CN103451849A - Nano-silver containing polybutylene succinate nano-fiber membrane, preparation method thereof and application - Google Patents
Nano-silver containing polybutylene succinate nano-fiber membrane, preparation method thereof and application Download PDFInfo
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- CN103451849A CN103451849A CN201210174899XA CN201210174899A CN103451849A CN 103451849 A CN103451849 A CN 103451849A CN 201210174899X A CN201210174899X A CN 201210174899XA CN 201210174899 A CN201210174899 A CN 201210174899A CN 103451849 A CN103451849 A CN 103451849A
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Abstract
The invention discloses a nano-silver containing polybutylene succinate nano-fiber membrane, a preparation method thereof and application. The nano-fiber membrane has fine biocompatibility, biodegradability, excellent mechanical and machining performances and effective broad-spectrum and long-acting antibacterial performance, silver nitrate is reduced into nano-silver particles in ethanol solution by taking PBS (polybutylene succinate) as base materials and by taking PVP (polyvinylpyrrolidone) as a stabilizing agent and a reducing agent, and the nano-silver particles are loaded in nano-fibers of the PBS by electrostatic spinning to obtain the nano-silver containing polybutylene succinate nano-fiber membrane. The nano-fiber membrane can be used for wound dressings, antibacterial filter membranes and medical devices.
Description
Technical field
The invention belongs to the nanofiber field, relate to especially poly butylene succinate nano fibrous membrane containing Nano Silver and its preparation method and application.
Background technology
The polymer nanofibre film for preparing the loading nano silvery particle by electrospinning becomes the hot issue of recent researcher's extensive concern.This nano composite material combines the special performance of nano-Ag particles and the excellent properties of polymer nanofiber.The polymer nanofibre film of electrospinning has the special performances such as specific area is large, porosity is high, at biomedical sectors such as tissue engineering bracket, skin repair and wound dressings, has broad application prospects.
The Nano Silver of diameter between 1-100nm has the physicochemical property more stable than conventional silver, higher surface-activity and lower toxicity in vivo.Aspect antibacterial applications, due to small size effect quantum effect and great specific area, Nano Silver has the antibacterial effect stronger than traditional inorganic antiseptic, and silver element can not make bacterium produce drug resistance, silver nano-grain is incorporated in polymer nanofiber, can give fiber effective anti-infective performance, thereby further enlarge its range of application at biomedical sector.
Poly butylene succinate (PBS) is a kind of novel biodegradable aliphatic polyester, there is the advantages such as good degradability, biocompatibility, mechanical property, processability, and, than PLGA, PGA, PLA etc., the production cost of PBS is lower.Correlative study shows that PBS can be used as a kind of potential biomaterial and is applied to the biomedical sectors such as organizational project, medicine release.Suttiphong has prepared the PBS nano fiber non-woven fabric and has studied its potential as tissue engineering material by electrostatic spinning technique.Because the PBS nano fiber non-woven fabric has distinctive character-high porosity, microcellular structure and large specific area, than general thin, to Gegenbaur's cell (SaOs-2), adhesion, growth and the activity on material has obvious facilitation to nano fiber non-woven fabric.But the PBS composite prepared containing Nano Silver by electrostatic spinning up to now, have not been reported.
Usually when preparing the electrospun fiber membrane of nano-Ag particles, can adopt at electrospinning process situ and generate nano-Ag particles, but this needs the cosolvent of selective polymer and silver ion, this cosolvent need to have good compatibility, and polymer need possess specific chemical group in order to can produce strong interaction with silver atoms, this just makes the electrospun fiber membrane for preparing nano-Ag particles be subject to the selection of cosolvent and the restriction of polymer chemistry structure, applicability a little less than.
Therefore, need to provide a kind of method for preparing the electrospun fiber membrane of nano-Ag particles, it can not be subject to the restriction of cosolvent and polymer chemistry structure, and applicability is strong.
Summary of the invention
First technical problem that the present invention will solve is to provide the poly butylene succinate nano fibrous membrane containing Nano Silver; This nano fibrous membrane has good biocompatibility, biological degradability, excellent mechanics and processing characteristics, also has potent, wide spectrum and long-acting anti-microbial property simultaneously.
Second technical problem that the present invention will solve is to provide the preparation method containing the poly butylene succinate nano fibrous membrane of Nano Silver; But by take PBS as base material, take polyvinylpyrrolidone PVP as stabilizing agent and reductant, be nano-Ag particles by silver nitrate reduction in ethanolic solution, by electrostatic spinning, nano-Ag particles be carried in the nanofiber of PBS, obtain the poly butylene succinate nano fibrous membrane containing Nano Silver.
The 3rd technical problem that the present invention will solve is to provide the application containing the poly butylene succinate nano fibrous membrane of Nano Silver, and it can be used for wound dressing, antibiotic filter membrane, medical device.
For solving the problems of the technologies described above, the invention provides the poly butylene succinate nano fibrous membrane containing Nano Silver, it is comprised of Nano Silver and poly butylene succinate fiber, nano-Ag particles is evenly distributed on poly butylene succinate fiber, wherein, fibre diameter is 50 ~ 500nm, and the nano-Ag particles diameter is 2 ~ 15nm.
110 ~ 120 ℃ of the fusing points of described poly butylene succinate, molecular weight 5 ~ 200,000.
For solving the problems of the technologies described above, the invention provides the preparation method containing the poly butylene succinate nano fibrous membrane of Nano Silver, comprise the following steps:
1) preparation of Nano Silver:
The ethanolic solution of silver nitrate is mixed with the ethanolic solution of polyvinylpyrrolidone, be stirred to solution colour and become peony by water white transparency, and no longer change, obtain the ethanolic solution containing nano-Ag particles;
2) contain the electrospinning of the poly butylene succinate fiber film of Nano Silver:
Poly butylene succinate is dissolved, the ethanolic solution containing nano-Ag particles that step 1) is obtained joins in poly butylene succinate solution, carry out electrostatic spinning after stirring, receive nano silk, obtain the poly butylene succinate nano fibrous membrane containing Nano Silver.
Further, in described step 1), the ethanolic solution concentration of silver nitrate is 0.001 ~ 0.03g/ml.
Further, in described step 1), the ethanolic solution concentration of polyvinylpyrrolidone is 0.02 ~ 0.2g/ml.
Further, in described step 1), the ethanolic solution of silver nitrate heats and stirs under 40 ~ 60 ℃ of conditions after mixing with the ethanolic solution of polyvinylpyrrolidone.
Further, the volume ratio containing the chloroformic solution of the ethanolic solution of nano-Ag particles and PBS described step 2) is 0.01 ~ 0.25.
Further, described step 2) in, the electrostatic spinning process parameter is as follows: voltage 15 ~ 30KV, and receiving range is 10 ~ 20cm, the empty internal diameter 0.2mm ~ 0.8mm of spinning, spinning speed is 30 ~ 80ul/min.
Described step 2) in, with aluminium foil or stainless steel stent, receive nano silk.
Step 2) nano fibrous membrane made at normal temperatures, vacuumize, can preserve afterwards.
For solving the problems of the technologies described above, the invention provides the application containing the poly butylene succinate nano fibrous membrane of Nano Silver, it can be used as wound dressing, antibiotic filter membrane, medical device.
The invention has the advantages that:
The present invention utilizes the distinctive chemical constitution of polyvinylpyrrolidone (PVP), when preparing nano-Ag particles, PVP can reduce on the one hand silver ion, can play the effect of stabilizing agent at the silver-colored particle surface of reduction by uniform fold again simultaneously, preparation process is simple, nano-Ag particles size uniform easy to operate, as to obtain, particle diameter is little;
The nano fibrous membrane that the present invention adopts method of electrostatic spinning to prepare can just be attached to previously prepared good nano-Ag particles one step in nanofiber, is not subject to the restriction of cosolvent and polymer chemistry structure, and applicability is strong;
The present invention uses nano-Ag particles, and its small-size effect, quantum effect and great specific area, have the antibacterial effect stronger than traditional inorganic antiseptic, makes the nano fibrous membrane made can be used as wound dressing, antibiotic filter membrane, medical device etc.
The accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the Nano Silver that makes of embodiment 1/PBS tunica fibrosa;
Fig. 2 is the transmission electron microscope picture of the Nano Silver that makes of embodiment 1/PBS tunica fibrosa;
Fig. 3 is the scanning electron microscope (SEM) photograph of the Nano Silver that makes of embodiment 2/PBS tunica fibrosa;
Fig. 4 is the transmission electron microscope picture of the Nano Silver that makes of embodiment 2/PBS tunica fibrosa.
The specific embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is further described.
Embodiment 1
Contain the preparation method of the poly butylene succinate nano fibrous membrane of Nano Silver, comprise the following steps:
Take 0.03 gram silver nitrate and 0.5 gram PVP is dissolved in respectively in the 10ml ethanolic solution, be stirred to fully and dissolve, the ethanolic solution of silver nitrate is added to rapidly in the ethanolic solution of PVP, be heated to 50 ° of C simultaneously, stir, become peony by water white transparency to solution colour, and no longer change, obtain stable nano-Ag particles;
Take 0.6 gram PBS and be dissolved in the 4ml chloroformic solution, be stirred to PBS and dissolve fully; The ethanolic solution of getting the nano-Ag particles of the above-mentioned preparation of 1ml joins in the chloroformic solution of PBS, stir until solution mixes, carry out electrospinning after standing, voltage is 20KV, and the syringe pump fltting speed is 50ul/min, and receiving range is 15cm, orifice diameter is 0.5mm, receive with aluminium foil, obtain the PBS nano fibrous membrane containing Nano Silver of electrospinning, vacuumize seals preservation after 24 hours.
Average fibre diameter is 450nm, and the average diameter of nano-Ag particles is 5nm.
Fig. 1 is the scanning electron microscope (SEM) photograph of the Nano Silver that makes of embodiment 1/PBS tunica fibrosa.
Fig. 2 is the transmission electron microscope picture of the Nano Silver that makes of embodiment 1/PBS tunica fibrosa.
Embodiment 2
Contain the preparation method of the poly butylene succinate nano fibrous membrane of Nano Silver, comprise the following steps:
Take 0.12 gram silver nitrate and 0.5 gram PVP is dissolved in respectively in the 10ml ethanolic solution, be stirred to fully and dissolve, the ethanolic solution of silver nitrate is added to rapidly in the ethanolic solution of PVP, be heated to 50 ° of C simultaneously, stir, become peony by water white transparency to solution colour, and no longer change, now obtain stable nano-Ag particles.
Take 0.6 gram PBS and be dissolved in the 4ml chloroformic solution, be stirred to PBS and dissolve fully; The ethanolic solution of getting the nano-Ag particles of the above-mentioned preparation of 1ml joins in the chloroformic solution of PBS, stir until solution mixes, carry out electrospinning after standing, voltage is 20KV, and the syringe pump fltting speed is 50ul/min, and receiving range is 15cm, orifice diameter is 0.5mm, receive with aluminium foil, obtain the PBS nano fibrous membrane containing Nano Silver of electrospinning, vacuumize seals preservation after 24 hours.
Average fibre diameter is 300nm, and the average diameter of nano-Ag particles is 8nm.
Fig. 3 is the scanning electron microscope (SEM) photograph of the Nano Silver that makes of embodiment 2/PBS tunica fibrosa.
Fig. 4 is the transmission electron microscope picture of the Nano Silver that makes of embodiment 2/PBS tunica fibrosa.
Embodiment 3
Contain the preparation method of the poly butylene succinate nano fibrous membrane of Nano Silver, comprise the following steps:
1) preparation of Nano Silver:
The ethanolic solution of silver nitrate is mixed with the ethanolic solution of polyvinylpyrrolidone, be stirred to solution colour and become peony by water white transparency, and no longer change, obtain the ethanolic solution containing nano-Ag particles;
2) contain the electrospinning of the poly butylene succinate fiber film of Nano Silver:
Poly butylene succinate is dissolved in chloroform, the ethanolic solution containing nano-Ag particles that step 1) is obtained joins in the chloroformic solution of poly butylene succinate, carry out electrostatic spinning after stirring, receive nano silk, obtain the poly butylene succinate nano fibrous membrane containing Nano Silver;
Wherein, in described step 1), the ethanolic solution concentration of silver nitrate is 0.001g/ml; In described step 1), the ethanolic solution concentration of polyvinylpyrrolidone is 0.02g/ml; Described step 2) volume ratio containing the chloroformic solution of the ethanolic solution of nano-Ag particles and PBS in is 0.01; Described step 2) in, the electrostatic spinning process parameter is as follows: voltage 15KV, and receiving range is 10cm, the empty internal diameter 0.2mm of spinning, spinning speed is 30ul/min.
Embodiment 4
Contain the preparation method of the poly butylene succinate nano fibrous membrane of Nano Silver, comprise the following steps:
1) preparation of Nano Silver:
The ethanolic solution of silver nitrate is mixed with the ethanolic solution of polyvinylpyrrolidone, be stirred to solution colour and become peony by water white transparency, and no longer change, obtain the ethanolic solution containing nano-Ag particles;
2) contain the electrospinning of the poly butylene succinate fiber film of Nano Silver:
Poly butylene succinate is dissolved in chloroform, the ethanolic solution containing nano-Ag particles that step 1) is obtained joins in the chloroformic solution of poly butylene succinate, carry out electrostatic spinning after stirring, receive nano silk, obtain the poly butylene succinate nano fibrous membrane containing Nano Silver;
Wherein, in described step 1), the ethanolic solution concentration of silver nitrate is 0.03g/ml; In described step 1), the ethanolic solution concentration of polyvinylpyrrolidone is 0.2g/ml; Described step 2) volume ratio containing the chloroformic solution of the ethanolic solution of nano-Ag particles and PBS in is 0.25; Described step 2) in, the electrostatic spinning process parameter is as follows: voltage 30KV, and receiving range is 20cm, the empty internal diameter 0.8mm of spinning, spinning speed is 80ul/min.
Obviously, the above embodiment of the present invention is only for example of the present invention clearly is described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here can't give all embodiments exhaustive.Every still row in protection scope of the present invention of apparent variation that technical scheme of the present invention extends out or change that belong to.
Claims (10)
1. contain the poly butylene succinate nano fibrous membrane of Nano Silver, it is characterized in that, it is comprised of Nano Silver and poly butylene succinate fiber, and nano-Ag particles is distributed on poly butylene succinate fiber, fibre diameter is 50 ~ 500nm, and the nano-Ag particles diameter is 2 ~ 15nm.
2. the poly butylene succinate nano fibrous membrane containing Nano Silver according to claim 1, is characterized in that 110 ~ 120 ℃ of the fusing points of described poly butylene succinate, molecular weight 5 ~ 200,000.
3. the preparation method of the poly butylene succinate nano fibrous membrane containing Nano Silver as claimed in claim 1 or 2, is characterized in that, comprises the following steps:
1) preparation of Nano Silver:
The ethanolic solution of silver nitrate is mixed with the ethanolic solution of polyvinylpyrrolidone, be stirred to solution colour and become peony by water white transparency, and no longer change, obtain the ethanolic solution containing nano-Ag particles;
2) contain the electrospinning of the poly butylene succinate fiber film of Nano Silver:
Poly butylene succinate is dissolved, the ethanolic solution containing nano-Ag particles that step 1) is obtained joins in poly butylene succinate solution, carry out electrostatic spinning after stirring, receive nano silk, obtain the poly butylene succinate nano fibrous membrane containing Nano Silver.
4. the preparation method of the poly butylene succinate nano fibrous membrane containing Nano Silver according to claim 3, is characterized in that, in described step 1), the ethanolic solution concentration of silver nitrate is 0.001 ~ 0.03g/ml.
5. the preparation method of the poly butylene succinate nano fibrous membrane containing Nano Silver according to claim 3, is characterized in that, in described step 1), the ethanolic solution concentration of polyvinylpyrrolidone is 0.02 ~ 0.2g/ml.
6. the preparation method of the poly butylene succinate nano fibrous membrane containing Nano Silver according to claim 3, it is characterized in that, in described step 1) the ethanolic solution of silver nitrate with under 40 ~ 60 ℃ of conditions, stir after the ethanolic solution of polyvinylpyrrolidone mixes.
7. the preparation method of the poly butylene succinate nano fibrous membrane containing Nano Silver according to claim 3, is characterized in that described step 2) in, poly butylene succinate is dissolved in chloroform.
8. the preparation method of the poly butylene succinate nano fibrous membrane containing Nano Silver according to claim 3, is characterized in that described step 2) in containing the volume ratio of the chloroformic solution of the ethanolic solution of nano-Ag particles and PBS, be 0.01 ~ 0.25.
9. the preparation method of the poly butylene succinate nano fibrous membrane containing Nano Silver according to claim 3, it is characterized in that, described step 2) in, the electrostatic spinning process parameter is as follows: voltage 15 ~ 30KV, receiving range is 10 ~ 20cm, the empty internal diameter 0.2mm ~ 0.8mm of spinning, spinning speed is 30 ~ 80ul/min.
10. according to the application of the arbitrary described poly butylene succinate nano fibrous membrane containing Nano Silver of claim 1 ~ 9, it is characterized in that, it can be used as wound dressing, antibiotic filter membrane, medical device.
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| CN104814542A (en) * | 2015-04-22 | 2015-08-05 | 中国科学院理化技术研究所 | Biodegradable environment-friendly mask |
| CN104872865A (en) * | 2015-06-04 | 2015-09-02 | 盐城工业职业技术学院 | Production method of biodegradable environment-friendly nanometer filter element for dustproof mask |
| CN105107015A (en) * | 2015-09-11 | 2015-12-02 | 江苏锦宇环境工程有限公司 | Preparation method of antibacterial healing-promoting biological foam dressing |
| CN106757788A (en) * | 2016-12-23 | 2017-05-31 | 杭州安诺过滤器材有限公司 | A kind of filter for infusion filtering nano fibrous membrane and preparation method thereof |
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| CN106757788A (en) * | 2016-12-23 | 2017-05-31 | 杭州安诺过滤器材有限公司 | A kind of filter for infusion filtering nano fibrous membrane and preparation method thereof |
| CN106757788B (en) * | 2016-12-23 | 2019-07-30 | 杭州安诺过滤器材有限公司 | A kind of filter for infusion filtering nano fibrous membrane and preparation method thereof |
| CN108396461A (en) * | 2018-03-01 | 2018-08-14 | 苏州甫众塑胶有限公司 | A kind of promoting healing nanofiber film dressing and preparation method thereof |
| CN108396461B (en) * | 2018-03-01 | 2020-09-15 | 山东朱氏堂医疗器械有限公司 | Healing-promoting nanofiber membrane dressing and preparation method thereof |
| CN110898678A (en) * | 2019-11-27 | 2020-03-24 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of degradable anti-haze fiber film |
| CN113336304A (en) * | 2021-05-06 | 2021-09-03 | 东南大学 | Preparation method and application of high-purity silver-doped bismuth tungstate nano antibacterial fiber membrane |
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