技术领域technical field
本发明涉及一种碳纳米管-细胞生长因子复合敷料的制备方法。 The invention relates to a preparation method of a carbon nanotube-cell growth factor composite dressing. the
背景技术Background technique
皮肤起着保护机体内环境并维持其稳定的作用，皮肤烧、创伤后治疗的最终目标就是促进创面愈合，重建或恢复皮肤屏障功能。随着对伤口愈合研究机制的深入，人们认识到使用敷料的目的远远不止是为了覆盖创面，还应具有吸附分泌物、杀灭细菌和促进伤口愈合的多重功效。纳米敷料具有很强的吸附性，能起到抗菌膜屏障作用，防止创面感染、出血，促进创面修复而成为近年来的研究热点。碳纳米管敷料是目前比较成熟的纳米辅料，具有一定的抗菌及促进创面愈合的疗效，并且毒副作用小，使用方便。但碳纳米管敷料的缺点是吸水性较差，随体性欠佳，对创面黏附性强，给换药带来一定的困难，还不能很好地促进创面愈合，因此有待于进一步研究改进。 The skin plays a role in protecting the internal environment of the body and maintaining its stability. The ultimate goal of skin burn and post-traumatic treatment is to promote wound healing and rebuild or restore the skin barrier function. With the in-depth research on the mechanism of wound healing, people realized that the purpose of using dressings is not only to cover the wound surface, but also to have multiple functions of absorbing secretions, killing bacteria and promoting wound healing. Nano dressings have strong adsorption, can act as an antibacterial film barrier, prevent wound infection and bleeding, and promote wound repair, which has become a research hotspot in recent years. Carbon nanotube dressing is a relatively mature nano-adjuvant at present, which has certain antibacterial and wound healing effects, and has less toxic and side effects and is easy to use. However, the disadvantages of carbon nanotube dressings are poor water absorption, poor body adaptability, strong adhesion to the wound surface, which brings certain difficulties to dressing changes, and cannot promote wound healing well, so further research and improvement are needed. the
发明内容Contents of the invention
本发明旨在提供一种碳纳米管-细胞生长因子复合敷料的制备方法。 The invention aims to provide a preparation method of a carbon nanotube-cell growth factor composite dressing. the
为了达到上述目的，本发明包括以下步骤： In order to achieve the above object, the present invention comprises the following steps:
1． 酸化碳纳米管： 1. Acidified carbon nanotubes:
（1）酸化碳纳米管：将85%-98.3%（重量百分比）的浓硫酸20～100ml 、 65%-85%（重量百分比）的浓硝酸10～50 ml和粒径为30 nm～500 nm碳纳米管0.1g～2.0g分散均匀后再放入60℃～100℃水浴中酸化0.5 h～2 h； (1) Acidify carbon nanotubes: add 85%-98.3% (weight percent) concentrated sulfuric acid 20-100ml, 65%-85% (weight percent) concentrated nitric acid 10-50ml and particle size 30nm-500nm 0.1g～2.0g of carbon nanotubes are uniformly dispersed and then acidified in a 60℃～100℃ water bath for 0.5h～2h;
（2）抽滤洗涤：用孔径为0.11μm-0. 33μm的抽滤膜进行抽滤，并用蒸馏水洗涤至洗涤液pH值5.0～8.0； (2) Suction filtration and washing: use a suction filtration membrane with a pore size of 0.11 μm-0.33 μm for suction filtration, and wash with distilled water until the pH value of the washing solution is 5.0-8.0;
（3）干燥称重：将经步骤（2）滤出的碳纳米管在40℃-70℃烘干； (3) Drying and weighing: dry the carbon nanotubes filtered out in step (2) at 40°C-70°C;
（4）溶解离心计算：将（3）得到的碳纳米管溶于50 ml蒸馏水中，室温超声分散0.5 h -3h， 再在8000rpm-20000rpm离心5mins～30 mins，然后沉淀干燥； (4) Calculation of dissolution and centrifugation: Dissolve the carbon nanotubes obtained in (3) in 50 ml of distilled water, disperse them ultrasonically at room temperature for 0.5 h -3 h, then centrifuge at 8000 rpm-20000 rpm for 5 mins to 30 mins, and then precipitate and dry;
2．制备碳纳米管-聚乙烯醇-细胞生长因子复合溶液： 2. Preparation of carbon nanotube-polyvinyl alcohol-cell growth factor composite solution:
(1)将碳纳米管加入去离子水分散均匀。 (1) Add carbon nanotubes to deionized water to disperse evenly. the
(2）以所得碳纳米管分散液为液体介质，加入聚乙烯醇中。在60℃～100℃下水浴加热，搅拌均匀； (2) Using the obtained carbon nanotube dispersion as a liquid medium, add it to polyvinyl alcohol. Heat in a water bath at 60°C to 100°C and stir evenly;
（3）向经上述步骤所得的溶液里面加入细胞生长因子粉剂或者细胞生长因子溶液，使细胞生长因子终浓度为0.01μg/ml～1000μg/ml，室温磁力振荡或者超声分散0.5 h～8 h。生物电镜表征显示其再将其分散均匀。 (3) Add cell growth factor powder or cell growth factor solution to the solution obtained through the above steps, so that the final concentration of cell growth factor is 0.01 μg/ml-1000 μg/ml, magnetically shake or ultrasonically disperse at room temperature for 0.5 h-8 h. Bioelectron microscopy characterization showed that it dispersed evenly. the
3．静电纺织： 3. Electrospinning:
将碳纳米管-聚乙烯醇-细胞生长因子复合溶液进行静电纺丝，设定电压范围20kv～70kv（10-200）。 Electrospin the carbon nanotube-polyvinyl alcohol-cell growth factor composite solution, and set the voltage range from 20kv to 70kv (10-200). the
采用本发明的制备方法可得到组织均匀、发珠较少，纤维平直、连续、直径均一的碳纳米管－聚乙烯醇-细胞生长因子复合无纺布材料，由这些纤维形成的无纺布是一种有纳米微孔的多孔材料，因此有更大的比表面积，并且层中孔隙保证了空气的流通，可阻隔水等液体的深入，这样不仅可以有效地保护伤口、防止感染，而且保证了伤口的通风，同时采用本发明的制备方法可很好地复合细胞生长因子而作为药物载体形成缓释控释体系，促进伤口的愈合，有利于伤口尽快复原。且很好地保证了细胞生长因子的活性 The preparation method of the present invention can obtain a carbon nanotube-polyvinyl alcohol-cell growth factor composite non-woven fabric material with uniform structure, fewer hair beads, straight, continuous and uniform diameter fibers, and the non-woven fabric formed by these fibers It is a porous material with nano-micropores, so it has a larger specific surface area, and the pores in the layer ensure the circulation of air and block the penetration of liquids such as water, which can not only effectively protect wounds and prevent infection, but also ensure Ventilation of the wound is improved, and at the same time, the preparation method of the present invention can be well compounded with cell growth factors and used as a drug carrier to form a slow-release and controlled-release system, which can promote wound healing and facilitate wound recovery as soon as possible. And well ensure the activity of cell growth factors
具体实施方式Detailed ways
实施例1： Example 1:
1． 酸化碳纳米管： 1. Acidified carbon nanotubes:
（1）酸化碳纳米管：将85%-98.3%的浓硫酸60ml 、 65%-85%的浓硝酸20 ml和粒径为30 nm～500 nm碳纳米管0.1g～2.0g超声分散0.5 h -3h，再放入60℃～100℃水浴中酸化0.5 h～2 h； (1) Acidification of carbon nanotubes: Ultrasonic dispersion of 60ml of 85%-98.3% concentrated sulfuric acid, 20ml of 65%-85% concentrated nitric acid and 0.1g-2.0g of carbon nanotubes with a particle size of 30 nm to 500 nm for 0.5 h -3h, then acidified in a water bath at 60°C to 100°C for 0.5h to 2h;
（2）抽滤洗涤：用孔径为0.11μm-0. 33μm的抽滤膜进行抽滤，并用蒸馏水洗涤至洗涤液pH值5.0～8.0； (2) Suction filtration and washing: use a suction filtration membrane with a pore size of 0.11 μm-0.33 μm for suction filtration, and wash with distilled water until the pH value of the washing solution is 5.0-8.0;
（3）干燥称重：将经步骤（2）滤出的碳纳米管在40℃-70℃烘干； (3) Drying and weighing: dry the carbon nanotubes filtered out in step (2) at 40°C-70°C;
（4）溶解离心计算：将（3）得到的碳纳米管溶于50 ml蒸馏水中，室温超声分散0.5 h -3h， 再在8000rpm-20000rpm离心5mins～30 mins，然后沉淀干燥； (4) Calculation of dissolution and centrifugation: Dissolve the carbon nanotubes obtained in (3) in 50 ml of distilled water, disperse them ultrasonically at room temperature for 0.5 h -3 h, then centrifuge at 8000 rpm-20000 rpm for 5 mins to 30 mins, and then precipitate and dry;
2．制备碳纳米管-聚乙烯醇-细胞生长因子复合溶液： 2. Preparation of carbon nanotube-polyvinyl alcohol-cell growth factor composite solution:
(1)将酸化得到的碳纳米管10mg放入烧杯中，加入去离子水1000ml，5 W～100 W磁力搅拌0.1 h～6 h，再10khz-40 khz频率超声分散0.5 h～3 h，得到均一、稳定、无沉淀的分散溶液。(2）以所得碳纳米管水分散液为液体介质，加入0.01ml-10ml（质量分数为1%-50%）的聚乙烯醇。在60℃～100℃下水浴加热1 h～3 h。持续搅拌，以保证最终所得为均一、稳定、不出现沉淀或者絮凝的分散液。 (1) Put 10 mg of acidified carbon nanotubes into a beaker, add 1000 ml of deionized water, stir with 5 W ~ 100 W magnetic force for 0.1 h ~ 6 h, and then ultrasonically disperse at 10khz-40khz frequency for 0.5 h ~ 3 h to obtain Uniform, stable, precipitate-free dispersion solution. (2) Using the obtained carbon nanotube water dispersion as a liquid medium, add 0.01ml-10ml (mass fraction: 1%-50%) of polyvinyl alcohol. Heat in a water bath at 60°C to 100°C for 1 h to 3 h. Stir continuously to ensure that the final result is a uniform, stable dispersion without precipitation or flocculation. the
（3）向经上述步骤所得的溶液里面加入细胞生长因子粉剂或者细胞生长因子溶液，使细胞生长因子终浓度为0.01μg/ml～1000μg/ml，室温磁力振荡或者超声分散0.5 h～8 h直至分散均匀。 (3) Add cell growth factor powder or cell growth factor solution to the solution obtained through the above steps, so that the final concentration of cell growth factor is 0.01 μg/ml to 1000 μg/ml, magnetic oscillation or ultrasonic dispersion at room temperature for 0.5 h to 8 h until Disperse evenly. the
3．静电纺织： 3. Electrospinning:
将碳纳米管-聚乙烯醇-细胞生长因子复合溶液倒入注射器中，并将注射器固定在注射泵上。打开高压发生器，开始静电纺丝，在收集介质（金属箔）上收集所得样品。设定电压范围20kv～70kv，进行静电纺织，得到无纺布。 Pour the carbon nanotube-polyvinyl alcohol-cell growth factor composite solution into the syringe, and fix the syringe on the syringe pump. Turn on the high voltage generator, start electrospinning, and collect the resulting sample on a collection medium (metal foil). The voltage range is set to 20kv-70kv, and electrostatic spinning is carried out to obtain non-woven fabrics. the
采用本发明的制备方法可得到组织均匀、发珠较少，纤维平直、连续、直径均一的碳纳米管－聚乙烯醇复合无纺布材料，由这些纤维形成的无纺布是一种有纳米微孔的多孔材料，因此有更大的比表面积，并且层中孔隙保证了空气的流通，可阻隔水等液体的深入，这样不仅可以有效地保护伤口、防止感染，而且保证了伤口的通风，同时采用本发明的制备方法可很好地复合细胞生长因子而作为药物载体 形成缓释控释体系，促进伤口的愈合，有利于伤口尽快复原。 Adopting the preparation method of the present invention can obtain the carbon nanotube-polyvinyl alcohol composite non-woven fabric material with uniform structure, fewer hair beads, straight, continuous and uniform diameter fibers, and the non-woven fabric formed by these fibers is an effective The nano-microporous porous material has a larger specific surface area, and the pores in the layer ensure the circulation of air and block the penetration of liquids such as water. This can not only effectively protect the wound and prevent infection, but also ensure the ventilation of the wound. At the same time, the preparation method of the present invention can be well compounded with cell growth factors and used as a drug carrier to form a slow-release and controlled-release system, which can promote wound healing and facilitate wound recovery as soon as possible. the
实施例2： Example 2:
1． 酸化碳纳米管： 1. Acidified carbon nanotubes:
（1）酸化碳纳米管：将85%-98.3%的浓硫酸60ml 、 65%-85%的浓硝酸20 ml和粒径为30 nm～500 nm碳纳米管0.1g～2.0g超声分散0.5 h -3h，再放入60℃～100℃水浴中酸化0.5 h～2 h； (1) Acidification of carbon nanotubes: Ultrasonic dispersion of 60ml of 85%-98.3% concentrated sulfuric acid, 20ml of 65%-85% concentrated nitric acid and 0.1g-2.0g of carbon nanotubes with a particle size of 30 nm to 500 nm for 0.5 h -3h, then acidified in a water bath at 60°C to 100°C for 0.5h to 2h;
（2）抽滤洗涤：用孔径为0.11μm-0. 33μm的抽滤膜进行抽滤，并用蒸馏水洗涤至洗涤液pH值5.0～8.0； (2) Suction filtration and washing: use a suction filtration membrane with a pore size of 0.11 μm-0.33 μm for suction filtration, and wash with distilled water until the pH value of the washing solution is 5.0-8.0;
（3）干燥称重：将经步骤（2）滤出的碳纳米管在40℃-70℃烘干； (3) Drying and weighing: dry the carbon nanotubes filtered out in step (2) at 40°C-70°C;
（4）溶解离心计算：将（3）得到的碳纳米管溶于50 ml蒸馏水中，室温超声分散0.5 h -3h， 再在8000rpm-20000rpm离心5mins～30 mins，然后沉淀干燥； (4) Calculation of dissolution and centrifugation: Dissolve the carbon nanotubes obtained in (3) in 50 ml of distilled water, disperse them ultrasonically at room temperature for 0.5 h -3 h, then centrifuge at 8000 rpm-20000 rpm for 5 mins to 30 mins, and then precipitate and dry;
2．制备碳纳米管-聚乙烯醇-细胞生长因子复合溶液： 2. Preparation of carbon nanotube-polyvinyl alcohol-cell growth factor composite solution:
(1)将酸化得到的碳纳米管10mg放入烧杯中，加入去离子水1000ml，5 W～100 W磁力搅拌0.1 h～6 h，再10khz-40 khz频率超声分散0.5 h～3 h，得到均一、稳定、无沉淀的分散溶液。(2）以所得碳纳米管水分散液为液体介质，加入0.01ml-10ml（质量分数为1%-50%）的聚乙烯醇。在60℃～100℃下水浴加热1 h～3 h。持续搅拌，以保证最终所得为均一、稳定、不出现沉淀或者絮凝的分 散液。 (1) Put 10 mg of acidified carbon nanotubes into a beaker, add 1000 ml of deionized water, stir with 5 W ~ 100 W magnetic force for 0.1 h ~ 6 h, and then ultrasonically disperse at 10khz-40khz frequency for 0.5 h ~ 3 h to obtain Uniform, stable, precipitate-free dispersion solution. (2) Using the obtained carbon nanotube water dispersion as a liquid medium, add 0.01ml-10ml (mass fraction: 1%-50%) of polyvinyl alcohol. Heat in a water bath at 60°C to 100°C for 1 h to 3 h. Stir continuously to ensure that the final result is a uniform, stable dispersion without precipitation or flocculation. the
（3）向经上述步骤所得的溶液里面加入细胞生长因子粉剂或者细胞生长因子溶液，使细胞生长因子终浓度为0.01μg/ml～1000μg/ml，室温磁力振荡或者超声分散0.5 h～8 h直至分散均匀。 (3) Add cell growth factor powder or cell growth factor solution to the solution obtained through the above steps, so that the final concentration of cell growth factor is 0.01 μg/ml to 1000 μg/ml, magnetic oscillation or ultrasonic dispersion at room temperature for 0.5 h to 8 h until Disperse evenly. the
3．静电纺织： 3. Electrospinning:
将碳纳米管-聚乙烯醇-细胞生长因子复合溶液进行静电纺丝，设定电压范围20kv～70kv。 The carbon nanotube-polyvinyl alcohol-cell growth factor composite solution is electrospun, and the voltage range is set to 20kv-70kv. the
采用本发明的制备方法可得到组织均匀、发珠较少，纤维平直、连续、直径均一的碳纳米管－聚乙烯醇复合无纺布材料，由这些纤维形成的无纺布是一种有纳米微孔的多孔材料，因此有更大的比表面积，并且层中孔隙保证了空气的流通，可阻隔水等液体的深入，这样不仅可以有效地保护伤口、防止感染，而且保证了伤口的通风，同时采用本发明的制备方法可很好地复合细胞生长因子而作为药物载体形成缓释控释体系，促进伤口的愈合，有利于伤口尽快复原。 Adopting the preparation method of the present invention can obtain the carbon nanotube-polyvinyl alcohol composite non-woven fabric material with uniform structure, fewer hair beads, straight, continuous and uniform diameter fibers, and the non-woven fabric formed by these fibers is an effective The nano-microporous porous material has a larger specific surface area, and the pores in the layer ensure the circulation of air and block the penetration of liquids such as water. This can not only effectively protect the wound and prevent infection, but also ensure the ventilation of the wound. , and at the same time, the preparation method of the present invention can be well compounded with cell growth factors and used as a drug carrier to form a slow-release and controlled-release system, which can promote wound healing and facilitate wound recovery as soon as possible. the
实施例3： Example 3:
1． 酸化碳纳米管： 1. Acidified carbon nanotubes:
（1）酸化碳纳米管：将85%-98.3%的浓硫酸60ml 、 65%-85%的浓硝酸20 ml和粒径为30 nm～500 nm碳纳米管0.1g～2.0g超声分散0.5 h -3h，再放入60℃～100℃水浴中酸化0.5 h～2 h； (1) Acidification of carbon nanotubes: Ultrasonic dispersion of 60ml of 85%-98.3% concentrated sulfuric acid, 20ml of 65%-85% concentrated nitric acid and 0.1g-2.0g of carbon nanotubes with a particle size of 30 nm to 500 nm for 0.5 h -3h, then acidified in a water bath at 60°C to 100°C for 0.5h to 2h;
（2）抽滤洗涤：用孔径为0.11μm-0. 33μm的抽滤膜进行抽滤，并用蒸馏水洗涤至洗涤液pH值5.0～8.0； (2) Suction filtration and washing: use a suction filtration membrane with a pore size of 0.11 μm-0.33 μm for suction filtration, and wash with distilled water until the pH value of the washing solution is 5.0-8.0;
（3）干燥称重：将经步骤（2）滤出的碳纳米管在40℃-70℃烘干； (3) Drying and weighing: dry the carbon nanotubes filtered out in step (2) at 40°C-70°C;
（4）溶解离心计算：将（3）得到的碳纳米管溶于50 ml蒸馏水中，室温超声分散0.5 h -3h， 再在8000rpm-20000rpm离心5mins～30 mins，然后沉淀干燥； (4) Calculation of dissolution and centrifugation: Dissolve the carbon nanotubes obtained in (3) in 50 ml of distilled water, disperse them ultrasonically at room temperature for 0.5 h -3 h, then centrifuge at 8000 rpm-20000 rpm for 5 mins to 30 mins, and then precipitate and dry;
2．制备碳纳米管-聚乙烯醇-细胞生长因子复合溶液： 2. Preparation of carbon nanotube-polyvinyl alcohol-cell growth factor composite solution:
(1)将酸化得到的碳纳米管10mg放入烧杯中，加入去离子水1000ml，5 W～100 W磁力搅拌0.1 h～6 h，再10khz-40 khz频率超声分散0.5 h～3 h，得到均一、稳定、无沉淀的分散溶液。 (1) Put 10 mg of acidified carbon nanotubes into a beaker, add 1000 ml of deionized water, stir with 5 W ~ 100 W magnetic force for 0.1 h ~ 6 h, and then ultrasonically disperse at 10khz-40khz frequency for 0.5 h ~ 3 h to obtain Uniform, stable, precipitate-free dispersion solution. the
(2）以所得碳纳米管水分散液为液体介质，加入0.01ml-10ml（质量分数为1%-50%）的聚乙烯醇。在60℃～100℃下水浴加热1 h～3 h。持续搅拌，以保证最终所得为均一、稳定、不出现沉淀或者絮凝的分散液。 (2) Using the obtained carbon nanotube water dispersion as a liquid medium, add 0.01ml-10ml (mass fraction: 1%-50%) of polyvinyl alcohol. Heat in a water bath at 60°C to 100°C for 1 h to 3 h. Stir continuously to ensure that the final result is a uniform, stable dispersion without precipitation or flocculation. the
（3）向经上述步骤所得的溶液里面加入细胞生长因子粉剂或者细胞生长因子溶液，使细胞生长因子终浓度为0.01μg/ml～1000μg/ml，室温磁力振荡或者超声分散0.5 h～8 h直至分散均匀。 (3) Add cell growth factor powder or cell growth factor solution to the solution obtained through the above steps, so that the final concentration of cell growth factor is 0.01 μg/ml to 1000 μg/ml, magnetic oscillation or ultrasonic dispersion at room temperature for 0.5 h to 8 h until Disperse evenly. the
3．静电纺织： 3. Electrospinning:
将碳纳米管-聚乙烯醇-细胞生长因子复合溶液进行静电纺丝，设定电压范围20kv～70kv。 The carbon nanotube-polyvinyl alcohol-cell growth factor composite solution is electrospun, and the voltage range is set to 20kv-70kv. the
采用本发明的制备方法可得到组织均匀、发珠较少，纤维平直、连续、直径均一的碳纳米管－聚乙烯醇复合无纺布材料，由这些纤维形成的无纺布是一种有纳米微孔的多孔材料，因此有更大的比表面 积，并且层中孔隙保证了空气的流通，可阻隔水等液体的深入，这样不仅可以有效地保护伤口、防止感染，而且保证了伤口的通风，同时采用本发明的制备方法可很好地复合细胞生长因子而作为药物载体形成缓释控释体系，促进伤口的愈合，有利于伤口尽快复原。 Adopting the preparation method of the present invention can obtain the carbon nanotube-polyvinyl alcohol composite non-woven fabric material with uniform structure, fewer hair beads, straight, continuous and uniform diameter fibers, and the non-woven fabric formed by these fibers is an effective Nano-microporous porous material, so it has a larger specific surface area, and the pores in the layer ensure the circulation of air and block the penetration of liquids such as water, which can not only effectively protect the wound and prevent infection, but also ensure the wound's health. Ventilation, and at the same time, the preparation method of the present invention can be well compounded with cell growth factors and used as a drug carrier to form a slow-release and controlled-release system, which can promote wound healing and facilitate wound recovery as soon as possible. the
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210330471XACN103041439A (en) | 2012-09-07 | 2012-09-07 | Carbon nanotube-cell growth factor composite dressing and preparation method thereof |
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210330471XACN103041439A (en) | 2012-09-07 | 2012-09-07 | Carbon nanotube-cell growth factor composite dressing and preparation method thereof |
| Publication Number | Publication Date |
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| CN103041439Atrue CN103041439A (en) | 2013-04-17 |
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210330471XAPendingCN103041439A (en) | 2012-09-07 | 2012-09-07 | Carbon nanotube-cell growth factor composite dressing and preparation method thereof |
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| CN106994188A (en)* | 2017-03-30 | 2017-08-01 | 中南大学湘雅三医院 | A kind of dressing repaired for radiotherapy |
| CN113398311A (en)* | 2021-05-25 | 2021-09-17 | 周建大 | Polymeric composite protective membrane loaded with nano antibacterial peptide, preparation method and application |
| CN113398311B (en)* | 2021-05-25 | 2022-08-02 | 周建大 | Polymeric composite protective membrane loaded with nano antibacterial peptide, preparation method and application |
| CN114159613A (en)* | 2021-11-08 | 2022-03-11 | 江苏大学 | A kind of antibacterial hemostatic composite dressing and preparation method thereof |
| CN114917394A (en)* | 2022-06-24 | 2022-08-19 | 宁夏医科大学 | Double-layer composite functional dressing carrying nano silver and growth factors and preparation method thereof |
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