CN115531610A - Fiber composite membrane, preparation method and application thereof - Google Patents
Fiber composite membrane, preparation method and application thereof Download PDFInfo
- Publication number
- CN115531610A CN115531610A CN202211398004.0A CN202211398004A CN115531610A CN 115531610 A CN115531610 A CN 115531610A CN 202211398004 A CN202211398004 A CN 202211398004A CN 115531610 A CN115531610 A CN 115531610A
- Authority
- CN
- China
- Prior art keywords
- polyvinyl alcohol
- fiber composite
- composite membrane
- dura mater
- core layer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- Materials For Medical Uses (AREA)
Abstract
The invention relates to the technical field of artificial dura mater spinalis, and in particular relates to a fiber composite membrane, a preparation method and application thereof. The fiber composite membrane comprises a core layer and a shell layer wrapping the core layer, wherein the core layer is composed of a spinning material and an antibacterial substance, and the shell layer is composed of methylacryloyl acylated polyvinyl alcohol-o-nitrobenzene hyaluronic acid-photoinitiator. The fiber composite membrane has the advantages of high gelling speed, good biomechanics and adhesiveness and low swelling rate, can be used as an artificial dura mater, and then effectively repairs dura mater damage to avoid cerebrospinal fluid leakage.
Description
Technical Field
The invention relates to the technical field of artificial dura mater spinalis, and in particular relates to a fiber composite membrane, a preparation method and application thereof.
Background
Cerebrospinal fluid leakage is a relatively common clinical complication in spinal and neurosurgical surgery. The dura mater is ruptured or damaged due to trauma, intraspinal tumor excision, dural dysplasia, dural ossification, involvement of intraspinal operations and the like, and cerebrospinal fluid leakage is caused. If not properly treated, the traditional Chinese medicine composition can cause a plurality of serious complications such as low intracranial pressure syndrome, acute airway obstruction, cerebrospinal fluid cyst, adhesive arachnoiditis, intravertebral infection and intracranial infection, arachnoiditis or meningitis, brain abscess, intracranial hemorrhage and the like, and even can endanger life. Therefore, how to effectively repair the ruptured or defective dura mater to prevent leakage of cerebrospinal fluid is a clinically urgent problem.
Currently, the methods for intraoperative dura mater repair mainly include direct suturing and dura mater replacement material suturing. Wherein, the direct sewing method can achieve the purpose of directly and effectively repairing the dura mater, but for the dura mater with defect in the art, the direct sewing often has overlarge tension, is easy to form clamping pressure on the medullary nerve of a user, needs fine operation, and can damage the spinal cord or the nerve if careless. Because the 'needle eye' caused by sewing the needle during sewing is difficult to achieve absolute watertight sewing, the risk of cerebrospinal fluid leakage still exists after the operation. In addition, suturing is limited for posterior and anterior surgical ventral dural rupture or defect.
Autologous or heterologous tissues (such as muscles, fat, fascia or dura mater and the like) are used as dura mater replacement materials to be matched with tension-reducing suture, so that the dura mater with certain defect can be repaired, but ideal watertight suture is still difficult to achieve, and scar tissue adhesion is easily formed after the dura mater replacement material suture method to cause nerve stimulation symptoms. With the development of biomaterials, more and more novel biomaterials have been applied to repair of dural damage. However, the existing dura mater repair materials generally have the problem of weak adhesion performance, can only be used as an auxiliary adhesive but not used alone, and still need to be covered on the surface of the dura mater after the dura mater is sewed up to achieve the effect of watertight repair. However, in the clinical operation process, the damaged position of the dura mater may be located in front of or at the side of the dura mater or at the nerve root sleeve, and these positions often cannot be sutured effectively, so that even if the artificial dura mater repair is adopted, the problem of poor repair effect still exists, and postoperative cerebrospinal fluid leakage still occurs possibly.
Therefore, the development of an artificial dura mater capable of effectively improving the repairing effect is urgently needed to be solved clinically.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a fiber composite membrane, a preparation method and application thereof. The fiber composite membrane is high in gelling speed, good in biomechanics and adhesion, low in swelling rate and degradable, can be used as an artificial dura mater, and then effectively repairs dura mater damage, and cerebrospinal fluid leakage is avoided.
The invention is realized by the following steps:
in a first aspect, the invention provides a fiber composite membrane for preparing an artificial dura mater, which comprises a core layer and a shell layer wrapping the core layer, wherein the core layer is made of a spinning material-an antibacterial substance, and the shell layer is made of methacrylated polyvinyl alcohol-o-nitrophenyl hyaluronic acid-a photoinitiator.
In an alternative embodiment, the core layer is composed of a collagen-nanoscopic antibacterial material;
preferably, the core layer is composed of type I collagen-nano silver, and the shell layer is composed of methacryloylated polyvinyl alcohol-o-nitrophenyl hyaluronic acid-phenyl-2, 4, 6-trimethylbenzoyl lithium phosphite.
In an alternative embodiment, the thickness of the fiber composite membrane is 100 to 1000 micrometers;
preferably, the fiber composite membrane is a coaxially oriented fiber;
preferably, each layer of fiber in the fiber composite membrane is arranged according to a certain shape and orientation;
preferably, each layer of fibers in the fiber composite membrane are arranged according to a certain orientation, wherein the certain shape of the fibers is a 90-degree rectangle, a 45-degree parallelogram and a 60-degree equilateral triangle;
preferably, each layer of fibers in the fiber composite membrane are arranged and superposed according to the shape orientation of the fibers of the first layer;
preferably, the diameter of the fiber in the fiber composite membrane is 400-1000 nanometers, the pore spacing is 100-300 micrometers, and the porosity is 75-90%.
In a second aspect, the present invention provides a method for preparing a fiber composite film for preparing an artificial dura mater, according to the foregoing embodiment, the spinning material-antibacterial substance and the methacrylated polyvinyl alcohol-o-nitrophenyl hyaluronic acid-photoinitiator are respectively processed by using a near-field direct writing printing technology to construct a core layer and a shell layer, and the shell layer wraps the core layer.
In an alternative embodiment, the preparation of the methacrylated polyvinyl alcohol-o-nitrophenyl hyaluronic acid-photoinitiator comprises: mixing methacryloylated polyvinyl alcohol, o-nitrophenyl hyaluronic acid, a photoinitiator and deionized water to form a mixed solution, wherein the ratio of the methacryloylated polyvinyl alcohol to the o-nitrophenyl hyaluronic acid to the photoinitiator in the mixed solution is as follows: 4-8wv%, 0.5-2wv%, and 0.5wv%.
In an alternative embodiment, the photoinitiator comprises lithium phenyl-2, 4, 6-trimethylbenzoylphosphite.
In an alternative embodiment, the preparation of the acrylated polyvinyl alcohol comprises: mixing polyvinyl alcohol and methacrylic anhydride and then reacting in a dark place;
preferably, the preparation of the acrylated polyvinyl alcohol comprises: dissolving the polyvinyl alcohol, mixing the dissolved polyvinyl alcohol with the methacrylic anhydride, reacting in a dark place, removing unreacted impurities, and freeze-drying by using a vacuum freeze-drying technology;
preferably, the preparation of the acrylated polyvinyl alcohol comprises: mixing the polyvinyl alcohol with deionized water, heating for dissolving, cooling, mixing with the methacrylic anhydride for light-resistant reaction, removing unreacted impurities, and freeze-drying by using a vacuum freeze-drying technology;
preferably, the step of removing unreacted impurities comprises: dialyzing the reacted solution for 6-8 days, and changing the water for dialysis every 4-8 hours;
preferably, the concentration of the polyvinyl alcohol is 4-10%, the dissolving temperature is 75-85 ℃, the cooling temperature is 45-55 ℃, and the ratio of the polyvinyl alcohol to the methacrylic anhydride is 1g:0.8-1.2mL, and the reaction time is 24-48 hours in a dark place.
In an alternative embodiment, the preparation of the spinning material-antibacterial substance comprises: dissolving a spinning material to form a material solution, and then mixing the material solution with an antibacterial substance to form a spinning solution;
wherein, the concentration of the spinning material in the spinning solution is 4-8%, and the concentration of the antibacterial substance in the spinning solution is 1-3mg/L;
preferably, the spun material comprises collagen, more preferably type I collagen;
preferably, the antibiotic substance includes nano silver.
In an alternative embodiment, the parameters of the near-field direct write printing technique include: the voltage is 2-6kV, the extrusion air pressure is 3-12kPa, the room temperature is high, the receiving distance of the electrode plate is 2-6mm, the inner diameter of the core layer spray head is 200-400 mu m, and the inner diameter of the shell layer spray head is 300-450 mu m.
In a third aspect, the present invention provides a use of the fiber composite membrane for preparing an artificial dura mater for spinal applications, as described in the previous embodiments.
The invention has the following beneficial effects: the embodiment of the invention provides a fiber composite membrane with a specific structure, which can be used as a suture-free artificial dura mater spinalis, has good biocompatibility, good biomechanical property, degradability, low swelling rate, high gelling speed and good adhesion property, and can sufficiently resist the pressure of cerebrospinal fluid after being adhered to the dura mater spinalis; meanwhile, the spinal cord and nerve repairing device can be free of suture, greatly shortens operation time, reduces risks of spinal cord and nerve injury, and can effectively reduce postoperative cerebrospinal fluid leakage complications particularly for injury repair of the front and the side of a dura mater and nerve root sleeve positions.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a schematic view of the fiber orientation of a fiber composite membrane provided by an embodiment of the present invention;
FIG. 2 is a schematic view of a coaxial fiber structure of a fiber composite membrane provided by an embodiment of the present invention;
fig. 3 is a schematic diagram illustrating a technical principle of near-field direct-writing printing of a fiber composite film according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The embodiment of the invention provides a fiber composite membrane for preparing an artificial dura mater, which comprises a core layer and a shell layer wrapping the core layer, wherein the core layer is made of a spinning material, namely an antibacterial substance, the spinning material can be collagen, preferably type I collagen, the antibacterial substance can be a nano antibacterial substance, such as nano silver, and the core layer can be made of the collagen, namely the nano antibacterial substance; for example, it is composed of type I collagen-nanosilver.
The shell layer is composed of methacryloylated polyvinyl alcohol-o-nitrobenzene hyaluronic acid-photoinitiator. The photoinitiator can be a photoinitiator in the prior art, but is preferably phenyl-2, 4, 6-trimethylbenzoyl lithium phosphite, which has small side effect on a human body and can ensure the safety of the fiber composite membrane. Thus, the shell layer may be composed of methacryloylated polyvinyl alcohol-o-nitrophenylhyaluronic acid-phenyl-2, 4, 6-trimethylbenzoyl lithium phosphite.
The fiber composite membrane with the structure is high in gelling speed, good in biomechanics and adhesion, low in swelling rate and degradable, can be used as a dura mater, and then can be used for effectively repairing dura mater damage to avoid cerebrospinal fluid leakage. Meanwhile, the antibacterial substance can be slowly released, and the antibacterial effect can be achieved.
Further, the fiber composite film is a coaxially oriented fiber (see fig. 1); each layer of fiber in the fiber composite membrane is arranged in an orientation manner according to a certain shape; for example, each layer of fibers is arranged in an orientation having a shape of 90-degree rectangle, 45-degree parallelogram and 60-degree equilateral triangle (see fig. 2); each layer of fiber in the fiber composite membrane is arranged and superposed according to the shape orientation of the fiber of the first layer; the thickness of the fiber composite membrane is 100-1000 microns; such as any value or range of values between 100-1000 microns, such as 100 microns, 200 microns, 300 microns, 400 microns, 500 microns, 600 microns, 700 microns, 800 microns, 900 microns, 1000 microns, etc., or any two values. The diameter of the fiber in the fiber composite membrane is 400-1000 nanometers, the pore space is 100-300 micrometers, and the porosity is 75-90%.
The embodiment of the invention provides a preparation method of a fiber composite membrane for preparing an artificial dura mater spinalis, which is characterized in that a spinning material, namely an antibacterial substance and a methacrylic acylated polyvinyl alcohol, o-nitrophenyl hyaluronic acid and a photoinitiator are respectively processed by utilizing a near-field direct writing printing technology to construct a core layer and a shell layer, and the core layer is wrapped by the shell layer. In particular, the amount of the solvent to be used,
firstly, adding polyvinyl alcohol (PVA for short in the whole text) into deionized water, performing constant-temperature magnetic stirring under the heating condition to fully dissolve the PVA, then stopping heating, adding methacrylic anhydride after the solution is cooled to a preset temperature, reacting under the dark condition, synthesizing a polyvinyl alcohol-methacrylic anhydride polymer (PVA-MA polymer for short in the whole text), then removing residual unreacted impurities, and performing vacuum freeze drying to obtain white spongy methacryloylated polyvinyl alcohol (PVA-MA for short in the whole text).
The method for removing unreacted impurities comprises the following steps: the solution after the reaction is transferred to a 10kda dialysis bag for dialysis, and deionized water is replaced every 4 to 8 hours for 6 to 8 days (e.g., 6 days, 6.5 days, 7 days, or 8 days) before impurities are removed.
Further, the concentration of polyvinyl alcohol is 4 to 10% (the concentration herein refers to the concentration of polyvinyl alcohol in the reaction mixture), for example, 4%, 5%, 6%, 7%, 8%, 9%, and 10%. The dissolution temperature is 75-85 deg.C, such as 75 deg.C, 76 deg.C, 77 deg.C, 78 deg.C, 79 deg.C, 80 deg.C, 81 deg.C, 82 deg.C, 83 deg.C, 84 deg.C, 85 deg.C, or any two values in the range of values. The predetermined temperature is 45-55 deg.C, such as 45 deg.C, 46 deg.C, 47 deg.C, 48 deg.C, 49 deg.C, 50 deg.C, 51 deg.C, 52 deg.C, 53 deg.C, 54 deg.C, 55 deg.C, or any two values forming a range value between 45-55 deg.C. The ratio of the polyvinyl alcohol to the methacrylic anhydride is 1g:0.8 to 1.2mL, for example, 1g: any value or range of any two values between 0.8 and 1.2 mL. The reaction time is 24-48 hours in a dark place. For example, any value or any two values between 24 and 48 hours such as 24 hours, 30 hours, 32 hours, 34 hours, 36 hours, 40 hours, 42 hours, and 48 hours forms a range value.
And secondly, mixing PVA-MA, o-nitrophenyl hyaluronic acid (HA-NB) and a photoinitiator, such as phenyl-2, 4, 6-trimethyl benzoyl lithium phosphite (LAP), dissolving the mixture in deionized water, and fully dissolving the mixture to obtain a water-soluble mixed solution.
Wherein the ratio of the methacryloylated polyvinyl alcohol, the o-nitrophenyl hyaluronic acid and the photoinitiator in the mixed solution is as follows: 4-8wv%, 0.5-2wv%, and 0.5wv%. wv% refers to the mass of the corresponding substance contained in the mixed solution per unit volume.
Thirdly, dissolving the spinning material to form a material solution, and then mixing the material solution with the antibacterial substance to form a spinning solution; for example, when the adopted spinning solution is type I collagen and the antibacterial substance is nano silver, the operation steps are as follows: dissolving the type I collagen in an acetic acid solution, then adding the nano silver, and fully and uniformly stirring.
Wherein the concentration of the spinning material in the spinning solution is 4-8%, for example, any value or a range value formed by any two values between 4-8% such as 4%, 5%, 6%, 7% and 8%, and the concentration of the antibacterial substance in the spinning solution is 1-3mg/L; for example, 1mg/L, 1.5mg/L, 2mg/L, 2.5mg/L, 3mg/L, and the like, or a range of any two values.
And fourthly, respectively processing the spinning materials, namely the antibacterial substance and the methacryloylated polyvinyl alcohol, the o-nitrobenzene hyaluronic acid and the photoinitiator by using a near-field direct writing printing technology to construct a core layer and a shell layer, and enabling the shell layer to wrap the core layer. See fig. 3.
Wherein the parameters of the near-field direct-write printing technology comprise: the voltage is 2-6kV, the extrusion air pressure is 3-12kPa, the temperature is room temperature, the electrode plate receiving distance is 2-6mm,200-400 μm, and the inner diameter of the shell layer spray head is 300-450 μm.
The invention provides an application of the fiber composite membrane for preparing the artificial dura mater spinalis in preparing the artificial dura mater spinalis.
The invention provides an artificial dura mater spinalis, which is prepared from the fiber composite membrane for preparing the artificial dura mater spinalis. The fiber composite membrane is pasted on an affected part and then irradiated, so that the fiber composite membrane is crosslinked to form stable hydrogel, the surface of the hydrogel can be detected to be smooth, no gap exists between the interface of the hydrogel and the dura mater and is tightly connected, then, the physiological saline is poured into the proximal end of the spinal cord, and the liquid seepage exists at the repaired part without dura mater defect.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a preparation method of a fiber composite membrane, which comprises the following steps:
preparation of PVA-MA: preferably, medical-grade PVA is adopted in this embodiment, and the PVA is sufficiently dissolved in deionized water at a first set temperature (for example, 85 degrees celsius), the concentration of the PVA can be controlled to be 4 to 8%, and when the PVA is dissolved and cooled to a second set temperature (for example, 45 degrees celsius), the PVA is stirred by a constant-temperature magnetic force, and the amount of PVA is 1g: adding methacrylic anhydride into the solution according to the proportion of 1mL of methacrylic anhydride, reacting for 24-48 hours in a dark environment, further transferring into a 10kda dialysis bag for dialysis, changing deionized water once at intervals of 6-8 hours, continuing for 1 week, removing residual unreacted impurities, and performing vacuum freeze drying to obtain white powdery PVA-MA.
1) Respectively taking 2g of PVA-MA, 0.25g of HA-NB and 0.5g of LAP material, mixing, dissolving in deionized water, fully dissolving to obtain a water-soluble PVA-MA/HA-NB/LAP mixed solution, and storing in dark place for later use;
2) Dissolving 2g of type I collagen in an acetic acid solution, adding 1mg/L of nano-silver, and fully and uniformly stirring for later use;
3) Setting technical parameters of near-field direct-write printing: the voltage is 2kV, the extrusion pressure is 3KPa, the room temperature is high, the electrode plate receiving distance is 2mm, the inner diameter of a core layer spray head is 300 mu m, and the inner diameter of a shell layer spray head is 350 mu m. The I-type collagen/nano-silver mixed solution is used as a core, the PVA-MA/HA-NB/LAP mixed solution is used as a shell, a near-field direct-writing printing technology is utilized to construct a fiber membrane with a core layer of the I-type collagen/nano-silver, a shell layer of the PVA-MA/HA-NB/LAP nano-fiber composite membrane, the membrane thickness is set to be 100 mu m, and the fiber membrane with internal formats of 90-degree parallel rectangles, 45-degree parallelograms and 60-degree equilateral triangles is respectively constructed.
The embodiment of the invention provides an application of the fiber composite membrane, which specifically comprises the following steps:
the prepared sterile PVA-MA/HA-NB/LAP/I type collagen/nano silver composite fiber membrane is attached to a bovine cervical spine spinal cord dura mater defect animal model (the dura mater is ligated at the far end of the spinal cord to close the far end), the fiber membrane can quickly absorb water in cerebrospinal fluid or blood and then is converted into a photosensitive gel precursor (the fiber membrane can be soaked by a small amount of physiological saline water directly if necessary), the fiber membrane can be subjected to bending plasticity along the amplitude of the dura mater sac to tightly adhere to the dura mater, the white fiber membrane can be converted into a transparent or semitransparent gel precursor at the moment, the fiber membrane is irradiated by a light source with the wavelength of 405nm for 15-30 seconds, then the fiber membrane quickly completes photocrosslinking to form stable composite hydrogel, the surface of the hydrogel is probed, no gap exists at the interface of the hydrogel and the dura mater is tightly connected, then physiological saline is infused into the near end of the spinal cord, and liquid seeps at the defect position of the dura is not found. Along with the degradation of the hydrogel, the nano silver is slowly released from the type I collagen scaffold, thereby achieving the antibacterial effect.
Example 2
The embodiment provides a preparation method of a fiber composite membrane, which comprises the following steps:
the fiber composite membrane was prepared using 3g of PVA-MA, 0.5g of HA-NB, 0.5g of LAP material, 3g of type I collagen, and 2mg/L of nano-silver as starting materials, and the rest of the procedure was the same as in example 1.
Example 3
The fiber composite membrane was prepared from 4g of PVA-MA, 1g of HA-NB, 0.5g of LAP, 4g of type I collagen, and 3mg/L of nanosilver as starting materials, and the procedure was the same as in example 1.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The fiber composite membrane for preparing the artificial dura mater spinalis is characterized by comprising a core layer and a shell layer wrapping the core layer, wherein the core layer is made of a spinning material-an antibacterial substance, and the shell layer is made of methacryloylated polyvinyl alcohol-o-nitrobenzene hyaluronic acid-a photoinitiator.
2. The fiber composite membrane for preparing an artificial dura mater according to claim 1, wherein the core layer is composed of collagen-nano antibacterial material;
preferably, the core layer is composed of type I collagen-nano silver, and the shell layer is composed of methacryloylated polyvinyl alcohol-o-nitrophenyl hyaluronic acid-phenyl-2, 4, 6-trimethylbenzoyl lithium phosphite.
3. The fiber composite membrane for preparing an artificial dura mater spinalis according to claim 1 or 2, wherein the thickness of the fiber composite membrane is 100-1000 microns;
preferably, the fiber composite membrane is a coaxial oriented fiber;
preferably, each layer of fiber in the fiber composite membrane is arranged according to a certain shape and orientation;
preferably, each layer of fibers in the fiber composite membrane are arranged according to the orientation of a certain shape in a 90-degree rectangle, a 45-degree parallelogram and a 60-degree equilateral triangle;
preferably, each layer of fibers in the fiber composite membrane are arranged and superposed according to the shape orientation of the fibers of the first layer;
preferably, the diameter of the fiber in the fiber composite membrane is 400-1000 nanometers, the pore spacing is 100-300 micrometers, and the porosity is 75-90%.
4. The method of claim 1, wherein the spinning material-antibacterial substance and the methacrylated polyvinyl alcohol-o-nitrophenyl hyaluronic acid-photoinitiator are separately treated by a near-field direct writing printing technique to construct a core layer and a shell layer, and the core layer is wrapped by the shell layer.
5. The method of claim 4, wherein the methacrylated polyvinyl alcohol-o-nitrophenyl hyaluronic acid-photoinitiator is prepared by: mixing methacryloylated polyvinyl alcohol, o-nitrophenyl hyaluronic acid, a photoinitiator and deionized water to form a mixed solution, wherein the ratio of the methacryloylated polyvinyl alcohol to the o-nitrophenyl hyaluronic acid to the photoinitiator in the mixed solution is as follows: 4-8wv%, 0.5-2wv%, 0.5wv%;
preferably, the photoinitiator comprises lithium phenyl-2, 4, 6-trimethylbenzoylphosphite.
6. The method of claim 5, wherein the preparation of the acrylated polyvinyl alcohol comprises: mixing polyvinyl alcohol and methacrylic anhydride and then reacting in a dark place;
preferably, the preparation of the acrylated polyvinyl alcohol comprises: dissolving the polyvinyl alcohol, mixing the dissolved polyvinyl alcohol with the methacrylic anhydride, reacting in a dark place, removing unreacted impurities, and freeze-drying by using a vacuum freeze-drying technology;
preferably, the preparation of the acrylated polyvinyl alcohol comprises: mixing the polyvinyl alcohol with deionized water, heating for dissolving, cooling, mixing with the methacrylic anhydride for light-resistant reaction, removing unreacted impurities, and freeze-drying by using a vacuum freeze-drying technology;
preferably, the step of removing unreacted impurities comprises: dialyzing the reacted solution for 6-8 days, and changing the water for dialysis every 4-8 hours;
preferably, the concentration of the polyvinyl alcohol is 4-10%, the dissolving temperature is 75-85 ℃, the cooling temperature is 45-55 ℃, and the ratio of the polyvinyl alcohol to the methacrylic anhydride is 1g:0.8-1.2mL, and the reaction time is 24-48 hours in dark.
7. The method of manufacturing according to claim 4, wherein the manufacturing of the spinning material-antibacterial substance includes: dissolving a spinning material to form a material solution, and then mixing the material solution with an antibacterial substance to form a spinning solution;
wherein, the concentration of the spinning material in the spinning solution is 4-8%, and the concentration of the antibacterial substance in the spinning solution is 1-3mg/L;
preferably, the spinning material comprises collagen, more preferably type I collagen;
preferably, the antibiotic substance includes nano silver.
8. The production method according to any one of claims 4 to 7, wherein the parameters of the near-field direct-write printing technique include: the voltage is 2-6kV, the extrusion pressure is 3-12kPa, the room temperature is high, the receiving distance of the electrode plate is 2-6mm, the inner diameter of the core layer spray head is 200-400 mu m, and the inner diameter of the shell layer spray head is 300-450 mu m.
9. Use of the fiber composite membrane for preparing an artificial dura mater spinalis according to claim 1 in preparing an artificial dura mater spinalis.
10. An artificial dura mater for spinal applications, which is prepared from the fiber composite film according to claim 1.
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Application publication date: 20221230 |