CN103451849B - Containing the poly butylene succinate nano fibrous membrane and its preparation method and application of Nano Silver - Google Patents
Containing the poly butylene succinate nano fibrous membrane and its preparation method and application of Nano Silver Download PDFInfo
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Abstract
The invention discloses the poly butylene succinate nano fibrous membrane and its preparation method and application 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; By with can PBS for base material, with polyvinylpyrrolidone PVP for stabilizing agent and reductant, be nano-Ag particles by silver nitrate reduction in ethanolic solution, by electrostatic spinning, nano-Ag particles is carried in the nanofiber of PBS, obtain containing Nano Silver poly butylene succinate nano fibrous membrane its can be used for wound dressing, antibacterial filter membrane, medical device.
Description
Technical field
The invention belongs to nanofiber field, particularly contain poly butylene succinate nano fibrous membrane of Nano Silver and its preparation method and application.
Background technology
The Nano Silver of diameter between 1-100nm has physicochemical property, higher surface-activity and the lower toxicity in vivo more stable than conventional silver.In antibacterial applications, due to small size effect quantum effect and great specific area, Nano Silver has the antibacterial effect stronger than conventional 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, thus expand its range of application at biomedical sector further.
The polymer nanofibre film preparing loaded with nano Argent grain 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 performance that it is special that the polymer nanofibre film of electrospinning has that specific area is large, porosity is high etc., has broad application prospects at biomedical sectors such as tissue engineering bracket, skin repair and wound dressings.
The preparation of the composite fibre of existing nano-Ag particles and polymer comprises four kinds of modes.
The first is that nano-Ag particles is directly scattered in polymer solution, carries out electrospinning and obtains composite fibre.The advantage of this method is the restriction not by cosolvent and polymeric chemical structure, and it can select various different solvent, polymer.But there is the problem that nano particle easily occurs to reunite in this method.In existing document, CN101077473 avoids occurring reuniting by additional Vltrasonic device, but thisly can increase equipment cost.
The second is that direct for silver ion (being generally nitrate powder) dissolving is carried out electrospinning in a polymer solution, by physics or chemical method, the silver ion in-situ reducing in solution or in fiber is become elemental silver afterwards, thus in polymer fiber, form equally distributed nano-Ag particles.Such as CN101096424.The advantage of this method is less by the restriction of cosolvent and polymeric chemical structure.But this method exists the problem of preparation process complexity, preparation condition harshness, such as CN101096424 needs to adopt UV-irradiation that silver nitrate is carried out photo-reduction.
The third is directly attached on surface treated polymer fiber by nano-Ag particles.The advantage of this method is the restriction not by cosolvent and polymeric chemical structure.But adhesion effect is high by the requirement of attachment condition, the surface treatment of polymer fiber is complicated.
4th kind is adopt to generate nano-Ag particles at electrospinning process situ.But this needs the cosolvent of selective polymer and silver ion, this cosolvent needs to have good compatibility, and polymer need possess specific chemical group can produce strong interaction with silver atoms.
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 compared to PLGA, PGA, PLA etc., the production cost of PBS is lower.Correlative study shows that PBS can be applied to the biomedical sector such as organizational project, insoluble drug release as a kind of potential biomaterial.Suttiphong has prepared PBS nano fiber non-woven fabric by electrostatic spinning technique and have studied its potential as tissue engineering material.Because PBS nano fiber non-woven fabric has distinctive character-high porosity, microcellular structure and large specific area, compared to general thin, nano fiber non-woven fabric has obvious facilitation to Gegenbaur's cell (SaOs-2) adhesion on material, growth and activity.But up to now, be have not been reported by the PBS composite of electrostatic spinning preparation containing Nano Silver.
To sum up, need a kind of preparation newly containing the method for poly butylene succinate nano fibrous membrane of Nano Silver, just can avoid the reunion of Argent grain under without the need to outer field action intervention, and step simply, conditional request is low.
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 of the poly butylene succinate nano fibrous membrane containing Nano Silver; By with can PBS for base material, with polyvinylpyrrolidone PVP for 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 of the poly butylene succinate nano fibrous membrane containing Nano Silver, and it can be used for wound dressing, antibacterial 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 made up 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 nano-Ag particles diameter is 2 ~ 15nm.
The fusing point of described poly butylene succinate 110 ~ 120 DEG C, molecular weight 5 ~ 200,000.
For solving the problems of the technologies described above, the invention provides the preparation method of the poly butylene succinate nano fibrous membrane containing Nano Silver, comprising the following steps:
1) preparation of Nano Silver:
The ethanolic solution of silver nitrate is mixed with the ethanolic solution of polyvinylpyrrolidone, is stirred to solution colour and becomes peony by water white transparency, and no longer change, obtain the ethanolic solution containing nano-Ag particles;
2) containing the electrospinning of the poly butylene succinate fiber film of Nano Silver:
Poly butylene succinate is dissolved, by step 1) obtain join in poly butylene succinate solution containing the ethanolic solution of nano-Ag particles, carry out electrostatic spinning after stirring, receive nano silk, obtain the poly butylene succinate nano fibrous membrane containing Nano Silver.
Further, described step 1) in the ethanol solution concentration of silver nitrate be 0.001 ~ 0.03g/ml.
Further, described step 1) in the ethanol solution concentration of polyvinylpyrrolidone be 0.02 ~ 0.2g/ml.
Further, described step 1) in the ethanolic solution of silver nitrate mix with the ethanolic solution of polyvinylpyrrolidone to heat afterwards and stir under 40 ~ 60 DEG C of conditions.
Further, described step 2) in be 0.01 ~ 0.25 containing the volume ratio of the ethanolic solution of nano-Ag particles and the chloroformic solution of PBS.
Further, described step 2) in electrostatic spinning process parameter as follows: voltage 15 ~ 30KV, receiving range is 10 ~ 20cm, and the empty internal diameter 0.2mm ~ 0.8mm of spinning, spinning speed is 30 ~ 80ul/min.
Described step 2) in receive nano silk with aluminium foil or stainless steel stent.
Step 2) obtained nano fibrous membrane at normal temperatures, vacuumize, can preserve afterwards.
For solving the problems of the technologies described above, the invention provides the application of the poly butylene succinate nano fibrous membrane containing Nano Silver, it can be used as wound dressing, antibacterial filter membrane, medical device.
The invention has the advantages that:
The present invention utilizes polyvinylpyrrolidone (PVP) distinctive chemical constitution, when preparing nano-Ag particles, PVP mono-can reduce aspect silver ion, simultaneously can play the effect of stabilizing agent on the Argent grain surface of reduction by uniform fold again, preparation process is simple, easy to operate, the nano-Ag particles size uniform obtained, particle diameter is little;
Previously prepared good nano-Ag particles one step can just be attached in nanofiber by the nano fibrous membrane that the present invention adopts method of electrostatic spinning to prepare, and be not subject to the restriction of cosolvent and polymeric chemical structure, 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 conventional inorganic antiseptic, make the nano fibrous membrane obtained can be used as wound dressing, antibacterial filter membrane, medical device etc.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of Nano Silver/PBS tunica fibrosa that embodiment 1 obtains;
Fig. 2 is the transmission electron microscope picture of Nano Silver/PBS tunica fibrosa that embodiment 1 obtains;
Fig. 3 is the scanning electron microscope (SEM) photograph of Nano Silver/PBS tunica fibrosa that embodiment 2 obtains;
Fig. 4 is the transmission electron microscope picture of Nano Silver/PBS tunica fibrosa that embodiment 2 obtains.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is further described.
Embodiment 1
Containing the preparation method of the poly butylene succinate nano fibrous membrane of Nano Silver, comprise the following steps:
Take 0.03 gram of silver nitrate and 0.5 gram of PVP is dissolved in 10ml ethanolic solution respectively, be stirred to and dissolve completely, the ethanolic solution of silver nitrate is added to rapidly in the ethanolic solution of PVP, be heated to 50 DEG C simultaneously, stir, become peony to solution colour by water white transparency, and no longer change, obtain stable nano-Ag particles;
Take 0.6 gram of PBS to be dissolved in 4ml chloroformic solution, be stirred to PBS and dissolve completely; The ethanolic solution getting the nano-Ag particles of the above-mentioned preparation of 1ml joins in the chloroformic solution of PBS, stir until solution mixes, electrospinning is carried out after leaving standstill, voltage is 20KV, and 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 sealed 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 Nano Silver/PBS tunica fibrosa that embodiment 1 obtains.
Fig. 2 is the transmission electron microscope picture of Nano Silver/PBS tunica fibrosa that embodiment 1 obtains.
Embodiment 2
Containing the preparation method of the poly butylene succinate nano fibrous membrane of Nano Silver, comprise the following steps:
Take 0.12 gram of silver nitrate and 0.5 gram of PVP is dissolved in 10ml ethanolic solution respectively, be stirred to and dissolve completely, the ethanolic solution of silver nitrate is added to rapidly in the ethanolic solution of PVP, be heated to 50 DEG C simultaneously, stir, become peony to solution colour by water white transparency, and no longer change, now obtain stable nano-Ag particles.
Take 0.6 gram of PBS to be dissolved in 4ml chloroformic solution, be stirred to PBS and dissolve completely; The ethanolic solution getting the nano-Ag particles of the above-mentioned preparation of 1ml joins in the chloroformic solution of PBS, stir until solution mixes, electrospinning is carried out after leaving standstill, voltage is 20KV, and 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 sealed 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 Nano Silver/PBS tunica fibrosa that embodiment 2 obtains.
Fig. 4 is the transmission electron microscope picture of Nano Silver/PBS tunica fibrosa that embodiment 2 obtains.
Embodiment 3
Containing 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, is stirred to solution colour and becomes peony by water white transparency, and no longer change, obtain the ethanolic solution containing nano-Ag particles;
2) containing the electrospinning of the poly butylene succinate fiber film of Nano Silver:
Poly butylene succinate is dissolved in chloroform, by step 1) obtain join in the chloroformic solution of poly butylene succinate containing the ethanolic solution of nano-Ag particles, electrostatic spinning is carried out after stirring, receive nano silk, obtain the poly butylene succinate nano fibrous membrane containing Nano Silver;
Wherein, described step 1) in the ethanol solution concentration of silver nitrate be 0.001g/ml; Described step 1) in the ethanol solution concentration of polyvinylpyrrolidone be 0.02g/ml; Described step 2) in be 0.01 containing the volume ratio of the ethanolic solution of nano-Ag particles and the chloroformic solution of PBS; Described step 2) in electrostatic spinning process parameter as follows: voltage 15KV, receiving range is 10cm, and the empty internal diameter 0.2mm of spinning, spinning speed is 30ul/min.
Embodiment 4
Containing 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, is stirred to solution colour and becomes peony by water white transparency, and no longer change, obtain the ethanolic solution containing nano-Ag particles;
2) containing the electrospinning of the poly butylene succinate fiber film of Nano Silver:
Poly butylene succinate is dissolved in chloroform, by step 1) obtain join in the chloroformic solution of poly butylene succinate containing the ethanolic solution of nano-Ag particles, electrostatic spinning is carried out after stirring, receive nano silk, obtain the poly butylene succinate nano fibrous membrane containing Nano Silver;
Wherein, described step 1) in the ethanol solution concentration of silver nitrate be 0.03g/ml; Described step 1) in the ethanol solution concentration of polyvinylpyrrolidone be 0.2g/ml; Described step 2) in be 0.25 containing the volume ratio of the ethanolic solution of nano-Ag particles and the chloroformic solution of PBS; Described step 2) in electrostatic spinning process parameter as follows: voltage 30KV, receiving range is 20cm, and 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 is clearly 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 cannot give exhaustive to all embodiments.Every belong to technical scheme of the present invention the apparent change of extending out or variation be still in the row of protection scope of the present invention.
Claims (4)
1., containing a preparation method for the poly butylene succinate nano fibrous membrane of Nano Silver, it is characterized in that, comprise the following steps:
1) preparation of Nano Silver:
The ethanolic solution of silver nitrate is mixed with the ethanolic solution of polyvinylpyrrolidone, is stirred to solution colour and becomes peony by water white transparency, and no longer change, obtain the ethanolic solution containing nano-Ag particles;
2) containing the electrospinning of the poly butylene succinate nano fibrous membrane of Nano Silver:
Poly butylene succinate is dissolved in chloroform, by step 1) obtain join in poly butylene succinate solution containing the ethanolic solution of nano-Ag particles, carry out electrostatic spinning after stirring, receive nano silk, obtain the poly butylene succinate nano fibrous membrane containing Nano Silver;
Step 1) in the ethanol solution concentration of silver nitrate be 0.001 ~ 0.03g/ml, the ethanol solution concentration of polyvinylpyrrolidone is 0.02 ~ 0.2g/ml;
Step 2) in be 0.01 ~ 0.25 containing the volume ratio of the ethanolic solution of nano-Ag particles and the chloroformic solution of PBS;
Electrostatic spinning process parameter is as follows: voltage 15 ~ 30KV, and receiving range is 10 ~ 20cm, spinneret orifice internal diameter 0.2mm ~ 0.8mm, and spinning speed is 30 ~ 80 μ l/min;
The described poly butylene succinate nano fibrous membrane containing Nano Silver is made up of Nano Silver and poly butylene succinate fiber, and nano-Ag particles is distributed on poly butylene succinate fiber, and fibre diameter is 50 ~ 500nm, and nano-Ag particles diameter is 2 ~ 15nm.
2. the preparation method of the poly butylene succinate nano fibrous membrane containing Nano Silver according to claim 1, is characterized in that, the fusing point of described poly butylene succinate 110 ~ 120 DEG C, molecular weight 5 ~ 200,000.
3. the preparation method of the poly butylene succinate nano fibrous membrane containing Nano Silver according to claim 1, it is characterized in that, described step 1) in the ethanolic solution of silver nitrate mix with the ethanolic solution of polyvinylpyrrolidone after stir under 40 ~ 60 DEG C of conditions.
4., according to the application containing the poly butylene succinate nano fibrous membrane of Nano Silver that the arbitrary described method of claims 1 to 3 prepares, it is characterized in that, it can be used as wound dressing, antibacterial filter membrane, medical device.
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