CN102071490A - Method for preparing organic photochromic nanofibers - Google Patents
Method for preparing organic photochromic nanofibers Download PDFInfo
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Abstract
The invention relates to a method for preparing organic photochromic nanofibers, and the method comprises the following steps: dissolving organic photochromic compounds into a polymer solution so as to obtain a spinning solution; and preparing the spinning solution into nanofibers by using an electrostatic spinning technology, wherein the organic photochromic materials are spirooxazine type, spiropyrane type, diarylethene type, fulgide type and azo dye type photochromic materials, and the like; and the polymer materials refer to polyvinylpyrrolidone resins, polystyrene resins, polymethylmethacrylate resins, polyvinyl alcohol, polyethylene terephthalate (PET) resins and the like. The organic photochromic nanofibers prepared by the method provided by the invention have high sensitivity and excellent endurance performance, and can be applied to clothing materials for garments, shoes and hats, daily fabrics for fabrics and carpets, polymer fibers for cosmetics, discoloration windows, displays, chemical sensors and optical storage devices; and in the military field, the prepared organic photochromic nanofibers can be used for battle fatigues, tents, military machinery, and the like.
Description
Technical field
The present invention relates to a kind of preparation method of nanofiber, particularly relate to a kind of preparation method of organic photochromic nanofiber.
Background technology
Organic photochromic material is a kind of new type functional material, because it is the reversible generation change color of energy under light action, aspects such as camouflage cryptic coloration in high-density optical information storing device, holographic false proof, nonlinear optics apparatus, military affairs and secret writing material, civilian commodity (weaving, optical mirror slip etc.) manufacturing are with a wide range of applications, and its potential range of application just constantly is extended to such as fields such as molecular switch, bioprobe, biological supermolecules.
Be divided into following a few class from structure, fulgide type, spiro-pyrans, spiral shell oxazine type, azo dye type, diarylethene derivatives type, phenoxy group naphthonaphthalene quinones etc.Photochromic principle, promptly compd A absorbs certain wavelength (λ
1) light after take place photochromicly, produce chromoplast B; And B is at another wavelength (λ
2) illumination penetrate after, or can be returned to A at a certain temperature, become shadow.Its variable color often links together with change of molecular structure, as tautomerism, cis-trans isomerism, open loop ring-closure reaction, is dimerization or redox reaction sometimes.
Functional photochromic compound is a micromolecule, is not easy to practical application, and traditional approach is that the employing dispersion method is dispersed in photochromic compounds in the polymer substrate, forms organic photochromic polymer thin-film material; Or the employing polymerization, be grafted to polymer lateral chain on by covalent bond the organic photochromic molecule or be embedded on the main polymer chain, form photochromic copolymer.The advantage of dispersion method is that technical process is simple, cost of manufacture is low, the range of choice of polymeric matrix is wide, but in film, photochromic compounds is separated easily, limited its concentration range, and in use the photochromic compounds molecule easily moves from polymeric matrix, influence the stability of photochromic properties, the thickness of this outer film often stops the complete variable color of film inside or influences the response speed of its photochromic reactions.And the method for polymerization, advantage is that the organic photochromic molecule is grafted on the polymer lateral chain by covalent bond or is embedded on owner's chain, improved the stability of organic variable color macromolecular material in the use effectively, its shortcoming is building-up process complexity, cost height, is difficult to satisfy practical application.
Along with the progress of science and technology and the raising of people's living standard, people are to the various clothes of clothes, shoes and hats and indoor decoration, therefore and the appearance requirement of other daily fabrics is more and more higher, photochromic material is introduced coated fabric and is beautified the developing direction that dress ornament and environment become function fabric.But the color fastness to washing of photochromic printing is low and photochromicly be subjected to the restriction of coating transparency and reduce color changeable effect, thereby can not satisfy the demand.
Summary of the invention
The object of the present invention is to provide the preparation method of this organic photochromic nanofiber.
The invention provides a kind of preparation method of organic photochromic nanofiber, it is characterized in that comprising the steps:
(1) preparation of spinning solution: take by weighing a certain amount of polymer, be dissolved in an amount of organic solvent, obtain the polymer solution of transparent and homogeneous; A certain amount of photochromic compounds is dissolved in this polymer solution, leaves standstill after stirring under the room temperature;
(2) preparation of composite nano fiber: adopt electrostatic spinning technique, with step (1) make the polymer dope of photochromic compounds carry out spinning, preparation organic photochromic nanofiber; Technical parameter is: DC voltage 6kV～50kV, the internal diameter of nozzle are 0.6～1.2 millimeter, and the angle of nozzle and horizontal plane is 15～30 degree, and nozzle is 12～20 centimetres to the curing distance of receiving screen.
Described photochromic compounds Wei Luo oxazine type or spiro-pyrans type or diarylethene type, its mass percent concentration is 0.02～20%.
Described polymer is polyvinylpyrrolidone resin or polystyrene resin or plexiglass, and its mass percent concentration is 5～15%.
Described organic solvent is chloroform and N, dinethylformamide or N, dinethylformamide or dimethyl sulfoxide (DMSO).
The present invention compares with prior art has outstanding feature and progress:
1. the present invention directly loads on photochromic compounds in the polymeric matrix, photochromic compounds is not only on the surface of fiber, but be dispersed in the nanofiber, can overcome the low shortcoming of color fastness to washing of photochromic printing coated fabric.
2. with respect to photochromic film material, the preparation of nanofiber has increased the organic photochromic molecule and evenly has been exposed at the surf zone of nanofiber and strolls, and overcomes thin-film material and delays photochromic metachromatic shortcoming.
3. the single fibrillose acquisition that has photochromic characteristic, the feasible exploitation that can carry out micron or nanoscale photoswitch.
4. adopt the method for electrostatic spinning, use a spot of polymer, just can obtain continuous fiber; Can overcome solvent spinning and be only applicable to be dissolvable in water polymer in the volatility volume; Simultaneously, other function ingredients can be added to the characteristic in the polymer solution, make it can be widely used in the preparation of the nanofiber of difference in functionality.
The specific embodiment
Below embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
(1) preparation of spinning solution: take by weighing 2.5 gram polymethyl methacrylate (PMMA) resins, be dissolved in chloroform (CHCl
3)) and N, dinethylformamide (DMF), chloroform and N, the dinethylformamide volume ratio is in 15: 1 the mixed solution, to leave standstill after the stirring and dissolving, can obtain the transparent and homogeneous mass percent concentration and be 5% PMMA solution.A certain amount of organic photochromic diarylvinylene compound is dissolved in the mixed solution of this PMMA, stirred 2 hours under the room temperature, leave standstill afterwards.
(2) preparation of composite nano fiber: adopt electrostatic spinning technique, use the PMMA solution of above-mentioned organic photochromic diarylvinylene compound to carry out spinning, preparation photochromic compounds/PMMA composite nano fiber.Technical parameter is: DC voltage 6kV, the internal diameter of nozzle are 0.6mm, and nozzle is 12cm to the curing distance of receiving screen, 25 ℃ of room temperatures.
The organic photochromic nanofiber of above-mentioned preparation is colourless; Its under UV-irradiation (254nm) be can be observed become redness immediately, being determined at the visible range with ultraviolet-visual spectrometer has tangible absorption band; When sample be put into visible light (＞400nm) irradiation is down return colourless again rapidly.This variable color process can be back and forth at least 400 times, and do not have performance loss.
Embodiment 2
(1) preparation of spinning solution: take by weighing 7.5 gram polystyrene (PS) resins, be dissolved in DMF, leave standstill after the stirring and dissolving, can obtain the PS solution of transparent and homogeneous mass percent concentration 15%.A certain amount of organic photochromic Luo oxazine compound is dissolved among the PS, stirs 2h under the room temperature, leave standstill afterwards.
(2) preparation of composite nano fiber: adopt electrostatic spinning technique, use the PS solution of above-mentioned organic photochromic Luo oxazine compound to carry out spinning, preparation organic photochromic Luo oxazine compound/PS nanofiber.Technical parameter is: DC voltage 15kV, the internal diameter of nozzle are 0.6mm, and the angle of nozzle and horizontal plane is 15, and nozzle is 20cm to the curing distance of receiving screen, 25 ℃ of room temperatures.
The organic photochromic nanofiber of above-mentioned preparation is colourless; Its under UV-irradiation (365nm) be can be observed become blueness immediately, being determined at the visible range with ultraviolet-visual spectrometer has tangible absorption band; When sample be put into visible light (＞400nm) can return colourlessly rapidly under the irradiation, perhaps as in the dark, move back gradually to colourless.
Embodiment 3
(1) preparation of spinning solution: take by weighing 5 gram polyvinylpyrrolidone (PVP) resins, be dissolved in dimethyl sulfoxide (DMSO), leave standstill after the stirring and dissolving, can obtain the PVP solution of transparent and homogeneous mass percent concentration 10%.A certain amount of organic photochromic spiropyran compounds is dissolved among the PVP, stirred 2 hours under the room temperature, leave standstill afterwards.
(2) preparation of composite nano fiber: adopt electrostatic spinning technique, use the PVP solution of above-mentioned photochromic compounds to carry out spinning, preparation organic photochromic spiropyran compounds/PVP nanofiber.Technical parameter is: DC voltage 10kV, the internal diameter of nozzle are 1.2mm, and the angle of nozzle and horizontal plane is 30, and nozzle is 20cm to the curing distance of receiving screen, 25 ℃ of room temperatures.
The organic photochromic nanofiber of above-mentioned preparation is colourless; Its under ultra violet lamp (365nm) be can be observed become blueness immediately, being determined at the visible range with ultraviolet-visual spectrometer has tangible absorption band; When sample be put into visible light (＞400nm) irradiation is down return colourlessly again rapidly, perhaps as in the dark, move back gradually to colourless.
Claims (4)
1. the preparation method of an organic photochromic nanofiber is characterized in that comprising the steps:
(1) preparation of spinning solution: take by weighing a certain amount of polymer, be dissolved in an amount of organic solvent, obtain the polymer solution of transparent and homogeneous; A certain amount of photochromic compounds is dissolved in this polymer solution, leaves standstill after stirring under the room temperature;
(2) preparation of composite nano fiber: adopt electrostatic spinning technique, with step (1) make the polymer dope of photochromic compounds carry out spinning, preparation organic photochromic nanofiber; Technical parameter is: DC voltage 6kV～50kV, the internal diameter of nozzle are 0.6～1.2 millimeter, and the angle of nozzle and horizontal plane is 15～30 degree, and nozzle is 12～20 centimetres to the curing distance of receiving screen.
2. the preparation method of organic photochromic nanofiber according to claim 1 is characterized in that described photochromic compounds Wei Luo oxazine type or spiro-pyrans type or diarylethene type, and its mass percent concentration is 0.02～20%.
3. the preparation method of organic photochromic nanofiber according to claim 1, it is characterized in that described polymer is polyvinylpyrrolidone resin or polystyrene resin or plexiglass, mass percent concentration is 5～15%.
4. the preparation method of organic photochromic nanofiber according to claim 1 is characterized in that described organic solvent is chloroform and N, dinethylformamide or N, dinethylformamide or dimethyl sulfoxide (DMSO).
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| CN102732994A (en) * | 2012-06-21 | 2012-10-17 | 精源(南通)化纤制品有限公司 | Restorable photochromic artificial hairline and its preparation method |
| CN102851770A (en) * | 2012-09-04 | 2013-01-02 | 昆山市万丰制衣有限责任公司 | Color-changing fabric and weaving method thereof |
| CN103556300A (en) * | 2013-10-25 | 2014-02-05 | 厦门翔鹭化纤股份有限公司 | Photochromic fiber as well as preparation method and application thereof |
| CN103590192A (en) * | 2013-10-15 | 2014-02-19 | 浙江三志纺织有限公司 | Preparation method of dispersible blue 2BLN/ polyacrylonitrile-based colored nanofiber membrane |
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2010
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Application publication date: 20110525 |