CN101096424A - A kind of gelatin nanofiber film containing nano silver and its preparation and application - Google Patents
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Abstract
本发明涉及一种含纳米银的明胶纳米纤维膜，包括明胶纳米纤维和均匀地分布在明胶纳米纤维的纳米银，纳米银颗粒附着在明胶的纳米纤维表面或嵌入纤维中，明胶纳米纤维平均直径为60～200nm，纳米银颗粒平均直径为4～50nm。其制备方法采用静电纺丝法：在明胶—甲酸溶液中加入硝酸银制成纺丝液，通过静电纺丝得到含银离子的纳米纤维膜，然后采用紫外光照射的方法，将纤维中的银离子还原成纳米银颗粒。含纳米银的明胶纳米纤维膜可应用于制成人工皮肤、医用敷料、止血材料、卫生棉等产品。
The invention relates to a gelatin nanofiber film containing nanosilver, comprising gelatin nanofibers and nanosilver uniformly distributed in the gelatin nanofibers, nanosilver particles attached to the surface of the gelatin nanofibers or embedded in the fibers, and the average diameter of the gelatin nanofibers 60-200nm, and the average diameter of nano-silver particles is 4-50nm. The preparation method adopts the electrospinning method: silver nitrate is added to the gelatin-formic acid solution to make a spinning solution, and the nanofiber membrane containing silver ions is obtained by electrospinning, and then the silver in the fiber is irradiated by ultraviolet light. The ions are reduced to nano silver particles. The gelatin nanofiber film containing nano-silver can be applied to make artificial skin, medical dressing, hemostatic material, sanitary napkin and other products.
Description
技术领域technical field
本发明涉及纳米纤维膜，具体涉及一种含纳米银的明胶纳米纤维膜及其制备方法和应用。The invention relates to a nanofiber film, in particular to a gelatin nanofiber film containing nano silver and its preparation method and application.
背景技术Background technique
目前纳米纤维的制造已成为世人瞩目的焦点之一。纳米纤维具有较小的直径和较大的比表面积，因此使纳米纤维具有广泛的用途。利用纳米纤维制成的无纺布具有高透气性的特征，再加上纳米纤维具有大的表面积，常用来制成医用敷料以促进伤口复原。纳米纤维膜具有高孔隙率，有利于伤口渗出液的蒸发，避免创面积；且氧气容易透过，有利于创面组织细胞呼吸、上皮组织的生长和再生，加快伤口的愈合。另外，纳米纤维还可用来制作高效率的过滤材料、防护服等。At present, the manufacture of nanofibers has become one of the focuses of the world. Nanofibers have smaller diameters and larger specific surface areas, thus making nanofibers versatile. Non-woven fabrics made of nanofibers have the characteristics of high air permeability, coupled with the large surface area of nanofibers, they are often used to make medical dressings to promote wound recovery. The nanofiber membrane has high porosity, which is conducive to the evaporation of wound exudate and avoids the wound area; and oxygen can easily pass through, which is conducive to the respiration of wound tissue cells, the growth and regeneration of epithelial tissue, and accelerates wound healing. In addition, nanofibers can also be used to make high-efficiency filter materials, protective clothing, etc.
银具有广谱抗菌的效果，是一种天然抗菌材料，使用也比较安全，因此具有广泛的使用范围。目前以纳米技术的方式制成或形成纳米级银细微颗粒，可以使银的活性变大，抗菌效果增强。将纳米银附着在纤维上可以成为抗菌纤维和抗菌面料。将纳米银复合到医用敷料中制成抗菌敷料，具有杀菌、抗炎、促进伤口愈合等诸多功效。在纳米纤维上附着纳米银，通常采用浸渍和涂布的方式，使纳米银附着于纳米纤维上而形成纳米银纤维。这些以浸渍或涂布的方法很难得到直径小至几个纳米的银颗粒，而且银颗粒在纤维表面上的分布难以达到非常均匀，同时还会使纳米银的使用量增大。采用静电纺丝的方法可以在纳米纤维中掺入纳米银，增强抗菌效果。Silver has a broad-spectrum antibacterial effect, is a natural antibacterial material, and is relatively safe to use, so it has a wide range of applications. At present, nano-scale silver fine particles are made or formed by means of nanotechnology, which can increase the activity of silver and enhance the antibacterial effect. Attaching nano silver to fibers can become antibacterial fibers and antibacterial fabrics. Compounding nano-silver into medical dressings to make antibacterial dressings has many functions such as sterilization, anti-inflammation, and promotion of wound healing. Nano-silver is attached to the nano-fiber, usually by means of impregnation and coating, so that the nano-silver is attached to the nano-fiber to form the nano-silver fiber. These impregnation or coating methods are difficult to obtain silver particles with a diameter as small as several nanometers, and the distribution of silver particles on the fiber surface is difficult to achieve very uniform, while also increasing the amount of nano-silver used. Nano-silver can be mixed into nanofibers by electrospinning to enhance the antibacterial effect.
在专利CN1851087A中涉及到用静电纺丝法制备含纳米银的纤维网，其方法是将纳米银颗粒均匀混合在聚丙烯溶液中形成纺丝液，再进行静电纺丝将纳米银颗粒掺入纤维中。这种方法制得的含纳米银纤维存在两个方面的缺点：一是纳米银颗粒的直径较大，为100～500纳米；二是纳米银粉体在聚合物溶液的混合过程中容易发生团聚，难以分散均匀。In the patent CN1851087A, it involves the preparation of fiber webs containing nano-silver by electrospinning. The method is to uniformly mix nano-silver particles in polypropylene solution to form a spinning solution, and then carry out electrospinning to incorporate nano-silver particles into the fiber. middle. There are two disadvantages in the nano-silver fiber prepared by this method: one is that the diameter of the nano-silver particles is relatively large, which is 100-500 nanometers; the other is that the nano-silver powder is prone to agglomeration during the mixing process of the polymer solution. , it is difficult to disperse evenly.
本发明是将纳米银的前驱体——硝酸银加入到明胶溶液中制成均匀的纺丝液，通过静电纺丝将银离子混入纤维中，然后通过光照还原的方法将纤维中的银离子还原成纳米银颗粒。这样纳米银颗粒直径可很小，低至几个纳米，而且纳米银颗粒可均匀地分布在纤维膜中，可利用纳米银的抗菌效果制成人工皮肤、医用敷料、止血材料、卫生棉等产品。In the present invention, silver nitrate, the precursor of nano-silver, is added to the gelatin solution to make a uniform spinning solution, and silver ions are mixed into the fiber by electrospinning, and then the silver ions in the fiber are reduced by the method of light reduction into silver nanoparticles. In this way, the diameter of nano-silver particles can be very small, as low as several nanometers, and nano-silver particles can be evenly distributed in the fiber film, and the antibacterial effect of nano-silver can be used to make artificial skin, medical dressings, hemostatic materials, sanitary napkins and other products. .
发明内容Contents of the invention
本发明要解决的技术问题之一是克服现有技术中纳米颗粒较大，纳米银粉体难以分散均匀的缺陷，提供了一种纳米银颗粒直径很小，纳米银颗粒可均匀地分布在纤维膜中的含纳米银的明胶纳米纤维膜。本发明提供的含纳米银的明胶纳米纤维膜包括明胶纳米纤维和均匀地分布在明胶纳米纤维的纳米银，利用明胶这种天然高分子材料，通过静电纺丝的方法在纳米纤维中嵌入纳米银或使纳米银附着在纤维表面上，明胶纳米纤维直径为60～200纳米，纳米银颗粒平均直径4～50nm。One of the technical problems to be solved by the present invention is to overcome the defects in the prior art that the nanoparticles are large and the nano-silver powder is difficult to disperse uniformly. A gelatin nanofiber film containing nanosilver in the film. The gelatin nanofiber film containing nanosilver provided by the present invention comprises gelatin nanofibers and nanosilver uniformly distributed in the gelatin nanofibers, utilizes gelatin, a natural polymer material, to embed nanosilver in the nanofibers by electrospinning Or make the nano-silver adhere to the surface of the fiber, the diameter of the gelatin nano-fiber is 60-200 nm, and the average diameter of the nano-silver particle is 4-50 nm.
本发明所要解决的另一技术问题是提供了一种含纳米银的明胶纳米纤维膜的制备方法，本制备方法采用静电纺丝方法，包括下列步骤：Another technical problem to be solved by the present invention is to provide a kind of preparation method of the gelatin nanofiber film containing nano silver, this preparation method adopts electrospinning method, comprises the following steps:
(1)制备明胶溶液：将明胶溶于甲酸中，磁力搅拌至完全溶解，呈透明的、亮黄色液体，即明胶-甲酸溶液；(1) Preparation of gelatin solution: dissolve gelatin in formic acid, stir magnetically until completely dissolved, and become transparent, bright yellow liquid, i.e. gelatin-formic acid solution;
(2)制备明胶-硝酸银溶液：在(1)制备的明胶-甲酸溶液中加入硝酸银粉末，继续搅拌1小时，至硝酸银完全溶解；(2) Prepare gelatin-silver nitrate solution: add silver nitrate powder to the gelatin-formic acid solution prepared in (1), and continue stirring for 1 hour until silver nitrate is completely dissolved;
(3)将(2)中制备的明胶-硝酸银溶液移入塑料针管中进行静电纺丝，静电纺丝工艺条件为：静电压为14～32千伏，接受距离为6～24厘米，纺丝速率为0.4毫升/小时，喷丝孔内径0.7毫米，纺丝在室温下进行；(3) Move the gelatin-silver nitrate solution prepared in (2) into a plastic needle tube for electrostatic spinning. The rate is 0.4 ml/hour, the inner diameter of the spinneret hole is 0.7 mm, and the spinning is carried out at room temperature;
(4)将静电纺丝制得的纳米纤维膜用紫外光照射进行光还原，使纤维中的银离子变成纳米银颗粒，其中纳米银颗粒大部分分布在纤维的表面；(4) The nanofiber film prepared by electrospinning is irradiated with ultraviolet light for photoreduction, so that the silver ions in the fiber become nano-silver particles, wherein most of the nano-silver particles are distributed on the surface of the fiber;
步骤(1)中的甲酸质量浓度为70％～90％；所得明胶-甲酸溶液浓度为14％～22％(克/毫升)；The mass concentration of formic acid in step (1) is 70% to 90%; the concentration of the obtained gelatin-formic acid solution is 14% to 22% (g/ml);
步骤(2)中所加入硝酸银粉末浓度为0.3％～6％。The concentration of the silver nitrate powder added in the step (2) is 0.3%-6%.
本发明所采用的静电纺丝方法制备的纳米银纤维膜可使纳米银与纳米纤维一次成形，让纳米银颗粒附着在明胶的纳米纤维表面或嵌入纤维中而形成纳米银纤维膜，可以有效地减少纳米银的脱落和团聚现象，避免了直接加入纳米银粉体，而且可减少制作纳米银纤维的银添加量，使形成的纳米银在纤维膜中更均匀地分布。The nano-silver fiber film prepared by the electrospinning method adopted in the present invention can form the nano-silver and the nano-fiber at one time, and allow the nano-silver particle to attach to the surface of the nano-fiber of gelatin or embed it in the fiber to form a nano-silver fiber film, which can effectively Reduce the shedding and agglomeration of nano-silver, avoid the direct addition of nano-silver powder, and reduce the amount of silver added to make nano-silver fibers, so that the formed nano-silver is more evenly distributed in the fiber film.
利用纳米银的抗菌效果，本发明的含纳米银的明胶纳米纤维膜可应用于制成人工皮肤、医用敷料、止血材料、卫生棉等产品。Utilizing the antibacterial effect of nano-silver, the gelatin nanofiber film containing nano-silver of the present invention can be applied to make artificial skin, medical dressing, hemostatic material, sanitary napkin and other products.
附图说明Description of drawings
图1实施例1所制得的纳米纤维膜材料的扫描电镜图；The scanning electron micrograph of the nanofiber membrane material that Fig. 1 embodiment 1 makes;
图2实施例2所制得的纳米纤维膜材料的扫描电镜图；The scanning electron micrograph of the nanofiber membrane material that Fig. 2 embodiment 2 makes;
图3实施例1所制得的纳米纤维膜材料的透射电镜图；The transmission electron microscope figure of the nanofiber membrane material that Fig. 3 embodiment 1 makes;
图4实施例2所制得的纳米纤维膜材料的透射电镜图。The transmission electron micrograph of the nanofiber membrane material prepared in embodiment 2 of Fig. 4 .
具体实施方式Detailed ways
下面结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。Below in conjunction with specific embodiment, further illustrate the present invention. It should be understood that these examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art may make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims of the present application.
实施例1Example 1
准确称取1.5克医用级明胶溶于10毫升甲酸浓溶液中，甲酸浓度为88％，密封后常温下磁力搅拌，待明胶完全溶解后加入0.0075克的硝酸银粉末，密封后继续在常温下磁力搅拌，待硝酸银完全溶解后形成亮黄色透明液体，静置15分钟后将纺丝液转移至塑料注射器中，电压为22kV，注射泵推进速度为0.4ml/h，采用铝箔接收，接收距离为14cm，喷丝孔直径为0.7mm，在铝箔上得到静电纺明胶/银纳米纤维膜，40℃下真空干燥24h，置于紫外灯下照射3h，得到含纳米银的明胶纳米纤维膜。得到的纤维平均直径为105nm，银颗粒的平均直径为11nm。Accurately weigh 1.5 grams of medical grade gelatin and dissolve it in 10 milliliters of formic acid concentrated solution. The formic acid concentration is 88%. After sealing, stir magnetically at room temperature. After the gelatin is completely dissolved, add 0.0075 grams of silver nitrate powder. After sealing, continue to magnetically stir at room temperature. Stir until the silver nitrate is completely dissolved to form a bright yellow transparent liquid. After standing still for 15 minutes, transfer the spinning solution to a plastic syringe with a voltage of 22kV and a syringe pump with a speed of 0.4ml/h. Aluminum foil is used for receiving, and the receiving distance is 14cm, spinneret diameter is 0.7mm, electrospun gelatin/silver nanofiber membrane was obtained on aluminum foil, vacuum dried at 40°C for 24h, placed under ultraviolet light for 3h, and gelatin nanofiber membrane containing nanosilver was obtained. The average diameter of the obtained fibers was 105 nm, and the average diameter of the silver particles was 11 nm.
实施例2Example 2
准确称取1.5克医用级明胶溶于10毫升甲酸浓溶液中，甲酸浓度为88％，密封后常温下磁力搅拌，待明胶完全溶解后加入0.0150克的硝酸银粉末，密封后继续在常温下磁力搅拌，待硝酸银完全溶解后形成亮黄色透明液体，静置15分钟后将纺丝液转移至塑料注射器中，电压为22kV，注射泵推进速度为0.4ml/h，采用铝箔接收，接收距离为14cm，喷丝孔直径为0.7mm，在铝箔上得到静电纺明胶/银纳米纤维膜，40℃下真空干燥24h，置于紫外灯下照射3h，得到含纳米银的明胶纳米纤维膜。得到的纤维平均直径为126nm，银颗粒的平均直径为13nm。Accurately weigh 1.5 grams of medical grade gelatin and dissolve it in 10 milliliters of formic acid concentrated solution. The formic acid concentration is 88%. After sealing, stir magnetically at room temperature. After the gelatin is completely dissolved, add 0.0150 grams of silver nitrate powder. After sealing, continue to magnetically stir at room temperature. Stir until the silver nitrate is completely dissolved to form a bright yellow transparent liquid. After standing still for 15 minutes, transfer the spinning solution to a plastic syringe with a voltage of 22kV and a syringe pump with a speed of 0.4ml/h. Aluminum foil is used for receiving, and the receiving distance is 14cm, spinneret diameter is 0.7mm, electrospun gelatin/silver nanofiber membrane was obtained on aluminum foil, vacuum dried at 40°C for 24h, placed under ultraviolet light for 3h, and gelatin nanofiber membrane containing nanosilver was obtained. The average diameter of the obtained fibers was 126 nm, and the average diameter of the silver particles was 13 nm.
实施例3Example 3
准确称取1.5克医用级明胶溶于10毫升甲酸浓溶液中，甲酸浓度为88％，密封后常温下磁力搅拌，待明胶完全溶解后加入0.0300克的硝酸银粉末，密封后继续在常温下磁力搅拌，待硝酸银完全溶解后形成亮黄色透明液体，静置15分钟后将纺丝液转移至塑料注射器中，电压为22kV，注射泵推进速度为0.4ml/h，采用铝箔接收，接收距离为14cm，喷丝孔直径为0.7mm，在铝箔上得到静电纺明胶/银纳米纤维膜，40℃下真空干燥24h，置于紫外灯下照射3h，得到含纳米银的明胶纳米纤维膜。得到的纤维平均直径为165nm，银颗粒的平均直径为17nm。Accurately weigh 1.5 grams of medical grade gelatin and dissolve it in 10 milliliters of formic acid concentrated solution, the concentration of formic acid is 88%. After sealing, stir magnetically at room temperature. After the gelatin is completely dissolved, add 0.0300 grams of silver nitrate powder. After sealing, continue to magnetically stir at room temperature. Stir until the silver nitrate is completely dissolved to form a bright yellow transparent liquid. After standing still for 15 minutes, transfer the spinning solution to a plastic syringe with a voltage of 22kV and a syringe pump with a speed of 0.4ml/h. Aluminum foil is used for receiving, and the receiving distance is 14cm, spinneret diameter is 0.7mm, electrospun gelatin/silver nanofiber membrane was obtained on aluminum foil, vacuum dried at 40°C for 24h, placed under ultraviolet light for 3h, and gelatin nanofiber membrane containing nanosilver was obtained. The average diameter of the obtained fibers was 165 nm, and the average diameter of the silver particles was 17 nm.
实施例4Example 4
准确称取1.5克医用级明胶溶于10毫升甲酸浓溶液中，甲酸浓度为88％，密封后常温下磁力搅拌，待明胶完全溶解后加入0.0450克的硝酸银粉末，密封后继续在常温下磁力搅拌，待硝酸银完全溶解后形成亮黄色透明液体，静置15分钟后将纺丝液转移至塑料注射器中，电压为22kV，注射泵推进速度为0.4ml/h，采用铝箔接收，接收距离为14cm，喷丝孔直径为0.7mm，在铝箔上得到静电纺明胶/银纳米纤维膜，40℃下真空干燥24h，置于紫外灯下照射3h，得到含纳米银的明胶纳米纤维膜。得到的纤维平均直径为189nm，银颗粒的平均直径为23nm。Accurately weigh 1.5 grams of medical grade gelatin and dissolve it in 10 milliliters of formic acid concentrated solution, the concentration of formic acid is 88%. After sealing, stir magnetically at room temperature. After the gelatin is completely dissolved, add 0.0450 grams of silver nitrate powder. After sealing, continue to magnetically stir at room temperature. Stir until the silver nitrate is completely dissolved to form a bright yellow transparent liquid. After standing still for 15 minutes, transfer the spinning solution to a plastic syringe with a voltage of 22kV and a syringe pump with a speed of 0.4ml/h. Aluminum foil is used for receiving, and the receiving distance is 14cm, spinneret hole diameter is 0.7mm, get electrospun gelatin/silver nanofiber film on aluminum foil, vacuum dry at 40 ℃ for 24h, put it under ultraviolet lamp for 3h, get the gelatin nanofiber film containing nano silver. The average diameter of the obtained fibers was 189 nm, and the average diameter of the silver particles was 23 nm.
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| CN109675084A (en) * | 2018-12-17 | 2019-04-26 | 深圳先进技术研究院 | Antiseptic dressing and its preparation method and application |
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| CN115216039A (en) * | 2022-08-18 | 2022-10-21 | 广东省科学院生物与医学工程研究所 | Preparation method and application of degradable antibacterial film |
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