Polycaprolactone self-diffusion transparent film material and preparation method thereof

Abstract

The invention discloses a polycaprolactone self-diffusion transparent film material and a preparation method thereof. In the preparation process, polycaprolactone is dissolved in an acid solvent to prepare a polycaprolactone solution, then the polycaprolactone solution is dropwise added into a deionized water bath, the polycaprolactone solution spontaneously diffuses on the water surface and then is solidified into a transparent thin film through phase inversion, and the polycaprolactone self-diffusion transparent thin film material is obtained. The preparation process is simple, a support body mold is not needed, the preparation cost is low, the obtained polycaprolactone film has excellent transparency, a film material with antibacterial performance can be obtained by adding an antibacterial material into a polymer solution or a water bath used for preparation, and the polycaprolactone film has wide application in the fields of biology, packaging materials and the like.

Description

Technical Field

[0001] The invention belongs to the technical field of polymer materials, and in particular relates to a polycaprolactone self-diffusion transparent film material and a preparation method thereof. Background Art

[0002] Polycaprolactone (PCL) films have been widely used in biomedicine and other fields due to their biodegradability and good biocompatibility. Currently, the commonly used preparation methods are mainly through solvent evaporation or melt cooling. The resulting PCL film material has low transparency and it is generally difficult to completely separate the film from the mold.

[0003] Non-solvent phase inversion is a common method for preparing asymmetric polymer membranes. This method is to dissolve the polymer in a suitable solvent or solvent mixture to obtain a casting solution; then gently pour the casting solution onto a support, scrape it into a membrane with a scraper, and quickly transfer it to a coagulation bath. At this time, the casting solution and the coagulation bath diffuse in both directions, and the polymer solution finally solidifies into a membrane. However, the preparation of traditional non-solvent phase inversion membranes often requires glass or non-woven fabrics as a support. Summary of the invention

[0004] In order to solve the deficiencies of the prior art, the present invention provides a polycaprolactone self-diffusion transparent film material and a preparation method thereof. The polycaprolactone film material of the present invention has excellent transparency, and is solidified into a film by phase inversion self-diffusion, without the need for a supporting mold, and can obtain a film material with antibacterial properties by adding an antibacterial material to the polymer solution or coagulation bath used in the preparation.

[0005] The technical solution adopted by the present invention is:

[0006] 1. A method for preparing a polycaprolactone self-diffusing transparent film material, the preparation method comprising the following steps:

[0007] S1, fully dissolving polycaprolactone in an acidic solvent, stirring and standing to defoam, to obtain a casting solution;

[0008] S2. Using deionized water as a coagulation bath, slowly drop the casting solution obtained in step S1 into the coagulation bath, and the casting solution spontaneously diffuses on the surface of the coagulation bath and solidifies into a transparent film through phase inversion, thereby obtaining a polycaprolactone self-diffusion transparent film material.

[0009] In step S1, the acidic solvent is formic acid or acetic acid, and may also be a mixed solvent of formic acid and acetic acid in a certain proportion.

[0010] In the step S1, the casting liquid is a 5% to 10% wt polycaprolactone solution.

[0011] In the step S2, the preparation temperature is room temperature.

[0012] In the step S2, the amount of the casting solution added is 0.01-0.03 g.

[0013] 2. A polycaprolactone self-diffusion transparent film material is prepared by a preparation method.

[0014] 3. Application of a polycaprolactone self-diffusing transparent film material in biological dressings or food preservation.

[0015] 4. A method for applying a polycaprolactone self-diffusing transparent film material to a biological dressing: by adding a drug that promotes wound healing to a casting solution or a coagulation bath, a drug-loaded polycaprolactone transparent film is prepared and applied to the wound, such as coating the wound, to visualize the wound healing condition.

[0016] The food is immersed in the casting liquid for 1-2 minutes, then taken out and placed in a coagulation bath for 1-2 minutes. After the food is solidified into a transparent film through phase inversion, the food coated with the film is placed at room temperature to dry.

[0017] The food is, for example, fruit.

[0018] The beneficial effects of the present invention are:

[0019] 1. The polycaprolactone self-diffusing transparent thin film material provided by the present invention has a simple preparation process and low preparation cost;

[0020] 2. The polycaprolactone self-diffusing transparent film material provided by the present invention has excellent transparency;

[0021] 3. The preparation of the polycaprolactone self-diffusion transparent film material provided by the present invention does not require a support mold, can self-diffusion into a film, and has a complete film structure. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is a real picture of the polycaprolactone self-diffusing transparent film material prepared in specific example 1 on the water surface.

[0023] Figure 2 This is a real picture of the polycaprolactone self-diffusing transparent film material obtained in specific example 1 after drying.

[0024] Figure 3 This is a scanning electron microscope image of the front side (exposed to air) of the polycaprolactone self-diffusion transparent film material in specific embodiment 1.

[0025] Figure 4 This is a scanning electron microscope image of the reverse side (contacting the coagulation bath) of the polycaprolactone self-diffusion transparent film material in specific embodiment 1.

[0026] Figure 5This is a diagram of the antibacterial zone experiment of the polycaprolactone self-diffusing transparent film material loaded with antibacterial drugs in specific example 6.

[0027] Figure 6 This is a physical picture of the polycaprolactone self-diffusing opaque film material on the water surface in specific comparative example 1.

[0028] Figure 7 This is a physical picture of the polycaprolactone self-diffusing opaque film material on the water surface in specific comparative example 2. DETAILED DESCRIPTION

[0029] The present invention will be further described in detail below in conjunction with the accompanying drawings and specific embodiments, but the present invention is not limited to the following embodiments.

[0030] Embodiments of the present invention are as follows:

[0031] Embodiment 1:

[0032] (1) Dissolve 1 g of polycaprolactone (PCL) particles in 9 g of acetic acid solvent, stir to dissolve, and let stand to defoam to obtain a casting solution with a PCL concentration of 10%; select deionized water as the coagulation bath.

[0033] (2) A small amount of PCL solution is taken and dropped into the coagulation bath. The PCL solution quickly diffuses in the coagulation bath and gradually solidifies to obtain a PCL film. Figure 1 As shown, the obtained film material is placed in an oven to dry, and the dried PCL film is as shown in Figure 2 The test results of the PCL film front side (in contact with air) are shown in Figure 3 As shown in Figure 2, it can be seen that there are small holes on the surface of the film; the test results of the reverse side of the PCL film (contacting the coagulation bath) are as follows Figure 4 As shown, it can be seen that the surface of the film is smooth and there is no small hole distribution.

[0034] Embodiment 2:

[0035] (1) Dissolve 0.5 g of polycaprolactone (PCL) particles in 9.5 g of acetic acid solvent, stir to dissolve, and let stand to defoam to obtain a casting solution with a PCL concentration of 5%; select deionized water as the coagulation bath.

[0036] (2) A small amount of PCL solution is taken and dropped into the coagulation bath. The PCL solution diffuses rapidly in the coagulation bath and gradually solidifies to obtain a PCL film.

[0037] Embodiment 3:

[0038] (1) Dissolve 0.8 g of polycaprolactone (PCL) particles in 9.2 g of acetic acid solvent, stir to dissolve, and let stand to defoam to obtain a casting solution with a PCL concentration of 8%; select deionized water as the coagulation bath.

[0039] (2) A small amount of PCL solution is taken and dropped into the coagulation bath. The PCL solution diffuses rapidly in the coagulation bath and gradually solidifies to obtain a PCL film.

[0040] Embodiment 4:

[0041] (1) Dissolve 1 g of polycaprolactone (PCL) particles in a mixed solvent of 4.5 g of acetic acid and 4.5 g of formic acid, stir to dissolve, and allow to stand to defoam to obtain a casting solution with a PCL concentration of 10%; select deionized water as a coagulation bath.

[0042] (2) A small amount of PCL solution is taken and dropped into the coagulation bath. The PCL solution diffuses rapidly in the coagulation bath and gradually solidifies to obtain a PCL film.

[0043] Embodiment 5:

[0044] (1) Dissolve 1 g of polycaprolactone (PCL) particles in a mixed solvent of 6 g of acetic acid and 3 g of formic acid, stir to dissolve, and allow to stand to defoam to obtain a casting solution with a PCL concentration of 10%; select deionized water as a coagulation bath.

[0045] (2) A small amount of PCL solution is taken and dropped into the coagulation bath. The PCL solution diffuses rapidly in the coagulation bath and gradually solidifies to obtain a PCL film.

[0046] Embodiment 6:

[0047] (1) Dissolve 1 g of polycaprolactone (PCL) particles in 9 g of acetic acid solvent, stir to dissolve, then add 0.1 g of polyhexamethylene biguanide salt, let stand to defoam, and obtain a casting solution with an antibacterial drug having a PCL concentration of 10%; select deionized water as the coagulation bath.

[0048] (2) A small amount of PCL solution was taken and dropped into the coagulation bath. The PCL solution diffused rapidly in the coagulation bath and gradually solidified to obtain a PCL film. The obtained film was subjected to an inhibition zone test. To facilitate the antibacterial test, the transparent film was placed on a white paper. The results are shown in Figure 2. Figure 5 As shown in the results, it can be seen that the PCL film has an obvious inhibition zone.

[0049] Comparative Example 1:

[0050] (1) Dissolve 1.5 g of polycaprolactone (PCL) particles in 8.5 g of acetic acid solvent, stir to dissolve, and let stand to defoam to obtain a casting solution with a PCL concentration of 15%; select deionized water as the coagulation bath.

[0051] (2) A small amount of PCL solution is taken and dropped into the coagulation bath. The PCL solution diffuses rapidly in the coagulation bath and gradually solidifies to obtain a PCL film. The obtained PCL film is as follows: Figure 6As shown in the results, it can be seen that when the polymer concentration exceeds 10%, a diffusible opaque film of polycaprolactone can be obtained.

[0052] Comparative Example 2:

[0053] (1) Dissolve 1.5 g of polycaprolactone (PCL) particles in 8.5 g of formic acid solvent, stir to dissolve, and let stand to defoam to obtain a casting solution with a PCL concentration of 15%; select deionized water as the coagulation bath.

[0054] (2) A small amount of PCL solution is taken and dropped into the coagulation bath. The PCL solution diffuses rapidly in the coagulation bath and gradually solidifies to obtain a PCL film. The obtained PCL film is as follows: Figure 7 As shown in the results, it can be seen that when the polymer concentration exceeds 10%, a diffusible opaque film of polycaprolactone can be obtained, and the size of the film when the solvent is formic acid is larger than that when the solvent is acetic acid.

[0055] The above specific implementation modes are used to explain the present invention rather than to limit the present invention. Any modification and change made to the present invention within the spirit of the present invention and the protection scope of the claims shall fall within the protection scope of the present invention.

[0056] The above description is only a preferred embodiment of the present invention, so all equivalent changes or modifications made according to the structure, characteristics and principles described in the scope of the patent application of the present invention are included in the scope of the patent application of the present invention.

Claims

1. A method for preparing a polycaprolactone self-diffusing transparent film material, characterized in that: The method comprises the following steps: S1, dissolving polycaprolactone in an acidic solvent, stirring and standing to defoam, to obtain a casting solution; S2. Using deionized water as a coagulation bath, drop the casting solution obtained in step S1 into the coagulation bath, and the casting solution diffuses spontaneously on the surface of the coagulation bath and solidifies into a transparent film through phase inversion, thereby obtaining a polycaprolactone self-diffusion transparent film material.

2. The method for preparing the polycaprolactone self-diffusing transparent thin film material according to claim 1, characterized in that: In the step S1, the acidic solvent is formic acid or acetic acid.

3. The method for preparing the polycaprolactone self-diffusing transparent thin film material according to claim 1, characterized in that: In the step S1, the casting liquid is a 5% to 10% wt polycaprolactone solution.

4. The method for preparing the polycaprolactone self-diffusing transparent thin film material according to claim 1, characterized in that: In the step S2, the preparation temperature is room temperature.

5. The method for preparing the polycaprolactone self-diffusing transparent thin film material according to claim 1, characterized in that: In the step S2, the amount of the casting solution added is 0.01-0.03 g.

6. A polycaprolactone self-diffusion transparent film material, characterized in that: The preparation method is described in any one of claims 1 to 5.

7. Use of the polycaprolactone self-diffusing transparent film material prepared by the preparation method according to any one of claims 1 to 5 in biological dressings or food preservation.

8. A method for applying the polycaprolactone self-diffusing transparent film material prepared by the preparation method according to any one of claims 1 to 5 to a biological dressing, characterized in that: By adding drugs that promote wound healing into the casting solution or the coagulation bath, a drug-loaded polycaprolactone transparent film is prepared and applied to the wound to visualize the wound healing status.

9. A method for preserving food using the polycaprolactone self-diffusing transparent film material prepared by the preparation method according to any one of claims 1 to 5, characterized in that: The food is immersed in the casting liquid for 1-2 minutes, then taken out and placed in a coagulation bath for 1-2 minutes. After the food is solidified into a transparent film through phase inversion, the food coated with the film is placed at room temperature to dry.

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