High-molecular absorbable oral cavity repairing film as well as preparation method and application thereof

Abstract

The invention provides a high-molecular absorbable oral repair membrane as well as a preparation method and application thereof. The preparation method comprises the following steps: preparation of a spinning solution, preparation of a primary product of the oral repair membrane, ultrasonic cleaning, drying and biaxial stretching treatment. The oral repair film is used for products for treating oral mucosa / tooth injury. According to the preparation method disclosed by the invention, the oral cavity repairing film with biodegradability and relatively good mechanical property is prepared through an electrostatic spinning technology, can play a role of an isolation barrier, also has excellent tissue regeneration guiding performance, and is beneficial to adhesion, proliferation and differentiation of cells.

Description

Technical Field

[0001] The present application relates to the technical field of biomedical materials, and in particular to a polymer absorbable oral repair membrane, and a preparation method and application thereof. Background Art

[0002] Dental implants have become an important means of restoring missing or missing teeth. However, insufficient bone mass due to various factors, such as natural atrophy of the alveolar ridge, trauma, and periodontal disease, reduces the success rate of implant restoration and limits the scope of their use. Guided tissue regeneration (GTR) can effectively address the problems of insufficient bone mass and alveolar bone defects. This technology involves placing a barrier membrane at the bone defect site to prevent fibroblasts from entering the bone defect while also promoting osteoblast adhesion, proliferation, and bone tissue regeneration.

[0003] Currently, the most commonly used biofilms on the market are divided into absorbable biofilms and non-absorbable biofilms. Non-absorbable membranes are mainly metal membranes and polymer membranes. This type of membrane material has excellent mechanical strength and can play a good shielding and supporting role. However, there are also huge defects. First, non-absorbable membranes are usually accompanied by the disadvantages of high hardness and poor comfort. They have poor fit with soft tissues and can irritate wounds during activities, triggering inflammatory reactions. Secondly, because the membrane cannot be absorbed and degraded in the body, a second operation is required to remove the implanted membrane from the damaged area, which not only increases the risk of infection but also prolongs the treatment and recovery time.

[0004] Collagen is one of the most widely used materials in biomedical applications. It has low immunogenicity, good coordination with host cells, biodegradability, high strength and toughness. Collagen is a structural protein with biological functions, accounting for 1 / 3 of the total protein in the human body. It is the main component of connective tissues or organs such as skin, cartilage, ligaments, and tendons. It can effectively promote cell division, proliferation and differentiation, induce platelet adhesion, promote platelet aggregation, and produce adhesion, compression and filling effects on wounds. However, the absorbable membrane in the existing technology is mainly collagen membrane, which has excellent biocompatibility and in vivo degradability. It has a high degree of compatibility with the soft tissue and bone tissue in the damaged area of ​​the human body, and can effectively cover the damaged area to allow bone tissue to grow in a shielded environment. At the same time, collagen-based absorbable biofilms do not require secondary surgery, reducing the risk of wound exposure and infection. However, in the application of collagen membranes, there is a problem of poor mechanical properties.

[0005] Therefore, providing a resorbable biomembrane with good mechanical properties is an important issue that needs to be addressed. Summary of the Invention

[0006] The present application provides a polymer absorbable oral repair membrane, and a preparation method and application thereof, to solve the above-mentioned problems mentioned in the background technology.

[0007] In one aspect, the present application provides a method for preparing a polymer absorbable oral repair membrane, the preparation method comprising the following steps: (1) Preparation of spinning solution: Add polycaprolactone to solvent A and stir until the mixture is uniform to obtain spinning solution A; add polyethylene glycol to solvent B and stir until the mixture is uniform to obtain spinning solution B; (2) Preparation of the initial oral repair membrane: Using a rotating drum as a receiving device, extract the spinning solution A with the first needle tube, and extract the spinning solution B with the second needle tube at the same time. Select two needles with a diameter of 10-24G and connect the first needle tube and the second needle tube respectively to perform electrospinning to obtain the initial oral repair membrane; (3) Ultrasonic cleaning: Take out the initial oral repair membrane and perform ultrasonic cleaning for 1-3 hours to obtain the initial oral repair membrane with polycaprolactone as the main component; (4) Drying: Drying the initial oral repair membrane after ultrasonic cleaning; (5) Biaxial stretching treatment: The oral repair membrane product after drying is stretched along two mutually perpendicular directions with a stretching ratio of 2-4 to obtain a finished oral repair membrane product.

[0008] Optionally, in the spinning solution A, the mass volume ratio of polycaprolactone to solvent A is 8-15% g / mL.

[0009] Optionally, in the spinning solution B, the mass volume ratio of polyethylene glycol to solvent B is 15-22% g / mL.

[0010] Optionally, solvent A includes any one of hexafluoroisopropanol, dichloromethane, chloroform, and DMF.

[0011] Optionally, solvent B includes any one of water, ethanol, DMSO, and DMF.

[0012] Optionally, the stirring speed during the preparation of spinning solution A and spinning solution B is 1000-5000 rpm.

[0013] Optionally, the parameters in the electrospinning process are: the flow rate of spinning solution A is 1-10 mL / h, the flow rate of spinning solution B is 5-15 mL / h, the receiving distance is 12-20 cm, the rotating drum speed is 50-200 r / min, the voltage is 12-30 KV, and the spinning time is 0.5-3 h.

[0014] Optionally, the temperature during the drying process is 30-50° C., and the drying time is 2 hours.

[0015] On the other hand, the present application also provides a polymer absorbable oral repair membrane, which is prepared by the above-mentioned preparation method.

[0016] On the other hand, the present application also provides an application of a polymer absorbable oral repair membrane, which is prepared by the above-mentioned preparation method, or is the above-mentioned oral repair membrane, and the oral repair membrane is used in products for treating oral mucosa / tooth damage.

[0017] The polymer absorbable oral restoration membrane provided in this application, as well as its preparation method and application, realizes the preparation of the polymer absorbable membrane and has the following beneficial effects compared with the existing technology: (1) The present application realizes the preparation of a polymer absorbable oral repair membrane through the above scheme. A spinning solution A containing polycaprolactone and a spinning solution B containing polyethylene glycol are obtained by mixing and stirring. Then, an oral repair membrane primary product whose main components are polycaprolactone and polyethylene glycol is obtained by electrospinning technology. Then, the oral repair membrane primary product is cleaned by ultrasonic wave to remove polyethylene glycol from the oral repair membrane primary product, thereby obtaining an oral repair membrane primary product with polycaprolactone as the main component. The membrane forms a larger pore size, which is conducive to providing a pore structure and increasing the three-dimensional pore size in space. When used, it is conducive to the flow of nutrients, tissue repair, guiding tissue regeneration performance, and cell adhesion, proliferation and differentiation, and has excellent mechanical properties and operability. At the same time, it can also improve hydrophilicity, which helps the oral repair membrane to be stably attached in the oral cavity during use, thereby preventing fibroblasts from entering the bone defect site and playing a better isolation role. Drying, and finally biaxial stretching are performed to improve the mechanical properties of the oral repair membrane, which well meets the mechanical properties requirements of oral tissue repair for the oral repair membrane. The present application prepares an oral repair membrane that has both biodegradability and good mechanical properties.

[0018] (2) By controlling the parameters during the electrospinning process, the thickness of the fibers ejected during the process can be controlled, and thus the pore size structure of the oral repair membrane can be controlled. This not only acts as an isolation barrier, but also has good performance in guiding tissue regeneration, which is beneficial to cell adhesion, proliferation and differentiation. Furthermore, after biaxial stretching treatment, the mechanical properties of the oral repair membrane, such as tensile strength and breaking strength, can be improved.

[0019] (3) The preparation method of the absorbable oral repair membrane provided in this application has the technical advantages of simple processing technology and easy operation.

[0020] (4) The absorbable oral repair membrane provided in this application can not only be used to prepare products for oral mucosa / tooth damage, but can also be used to prepare skin repair membranes that need to adhere to the skin surface. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, a brief introduction will be given below to the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without any creative work.

[0022] Figure 1 A physical picture of the initial oral repair membrane provided in Example 2 of the present application; Figure 2 This is a longitudinal stretch diagram of the oral restoration membrane provided in Example 2 of the present application; Figure 3 This is a transverse stretching diagram of the oral restoration membrane provided in Example 2 of the present application. DETAILED DESCRIPTION

[0023] To make the purpose, technical solutions, and advantages of the embodiments of this application more clear, the technical solutions in the embodiments of this application are clearly and completely described below. Obviously, the described embodiments are part of the embodiments of this application, not all of them. Based on the embodiments in this application, all other embodiments obtained by ordinary technicians in this field without making creative efforts also fall within the scope of protection of this application.

[0024] In one aspect, the present application provides a method for preparing a polymer absorbable oral repair membrane, the preparation method comprising the following steps: (1) Preparation of spinning solution: Add polycaprolactone to solvent A and stir until the mixture is uniform to obtain spinning solution A; add polyethylene glycol to solvent B and stir until the mixture is uniform to obtain spinning solution B; (2) Preparation of the initial oral repair membrane: Using a rotating drum as a receiving device, extract the spinning solution A with the first needle tube, and extract the spinning solution B with the second needle tube at the same time. Select two needles with a diameter of 10-24G and connect the first needle tube and the second needle tube respectively to perform electrospinning to obtain the initial oral repair membrane; (3) Ultrasonic cleaning: Take out the initial oral repair membrane and perform ultrasonic cleaning for 1-3 hours to obtain the initial oral repair membrane with polycaprolactone as the main component; (4) Drying: Drying the initial oral repair membrane after ultrasonic cleaning; (5) Biaxial stretching treatment: The oral repair membrane product after drying is stretched along two mutually perpendicular directions with a stretching ratio of 2-4 to obtain a finished oral repair membrane product.

[0025] Specifically, during the treatment of tooth damage, insufficient bone mass limits the therapeutic effect. By placing the polymer absorbable oral repair membrane prepared in this application at the bone defect site, fibroblasts are prevented from entering the bone defect site, while promoting the adhesion and proliferation of osteoblasts and bone tissue regeneration, playing an important and positive role in oral treatment.

[0026] In the preparation process of the oral prosthetic membrane of the present application, polycaprolactone and solvent A are first mixed to obtain spinning solution A, and polyethylene glycol is simultaneously mixed with solvent B to obtain spinning solution B. Electrospinning is then performed using electrospinning technology to produce a preliminary oral prosthetic membrane whose main components are polycaprolactone and polyethylene glycol. The preliminary oral prosthetic membrane is then ultrasonically cleaned. Since polyethylene glycol (PEG) is soluble in water, while polycaprolactone (PCL) is insoluble in water, ultrasonic cleaning can remove the polyethylene glycol from the preliminary oral prosthetic membrane, thereby obtaining a preliminary oral prosthetic membrane with polycaprolactone as the main component. The removal of polyethylene glycol can also form a larger pore size in the oral prosthetic membrane, which is beneficial for providing a pore structure and increasing the three-dimensional pore size in space. This facilitates the flow of nutrients during use and promotes tissue repair. It also improves hydrophilicity, which helps the oral prosthetic membrane to adhere stably in the oral cavity during use, thereby preventing fibroblasts from entering the bone defect site and providing a good isolation effect. By removing polyethylene glycol from the initial oral repair membrane, a finished oral repair membrane with a specific pore structure can be obtained, so that the oral repair membrane can be applied to different oral diseases, making the use of the oral repair membrane more extensive.

[0027] After ultrasonic cleaning, the initial oral repair membrane is dried for easy storage. The initial oral repair membrane after drying is subjected to biaxial stretching in two mutually perpendicular directions, namely longitudinal stretching and transverse stretching, and the longitudinal stretching and transverse stretching have the same stretching ratio of 2-4, to obtain a finished oral repair membrane. Finally, it is cut and packaged according to the required specifications and sterilized for clinical use. Biaxial stretching can make the polymer chains tend to align in a direction parallel to the plane of the film, improve the overall strength and uniformity of the oral repair membrane, reduce the strength difference of the oral repair membrane in different directions, and greatly improve the mechanical properties of the oral repair membrane, such as tensile strength and suture tearing force.

[0028] Polycaprolactone has excellent biocompatibility, bioretention properties, and biodegradability. It is gradually absorbed and excreted by the body during use. Oral prosthetic membranes made primarily of polycaprolactone adhere well to soft tissue and do not trigger an inflammatory response. Furthermore, if the damaged area requires reoperation, the membrane does not need to be removed, shortening the treatment cycle and making the patient experience more comfortable. Polyethylene glycol (PEG) is a commonly used polymer with excellent chemical stability. It is not susceptible to chemical reactions under normal conditions and can withstand certain temperature and pH fluctuations. It has low toxicity and is relatively safe for humans and the environment. In pharmaceutical applications, it is often used as an excipient to reduce the toxic side effects of drugs and minimize potential environmental hazards. PEG is also miscible with water in all proportions, making it easily dispersed and soluble in aqueous systems, demonstrating its hydrophilic nature.

[0029] Furthermore, the oral restoration membrane has a thickness of 0.4-0.7 mm before biaxial stretching treatment, and a thickness of 0.15-0.44 mm after biaxial stretching treatment, and is applicable to various usage environments.

[0030] The present application achieves the preparation of a polymer absorbable oral repair membrane through the above scheme. A spinning solution A containing polycaprolactone is obtained by mixing and stirring, and a spinning solution B containing polyethylene glycol is simultaneously added. Then, electrospinning is performed to obtain a preliminary oral repair membrane whose main components are polycaprolactone and polyethylene glycol. The preliminary oral repair membrane is then ultrasonically cleaned to remove the polyethylene glycol from the preliminary oral repair membrane, thereby obtaining a preliminary oral repair membrane with polycaprolactone as the main component. The larger pore size is formed, which is conducive to providing a pore structure and increasing the three-dimensional pore size in space. During use, it facilitates the flow of nutrients, promotes tissue repair, guides tissue regeneration, and promotes cell adhesion, proliferation, and differentiation. It also has excellent mechanical properties and operability. At the same time, it can also improve hydrophilicity, which helps the oral repair membrane to adhere stably in the oral cavity during use, thereby preventing fibroblasts from entering the bone defect site and providing a good isolation effect. Drying and finally biaxial stretching are performed to improve the mechanical properties of the oral repair membrane, which well meets the mechanical property requirements of oral tissue repair for oral repair membranes. The present application prepares an oral repair membrane that has both biodegradability and good mechanical properties.

[0031] Optionally, in the spinning solution A, the mass volume ratio of polycaprolactone to solvent A is 8-15% g / mL.

[0032] Optionally, in the spinning solution B, the mass volume ratio of polyethylene glycol to solvent B is 15-22% g / mL.

[0033] Specifically, if the concentration of the spinning solution is too high, the diameter of the ejected fibers may increase, and even a beaded structure may appear. If the concentration is too low, the polymer chains may not be entangled enough, and the viscosity may be low, which may lead to fiber breakage and discontinuity. Therefore, controlling the concentrations of spinning solution A and spinning solution B can make the ejected fibers uniform in fineness and continuity, and thus make the oral repair membrane have a uniform pore structure, which can improve the stability with soft tissue while playing a good isolation role. In particular, the concentration of spinning solution B has a greater influence on the pore structure of the prepared oral repair membrane. The increase in the concentration of polyethylene glycol in spinning solution B increases the pore structure of the oral repair membrane. By adjusting the concentrations of spinning solution A and spinning solution B, the pore size of the oral repair membrane can be controlled, and thus the mechanical properties of the oral repair membrane can be controlled. Optionally, solvent A includes any one of hexafluoroisopropanol, dichloromethane, chloroform, and DMF.

[0034] Optionally, solvent B includes any one of water, ethanol, DMSO, and DMF.

[0035] Optionally, the stirring speed during the preparation of the spinning solution A and the spinning solution B is 1000-5000 rpm, and the stirring time is 10-50 min.

[0036] Optionally, the parameters in the electrospinning process are: the flow rate of spinning solution A is 1-10 mL / h, the flow rate of spinning solution B is 5-15 mL / h, the receiving distance is 12-20 cm, the rotating drum speed is 50-200 r / min, the voltage is 12-30 KV, and the spinning time is 0.5-3 h.

[0037] Specifically, by controlling the parameters during the electrospinning process, the thickness of the ejected fibers can be controlled, and thus the pore size structure of the oral prosthetic membrane can be manipulated. This not only acts as an isolation barrier but also effectively guides tissue regeneration, facilitating cell adhesion, proliferation, and differentiation. Furthermore, through biaxial stretching, the membrane's mechanical properties, such as tensile strength, can be enhanced.

[0038] At the same time, by controlling the flow rates of the spinning solution A and the spinning solution B, the thickness of the ejected fibers can be controlled, thereby controlling the pore size structure of the oral repair membrane.

[0039] Furthermore, the flow rate ratio of spinning solution A and spinning solution B is always adjusted at a speed of 1:2, and the needle diameter of spinning solution A is smaller than the needle diameter of spinning solution B. The ratio of the two needle diameters is 1:1.5-2. By adjusting the flow rate of the spinning solution, the needle diameter during the electrospinning process, and the concentration of the spinning solution, multiple conditions are controlled synergistically, thereby controlling the pore structure of the oral repair membrane and improving the mechanical properties of the oral repair membrane.

[0040] Optionally, the temperature during the drying process is 30-50° C., and the drying time is 2 hours.

[0041] On the other hand, the present application also provides a polymer absorbable oral repair membrane, which is prepared by the above-mentioned preparation method.

[0042] On the other hand, the present application also provides an application of a polymer absorbable oral repair membrane, which is prepared by the above-mentioned preparation method, or is the above-mentioned oral repair membrane, and the oral repair membrane is used in products for treating oral mucosa / tooth damage.

[0043] Specifically, the absorbable oral repair membrane provided in the present application can not only be used to prepare products for oral mucosa / tooth damage, but can also be used to prepare skin repair membranes that need to adhere to the skin surface.

[0044] The technical solution of this application is described in detail below with reference to specific embodiments.

[0045] Example 1 A method for preparing a polymer absorbable oral repair membrane, the method comprising the following steps: (1) Preparation of spinning solution: polycaprolactone was added to solvent A (hexafluoroisopropanol) and stirred at a speed of 1000 rpm until the mixture was uniformly mixed to obtain a spinning solution A with a mass volume ratio of 8% g / mL; polyethylene glycol was added to solvent B (water, selected from purified water) and stirred at a speed of 1000 rpm until the mixture was uniformly mixed to obtain a spinning solution B with a mass volume ratio of 15% g / mL; (2) Preparation of the initial oral repair membrane: Using a rotating drum as a receiving device, the first needle tube was used to extract the spinning solution A, and the second needle tube was used to extract the spinning solution B, and electrospinning was performed to obtain the initial oral repair membrane; the parameters in the electrospinning process were: the diameter of the needle connected to the first needle tube was 10G, the diameter of the needle connected to the second needle tube was 12G, the flow rate of the spinning solution A was 1mL / h, the flow rate of the spinning solution B was 5mL / h, the receiving distance was 12cm, the rotating drum speed was 50r / min, the voltage was 12KV, and the spinning time was 0.5h.

[0046] (3) Ultrasonic cleaning: Take out the initial oral repair membrane and perform ultrasonic cleaning for 1 hour to obtain the initial oral repair membrane with polycaprolactone as the main component; (4) Drying: Dry the initial oral repair membrane after ultrasonic cleaning at 30°C for 2 hours; (5) Biaxial stretching: The dried oral restoration membrane is stretched along two mutually perpendicular directions with a stretching ratio of 2 to obtain a finished oral restoration membrane. When used, it is cut according to the required specifications and then sterilized for clinical use.

[0047] Example 2 A method for preparing a polymer absorbable oral repair membrane, the method comprising the following steps: (1) Preparation of spinning solution: polycaprolactone was added to solvent A (hexafluoroisopropanol), and the mixture was stirred at a speed of 2000 rpm until uniformly mixed, to obtain a spinning solution A with a mass volume ratio of 12% g / mL; polyethylene glycol was added to solvent B (water, selected from purified water), and the mixture was stirred at a speed of 2000 rpm until uniformly mixed, to obtain a spinning solution B with a mass volume ratio of 18% g / mL; (2) Preparation of the initial oral repair membrane: Using a rotating drum as a receiving device, the first needle tube was used to extract the spinning solution A, and the second needle tube was used to extract the spinning solution B, and electrospinning was performed to obtain the initial oral repair membrane; the parameters in the electrospinning process were: the diameter of the needle connected to the first needle tube was 12G, the diameter of the needle connected to the second needle tube was 24G, the flow rate of the spinning solution A was 6mL / h, the flow rate of the spinning solution B was 12mL / h, the receiving distance was 16cm, the rotating drum speed was 150r / min, the voltage was 16KV, and the spinning time was 2h.

[0048] (3) Ultrasonic cleaning: Take out the initial oral repair membrane and perform ultrasonic cleaning for 2 hours to obtain the initial oral repair membrane with polycaprolactone as the main component, such as Figure 1 As shown; (4) Drying: Dry the initial oral repair membrane after ultrasonic cleaning at 40°C for 2 hours; (5) Biaxial stretching treatment: The oral repair membrane after drying is stretched along two mutually perpendicular directions with a stretching ratio of 3 to obtain a finished oral repair membrane, such as Figure 1 When in use, cut according to the required specifications and then sterilize for clinical use.

[0049] Example 3 A method for preparing a polymer absorbable oral repair membrane, the method comprising the following steps: (1) Preparation of spinning solution: polycaprolactone was added to solvent A (hexafluoroisopropanol) and stirred at a speed of 5000 rpm until the mixture was uniformly mixed to obtain a spinning solution A with a mass volume ratio of 15% g / mL; polyethylene glycol was added to solvent B (water, selected from purified water) and stirred at a speed of 5000 rpm until the mixture was uniformly mixed to obtain a spinning solution B with a mass volume ratio of 22% g / mL; (2) Preparation of the initial oral repair membrane: Using a rotating drum as a receiving device, the first needle tube was used to extract the spinning solution A, and the second needle tube was used to extract the spinning solution B, and electrospinning was performed to obtain the initial oral repair membrane; the parameters in the electrospinning process were: the diameter of the first needle tube was 10G, the diameter of the second needle tube was 18G, the flow rate of the spinning solution A was 10mL / h, the flow rate of the spinning solution B was 15mL / h, the receiving distance was 20cm, the rotating drum speed was 200r / min, the voltage was 30KV, and the spinning time was 3h.

[0050] (3) Ultrasonic cleaning: Take out the initial oral repair membrane and perform ultrasonic cleaning for 3 hours to obtain the initial oral repair membrane with polycaprolactone as the main component; (4) Drying: Dry the initial oral repair membrane after ultrasonic cleaning at 50°C for 2 hours; (5) Biaxial stretching: The dried oral restoration membrane is stretched along two mutually perpendicular directions with a stretching ratio of 4 to obtain a finished oral restoration membrane. When used, it is cut according to the required specifications and then sterilized for clinical use.

[0051] Comparative Example 1 A method for preparing a polymer absorbable oral repair membrane, the method comprising the following steps: The difference from Example 2 is that: The ultrasonic cleaning process in step (3) was not performed.

[0052] Comparative Example 2 A method for preparing a polymer absorbable oral repair membrane, the method comprising the following steps: The difference from Example 2 is that: The biaxial stretching process in step (5) was not performed.

[0053] Comparative Example 3 A method for preparing a polymer absorbable oral repair membrane, the method comprising the following steps: The difference from Example 2 is that: The ultrasonic cleaning process in step (3) and the biaxial stretching process in step (5) were not performed.

[0054] Experimental Example 1 The oral prosthetic membranes obtained in Examples 1-3 were subjected to mechanical property testing, including tensile strength, elongation at break, and suture tear force. The oral prosthetic membrane samples used in these tests had a size of 30 x 10 x 0.45 mm (length x width x thickness). At least three replicates were run for each test, and the average value was calculated to produce the results shown in Table 1.

[0055] The tensile strength was measured using the GB / T1040.3-2006 method.

[0056] The elongation at break and the tear strength of sutures were determined according to the GB / T 1040.1-2018 method.

[0057] Taking Example 2 as an example, Figure 2 The figure shown is a longitudinal stretching diagram of the oral repair membrane provided in Example 2. Figure 3 This is a transverse stretching diagram of the oral restoration film provided in Example 2.

[0058] Table 1 As can be seen from Table 1, the mechanical properties of the oral repair membranes provided by Examples 1 to 3 of the present application are stronger than those of Comparative Examples 1 to 3. By comparing Examples 1 to 3 with Comparative Example 1, the mechanical properties of the oral repair membrane are enhanced after the polyethylene glycol is removed by ultrasonic cleaning. At the same time, by comparing Examples 1 to 3 with Comparative Example 2, it is shown that the elongation at break of the oral repair membrane is reduced by biaxial stretching, and the biaxial stretching makes the orientation of the molecular chains in the oral repair membrane more orderly, thereby significantly improving the tensile strength and suture tearing force. After biaxial stretching treatment, the oral repair membrane meets the requirements for the treatment of oral mucosa / tooth damage while greatly improving the mechanical properties of the oral repair membrane. By making the polymer chains tend to be arranged in a direction parallel to the film plane, the overall strength and uniformity of the oral repair membrane are improved, and the strength difference of the oral repair membrane in different directions is reduced. In Comparative Example 3, biaxial stretching was not performed and the polyethylene glycol was not washed off, and its mechanical properties were much weaker than those of Examples 1 to 3 and Comparative Examples 1 and 2. This shows that in this application, by washing off the polyethylene glycol in the initial oral repair membrane and performing biaxial stretching at the same time, the two operations work synergistically to improve the mechanical properties of the oral repair membrane.

[0059] Comparing Example 1, Example 2 and Example 3, the tensile strength, elongation at break and suture tearing force of the oral repair membrane provided by Example 2 are higher than those of Example 1 and Example 3, especially the elongation at break is significantly improved. In Example 2, by controlling the flow rate ratio of spinning solution A and spinning solution B to 1:2, the diameter ratio of the first needle tube to the second needle tube to 1:2, and controlling the concentrations of spinning solution A and spinning solution B at the same time, multiple conditions are coordinated to control the pore structure of the oral repair membrane, thereby improving the mechanical properties of the oral repair membrane.

[0060] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit them. Although the present application has been described in detail with reference to the above embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the above embodiments, or make equivalent replacements for some or all of the technical features therein. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A method for preparing a polymer absorbable oral repair membrane, characterized in that: The preparation method comprises the following steps: (1) Preparation of spinning solution: Add polycaprolactone to solvent A and stir until the mixture is uniform to obtain spinning solution A; add polyethylene glycol to solvent B and stir until the mixture is uniform to obtain spinning solution B; (2) Preparation of the initial oral repair membrane: using a rotating drum as a receiving device, extracting the spinning solution A with a first needle tube, and extracting the spinning solution B with a second needle tube, selecting two needles with a diameter of 10-24G and connecting them to the first needle tube and the second needle tube respectively, and performing electrospinning to obtain the initial oral repair membrane; (3) Ultrasonic cleaning: taking out the oral repair membrane product and performing ultrasonic cleaning for 1-3 hours to obtain the oral repair membrane product with polycaprolactone as the main component; (4) Drying: Drying the initial oral repair membrane after ultrasonic cleaning; (5) Biaxial stretching treatment: The oral repair membrane product after drying is stretched along two mutually perpendicular directions with a stretching ratio of 2-4 to obtain a finished oral repair membrane product.

2. The method for preparing the polymer absorbable oral repair membrane according to claim 1, characterized in that: In the spinning solution A, the mass volume ratio of the polycaprolactone to the solvent A is 8-15% g / mL.

3. The method for preparing the polymer absorbable oral repair membrane according to claim 1, characterized in that: In the spinning solution B, the mass volume ratio of the polyethylene glycol to the solvent B is 15-22% g / mL.

4. The method for preparing the polymer absorbable oral repair membrane according to claim 1, characterized in that: The solvent A includes any one of hexafluoroisopropanol, dichloromethane, chloroform, and DMF.

5. The method for preparing the polymer absorbable oral repair membrane according to claim 1, characterized in that: The solvent B includes any one of water, ethanol, DMSO and DMF.

6. The method for preparing the polymer absorbable oral repair membrane according to claim 1, characterized in that: The stirring speed during the preparation of the spinning solution A and the spinning solution B is 1000-5000 rpm.

7. The method for preparing a polymer absorbable oral repair membrane according to claim 1, characterized in that: The parameters in the electrospinning process are: the flow rate of spinning solution A is 1-10 mL / h, the flow rate of spinning solution B is 5-15 mL / h, the receiving distance is 12-20 cm, the rotating drum speed is 50-200 r / min, the voltage is 12-30 KV, and the spinning time is 0.5-3 h.

8. The method for preparing the polymer absorbable oral repair membrane according to any one of claims 1 to 7, characterized in that: The temperature during the drying process is 30-50° C., and the drying time is 2 hours.

9. A polymer absorbable oral repair membrane, characterized in that: The oral repair membrane is prepared by the preparation method according to any one of claims 1 to 8.

10. An application of a polymer absorbable oral repair membrane, characterized in that: The oral repair membrane is prepared by the preparation method according to any one of claims 1 to 8, or is the oral repair membrane according to claim 9, and the oral repair membrane is used in a product for treating oral mucosa / tooth damage.

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