Medical cast film material as well as preparation method and equipment thereof

Abstract

The invention relates to the technical field of medical material preparation, in particular to a medical cast film material and a preparation method and equipment thereof. Adding EGF gelatin microspheres based on the matrix solution to prepare an inner-layer membrane casting solution; adding nano-silver-loaded mesoporous silica based on the matrix solution to prepare an intermediate layer casting solution; dissolving PU (Polyurethane) and dopamine modified nano SiO2 in DMF (Dimethyl Formamide) to prepare an outer layer membrane casting solution; then casting an outer layer membrane casting solution in a mold at the temperature of 10 DEG C below zero, and curing for 5 minutes; a DA-PEG solution is sprayed; casting a middle layer membrane casting solution on the cured outer layer; casting an inner layer membrane casting solution on the middle layer; and finally, supercritical CO2 drying and gamma-ray irradiation crosslinking are carried out, so that the technical problems that in the prior art, a medical cast film material is insufficient in interlayer bonding strength in clinical application, and the thermal stability of active components is poor are solved.

Description

Technical Field

[0001] The present invention relates to the technical field of medical material preparation, in particular to a medical cast film material and a preparation method and equipment thereof. Background Art

[0002] Medical cast film materials, as an important class of biomedical materials, are widely used in post-surgical wound coverage, tissue repair, adhesion prevention, and as sustained-release drug carriers. Core performance requirements include excellent biocompatibility to prevent immune rejection, suitable mechanical strength to adapt to the complex mechanical environment in the body, a controllable degradation rate to match the tissue regeneration cycle, and multifunctional integration (such as antibacterial, healing-promoting, and adhesion-preventing).

[0003] However, the medical cast film materials in the prior art have insufficient interlayer bonding strength and poor thermal stability of active ingredients in clinical applications. Summary of the Invention

[0004] The purpose of the present invention is to provide a medical cast film material and a preparation method and equipment thereof, aiming to solve the technical problems of insufficient interlayer bonding strength and poor thermal stability of active ingredients in the existing medical cast film materials in clinical applications.

[0005] To achieve the above object, the present invention adopts a medical cast film material comprising a contact layer, an intermediate layer and an outer layer, wherein the intermediate layer is arranged on one side of the outer layer, and the contact layer is arranged on the side of the intermediate layer away from the outer layer;

[0006] The outer layer is polyurethane with a thickness of 20±5 μm;

[0007] The intermediate layer contains silver-loaded mesoporous silica with a silver loading of 8 wt%;

[0008] The contact layer contains EGF gelatin microspheres with a particle size of 10-50 μm.

[0009] The present invention also provides a method for preparing a medical cast film material, which is used to prepare the medical cast film material as described above.

[0010] The steps include:

[0011] First, prepare the matrix solution for use;

[0012] Then, EGF gelatin microspheres were added to the matrix solution to prepare the inner layer casting solution; nanosilver@mesoporous silica was added to the matrix solution to prepare the middle layer casting solution; PU and dopamine-modified nano-SiO2 were dissolved in DMF to prepare the outer layer casting solution;

[0013] Then, the outer layer casting solution was cast in a -10℃ mold and cured for 5 minutes; and the DA-PEG solution was sprayed;

[0014] Casting the intermediate layer casting liquid on the solidified outer layer;

[0015] Just cast the inner layer casting liquid on the middle layer;

[0016] Finally, supercritical CO2 drying and γ-ray irradiation cross-linking were performed.

[0017] The matrix solution is composed of polycaprolactone, silk fibroin, and modified chitosan in a weight ratio of 5:3:2, the solvent is hexafluoroisopropanol, and the solid content is 10 wt%.

[0018] The composition of the inner layer casting solution is as follows: matrix solution + 5 mg / mL EGF gelatin microspheres;

[0019] The composition of the intermediate layer casting solution is as follows: matrix solution + 8wt% nanosilver@mesoporous silica;

[0020] The composition of the outer layer casting solution is as follows: PU+0.5wt% dopamine modified nano-SiO2, and the solvent is DMF.

[0021] When spraying DA-PEG solution on the surface of the cured outer layer, the concentration of DA-PEG solution was 2 mg / mL and the spraying amount was 0.3 mL / cm 2 .

[0022] The present invention also provides a preparation device for preparing the matrix solution in the preparation method of the medical cast film material as described above.

[0023] It includes a frame, two shafts, a stirring tank, a cover plate, a stirring motor, a stirring rod and a synergistic mechanism, one end of the two shafts is rotatably connected to the frame, and the other end of the two shafts is fixedly connected to the stirring tank, the cover plate is arranged on the stirring tank, the stirring motor is installed on the cover plate, the output end of the stirring motor is fixedly connected to the stirring rod, and the synergistic mechanism is arranged on the frame.

[0024] Among them, the efficiency-enhancing mechanism includes a dual-axis motor, a disc, a supporting rod, a force block and a lifting assembly. The dual-axis motor is installed on the frame, and the two output ends of the dual-axis motor are respectively connected to the disc and the lifting assembly. The force block is fixedly connected to one of the shafts, and the force block has a force groove. One end of the supporting rod is fixedly connected to the disc, and the other end of the supporting rod is placed in the force groove.

[0025] Among them, the lifting includes a cam, a sliding part, an arc block and a round rod, the cover plate is slidably connected to the stirring tank, the cam is fixedly connected to the output end corresponding to the dual-axis motor, the sliding part is slidably connected to the frame, the arc block is fixedly connected to the sliding part, the arc block has an arc hole, one end of the round rod is fixedly connected to the cover plate, and the other end of the round rod is placed in the arc hole.

[0026] The present invention discloses a medical cast film material and a preparation method and equipment thereof. When used, first, a matrix solution is prepared for use; then, EGF gelatin microspheres are added to the matrix solution to prepare an inner layer casting solution; nanosilver@mesoporous silica is added to the matrix solution to prepare an intermediate layer casting solution; PU and dopamine-modified nano-SiO2 are dissolved in DMF to prepare an outer layer casting solution; then, the outer layer casting solution is cast in a mold at -10°C and cured for 5 minutes; and a DA-PEG solution is sprayed; the intermediate layer casting solution is cast on the cured outer layer; and the inner layer casting solution is cast on the intermediate layer; finally, supercritical CO2 drying and gamma-ray irradiation cross-linking are performed. In this way, the technical problems of insufficient interlayer bonding strength and poor thermal stability of active ingredients in the medical cast film materials of the prior art in clinical applications are solved.

[0027] In the present invention, a DA-PEG solution is sprayed after the outer layer is cured, and the catechol group of dopamine is used to form a covalent bond with the matrix material (such as PU, PCL), thereby significantly improving the interlayer bonding force.

[0028] In addition, a low-temperature casting process of -10°C to -20°C is used, combined with supercritical CO2 drying (non-thermal solvent removal) and γ-ray irradiation cross-linking (non-thermal cross-linking) to improve the EGF activity retention rate, extend the antibacterial effect of nanosilver, and extend the EGF sustained-release time, thereby achieving efficient protection and long-term release of active ingredients.

[0029] A high-porosity structure (>85%) is formed by supercritical CO2 drying, and γ-ray irradiation is used to induce the formation of a cross-linked network between PCL and SF molecular chains, thereby improving the tensile strength, taking into account both permeability and mechanical properties, and meeting clinical needs for material versatility. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0031] Figure 1 It is a schematic structural diagram of the medical cast membrane material of the present invention.

[0032] Figure 2 The present invention is a flow chart of the method for preparing the medical cast membrane material.

[0033] Figure 3 It is a structural schematic diagram of the preparation equipment of the present invention.

[0034] Figure 4 It is a front view of the preparation equipment of the present invention.

[0035] Figure 5 The present invention Figure 4 AA line structural cross-sectional view.

[0036] Figure 6 The present invention Figure 4 BB line structural cross-sectional view.

[0037] A1-contact layer, A2-middle layer, A3-outer layer, 101-frame, 102-shaft, 103-mixing tank, 104-cover, 105-mixing motor, 106-mixing rod, 107-dual-axis motor, 108-disc, 109-support rod, 110-force block, 111-cam, 112-sliding part, 113-arc block, 114-round rod, 115-force groove, 116-arc hole. DETAILED DESCRIPTION

[0038] The embodiments of the present invention are described in detail below. Examples of the embodiments are shown in the accompanying drawings. The embodiments described below with reference to the accompanying drawings are exemplary and are intended to be used to explain the present invention, but should not be understood as limiting the present invention.

[0039] See also Figure 1 , Figure 1 It is a schematic structural diagram of the medical cast membrane material of the present invention.

[0040] The present invention provides a medical cast film material, comprising a contact layer A1, an intermediate layer A2 and an outer layer A3, wherein the intermediate layer A2 is arranged on one side of the outer layer A3, and the contact layer A1 is arranged on the side of the intermediate layer A2 away from the outer layer A3;

[0041] The outer layer A3 is polyurethane with a thickness of 20±5 μm;

[0042] The intermediate layer A2 contains silver-loaded mesoporous silica with a silver loading of 8 wt%;

[0043] The contact layer A1 contains EGF gelatin microspheres with a particle size of 10-50 μm.

[0044] See also Figure 2 , Figure 2 The present invention is a flow chart of a method for preparing a medical cast film material.

[0045] The present invention also provides a method for preparing a medical cast film material, which is used to prepare the medical cast film material as described above.

[0046] The steps include:

[0047] First, prepare the matrix solution for use;

[0048] Then, EGF gelatin microspheres were added to the matrix solution to prepare the inner layer casting solution; nanosilver@mesoporous silica was added to the matrix solution to prepare the middle layer A2 casting solution; PU and dopamine-modified nano-SiO2 were dissolved in DMF to prepare the outer layer A3 casting solution;

[0049] Then, the outer layer A3 casting solution was cast in a -10℃ mold and cured for 5 minutes; and the DA-PEG solution was sprayed;

[0050] Casting the middle layer A2 casting liquid on the solidified outer layer A3;

[0051] Cast the inner layer casting liquid on the middle layer A2;

[0052] Finally, supercritical CO2 drying and γ-ray irradiation cross-linking were performed.

[0053] The matrix solution is composed of polycaprolactone, silk fibroin, and modified chitosan in a weight ratio of 5:3:2, the solvent is hexafluoroisopropanol, and the solid content is 10 wt%.

[0054] The composition of the inner layer casting solution is as follows: matrix solution + 5 mg / mL EGF gelatin microspheres;

[0055] The composition of the casting solution of the intermediate layer A2 is as follows: matrix solution + 8wt% nanosilver@mesoporous silica;

[0056] The composition of the outer layer A3 casting solution is as follows: PU+0.5wt% dopamine-modified nano-SiO2, and the solvent is DMF.

[0057] When the DA-PEG solution was sprayed on the surface of the cured outer layer A3, the concentration of the DA-PEG solution was 2 mg / mL and the spraying amount was 0.3 mL / cm 2 .

[0058] During specific use, first, a matrix solution is prepared for use; then, EGF gelatin microspheres are added to the matrix solution to prepare an inner layer casting liquid; nanosilver@mesoporous silica is added to the matrix solution to prepare an intermediate layer A2 casting liquid; PU and dopamine-modified nano-SiO2 are dissolved in DMF to prepare an outer layer A3 casting liquid; then, the outer layer A3 casting liquid is cast in a -10°C mold and cured for 5 minutes; and a DA-PEG solution is sprayed; the intermediate layer A2 casting liquid is cast on the cured outer layer A3; the inner layer casting liquid is cast on the intermediate layer A2; finally, supercritical CO2 drying and gamma-ray irradiation cross-linking are performed, thereby solving the technical problems of insufficient interlayer bonding strength and poor thermal stability of active ingredients in the existing medical cast film materials in clinical applications.

[0059] In the present invention, a DA-PEG solution is sprayed after the outer layer A3 is cured, and the catechol group of dopamine is used to form a covalent bond with the matrix material (such as PU, PCL), thereby significantly improving the interlayer bonding force.

[0060] In addition, a low-temperature casting process of -10°C to -20°C is used, combined with supercritical CO2 drying (non-thermal solvent removal) and γ-ray irradiation cross-linking (non-thermal cross-linking) to improve the EGF activity retention rate, extend the antibacterial effect of nanosilver, and extend the EGF sustained-release time, thereby achieving efficient protection and long-term release of active ingredients.

[0061] A high-porosity structure (>85%) is formed by supercritical CO2 drying, and γ-ray irradiation is used to induce the formation of a cross-linked network between PCL and SF molecular chains, thereby improving the tensile strength, taking into account both permeability and mechanical properties, and meeting clinical needs for material versatility.

[0062] See also Figures 3 to 6 ,in Figure 3 It is a structural schematic diagram of the preparation equipment of the present invention. Figure 4 It is a front view of the preparation equipment of the present invention. Figure 5 The present invention Figure 4 AA line structural cross-sectional view. Figure 6 The present invention Figure 4 BB line structural cross-sectional view.

[0063] The present invention also provides a preparation device for preparing the matrix solution in the preparation method of the medical cast film material as described above.

[0064] It includes a frame 101, two shafts 102, a stirring tank 103, a cover 104, a stirring motor 105, a stirring rod 106 and an enhancement mechanism. One end of the two shafts 102 is rotatably connected to the frame 101, and the other end of the two shafts 102 is fixedly connected to the stirring tank 103. The cover 104 is arranged on the stirring tank 103, and the stirring motor 105 is installed on the cover 104. The output end of the stirring motor 105 is fixedly connected to the stirring rod 106, and the enhancement mechanism is arranged on the frame 101.

[0065] According to this specific embodiment, when preparing the matrix solution, the raw materials for preparing the matrix solution are added to the stirring tank 103, and the stirring motor 105 is started. The stirring motor 105 drives the stirring rod 106 to stir and disperse the raw materials. At the same time, the synergistic mechanism is started. The synergistic mechanism drives the two shafts 102 to rotate on the frame 101, and then drives the stirring tank 103 to rotate, driving the material in the stirring tank 103 to shake, thereby improving the stirring and dispersion effect.

[0066] Among them, the efficiency-enhancing mechanism includes a dual-axis motor 107, a disc 108, a supporting rod 109, a force block 110 and a lifting assembly. The dual-axis motor 107 is installed on the frame 101, and the two output ends of the dual-axis motor 107 are respectively connected to the disc 108 and the lifting assembly. The force block 110 is fixedly connected to one of the shafts 102, and the force block 110 has a force groove 115. One end of the supporting rod 109 is fixedly connected to the disc 108, and the other end of the supporting rod 109 is placed in the force groove 115.

[0067] According to this specific embodiment, when the stirring rod 106 stirs and disperses the material, the dual-axis motor 107 is started, and one of the output ends of the dual-axis motor 107 drives the disc 108 to rotate. When the disc 108 rotates, it drives the supporting rod 109 to slide in the force groove 115. The supporting rod 109 slides in the force groove 115 and drives the force block 110 to swing. The swing of the force block 110 can drive the corresponding shaft 102 to rotate on the frame 101, thereby driving the stirring tank 103 to swing.

[0068] Among them, the lifting includes a cam 111, a sliding member 112, an arc block 113 and a round rod 114, the cover plate 104 is slidingly connected to the stirring tank 103, the cam 111 is fixedly connected to the output end corresponding to the dual-axis motor 107, the sliding member 112 is slidingly connected to the frame 101, the arc block 113 is fixedly connected to the sliding member 112, the arc block 113 has an arc hole 116, one end of the round rod 114 is fixedly connected to the cover plate 104, and the other end of the round rod 114 is placed in the arc hole 116.

[0069] For this specific embodiment, when the dual-axis motor 107 is working, the output end of the dual-axis motor 107 away from the disc 108 drives the cam 111 to rotate, and the cam 111 presses against the sliding member 112 to slide on the frame 101, and the sliding member 112 drives the arc block 113 to move upward, and the arc block 113 then drives the cover plate 104 to move upward through the round rod 114. After moving to the specified position, the cam 111 no longer presses against the sliding member 112. At this time, the cover plate 104 is reset with gravity, thereby driving the stirring motor 105 and the stirring rod 106 to move back and forth up and down, further improving the stirring effect.

[0070] The medical cast film material and its preparation method and equipment of the present invention are used as follows: first, a matrix solution is prepared for use; then, EGF gelatin microspheres are added to the matrix solution to prepare an inner layer casting solution; nanosilver@mesoporous silica is added to the matrix solution to prepare an intermediate layer A2 casting solution; PU and dopamine-modified nano-SiO2 are dissolved in DMF to prepare an outer layer A3 casting solution; then, the outer layer A3 casting solution is cast in a -10°C mold and cured for 5 minutes; and a DA-PEG solution is sprayed; the intermediate layer A2 casting solution is cast on the cured outer layer A3; and the inner layer casting solution is cast on the intermediate layer A2; finally, supercritical CO2 drying and gamma-ray irradiation cross-linking are performed, thereby solving the technical problems of insufficient interlayer bonding strength and poor thermal stability of active ingredients in clinical applications of medical cast film materials in the prior art.

[0071] In the present invention, a DA-PEG solution is sprayed after the outer layer A3 is cured, and the catechol group of dopamine is used to form a covalent bond with the matrix material (such as PU, PCL), thereby significantly improving the interlayer bonding force.

[0072] In addition, a low-temperature casting process of -10°C to -20°C is used, combined with supercritical CO2 drying (non-thermal solvent removal) and γ-ray irradiation cross-linking (non-thermal cross-linking) to improve the EGF activity retention rate, extend the antibacterial effect of nanosilver, and extend the EGF sustained-release time, thereby achieving efficient protection and long-term release of active ingredients.

[0073] A high-porosity structure (>85%) is formed by supercritical CO2 drying, and γ-ray irradiation is used to induce the formation of a cross-linked network between PCL and SF molecular chains, thereby improving the tensile strength, taking into account both permeability and mechanical properties, and meeting clinical needs for material versatility.

[0074] In addition, when preparing the matrix solution, the raw materials for preparing the matrix solution are added into the stirring tank 103, and the stirring motor 105 is started. The stirring motor 105 drives the stirring rod 106 to stir and disperse the raw materials. At the same time, the synergistic mechanism is started. The synergistic mechanism drives the two shafts 102 to rotate on the frame 101, and then drives the stirring tank 103 to rotate, driving the material in the stirring tank 103 to shake, thereby improving the stirring and dispersion effect.

[0075] When the stirring rod 106 stirs and disperses the material, the dual-axis motor 107 is started, and one of the output ends of the dual-axis motor 107 drives the disc 108 to rotate. When the disc 108 rotates, it drives the supporting rod 109 to slide in the force groove 115. When the supporting rod 109 slides in the force groove 115, it drives the force block 110 to swing. The swing of the force block 110 can drive the corresponding shaft 102 to rotate on the frame 101, thereby driving the stirring tank 103 to swing.

[0076] When the dual-axis motor 107 is working, the output end of the dual-axis motor 107 away from the disc 108 drives the cam 111 to rotate, and the cam 111 presses against the sliding member 112 to slide on the frame 101, and the sliding member 112 drives the arc block 113 to move upward, and the arc block 113 then drives the cover plate 104 to move upward through the round rod 114. After moving to the specified position, the cam 111 no longer presses against the sliding member 112. At this time, the cover plate 104 is reset with gravity, thereby driving the stirring motor 105 and the stirring rod 106 to move back and forth up and down, further improving the stirring effect.

[0077] The above disclosure is only a preferred embodiment of the present invention, and certainly cannot be used to limit the scope of the rights of the present invention. Ordinary technicians in this field can understand that all or part of the processes of the above embodiment and equivalent changes made in accordance with the claims of the present invention are still within the scope of the invention.

Claims

1. A medical cast film material, characterized in that: It comprises a contact layer, an intermediate layer and an outer layer, wherein the intermediate layer is arranged on one side of the outer layer, and the contact layer is arranged on a side of the intermediate layer away from the outer layer; The outer layer is polyurethane with a thickness of 20±5 μm; The intermediate layer contains silver-loaded mesoporous silica with a silver loading of 8 wt%; The contact layer contains EGF gelatin microspheres with a particle size of 10-50 μm.

2. A method for preparing a medical cast film material, for preparing the medical cast film material according to claim 1, characterized in that: The steps include: First, prepare the matrix solution for use; Then, EGF gelatin microspheres were added to the matrix solution to prepare the inner layer casting solution; nanosilver@mesoporous silica was added to the matrix solution to prepare the middle layer casting solution; PU and dopamine-modified nano-SiO2 were dissolved in DMF to prepare the outer layer casting solution; Then, the outer layer casting solution was cast in a -10°C mold and cured for 5 minutes; and the DA-PEG solution was sprayed; Casting the intermediate layer casting liquid on the solidified outer layer; Just cast the inner layer casting liquid on the middle layer; Finally, supercritical CO2 drying and γ-ray irradiation cross-linking were performed.

3. The method for preparing a medical cast film material according to claim 2, wherein: The matrix solution is composed of polycaprolactone, silk fibroin, and modified chitosan in a weight ratio of 5:3:2, the solvent is hexafluoroisopropanol, and the solid content is 10 wt%.

4. The method for preparing a medical cast film material according to claim 3, wherein: The composition of the inner layer casting solution is as follows: matrix solution + 5 mg / mL EGF gelatin microspheres; The composition of the intermediate layer casting solution is as follows: matrix solution + 8wt% nanosilver@mesoporous silica; The composition of the outer layer casting solution is as follows: PU+0.5wt% dopamine modified nano-SiO2, and the solvent is DMF.

5. The method for preparing a medical cast film material according to claim 4, wherein: When spraying DA-PEG solution on the surface of the cured outer layer, the concentration of DA-PEG solution was 2 mg / mL and the spraying volume was 0.3 mL / cm 2 .

6. A preparation device for preparing the matrix solution in the preparation method of the medical cast film material according to claim 5, characterized in that: It includes a frame, two shafts, a stirring tank, a cover plate, a stirring motor, a stirring rod and a synergistic mechanism, one end of the two shafts is rotatably connected to the frame, and the other end of the two shafts is fixedly connected to the stirring tank, the cover plate is arranged on the stirring tank, the stirring motor is installed on the cover plate, the output end of the stirring motor is fixedly connected to the stirring rod, and the synergistic mechanism is arranged on the frame.

7. The preparation device according to claim 6, characterized in that The efficiency-enhancing mechanism includes a dual-axis motor, a disc, a supporting rod, a force block and a lifting assembly. The dual-axis motor is installed on the frame. The two output ends of the dual-axis motor are respectively connected to the disc and the lifting assembly. The force block is fixedly connected to one of the shafts. The force block has a force groove. One end of the supporting rod is fixedly connected to the disc, and the other end of the supporting rod is placed in the force groove.

8. The preparation device according to claim 7, characterized in that The lifting mechanism includes a cam, a sliding member, an arc block and a round rod. The cover plate is slidably connected to the stirring tank, the cam is fixedly connected to the output end corresponding to the dual-axis motor, the sliding member is slidably connected to the frame, the arc block is fixedly connected to the sliding member, the arc block has an arc hole, one end of the round rod is fixedly connected to the cover plate, and the other end of the round rod is placed in the arc hole.

Images