of the present invention disclose the following technical solutions:

[0008] A method for preparing a medical PTFE etched tube, the operating steps of which are:

[0009] S1: Pull the PTFE tube into the cleaning tank for ultrasonic cleaning, then pull it into the dryer and dry it with a clean air drying device at a drying temperature of 45-60°C;

[0010] S2: The dried PTFE tube is subjected to plasma surface activation treatment and then passed into an etching tank for etching. During the etching process, a rotating conveyor is used to ensure that the surface of the PTFE tube is evenly etched, and the etching time is controlled within 2-5 minutes;

[0011] S3: The etched PTFE pipe passes through a multi-stage pure water rinse tank in turn to remove the etching solution and other impurities remaining on the surface. The pipe is then dried using a clean hot air drying device. The drying process needs to be carried out in a clean room to ensure the cleanliness of the pipe surface.

[0012] A further technical solution is that the cleaning tank contains a mixed solution of anhydrous ethanol and deionized water, with a mass ratio of 1:0.8-1.1.

[0013] A further technical solution is that the temperature of the cleaning tank is controlled at 40-50° C. and the cleaning time is 10-15 minutes.

[0014] A further technical solution is that the plasma surface activation treatment parameters are: plasma treatment power is 80-200W, and frequency is 13.56MHz.

[0015] A further technical solution is that the etching solution in the etching tank is sodium naphthalene etching solution.

[0016] A further technical solution is that an etching stabilizer is added to the etching solution, and the added amount is 2-5% of the total amount of the etching solution.

[0017] A further technical solution is that the etching stabilizer preparation method is:

[0018] K1: By weight, 18-32 parts of 5-fluoro-1-naphthylamine, 5-10 parts of O,O-dimethylphosphoryl chloride, 0.05-0.5 parts of aluminum chloride, and 200-300 parts of DMF are placed in a stirring tank, the reaction temperature is controlled at 60-80°C, and the reaction time is 3-12 hours;

[0019] K2: Add 0.03-0.8 parts of acrylic-cage polysilsesquioxane (CAS: 1620202-27-8) and 2-5 parts of triethylamine, stir and react at 60-80° C. for 1-4 hours, and distill off DMF to obtain an etching stabilizer.

[0020] A further technical solution is that the temperature of the rinsing water is controlled between 20-30° C. and the rinsing time is 5-10 minutes.

[0021] A further technical solution is that the rinsing water is high-purity water with a resistivity of ≥15MΩ·cm.

[0022] A further technical solution is that the drying temperature is controlled between 60-80° C. and the drying time is 10-15 minutes.

[0023] Stabilizer synthesis reaction mechanism:

[0024] The reaction process includes two main stages: first, 5-fluoro-1-naphthylamine undergoes an acylation reaction with O,O-dimethylphosphoryl chloride to generate phosphoryl ester 5-fluoro-1-naphthylamine; then, the amino group in the product undergoes an addition reaction with acrylic acid-cage polysilsesquioxane.

[0025] 1. Acylation reaction mechanism:

[0026] 5-Fluoro-1-naphthylamine acts as a nucleophile, and its amino nitrogen (with a lone pair of electrons) initiates a nucleophilic attack on the phosphoryl group in O,O-dimethylphosphoryl chloride. This nucleophilic attack results in the attack of the carbonyl carbon in O,O-dimethylphosphoryl chloride, followed by the formation of an intermediate containing a four-coordinated phosphorus intermediate and a good leaving group (i.e., chloride ion). By eliminating the chloride ion, the phosphoryl ester 5-fluoro-1-naphthylamine is formed. This step involves the formation of a P=O bond, which is a relatively stable structure because the phosphoryl group has a strong electron-withdrawing ability that can stabilize the adjacent nitrogen anion.

[0027] 2. Amino addition reaction mechanism:

[0028] In the second stage, the amino group of the newly formed phosphoryl ester 5-fluoro-1-naphthylamine again acts as a nucleophile to attack the acrylate double bond in the acrylic-cage polysilsesquioxane. This process follows the Michael addition reaction mechanism to form a stable addition product.

[0029] Technical effect:

[0030] Compared with traditional methods, this method has the following advantages:

[0031] 1. Improve stability:

[0032] Through these chemical modifications, especially the introduction of phosphoryl ester groups and cage-shaped polysilsesquioxanes, the stability of fluoronaphthalene can be significantly enhanced. This stability mainly comes from the amphiphilic cage structure and the electron-attracting ability of the phosphoryl group, which work together to slow down the invasion of chemical forces.

[0033] 2. Slow down the decomposition rate:

[0034] During the etching process, sodium naphthalene usually encounters the problem of rapid decomposition. Modified fluoronaphthalene, as a stabilizing agent for etching treatment agents, can effectively slow down this decomposition process and improve treatment efficiency and safety.

[0035] 3. Improve interface properties:

[0036] The introduction of phosphoester groups improves the interfacial properties of the material, such as reducing surface tension and enhancing the overall corrosion resistance, oxidation resistance and stability of the material. DETAILED DESCRIPTION

[0037] The technical solution of the present invention is further described below by specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0038] Interface property test

[0039] Test method: Use a contact angle meter to test the water contact angle of etched PTFE pipes to evaluate changes in surface tension. Select PTFE pipe samples before and after etching, measure the contact angle of water droplets on their surfaces, and compare and analyze.

[0040] Example 1

[0041] A method for preparing a medical PTFE etched tube, the operating steps of which are:

[0042] S1: The PTFE tube is pulled into a cleaning tank for ultrasonic cleaning, and then pulled into a dryer for drying by a clean air drying device at a drying temperature of 45°C;

[0043] S2: The dried PTFE tube is subjected to plasma surface activation treatment and then passed into an etching tank for etching. During the etching process, a rotating conveyor is used to ensure that the surface of the PTFE tube is etched evenly, and the etching time is controlled within 2 minutes;

[0044] S3: The etched PTFE pipe passes through a multi-stage pure water rinse tank in turn to remove the etching solution and other impurities remaining on the surface. The pipe is then dried using a clean hot air drying device. The drying process needs to be carried out in a clean room to ensure the cleanliness of the pipe surface.

[0045] The cleaning tank contains a mixed solution of anhydrous ethanol and deionized water, with a mass ratio of 1:0.8.

[0046] The temperature of the cleaning tank was controlled at 40°C and the cleaning time was 10 minutes.

[0047] The plasma surface activation treatment parameters are: plasma treatment power is 80W, and frequency is 13.56MHz.

[0048] The etching solution in the etching tank is selected from sodium naphthalene etching solution.

[0049] The etching stabilizer is added to the etching solution in an amount of 2% of the total amount of the etching solution. The preparation method is as follows:

[0050] K1: 18 g 5-fluoro-1-naphthylamine, 5 g O,O-dimethylphosphoryl chloride, 0.05 g aluminum chloride, and 200 g DMF were placed in a stirred tank, the reaction temperature was controlled at 60° C., and the reaction time was 3 hours;

[0051] K2: Add 0.03 g of acrylic acid-cage polysilsesquioxane (CAS: 1620202-27-8) and 2 g of triethylamine, stir and react at 60° C. for 1 hour, and distill off DMF to obtain an etching stabilizer.

[0052] The rinsing water temperature was controlled at 20° C. and the rinsing time was 5 minutes.

[0053] The rinsing water is high-purity water with a resistivity of ≥15MΩ·cm.

[0054] The drying temperature was controlled at 60° C. and the drying time was 10 minutes.

[0055] The water contact angle of the PTFE etched tube prepared in this example was measured by a contact angle meter and was 88°.

[0056] Example 2

[0057] A method for preparing a medical PTFE etched tube, the operating steps of which are:

[0058] S1: The PTFE tube is pulled into a cleaning tank for ultrasonic cleaning, and then pulled into a dryer for drying by a clean air drying device at a drying temperature of 50°C;

[0059] S2: The dried PTFE tube is subjected to plasma surface activation treatment and then passed into an etching tank for etching. During the etching process, a rotating conveyor is used to ensure that the surface of the PTFE tube is etched evenly, and the etching time is controlled within 3 minutes;

[0060] S3: The etched PTFE pipe passes through a multi-stage pure water rinse tank in turn to remove the etching solution and other impurities remaining on the surface. The pipe is then dried using a clean hot air drying device. The drying process needs to be carried out in a clean room to ensure the cleanliness of the pipe surface.

[0061] The cleaning tank contains a mixed solution of anhydrous ethanol and deionized water, with a mass ratio of 1:0.9.

[0062] The temperature of the cleaning tank was controlled at 45°C and the cleaning time was 12 minutes.

[0063] The plasma surface activation treatment parameters are: plasma treatment power is 120W, and frequency is 13.56MHz.

[0064] The etching solution in the etching tank is selected from sodium naphthalene etching solution.

[0065] The etching stabilizer is added to the etching solution in an amount of 3% of the total amount of the etching solution. The preparation method is as follows:

[0066] K1: 24 g of 5-fluoro-1-naphthylamine, 7 g of O,O-dimethylphosphoryl chloride, 0.2 g of aluminum chloride, and 235 g of DMF were placed in a stirred tank, the reaction temperature was controlled at 70° C., and the reaction time was 6 hours;

[0067] K2: Add 0.3 g of acrylic-cage polysilsesquioxane (CAS: 1620202-27-8) and 3 g of triethylamine, stir and react at 70° C. for 2 hours, and distill off DMF to obtain an etching stabilizer.

[0068] The rinsing water temperature was controlled at 25° C., and the rinsing time was 7 minutes.

[0069] The rinsing water is high-purity water with a resistivity of ≥15MΩ·cm.

[0070] The drying temperature was controlled at 70° C. and the drying time was 12 minutes.

[0071] The water contact angle of the PTFE etched tube prepared in this example was measured by a contact angle meter and was 84°.

[0072] Example 3

[0073] A method for preparing a medical PTFE etched tube, the operating steps of which are:

[0074] S1: The PTFE tube is pulled into a cleaning tank for ultrasonic cleaning, and then pulled into a dryer for drying by a clean air drying device at a drying temperature of 55°C;

[0075] S2: The dried PTFE tube is subjected to plasma surface activation treatment and then passed into an etching tank for etching. During the etching process, a rotating conveyor is used to ensure that the surface of the PTFE tube is etched evenly, and the etching time is controlled within 4 minutes;

[0076] S3: The etched PTFE pipe passes through a multi-stage pure water rinse tank in turn to remove the etching solution and other impurities remaining on the surface. The pipe is then dried using a clean hot air drying device. The drying process needs to be carried out in a clean room to ensure the cleanliness of the pipe surface.

[0077] The cleaning tank contains a mixed solution of anhydrous ethanol and deionized water in a mass ratio of 1:1.

[0078] The temperature of the cleaning tank was controlled at 45°C and the cleaning time was 13.5 minutes.

[0079] The plasma surface activation treatment parameters are: plasma treatment power is 150W, and frequency is 13.56MHz.

[0080] The etching solution in the etching tank is selected from sodium naphthalene etching solution.

[0081] The etching stabilizer is added to the etching solution in an amount of 4% of the total amount of the etching solution. The preparation method is as follows:

[0082] K1: 28 g of 5-fluoro-1-naphthylamine, 8.5 g of O,O-dimethylphosphoryl chloride, 0.35 g of aluminum chloride, and 285 g of DMF were placed in a stirred tank, the reaction temperature was controlled at 70° C., and the reaction time was 10 hours;

[0083] K2: Add 0.6 g of acrylic acid-cage polysilsesquioxane (CAS: 1620202-27-8) and 4 g of triethylamine, stir and react at 75° C. for 3 hours, and distill off DMF to obtain an etching stabilizer.

[0084] The rinsing water temperature was controlled at 25° C., and the rinsing time was 8 minutes.

[0085] The rinsing water is high-purity water with a resistivity of ≥15 MΩ·cm.

[0086] The drying temperature was controlled at 70° C. and the drying time was 13 minutes.

[0087] The water contact angle of the PTFE etched tube prepared in this example was measured by a contact angle meter and was 85°.

[0088] Example 4

[0089] A method for preparing a medical PTFE etched tube, the operating steps of which are:

[0090] S1: The PTFE tube is pulled into a cleaning tank for ultrasonic cleaning, and then pulled into a dryer for drying by a clean air drying device at a drying temperature of 60°C;

[0091] S2: The dried PTFE tube is subjected to plasma surface activation treatment and then passed into an etching tank for etching. During the etching process, a rotating conveyor is used to ensure that the surface of the PTFE tube is etched evenly, and the etching time is controlled within 5 minutes;

[0092] S3: The etched PTFE pipe passes through a multi-stage pure water rinse tank in turn to remove the etching solution and other impurities remaining on the surface. The pipe is then dried using a clean hot air drying device. The drying process needs to be carried out in a clean room to ensure the cleanliness of the pipe surface.

[0093] The cleaning tank contains a mixed solution of anhydrous ethanol and deionized water, with a mass ratio of 1:1.1.

[0094] The temperature of the cleaning tank was controlled at 50°C and the cleaning time was 15 minutes.

[0095] The plasma surface activation treatment parameters are: plasma treatment power is 200W, and frequency is 13.56MHz.

[0096] The etching solution in the etching tank is selected from sodium naphthalene etching solution.

[0097] The etching stabilizer is added to the etching solution in an amount of 5% of the total amount of the etching solution. The preparation method is as follows:

[0098] K1: 32 g of 5-fluoro-1-naphthylamine, 10 g of O,O-dimethylphosphoryl chloride, 0.5 g of aluminum chloride, and 300 g of DMF were placed in a stirred tank, the reaction temperature was controlled at 80° C., and the reaction time was 12 hours;

[0099] K2: Add 0.8 g of acrylic acid-cage polysilsesquioxane (CAS: 1620202-27-8) and 5 g of triethylamine, stir and react at 80° C. for 4 hours, and distill off DMF to obtain an etching stabilizer.

[0100] The rinsing water temperature was controlled at 30° C., and the rinsing time was 10 minutes.

[0101] The rinsing water is high-purity water with a resistivity of ≥15 MΩ·cm.

[0102] The drying temperature is controlled at 80° C. and the drying time is 15 minutes.

[0103] The water contact angle of the PTFE etched tube prepared in this example was measured by a contact angle meter and was 82°.

[0104] Comparative Example 1

[0105] A method for preparing a medical PTFE etched tube, the operating steps of which are:

[0106] S1: The PTFE tube is pulled into a cleaning tank for ultrasonic cleaning, and then pulled into a dryer for drying by a clean air drying device at a drying temperature of 45°C;

[0107] S2: The dried PTFE tube is subjected to plasma surface activation treatment and then passed into an etching tank for etching. During the etching process, a rotating conveyor is used to ensure that the surface of the PTFE tube is etched evenly, and the etching time is controlled within 2 minutes;

[0108] S3: The etched PTFE pipe passes through a multi-stage pure water rinse tank in turn to remove the etching solution and other impurities remaining on the surface. The pipe is then dried using a clean hot air drying device. The drying process needs to be carried out in a clean room to ensure the cleanliness of the pipe surface.

[0109] The cleaning tank contains a mixed solution of anhydrous ethanol and deionized water, with a mass ratio of 1:0.8.

[0110] The temperature of the cleaning tank was controlled at 40°C and the cleaning time was 10 minutes.

[0111] The plasma surface activation treatment parameters are: plasma treatment power is 80W, and frequency is 13.56MHz.

[0112] The etching solution in the etching tank is selected from sodium naphthalene etching solution.

[0113] The rinsing water temperature was controlled at 20° C. and the rinsing time was 5 minutes.

[0114] The rinsing water is high-purity water with a resistivity of ≥15 MΩ·cm.

[0115] The drying temperature was controlled at 60° C. and the drying time was 10 minutes.

[0116] The water contact angle of the PTFE etched tube prepared in this example was measured by a contact angle meter and was 108°.

[0117] Comparative Example 2

[0118] A method for preparing a medical PTFE etched tube, the operating steps of which are:

[0119] S1: The PTFE tube is pulled into a cleaning tank for ultrasonic cleaning, and then pulled into a dryer for drying by a clean air drying device at a drying temperature of 45°C;

[0120] S2: The dried PTFE tube is subjected to plasma surface activation treatment and then passed into an etching tank for etching. During the etching process, a rotating conveyor is used to ensure that the surface of the PTFE tube is etched evenly, and the etching time is controlled within 2 minutes;

[0121] S3: The etched PTFE pipe passes through a multi-stage pure water rinse tank in turn to remove the etching solution and other impurities remaining on the surface. The pipe is then dried using a clean hot air drying device. The drying process needs to be carried out in a clean room to ensure the cleanliness of the pipe surface.

[0122] The cleaning tank contains a mixed solution of anhydrous ethanol and deionized water, with a mass ratio of 1:0.8.

[0123] The temperature of the cleaning tank was controlled at 40°C and the cleaning time was 10 minutes.

[0124] The plasma surface activation treatment parameters are: plasma treatment power is 80W, and frequency is 13.56MHz.

[0125] The etching solution in the etching tank is selected from sodium naphthalene etching solution.

[0126] The etching stabilizer is added to the etching solution in an amount of 2% of the total amount of the etching solution. The preparation method is as follows:

[0127] K1: 18 g of 5-fluoro-1-naphthylamine, 0.05 g of aluminum chloride, and 200 g of DMF were placed in a stirred tank, the reaction temperature was controlled at 60° C., and the reaction time was 3 hours;

[0128] K2: Add 0.03 g of acrylic acid-cage polysilsesquioxane (CAS: 1620202-27-8) and 2 g of triethylamine, stir and react at 60° C. for 1 hour, and distill off DMF to obtain an etching stabilizer.

[0129] The rinsing water temperature was controlled at 20° C. and the rinsing time was 5 minutes.

[0130] The rinsing water is high-purity water with a resistivity of ≥15MΩ·cm.

[0131] The drying temperature was controlled at 60° C. and the drying time was 10 minutes.

[0132] The water contact angle of the PTFE etched tube prepared in this example was measured by a contact angle meter and was 94°.

[0133] Comparative Example 3

[0134] A method for preparing a medical PTFE etched tube, the operating steps of which are:

[0135] S1: The PTFE tube is pulled into a cleaning tank for ultrasonic cleaning, and then pulled into a dryer for drying by a clean air drying device at a drying temperature of 45°C;

[0136] S2: The dried PTFE tube is subjected to plasma surface activation treatment and then passed into an etching tank for etching. During the etching process, a rotating conveyor is used to ensure that the surface of the PTFE tube is etched evenly, and the etching time is controlled within 2 minutes;

[0137] S3: The etched PTFE pipe passes through a multi-stage pure water rinse tank in turn to remove the etching solution and other impurities remaining on the surface. The pipe is then dried using a clean hot air drying device. The drying process needs to be carried out in a clean room to ensure the cleanliness of the pipe surface.

[0138] The cleaning tank contains a mixed solution of anhydrous ethanol and deionized water, with a mass ratio of 1:0.8.

[0139] The temperature of the cleaning tank was controlled at 40°C and the cleaning time was 10 minutes.

[0140] The plasma surface activation treatment parameters are: plasma treatment power is 80W, and frequency is 13.56MHz.

[0141] The etching solution in the etching tank is selected from sodium naphthalene etching solution.

[0142] The etching stabilizer is added to the etching solution in an amount of 2% of the total amount of the etching solution. The preparation method is as follows:

[0143] K1: 18 g 5-fluoro-1-naphthylamine, 5 g O,O-dimethylphosphoryl chloride, 0.05 g aluminum chloride, and 200 g DMF were placed in a stirred tank, the reaction temperature was controlled at 60° C., and the reaction time was 3 hours;

[0144] K2: Add 2 g of triethylamine, stir and react at 60° C. for 1 hour, and distill off DMF to obtain an etching stabilizer.

[0145] The rinsing water temperature was controlled at 20° C. and the rinsing time was 5 minutes.

[0146] The rinsing water is high-purity water with a resistivity of ≥15 MΩ·cm.

[0147] The drying temperature was controlled at 60° C. and the drying time was 10 minutes.

[0148] The water contact angle of the PTFE etched tube prepared in this example was measured by a contact angle meter and was 98°.

[0149] The above specific implementation scheme and corresponding test results indicate that the modified etching solution by introducing phosphoryl ester groups significantly improves the interfacial properties of the material, reduces the surface tension, improves the corrosion resistance and oxidation resistance of the material, and significantly improves the overall performance of the PTFE pipe.

[0150] The applicant declares that the present invention is further illustrated by the above embodiments, but the present invention is not limited to the above embodiments, that is, it does not mean that the present invention must rely on the above embodiments to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of various raw materials of the product of the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims

1. A method for preparing a medical PTFE etching tube, the operating steps of which are: S1: Pull the PTFE tube into the cleaning tank for ultrasonic cleaning, then pull it into the dryer and dry it with a clean air drying device at a drying temperature of 45-60°C; S2: The dried PTFE tube is subjected to plasma surface activation treatment and then passed into an etching tank for etching. During the etching process, a rotating conveyor is used to ensure that the surface of the PTFE tube is evenly etched, and the etching time is controlled within 2-5 minutes; S3: The etched PTFE pipe passes through a multi-stage pure water rinse tank in turn to remove the etching solution and other impurities remaining on the surface. The pipe is then dried using a clean hot air drying device. The drying process needs to be carried out in a clean room to ensure the cleanliness of the pipe surface.

2. The method for preparing a medical PTFE etched tube according to claim 1, characterized in that: The cleaning tank contains a mixed solution of anhydrous ethanol and deionized water, with a mass ratio of 1:0.8-1.

1.

3. The method for preparing a medical PTFE etched tube according to claim 1, characterized in that: The temperature of the cleaning tank is controlled at 40-50°C, and the cleaning time is 10-15 minutes.

4. The method for preparing a medical PTFE etched tube according to claim 1, characterized in that: The plasma surface activation treatment parameters are: plasma treatment power is 80-200W, and frequency is 13.56MHz.

5. The method for preparing a medical PTFE etched tube according to claim 1, characterized in that: The etching solution in the etching tank is selected from sodium naphthalene etching solution.

6. The method for preparing a medical PTFE etching tube according to claim 5, characterized in that: An etching stabilizer is added to the etching solution, and the added amount is 2-5% of the total amount of the etching solution.

7. The method for preparing a medical PTFE etching tube according to claim 6, characterized in that: The etching stabilizer preparation method is: K1: By weight, 18-32 parts of 5-fluoro-1-naphthylamine, 5-10 parts of O,O-dimethylphosphoryl chloride, 0.05-0.5 parts of aluminum chloride, and 200-300 parts of DMF are placed in a stirring tank, the reaction temperature is controlled at 60-80°C, and the reaction time is 3-12 hours; K2: Add 0.03-0.8 parts of acrylic-cage polysilsesquioxane and 2-5 parts of triethylamine, stir and react at 60-80° C. for 1-4 hours, and remove DMF by distillation to obtain an etching stabilizer.

8. The method for preparing a medical PTFE etched tube according to claim 1, characterized in that: The temperature of the rinsing water is controlled between 20-30° C., and the rinsing time is 5-10 minutes.

9. The method for preparing a medical PTFE etching tube according to claim 1, characterized in that: The rinsing water is high-purity water with a resistivity of ≥15MΩ·cm.

10. The method for preparing a medical PTFE etched tube according to claim 1, characterized in that: The drying temperature is controlled between 60-80° C., and the drying time is 10-15 minutes.

Citation Information

Patent Citations

  • Data processing apparatus, data processing method, and data processing program

    JP2022081112A