A method for preparing a precision infusion hydrophilic pore membrane

Abstract

The application relates to a preparation method of a precision infusion hydrophilic nuclear pore membrane, comprising the following steps: preparing a nuclear pore membrane by using a characteristic base material; obtaining a nanoscale nuclear pore membrane after plasma surface treatment of the nuclear pore membrane; and obtaining a hydrophilic nuclear pore membrane after a grafting reaction is initiated between the nanoscale nuclear pore membrane and a characteristic solution. According to the technical scheme provided by the application, the membrane pore size is adjusted to the nanoscale after plasma surface treatment of the nuclear pore membrane, the nuclear pore membrane pore distribution is more uniform, when the hydrophilic nuclear pore membrane is applied to clinical infusion, bacteria with smaller particle sizes can be filtered out, and fine blood filtration is realized; in addition, in the modification grafting reaction process, vinyl pyrrolidone is used to replace acrylic acid in the prior art, harm to the human body can be avoided, other impurities can be prevented from polluting the modified hydrophilic nuclear pore membrane, the reliability and stability of the hydrophilic nuclear pore membrane are improved, and the service life of the hydrophilic nuclear pore membrane is prolonged.

Description

Technical Field

[0001] This invention belongs to the field of nuclear pore membrane manufacturing technology, and particularly relates to a method for preparing a precision infusion hydrophilic nuclear pore membrane. Background Technology

[0002] Currently, intravenous injectors used in clinical medicine in China typically include a syringe body containing a filter membrane. This membrane removes impurities from the medication, preventing them from entering the bloodstream and contaminating the blood, potentially causing other inflammations. Existing filter membranes are usually cellulose membranes, with pore sizes typically around 15 micrometers. The relatively large pore size of cellulose membranes makes it difficult to filter out bacteria with smaller particle sizes. Nuclear pore membranes, on the other hand, are based on a polymer film. They are created by uniformly irradiating with heavy ions to obtain latent tracks, followed by chemical etching to achieve uniform pore size, distribution, and through-holes. The pore size of nuclear pore membranes can be precisely controlled by adjusting the etching method. The pore size determines the scale of substances retained. Nuclear pore membranes have even smaller pore sizes, and in recent years, they have been increasingly used in intravenous injectors to improve the filtration accuracy of medications.

[0003] In the prior art, patent document with authorization announcement number "CN109078503B" discloses a process for hydrophilicating PET precision infusion filtration nucleopore membranes, including steps such as preparing an initiation bath, initiation treatment, preparing a grafting bath, and grafting treatment. This patented technology modifies the nucleopore membrane through a grafting reaction, giving it better mechanical properties and enhanced surface hydrophilicity, resulting in good stability. However, the pore diameter of existing nucleopore membranes is multidimensionally in the micrometer range, making them difficult to apply to applications requiring fine blood filtration. Furthermore, the acrylic acid used in the grafting reaction of the aforementioned patented technology is an unsaturated fatty acid with a pungent odor and corrosive properties. When some acrylic acid enters the human body with the medication, it can damage the skin, eyes, respiratory tract, and other organs. In addition, acrylic acid is chemically reactive, and the grafting reaction process of the aforementioned patented technology is completely exposed to the external environment, making it prone to reduction reactions with hydrogen in the air, affecting the reliability, stability, and service life of the resulting modified nucleopore membrane. Summary of the Invention

[0004] To address the aforementioned technical problems, this invention provides a method for preparing a precision infusion hydrophilic nuclear pore membrane.

[0005] This invention provides a method for preparing a precision infusion hydrophilic nuclear pore membrane, comprising the following steps: Step 1: Prepare a nuclear pore membrane using a characteristic substrate; Step 2: After performing plasma surface treatment on the nuclear pore membrane described in Step 1 using a plasma surface treatment instrument, a nanoscale nuclear pore membrane is obtained; Step 3: Provide a characteristic solution and an initiator. The concentration of the characteristic solution is 2%-5%, and the characteristic solution includes vinylpyrrolidone. Under the action of the initiator, the nanoscale nuclear pore membrane obtained in Step 2 undergoes a grafting reaction with the characteristic solution to obtain a hydrophilic nuclear pore membrane.

[0006] The preparation method of the precision infusion hydrophilic nuclear pore membrane further includes the following steps: first, cleaning the hydrophilic nuclear pore membrane with a cleaning solution, and then drying the hydrophilic nuclear pore membrane.

[0007] The hydrophilic nucleopore membrane is cleaned by spraying with a cleaning solution.

[0008] The cleaning solution is an aqueous solution of methanol, ethanol, or acetone.

[0009] The feature substrate mentioned in step one is a PET polyester film or a PC polycarbonate film, and the pore size of the core pore membrane is 0.22-5.0 μm.

[0010] In step two, the process parameters for plasma surface treatment of the nuclear pore mold include: the plasma surface treatment instrument uses oxygen as the working gas, the oxygen flow rate is at least 20 mL / min, the vacuum degree of the plasma surface treatment instrument is below 0.2 Pa, and the plasma surface treatment duration is 1 h-2 h.

[0011] In step three, the grafting reaction is carried out in a sealed container, and nitrogen gas is introduced into the sealed container as a protective gas.

[0012] The process parameters for the grafting reaction include: the temperature of the grafting reaction is 50-80℃, and the duration of the grafting reaction is 6-8h.

[0013] The characteristic solution also includes hydroxyethyl acrylate.

[0014] The initiator is azobisisobutyronitrile at a concentration of 1%.

[0015] The beneficial effects of this invention are as follows: Firstly, by employing the technical solution provided by this invention, the nuclear pore membrane undergoes plasma surface treatment. This plasma treatment process uses high-energy active particles to deeply clean, activate, and etch the material surface, finely adjusting the pore size of the nuclear pore membrane to the nanoscale and making the pore distribution more uniform. Finally, a nanoscale nuclear pore membrane is obtained. When this modified nuclear pore membrane is applied to clinical infusions, it can filter out bacteria with even smaller particle sizes, making it suitable for applications involving fine filtration of blood. Secondly, in the modification grafting reaction process, vinylpyrrolidone is used instead of acrylic acid in the prior art. Vinylpyrrolidone has higher safety for the human body, avoiding damage to internal organs. Furthermore, vinylpyrrolidone is chemically inert, and the grafting reaction process in this invention is carried out in a closed container, protected by nitrogen gas, preventing vinylpyrrolidone from reacting chemically with other substances in the air. This improves the reliability and stability of the obtained modified hydrophilic nuclear pore membrane and helps extend its service life. Attached Figure Description

[0016] Figure 1 This is a process flow diagram of the present invention. Detailed Implementation

[0017] The technical solution of the present invention will be further described below with reference to the accompanying drawings, but the scope of protection claimed is not limited thereto; This invention provides a method for preparing a precision infusion hydrophilic nuclear pore membrane, such as... Figure 1 As shown, it includes the following steps: Step 1: Prepare a nuclear pore membrane using a characteristic substrate; Step 2: After performing plasma surface treatment on the nuclear pore membrane described in Step 1 using a plasma surface treatment instrument, a nanoscale nuclear pore membrane is obtained; Step 3: Provide a characteristic solution and an initiator. The concentration of the characteristic solution is 2%-5%, and the characteristic solution includes vinylpyrrolidone. Under the action of the initiator, the nanoscale nuclear pore membrane obtained in Step 2 undergoes a grafting reaction with the characteristic solution to obtain a hydrophilic nuclear pore membrane.

[0018] The technical solution provided by this invention first involves plasma surface treatment of the nuclear pore membrane. This plasma treatment process uses high-energy active particles to deeply clean, activate, and etch the material surface, finely adjusting the pore size of the nuclear pore membrane to the nanoscale and making the pore distribution more uniform. This results in a nanoscale nuclear pore membrane. When applied to clinical infusions, this modified nuclear pore membrane can filter out bacteria with even smaller particle sizes, making it suitable for fine filtration of blood. Secondly, in the modification grafting reaction, vinylpyrrolidone is used instead of acrylic acid in the prior art. Vinylpyrrolidone has higher safety for the human body, avoiding damage to internal organs. Furthermore, vinylpyrrolidone is chemically inert, and the grafting reaction in this invention is carried out in a closed container with nitrogen as a protective gas, preventing vinylpyrrolidone from reacting chemically with other substances in the air. This improves the reliability and stability of the resulting modified hydrophilic nuclear pore membrane and helps extend its service life.

[0019] Specifically, the preparation method of the precision infusion hydrophilic nuclear pore membrane further includes the following steps: first, cleaning the hydrophilic nuclear pore membrane with a cleaning solution, and then drying the hydrophilic nuclear pore membrane. The cleaning solution is applied to the hydrophilic nuclear pore membrane by spraying. Preferably, the cleaning solution is an aqueous solution of methanol, ethanol, or acetone.

[0020] In addition, the feature substrate mentioned in step one is a PET polyester film or a PC polycarbonate film, and the pore size of the core-pore membrane is 0.22-5.0 μm. In step two, the process parameters for plasma surface treatment of the core-pore mold include: the plasma surface treatment instrument uses oxygen as the working gas, the oxygen flow rate is at least 20 mL / min, the vacuum degree of the plasma surface treatment instrument is below 0.2 Pa, and the plasma surface treatment duration is 1-2 hours. In step three, the grafting reaction is carried out in a sealed container, and nitrogen is introduced into the sealed container as a protective gas. The process parameters for the grafting reaction include: the grafting reaction temperature is 50-80℃, and the grafting reaction duration is 6-8 hours. Preferably, the feature solution also includes hydroxyethyl acrylate. The initiator is azobisisobutyronitrile (AIB) at a concentration of 1%. By employing the technical solution of this invention, the grafting reaction is carried out in a sealed container, and inert nitrogen gas is introduced as a protective gas. This avoids chemical reactions between vinylpyrrolidone and other substances in the air, improves the reliability and stability of the prepared modified hydrophilic nucleoporous membrane, and helps to extend its service life.

[0021] Example 1: Example 1 provides a method for preparing a precision infusion hydrophilic nuclear pore membrane, comprising the following steps: Step 1: A core-pore membrane was prepared using PET polyester with a thickness of 0.22 μm as the substrate; Step 2: The nuclear pore membrane described in Step 1 is subjected to plasma surface treatment using a plasma surface treatment instrument. The plasma surface treatment instrument uses oxygen as the working gas, the oxygen flow rate is 20 mL / min, the vacuum degree of the plasma surface treatment instrument is below 0.2 Pa, and the plasma surface treatment duration is 1 h, thereby obtaining a nanoscale nuclear pore membrane. Step 3: Using 1% azobisisobutyronitrile as an initiator and 5% vinylpyrrolidone aqueous solution as a characteristic solution, the nanoscale nuclear pore membrane is immersed in the characteristic solution, and nitrogen gas is introduced into the characteristic solution as a protective gas. Under the action of the initiator, the nanoscale nuclear pore membrane and the characteristic solution are initiated to undergo a grafting reaction. The grafting reaction temperature is set at 80°C, and the duration of the grafting reaction is set at 8 hours to obtain a hydrophilic nuclear pore membrane. Step 4: First, clean the hydrophilic nuclear pore membrane with an acetone aqueous solution, and then dry the hydrophilic nuclear pore membrane.

[0022] Example 2: Example 2 provides a method for preparing a precision infusion hydrophilic nuclear pore membrane, comprising the following steps: Step 1: A core-pore membrane was prepared using a 3μm thick PC polycarbonate substrate. Step 2: The nuclear pore membrane described in Step 1 is subjected to plasma surface treatment using a plasma surface treatment instrument. The plasma surface treatment instrument uses oxygen as the working gas, the oxygen flow rate is 20 mL / min, the vacuum degree of the plasma surface treatment instrument is below 0.2 Pa, and the plasma surface treatment duration is 1.5 h, thereby obtaining a nanoscale nuclear pore membrane. Step 3: Using 1% azobisisobutyronitrile as an initiator and 2% hydroxyethyl acrylate aqueous solution as a characteristic solution, the nanoscale nuclear pore membrane is immersed in the characteristic solution, and nitrogen gas is introduced into the characteristic solution as a protective gas. Under the action of the initiator, the nanoscale nuclear pore membrane and the characteristic solution initiate a grafting reaction. The grafting reaction temperature is set at 50°C, and the duration of the grafting reaction is set at 8 hours to obtain a hydrophilic nuclear pore membrane. Step 4: First, clean the hydrophilic nuclear pore membrane with a methanol aqueous solution, and then dry the hydrophilic nuclear pore membrane.

[0023] Example 3: Example 4 provides a method for preparing a precision infusion hydrophilic nuclear pore membrane, comprising the following steps: Step 1: A core-pore membrane was prepared using PET polyester with a thickness of 5 μm as the substrate; Step 2: The nuclear pore membrane described in Step 1 is subjected to plasma surface treatment using a plasma surface treatment instrument. The plasma surface treatment instrument uses oxygen as the working gas, the oxygen flow rate is 20 mL / min, the vacuum degree of the plasma surface treatment instrument is below 0.2 Pa, and the plasma surface treatment duration is 2 h, thereby obtaining a nanoscale nuclear pore membrane. Step 3: Using 1% azobisisobutyronitrile as an initiator and 3% vinylpyrrolidone aqueous solution as a characteristic solution, the nanoscale nuclear pore membrane is immersed in the characteristic solution, and nitrogen gas is introduced into the characteristic solution as a protective gas. Under the action of the initiator, the nanoscale nuclear pore membrane and the characteristic solution are initiated to undergo a grafting reaction. The grafting reaction temperature is set at 70°C, and the duration of the grafting reaction is set at 7 hours to obtain a hydrophilic nuclear pore membrane. Step 4: First, clean the hydrophilic nuclear pore membrane with an ethanol-water solution, and then dry the hydrophilic nuclear pore membrane.

[0024] The hydrophilic contact angles of the hydrophilic nucleoporous membranes prepared in Examples 1 to 3 were measured. The measurement method was as follows: using an SDC-200S contact angle measuring instrument produced by Dongguan Shengding Precision Instruments Co., Ltd., deionized water was used as the droplet, and a total volume of 2 μL of deionized water was dropped onto the surface of the hydrophilic nucleoporous membranes prepared in Examples 1 to 3 one by one using the seat drop method. With the arc-shaped surface of the droplet as the reference, the contact edge between the droplet and the hydrophilic nucleoporous membrane was tangented, and the hydrophilic contact angle data were measured and are shown in Table 1.

[0025] Table 1 Hydrophilic properties of nuclear pore membranes As can be seen from Examples 1 to 3, by applying plasma surface treatment to the nuclear pore membrane before the grafting reaction, the pore size of the nuclear pore membrane is optimized and adjusted, and the hydrophilicity of the nuclear pore membrane is improved. The hydrophilic contact angle of the prepared hydrophilic nuclear pore membrane is less than 30°. The hydrophilic nuclear pore membranes prepared in Examples 1 to 3 exhibit good hydrophilicity, which improves the compatibility between the hydrophilic nuclear pore membrane and the drug solution.

Claims

1. A method for preparing a precision infusion hydrophilic nuclear pore membrane, characterized in that: Includes the following steps: Step 1: Prepare a nuclear pore membrane using a characteristic substrate; Step 2: After performing plasma surface treatment on the nuclear pore membrane described in Step 1 using a plasma surface treatment instrument, a nanoscale nuclear pore membrane is obtained; Step 3: Provide a characteristic solution and an initiator. The concentration of the characteristic solution is 2%-5%, and the characteristic solution includes vinylpyrrolidone. Under the action of the initiator, the nanoscale nuclear pore membrane obtained in Step 2 undergoes a grafting reaction with the characteristic solution to obtain a hydrophilic nuclear pore membrane.

2. The method for preparing a precision infusion hydrophilic nucleoporous membrane as described in claim 1, characterized in that: The preparation method of the precision infusion hydrophilic nuclear pore membrane further includes the following steps: first, cleaning the hydrophilic nuclear pore membrane with a cleaning solution, and then drying the hydrophilic nuclear pore membrane.

3. The method for preparing a precision infusion hydrophilic nucleoporous membrane as described in claim 2, characterized in that: The hydrophilic nucleopore membrane is cleaned by spraying with a cleaning solution.

4. A method for preparing a precision infusion hydrophilic nucleoporous membrane as described in claim 2 or 3, characterized in that: The cleaning solution is an aqueous solution of methanol, ethanol, or acetone.

5. The method for preparing a precision infusion hydrophilic nucleoporous membrane as described in claim 1, characterized in that: The feature substrate mentioned in step one is a PET polyester film or a PC polycarbonate film, and the pore size of the core pore membrane is 0.22-5.0 μm.

6. The method for preparing a precision infusion hydrophilic nucleoporous membrane as described in claim 1, characterized in that: In step two, the process parameters for plasma surface treatment of the nuclear pore mold include: the plasma surface treatment instrument uses oxygen as the working gas, the oxygen flow rate is at least 20 mL / min, the vacuum degree of the plasma surface treatment instrument is below 0.2 Pa, and the plasma surface treatment duration is 1 h-2 h.

7. The method for preparing a precision infusion hydrophilic nucleoporous membrane as described in claim 1, characterized in that: In step three, the grafting reaction is carried out in a sealed container, and nitrogen gas is introduced into the sealed container as a protective gas.

8. A method for preparing a precision infusion hydrophilic nucleoporous membrane as described in claim 6 or 7, characterized in that: The process parameters for the grafting reaction include: the temperature of the grafting reaction is 50-80℃, and the duration of the grafting reaction is 6-8h.

9. The method for preparing a precision infusion hydrophilic nucleoporous membrane as described in claim 1, characterized in that: The characteristic solution also includes hydroxyethyl acrylate.

10. The method for preparing a precision infusion hydrophilic nucleoporous membrane as described in claim 1, characterized in that: The initiator is azobisisobutyronitrile at a concentration of 1%.

Images