CN102127825B - Preparation method of polymer fluorescent colorful fibre - Google Patents
Preparation method of polymer fluorescent colorful fibre Download PDFInfo
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- CN102127825B CN102127825B CN2010106019817A CN201010601981A CN102127825B CN 102127825 B CN102127825 B CN 102127825B CN 2010106019817 A CN2010106019817 A CN 2010106019817A CN 201010601981 A CN201010601981 A CN 201010601981A CN 102127825 B CN102127825 B CN 102127825B
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- polymer
- quantum dot
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- colorful
- spinning
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- 239000000835 fiber Substances 0.000 title claims abstract description 47
- 229920000642 polymer Polymers 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 24
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical class [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000009987 spinning Methods 0.000 claims abstract description 15
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 239000002096 quantum dot Substances 0.000 claims description 38
- 239000004793 Polystyrene Substances 0.000 claims description 19
- 239000007864 aqueous solution Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 229920002223 polystyrene Polymers 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 9
- 239000000376 reactant Substances 0.000 claims description 8
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 239000005030 aluminium foil Substances 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000005034 decoration Methods 0.000 abstract description 2
- 238000000151 deposition Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 238000002189 fluorescence spectrum Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 2
- 241000220317 Rosa Species 0.000 description 1
- AQCDIIAORKRFCD-UHFFFAOYSA-N cadmium selenide Chemical compound [Cd]=[Se] AQCDIIAORKRFCD-UHFFFAOYSA-N 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000007877 drug screening Methods 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a preparation method of a polymer fluorescent colorful fibre, belonging to the preparation field of fluorescent fibres and aiming to solve the technical problem that CdSe quantum dots are difficult to disperse into polymers for electrostatic spinning. The method provided by the invention comprises the following steps of: firstly, preparing CdSe quantum dots with different emitting light peak positions, and then mixing; secondly, depositing with ethanol and extracting with toluene; thirdly, preparing a polymer spinning solution; and fourthly, spinning the polymer spinning solution obtained in the third step into a fibre through a spinning process to obtain the polymer fluorescent colorful fibre. The fibre prepared by the invention can present red, orange, yellow, green and cyan lights under an ultraviolet light with the wavelength of 365 nm. The method has the advantages of simple process, economy, high spinning efficiency and easiness in controlling reaction conditions. The polymer fluorescent colorful fibre is applied to the aspects such as fluorescent anti-counterfeiting brands, paper and fluorescent decoration, fluorescent ink and clothes products.
Description
Technical field
The invention belongs to the preparation field of fluorescent fiber.Cadmium selenide (CdSe) has good optical characteristics and stability; Have wide practical use in fields such as luminescent device, optical bio marks; The present invention disperses to be coated in polystyrene (PS) fiber through toluene, has obtained to appear the colorful fiber of corresponding quantum dot fluorescent characteristic.
Background technology.
Along with progress of science and technology, new fluorescent fiber continues to bring out, it., the photosensitive colour-changing material. the fluorescence ornament materials. a plurality of fields such as optical recording material, storage fiber optics, fiber optics, anti-false fiber, optical fiber have a wide range of applications.Quantum dot is owing to quantum-mechanical marvellous rule has significant dimensional effect; Basically the light that is higher than specific thresholding all can absorb; And an organic dye molecule only could be raised to higher excitation state from ground state behind the photon that absorbs appropriate energy, and used light must be accurate wavelength or color, and these are obviously different with the semiconductor bulk phase material; And quantum dot will absorb the photon that all are higher than its band-gap energy, but the optical wavelength of being launched (being color) has size-dependent again very much.So the nano semiconductor material of single kind just can produce an emission wavelength label family different, that color is clearly demarcated by change in size, this is that dye molecule can't be realized at all.Compare with traditional dye molecule, quantum dot has multiple advantage really.Inorganic crystallites can be born exciting and light emission repeatedly, and organic molecule can decompose. and lasting stability can let the researcher observe cell and tissue for more time, and has no to carry out the modifying interface connection difficultly.Measuring in the benefit of a maximum is that abundant color is arranged.The complexity of living things system often need be observed several kinds of components simultaneously; If dye with dye molecule; Then need the light of different wave length to excite, measure in point and then do not have this problem, use the nanocrystal of different sizes (and then different colors) to come the different biomolecule of mark.Use single light source just can make the different particles can be by immediately monitoring.The special optical property of quantum dot makes it in researchs such as biochemistry, molecular biology, cell biology, proteomics, drug screening, interaction of biomacromolecules, great application prospect arranged.But because the toxicity and the fluorescence unstability of quantum dot make it be difficult to use, it is a kind of ideal means that quantum dot is coated.Because of it forms spinning solution owing to reasons such as skin effect make quantum dot be difficult to be dispersed in uniformly in polymer solution, can not adopt electrostatic spinning technique to prepare fluorescent fiber.The CdS quantum dot is coated on water soluble (CO) polymers with generated in-situ way and processes fluorescent fiber at present..
Summary of the invention
The present invention will solve the CdSe quantum dot and be difficult to be dispersed in the technical problem of carrying out electrostatic spinning in the polymer; And provide a kind of polymer fluorescent colorful fiber preparation method.The present invention provides a kind of new way for the preparation fluorescent fiber.
The colorful fiber preparation method of polymer fluorescent is undertaken by following step among the present invention: one, 150mL absolute ethyl alcohol and 40mL oleic acid are mixed, add the 50mLNaOH aqueous solution and 50mLCd (CH successively
3COO)
22H
2The O aqueous solution (white solution) adds 50mL Na again
2SeSO
3Solution is placed 3～5min (yellow solution) and is obtained reactant liquor, presses 5 parts of reactant liquors of aforesaid operations preparation then; Be transferred to and react 0.5h, 1.5h, 2h, 4h and 12h in the different agitated reactors respectively; Be reflected under closed reactor, 40～150 ℃ of conditions of temperature and carry out, in the reaction time, obtain to contain the different CdSe quantum dot mixtures of launching the photopeaks position; The above-mentioned CdSe quantum dot mixture that contains is mixed, obtain quantum dot mixture A; Two, obtain quantum dot mixture A with the precipitation with alcohol step 1, use extracted in toluene then, get upper strata liquid (upper strata liquid is rose); Three, polystyrene (PS) is added in the liquid of upper strata, the mass concentration of polystyrene is 25%～35%, and CdSe quantum dot gross mass is 2%～4% of a polystyrene quality; Ultrasonic being dispersed to evenly obtains polymer dope; Four, through spinning technique the polymer dope that step 3 obtains is spun into fiber; Promptly obtain the colorful fiber of polymer fluorescent; Wherein the mass concentration of the NaOH aqueous solution is 6%～8% in the step 1, Cd (CH
3COO)
22H
2The mass concentration of the O aqueous solution is 2%～3%, Na
2SeSO
3The mass concentration of solution is 2%.
The present invention is a bridge with toluene, obtains uniform spinning solution, has solved CdSe quantum dot difficulty and has been dispersed in this difficult problem in the polystyrene; And pass through method of extraction; Cast out deposition that the common purifying of quantum dot uses and method such as centrifugal, reduced cost, cadmium selenide is dissolved in through toluene has been coated in the PS fiber in the chemical fibre manufacture process; Obtain appearing the colorful fiber of corresponding quantum dot fluorescent characteristic, the preparation fiber can present red, orange, yellow, green, cyan light under 365nm wavelength ultraviolet light.This method technology is simple, economy, spinning efficiency are high, easy control of reaction conditions.Be applied in fluorescence falsification preventing trade mark, paper and fluorescence decoration, fluorescent ink, clothing products aspect.
Description of drawings
Fig. 1 is the fluorescence spectrum figure of different size quantum dot, respectively corresponding 0.5h, 1.5h, 2h, 4h and 12h of peak from left to right among the figure; Fig. 2 is the fluorescence spectrum figure of the colorful fiber of the specific embodiment eight preparation polymer fluorescents.
The specific embodiment
The specific embodiment one: the colorful fiber preparation method of polymer fluorescent is undertaken by following step in this embodiment: one, 150mL absolute ethyl alcohol and 40mL oleic acid are mixed, add the 50mLNaOH aqueous solution and 50mLCd (CH successively
3COO)
22H
2The O aqueous solution wherein, adds 50mL Na again
2SeSO
3Solution; Place 3～5min and obtain reactant liquor, press 5 parts of reactant liquors of aforesaid operations preparation then, be transferred to and react 0.5h, 1.5h, 2h, 4h and 12h in the different agitated reactors respectively; Be reflected under closed reactor, 40～150 ℃ of conditions of temperature and carry out; Acquisition contains the CdSe quantum dot mixture of different emission photopeaks position, and the above-mentioned CdSe quantum dot mixture that contains is mixed, and obtains quantum dot mixture A; Two, obtain quantum dot mixture A with the precipitation with alcohol step 1, use extracted in toluene then, get upper strata liquid; Three, polystyrene (PS) is added in the liquid of upper strata, the mass concentration of polystyrene is 25%～35%, and CdSe quantum dot gross mass is 2%～4% of a polystyrene quality; Ultrasonic being dispersed to evenly obtains polymer dope; Four, through spinning technique the polymer dope that step 3 obtains is spun into fiber; Promptly obtain the colorful fiber of polymer fluorescent; Wherein the mass concentration of the NaOH aqueous solution is 6%～8% in the step 1, Cd (CH
3COO)
22H
2The mass concentration of the O aqueous solution is 2%～3%, Na
2SeSO
3The mass concentration of solution is 2%.
This embodiment prepares fiber can present red, orange, yellow, green, cyan light under 365nm wavelength ultraviolet light.
The specific embodiment two: what this embodiment and the specific embodiment one were different is: the said reaction temperature of step 1 is 80～100 ℃.Other step is identical with the specific embodiment one with parameter.
The specific embodiment three: what this embodiment was different with the specific embodiment one or two is: the required supersonic frequency of ultrasonic dispersion is 80Hz in the step 3.Other step is identical with the specific embodiment one or two with parameter.
The specific embodiment four: what this embodiment was different with one of specific embodiment one to three is: CdSe quantum dot gross mass is 2.5%～3.5% of a polystyrene quality in the step 3.Other step is identical with one of specific embodiment one to three with parameter.
The specific embodiment five: what this embodiment was different with one of specific embodiment one to three is: CdSe quantum dot gross mass is 3.0% of a polystyrene quality in the step 3.Other step is identical with one of specific embodiment one to three with parameter.
The specific embodiment six: what this embodiment was different with one of specific embodiment one to four is: the said spinning technique of step 4 is fiber elongation method, rotary spinning or electrostatic spinning.Other step is identical with one of specific embodiment one to four with parameter.
The specific embodiment seven: what this embodiment and the specific embodiment six were different is: copper wire is as anode in the said electrostatic spinning, and aluminium foil is as negative electrode, and fixed negative pole and anode distance are 15cm, electrostatic spinning under 12kv voltage.Other step and parameter and specific embodiment six phase are together.
The specific embodiment eight: the colorful fiber preparation method of polymer fluorescent is undertaken by following step in this embodiment of this enforcement: one, 150mL absolute ethyl alcohol and 40mL oleic acid are mixed, add the 50mLNaOH aqueous solution and 50mLCd (CH successively
3COO)
22H
2The O aqueous solution wherein, adds 50mL Na again
2SeSO
3Solution; Leave standstill 5min and obtain reactant liquor, press 5 parts of reactant liquors of aforesaid operations preparation then, be transferred to and react 0.5h, 1.5h, 2h, 4h and 12h in the different agitated reactors respectively; Be reflected under closed reactor, 100 ℃ of conditions of temperature and see Fig. 1); Acquisition contains the CdSe quantum dot mixture of different emission photopeaks position, and the above-mentioned CdSe quantum dot mixture that contains is mixed, and obtains quantum dot mixture A; Two, obtain quantum dot mixture A with the precipitation with alcohol step 1, use extracted in toluene then, get upper strata liquid; Three, polystyrene (PS) is added in the liquid of upper strata, the mass concentration of polystyrene is 30%, and CdSe quantum dot quality is 3% with the ratio of polystyrene quality; Ultrasonic being dispersed to evenly obtains polymer dope; Four, through electrostatic spinning the polymer dope that step 3 obtains is spun into fiber, copper wire is as anode in the electrostatic spinning, and aluminium foil is as negative electrode, and fixed negative pole and anode distance are 15cm, electrostatic spinning under 12kv voltage; Promptly obtain the colorful fiber of polymer fluorescent; Wherein the mass concentration of the NaOH aqueous solution is 7% in the step 1, Cd (CH
3COO)
22H
2The mass concentration of the O aqueous solution is 2%, Na
2SeSO
3The mass concentration of solution is 2%.
The fluorescence spectrum of the colorful fiber of polymer fluorescent of this embodiment preparation is as shown in Figure 2, can be known that by Fig. 2 the fluorescent fiber of preparation can present red, orange, yellow, green, cyan light under 365nm wavelength ultraviolet light.
Claims (7)
1. colorful fiber preparation method of polymer fluorescent is characterized in that the colorful fiber preparation method of polymer fluorescent undertaken by following step:
One, 150mL absolute ethyl alcohol and 40mL oleic acid are mixed, add the 50mL NaOH aqueous solution and 50mLCd (CH successively
3COO)
22H
2The O aqueous solution adds 50mL Na again
2SeSO
3Solution; Place 3～5min and obtain reactant liquor, press 5 parts of reactant liquors of aforesaid operations preparation then, be transferred to and react 0.5h, 1.5h, 2h, 4h and 12h in the different agitated reactors respectively; Be reflected under closed reactor, 40～150 ℃ of conditions of temperature and carry out; Acquisition contains the CdSe quantum dot mixture of different emission photopeaks position, and the above-mentioned CdSe quantum dot mixture that contains is mixed, and obtains quantum dot mixture A;
Two, obtain quantum dot mixture A with the precipitation with alcohol step 1, use extracted in toluene then, get upper strata liquid;
Three, polystyrene is added in the liquid of upper strata, the mass concentration of polystyrene is 25%～35%, and CdSe quantum dot gross mass is 2%～4% of a polystyrene quality; Ultrasonic being dispersed to evenly obtains polymer dope;
Four, through spinning technique the polymer dope that step 3 obtains is spun into fiber; Promptly obtain the colorful fiber of polymer fluorescent; Wherein the mass concentration of the NaOH aqueous solution is 6%～8% in the step 1, Cd (CH
3COO)
22H
2The mass concentration of the O aqueous solution is 2%～3%, Na
2SeSO
3The mass concentration of solution is 2%.
2. the colorful fiber preparation method of a kind of polymer fluorescent according to claim 1 is characterized in that the said reaction temperature of step 1 is 80～100 ℃.
3. the colorful fiber preparation method of a kind of polymer fluorescent according to claim 2 is characterized in that the required supersonic frequency of ultrasonic dispersion is 80Hz in the step 3.
4. the colorful fiber preparation method of a kind of polymer fluorescent according to claim 3 is characterized in that CdSe quantum dot gross mass is 2.5%～3.5% of a polystyrene quality in the step 3.
5. the colorful fiber preparation method of a kind of polymer fluorescent according to claim 3 is characterized in that CdSe quantum dot gross mass is 3.0% of a polystyrene quality in the step 3.
6. according to the colorful fiber preparation method of the described a kind of polymer fluorescent of each claim among the claim 1-5, it is characterized in that the said spinning technique of step 4 is fiber elongation method, rotary spinning or electrostatic spinning.
7. the colorful fiber preparation method of a kind of polymer fluorescent according to claim 6 is characterized in that copper wire is as anode in the said electrostatic spinning, and aluminium foil is as negative electrode, and fixed negative pole and anode distance are 15cm, electrostatic spinning under 12kv voltage.
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| CN2010106019817A CN102127825B (en) | 2010-12-23 | 2010-12-23 | Preparation method of polymer fluorescent colorful fibre |
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| CN102127825A CN102127825A (en) | 2011-07-20 |
| CN102127825B true CN102127825B (en) | 2012-06-27 |
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| CN102693679A (en) * | 2012-05-30 | 2012-09-26 | 广东普加福光电科技有限公司 | Anti-counterfeiting identification method by aid of quantum points |
| CN105860686A (en) * | 2016-06-17 | 2016-08-17 | 武汉工程大学 | Nanometer fluorescence fiber anti-fake waterborne glazing oil and preparation method thereof |
| CN105949622B (en) * | 2016-06-17 | 2018-11-06 | 武汉工程大学 | A kind of nano fluorescence fiber false-proof film and preparation method thereof |
| CN106283398B (en) * | 2016-10-26 | 2019-09-24 | 南方科技大学 | A method for preparing quantum rod/polymer fiber membrane by electrospinning technology |
| CN108239797B (en) * | 2018-01-05 | 2021-09-03 | 京东方科技集团股份有限公司 | Preparation method of polyester fiber and polyester fiber |
| CN110644071B (en) * | 2019-09-25 | 2022-04-26 | 武汉纺织大学 | Centrifugal spinning preparation method of photoluminescent fiber |
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| US7999455B2 (en) * | 2006-11-13 | 2011-08-16 | Research Triangle Institute | Luminescent device including nanofibers and light stimulable particles disposed on a surface of or at least partially within the nanofibers |
| CN101096687B (en) * | 2007-07-11 | 2012-08-29 | 武汉大学 | Method for preparing cadmium selenide quantum dots by using microbial cells |
| US8714776B2 (en) * | 2008-05-13 | 2014-05-06 | Research Triangle Institute | Porous and non-porous nanostructures and application thereof |
| CN101338189A (en) * | 2008-08-27 | 2009-01-07 | 吉林大学 | High-voltage electrospinning preparation method of multiple fluorescence-encoded microspheres |
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