CN103806115A - Glowing nanometer fibre with biocompatibility and preparation method of glowing nanometer fibre - Google Patents

Glowing nanometer fibre with biocompatibility and preparation method of glowing nanometer fibre Download PDF

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Publication number
CN103806115A
CN103806115A CN201210456323.2A CN201210456323A CN103806115A CN 103806115 A CN103806115 A CN 103806115A CN 201210456323 A CN201210456323 A CN 201210456323A CN 103806115 A CN103806115 A CN 103806115A
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preparation
fibre
glowing
biocompatibility
particles
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CN103806115B (en
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周涓
朱君
施丽君
何丹农
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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Abstract

The invention relates to a preparation method of a glowing nanometer fibre with the biocompatibility. The preparation method comprises the following steps of dissolving carbon nanometer particles in a solvent, adding a high molecular material under a stirring condition in the mass ratio of the high molecular material to the carbon nanometer particles being (0.5:1)-(1:2), and stirring for 1-3 hours so as to obtain a uniform spinning fluid ultimately; injecting a spinning liquid into a needle cylinder, regulating an electrostatic spinning technology, collecting a layer of uniform white fibres which are collected from a receiving aluminum foil; and putting the white fibres into a high-temperature pipe-shaped atmosphere furnace, inputting nitrogen, heating to 600-1000 DEG C, carrying out heat preservation for 1-5 hours, and finally cooling to the room temperature so as to obtain the glowing nanometer fibre containing the carbon nanometer particles. The obtained fibre has the good biocompatibility, meanwhile, the fibres have a glowing property, the glowing nanometer fibre is suitable for being used in a biomedical field, and the glowing nanometer fibre is particularly utilized as a bracket material and is convenient to anaphase observation. The preparation method provided by the invention is simple, the production cost is low, and the preparation method can further meet the production and application requirements.

Description

A kind of luminous nano fibre with biocompatibility and preparation method thereof
Technical field
The present invention relates to a kind of nanofiber and preparation method thereof, be specifically related to good luminous nano fibre of a kind of biocompatibility and preparation method thereof.This method belongs to the technology of preparing of fluorescent nano-fiber, and prepared material can be widely used in biology, medicine and other fields.
Background technology
Electrostatic spinning technique is one and prepares the simple and effective technology of nanometer stage material.Polymer melt or solution, under high-pressure electrostatic effect, utilize electric field force to overcome polymer solution surface tension and form one charged injection stream, and solvent evaporates is solidified afterwards, and nano-scale fiber is arranged on collecting board disorderly, forms similar non-woven fabrics fiber film.Electrostatic spinning technique has been advantageously applied to prepares silk fibroin nano-fiber film, and prepared tunica fibrosa has the Morphological Features that fibre number is thin, surface area is large, porosity is high and can be used as the porous support of Growth of Cells, promotes migration and the propagation of cell; Also can be used as artificial graft's blood vessel, surface of a wound cladding material and pharmaceutical carrier, be widely used as organizational project and bio-medical engineering material.
In recent years, prepare many functional nano fibers by electrostatic spinning technique, made it be applied to better technical field of biological material.Up to the present, prepared as functional fibres such as antibacterial nano fiber, hemostasis nanofiber, fluorescent nano-fibers.Wherein, Chinese scholars is prepared fluorescent nano-fiber by electrostatic spinning technique, has obtained some achievements in research.In addition, also reported multi-functional magnetic~fluorescent nano-fiber.But these are semi-conducting material, rare earth material etc. for the fluorescent nano material of filling, and these materials do not possess good biological safety, and therefore these fluorescent nano-fibers are not suitable for biological field.
In recent years, there is a kind of novel fluorescent carbon nano material---fluorescent carbon nano-particles, there is abundant photoluminescent property, and with quantum dot, the comparison of up-conversion luminescence nano particle, fluorescent carbon nano-particles is except good stability, luminous intensity advantages of higher, surface has abundant oxy radical, easily functionalization.The most important thing is to have low toxicity characteristic, scientist extracts carbon nanometer from copolymerization sugar, then in zooblast, checks the toxicity of these nano particles, found that, even under very high concentration, these nano particles also only have very little toxicity, or even nontoxic.Thereby development carbon nano-particles has important practical significance in the application of biomedicine field.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of luminous nano fibre with biocompatibility and preparation method thereof.The method is scattered in carbon nano-particles in solvent, compound with macromolecular material, is mixed to form spinning solution, then prepares the good luminous nano fibre of biocompatibility by electrostatic spinning technique.
A preparation method with the luminous nano fibre of biocompatibility, is characterized in that, comprises the following steps:
1) carbon nano-particles is dissolved in solvent, ultrasound condition 0.5~4 hour, making its mass concentration is 0.01~0.5 grams per milliliter; Under stirring condition, add macromolecular material, make itself and carbon nano-particles mass ratio 0.5:1~1:2, stir 1~3 hour, finally obtain uniform spinning solution;
2) above-mentioned spinning solution is poured into syringe, regulate electrostatic spinning process, on reception aluminium foil, collect the uniform white fiber of one deck;
3) above-mentioned white fiber is put into high-temperature tubular atmosphere furnace, pass into nitrogen, be warming up to 600~1000 ℃, be incubated 1~5 hour, be finally cooled to room temperature, obtain the luminous nano fibre containing carbon nano-particles.
The particle diameter of described carbon nano-particles is 50~300 nanometers.
Described solvent is water, ethanol, chloroform, N, a kind of or its combination in N~dimethyl formamide, dimethyl sulfoxide (DMSO), ether, hexafluoroisopropanol, formic acid.
Described macromolecular material is the one in carboxymethyl cellulose, polyvinylpyrrolidone, chitin, shitosan, PLA, polyglycolic acid, polycaprolactone, poly-hydroxy fatty acid, fibroin albumen, collagen.
Described electrostatic spinning process is 10~20 kilovolts of voltages, 0.1~0.5 ml/hour of liquid inventory, and receiving range is 10~20 centimetres.
A kind of luminous nano fibre with biocompatibility is prepared by said method.
The invention has the advantages that: by electrostatic spinning technique, prepare nano level composite fibre.This fiber had both had good biocompatibility, had both again luminescent properties simultaneously, was more suitable for biomedical sector, can serve as especially a kind of timbering material, was convenient to later stage observation.Preparation technology of the present invention is simple, and production cost is low, can further meet the demand of producing and applying.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of the prepared nano fibrous membrane of embodiment 1.
Fig. 2 is the stereoscan photograph of the prepared nano fibrous membrane of embodiment 2.
Fig. 3 is the emission spectrum of the prepared nano fibrous membrane of embodiment 3.
Fig. 4 is the emission spectrum of the prepared nano fibrous membrane of embodiment 4.
The specific embodiment
By specific embodiment, technical scheme of the present invention is further described below.Following embodiment further illustrates of the present invention, and does not limit the scope of the invention.
Embodiment 1:
1) 0.5 gram, the carbon nano-particles of 100 nanometers are dissolved in 10 ml waters, ultrasound condition 0.5 hour, making its mass concentration is 0.05 grams per milliliter.Under stirring condition, add 1 gram of polyvinylpyrrolidone, stir 1 hour, finally obtain uniform spinning solution.
2) above-mentioned spinning solution is poured into syringe, 10 kilovolts of regulation voltages, 0.1 ml/hour of liquid inventory, receiving range is 10 centimetres, on reception aluminium foil, collects the uniform white fiber of one deck.
3) above-mentioned white fiber is put into high-temperature tubular atmosphere furnace, pass into nitrogen, be warming up to 600 ℃, be incubated 3 hours, be finally cooled to room temperature, obtain the luminous nano fibre containing carbon nano-particles.
Fig. 1 is the stereoscan photograph of prepared nano fibrous membrane.As seen from the figure, the diameter of nanofiber is 500 nanometers.
Embodiment 2:
1) 1 gram, the carbon nano-particles of 300 nanometers are dissolved in ethanol/chloroform of 10 milliliters of 1:1, ultrasound condition 1 hour, making its mass concentration is 0.1 grams per milliliter.Under stirring condition, add 0.5 gram of PLA, stir 2 hours, finally obtain uniform spinning solution.
2) above-mentioned spinning solution is poured into syringe, 15 kilovolts of regulation voltages, 0.1 ml/hour of liquid inventory, receiving range is 10 centimetres, on reception aluminium foil, collects the uniform white fiber of one deck.
3) above-mentioned white fiber is put into high-temperature tubular atmosphere furnace, pass into nitrogen, be warming up to 800 ℃, be incubated 2 hours, be finally cooled to room temperature, obtain the luminous nano fibre containing carbon nano-particles.
Fig. 2 is the stereoscan photograph of prepared nano fibrous membrane.As seen from the figure, the diameter of nanofiber is 1000 nanometers.
Embodiment 3:
1) 0.1 gram, the carbon nano-particles of 200 nanometers are dissolved in 10 milliliters of ethanol, ultrasound condition 1 hour, making its mass concentration is 0.01 grams per milliliter.Under stirring condition, add 0.2 gram of shitosan, stir 3 hours, finally obtain uniform spinning solution.
2) above-mentioned spinning solution is poured into syringe, 20 kilovolts of regulation voltages, 0.2 ml/hour of liquid inventory, receiving range is 15 centimetres, on reception aluminium foil, collects the uniform white fiber of one deck.
3) above-mentioned white fiber is put into high-temperature tubular atmosphere furnace, pass into nitrogen, be warming up to 600 ℃, be incubated 2 hours, be finally cooled to room temperature, obtain the luminous nano fibre containing carbon nano-particles.
Fig. 3 is take 800 nm as excitation wavelength, the emission spectrum of nano fibrous membrane.As seen from the figure, the emission wavelength of nano fibrous membrane is 530 nm, and intensity is 1040.
Embodiment 4:
1) 0.2 gram, the carbon nano-particles of 50 nanometers are dissolved in 10 ml waters, ultrasound condition 2 hours, making its mass concentration is 0.02 grams per milliliter.Under stirring condition, add 0.2 gram of fibroin albumen, stir 3 hours, finally obtain uniform spinning solution.
2) above-mentioned spinning solution is poured into syringe, 15 kilovolts of regulation voltages, 0.2 ml/hour of liquid inventory, receiving range is 10 centimetres., on reception aluminium foil, collect the uniform white fiber of one deck.
3) above-mentioned white fiber is put into high-temperature tubular atmosphere furnace, pass into nitrogen, be warming up to 600 ℃, be incubated 1 hour, be finally cooled to room temperature, obtain the luminous nano fibre containing carbon nano-particles.
Fig. 4 is take 800 nm as excitation wavelength, the emission spectrum of nano fibrous membrane.As seen from the figure, the emission wavelength of nano fibrous membrane is 540 nm, and intensity is 105.

Claims (6)

1. a preparation method with the luminous nano fibre of biocompatibility, is characterized in that, comprises the following steps:
1) carbon nano-particles is dissolved in solvent, ultrasound condition 0.5~4 hour, making its mass concentration is 0.01~0.5 grams per milliliter; Under stirring condition, add macromolecular material, make itself and carbon nano-particles mass ratio 0.5:1~1:2, stir 1~3 hour, finally obtain uniform spinning solution;
2) above-mentioned spinning solution is poured into syringe, regulate electrostatic spinning process, on reception aluminium foil, collect the uniform white fiber of one deck;
3) above-mentioned white fiber is put into high-temperature tubular atmosphere furnace, pass into nitrogen, be warming up to 600~1000 ℃, be incubated 1~5 hour, be finally cooled to room temperature, obtain the luminous nano fibre containing carbon nano-particles.
2. a kind of preparation method of the luminous nano fibre with biocompatibility according to claim 1, is characterized in that, the particle diameter of described carbon nano-particles is 50~300 nanometers.
3. a kind of preparation method of the luminous nano fibre with biocompatibility according to claim 1, it is characterized in that, described solvent is water, ethanol, chloroform, N, a kind of or its combination in N~dimethyl formamide, dimethyl sulfoxide (DMSO), ether, hexafluoroisopropanol, formic acid.
4. a kind of preparation method of the luminous nano fibre with biocompatibility according to claim 1, it is characterized in that, described macromolecular material is the one in carboxymethyl cellulose, polyvinylpyrrolidone, chitin, shitosan, PLA, polyglycolic acid, polycaprolactone, poly-hydroxy fatty acid, fibroin albumen, collagen.
5. a kind of preparation method of the luminous nano fibre with biocompatibility according to claim 1, is characterized in that, described electrostatic spinning process is 10~20 kilovolts of voltages, 0.1~0.5 ml/hour of liquid inventory, and receiving range is 10~20 centimetres.
6. a luminous nano fibre with biocompatibility, is characterized in that, prepares according to the method described in claim 1~7 any one.
CN201210456323.2A 2012-11-14 2012-11-14 A kind of luminous nano fibre with biocompatibility and preparation method thereof Expired - Fee Related CN103806115B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105924983A (en) * 2016-05-13 2016-09-07 东莞市联洲知识产权运营管理有限公司 Color-changeable fibroin particles and preparation method thereof
CN106947466A (en) * 2017-03-30 2017-07-14 延边大学 The preparation method of carbon point porous inorganic oxide composite nano fiber

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1876902A (en) * 2006-07-10 2006-12-13 东华大学 Atmosphere controllable static spinning device and industrial application thereof
CN101244902A (en) * 2007-06-15 2008-08-20 东华大学 Fluorescence fibre for reinforcing concrete, production and application thereof
JP2010236117A (en) * 2009-03-31 2010-10-21 Unitika Ltd Luminescent fibrous structural material
CN101962818A (en) * 2010-09-08 2011-02-02 黑龙江大学 Preparation method of doping type fluorescent micron-nano fibers

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1876902A (en) * 2006-07-10 2006-12-13 东华大学 Atmosphere controllable static spinning device and industrial application thereof
CN101244902A (en) * 2007-06-15 2008-08-20 东华大学 Fluorescence fibre for reinforcing concrete, production and application thereof
JP2010236117A (en) * 2009-03-31 2010-10-21 Unitika Ltd Luminescent fibrous structural material
CN101962818A (en) * 2010-09-08 2011-02-02 黑龙江大学 Preparation method of doping type fluorescent micron-nano fibers

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105924983A (en) * 2016-05-13 2016-09-07 东莞市联洲知识产权运营管理有限公司 Color-changeable fibroin particles and preparation method thereof
CN105924983B (en) * 2016-05-13 2018-08-24 崔金芬 A kind of changeable colour fibroin particle and preparation method thereof
CN106947466A (en) * 2017-03-30 2017-07-14 延边大学 The preparation method of carbon point porous inorganic oxide composite nano fiber
CN106947466B (en) * 2017-03-30 2019-11-15 延边大学 Carbon dots-porous inorganic oxide composite nano fiber preparation method

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