CN104372617A - Method for preparing structural color carbon fibers based on P(NIPAAm-co-HEAC) nano-spheres - Google Patents
Method for preparing structural color carbon fibers based on P(NIPAAm-co-HEAC) nano-spheres Download PDFInfo
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- CN104372617A CN104372617A CN201410647400.1A CN201410647400A CN104372617A CN 104372617 A CN104372617 A CN 104372617A CN 201410647400 A CN201410647400 A CN 201410647400A CN 104372617 A CN104372617 A CN 104372617A
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Abstract
The invention relates to a method for preparing structural color carbon fibers based on P(NIPAAm-co-HEAC) nano-spheres. The method comprises the following steps: taking N-isopropylacrylamide, hydroxyethyl acrylate, N,N-methylene bisacrylamide and sodium dodecyl sulfate as starting raw materials; preparing the P(NIPAAm-co-HEAC) nano-spheres by adopting an emulsion polymerization method; mixing the P(NIPAAm-co-HEAC) nano-spheres with ultrapure water to obtain a dispersed solution; putting the dispersed solution into an annular metal container and putting the carbon fibers to the center of the container; carrying out electrophoretic deposition by an additional electric field, and pulling out the fibers from the container at constant speed; and drying at room temperature to obtain the product. The structural color carbon fibers prepared by the method provided by the invention have good optical performance and toxic chemical dyes are not needed; and the method is simple and feasible and has an important reference value for reducing the environmental pollution of a dyeing and finishing industry.
Description
Technical field
The invention belongs to stock-dye field, particularly one prepares the method for schemochrome carbon fiber based on P (NIPAAm-co-HEAC) nanosphere.
Background technology
Traditional dyeing course can produce the industrial wastewater containing a large amount of heavy metal ion and poisonous dyestuff intermediate, these waste water containing a large amount of harmful chemical are drained into rivers,lakes and seas, and meeting serious environment pollution, causes very serious negative effect to human society.The contradiction that can solve well between traditional dyeing and environmental pollution and structure is added lustre to.Schemochrome makes light wave and body surface micro-structural generation diffraction, scattering or interference and the physical process of the shades of colour produced, and is the biomimetic concept of the structure coloring such as feather, opal coming from occurring in nature butterfly's wing, birds.If schemochrome can be formed on the surface of fiber or fabric, just can overcome the defect in traditional dyeing process well and bring up intelligent structure coloring fiber.
In schemochrome fiber research field, researcher both domestic and external, in continuous exploration, actively seeks the route of simple to operate, effective imparting fiber color.K.Q.Zhang etc. report at J.Fiber Bioeng.Inform.Vol.2 (2010) pp.214-218 and assemble one deck SiO on the surface of glass fibre by the method dipping deposition
2nanosphere, has obtained structure color fibre, but this method lacks long-range order; H.Z.Wang etc. report at fiberglass surfacing self assembly one deck opal structural in Chemical Communications Vol.47 (2011) pp.12801-12803, thus realize the target of fiberglass surfacing schemochrome, but the SiO used
2adhesion between nanosphere and fiber is not strong.M.Skorobogatiy seminars of Canada etc. are at OpticsExpress, the effect that polymer photon crystal fiber (PBG Bragg Fiber) have also discovered schemochrome is prepared in Vol.16 (2008) pp.15677-15693, due to the difference of refractive index between sandwich construction, when incident light is propagated in the optical fiber of its PMMA/PS sandwich construction prepared, part light appears from optical fiber, macroscopically also can observe bright color, this is utilize two-dimensional photon crystal structure to prepare schemochrome fiber to provide necessary theoretical foundation and experiment condition, but prerequisite to have external light source.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method preparing schemochrome carbon fiber based on P (NIPAAm-co-HEAC) nanosphere, schemochrome fiber prepared by the method has good optical property, without the need to toxic chemical dyestuff, method is simple, has important reference value to the environmental pollution reducing dyeing and finishing industry.
One of the present invention prepares the method for schemochrome carbon fiber based on P (NIPAAm-co-HEAC) nanosphere, comprising:
(1) NIPA, N, N is taken under room temperature '-methylene-bisacrylamide, hydroxy-ethyl acrylate, dodecyl sodium sulfate and ultra-pure water, stirring and dissolving obtains reaction solution; Pass into nitrogen, heating, adds initator and carries out emulsion polymerization 1-6h, be cooled to room temperature, the emulsion obtained is carried out centrifuge washing, obtain P (NIPAAm-co-HEAC) nanosphere; Wherein the mass ratio of NIPA and hydroxy-ethyl acrylate is 5:1-40:1; NIPA, N, N ' mass ratio of-methylene-bisacrylamide and dodecyl sodium sulfate is 10:1:1-25:1:1.
(2) carbon fiber is positioned in ethanolic solution, acetone soln, ultra-pure water successively carries out ultrasonic cleaning, finally dry;
(3) P (NIPAAm-co-HEAC) nanosphere in step (1) and ultra-pure water are mixed to get dispersion liquid, and dispersion liquid is placed in endless metal container, carbon fiber in step (2) is placed in container center place, by extra electric field electrophoretic deposition, then fiber is at the uniform velocity pulled out from container, dry under normal temperature, obtain the schemochrome fiber of P (NIPAAm-co-HEAC) nanosphere assembling.
Stirring in described step (1) is magnetic agitation, and mixing speed is 400-900rpm.
Centrifugal rotational speed in described step (1) is 8500-9500rpm.
Initator in described step (1) is the one in ammonium persulfate, potassium peroxydisulfate, and adding speed is 10ml/30s-10ml/60s, and the mass ratio of NIPA and initator is 15:1-25:1.
Heating-up temperature in described step (1) is 65-75 DEG C, and heat time heating time is 50-70min.
The concentration of the ethanolic solution in described step (2) is 90%-99%, and the concentration of acetone soln is 90%-99%, and ultrapure resistivity of water is 18.2M Ω cm
-1.
The ultrasonic cleaning time in described step (2) is respectively 25 ~ 30min.
Electrophoretic deposition parameter in described step (3) is: electrophoretic voltage 1.6-3.0V, sedimentation time 20s-300s.
Drying time in described step (3) is 0.5-1.5h.
beneficial effect
(1) the present invention is simple to operate, effective, has industrial applications potentiality;
(2) the schemochrome fiber prepared by the present invention has excellent optical property;
(3) the present invention is without the need to chemical dye, has important reference value to the environmental pollution reducing Dyeing & Finishing Industry.
Accompanying drawing explanation
Fig. 1 is the FE-SEM picture of P (NIPAAm-co-HEAC) nanosphere that emulsion polymerisation obtains;
Fig. 2 is the green schemochrome carbon fiber optical microscope photograph that electrophoretic deposition obtains;
Fig. 3 is the yellow schemochrome carbon fiber optical microscope photograph that electrophoretic deposition obtains;
Fig. 4 is the reflectance spectrum of the schemochrome carbon fiber that embodiment 3 obtains.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
(1) 1g NIPA, 0.1gN is taken, N '-methylene-bisacrylamide, 0.1g hydroxy-ethyl acrylate, 0.1g dodecyl sodium sulfate, the there-necked flask magnetic agitation rotating speed that 120g ultra-pure water puts into 250ml is 400rpm, obtains reaction solution.Keep flow velocity to pass into nitrogen, heat 1h when 70 DEG C, potassium peroxydisulfate (KPS) 0.10g adding prior wiring solution-forming carries out emulsion polymerization 3h, and adding speed is 10ml/30s, is cooled to room temperature, and the emulsion obtained is carried out centrifuge washing.Centrifuge speed is set as 9000rpm, obtains P (NIPAAm-co-HEAC) nanosphere.Fig. 1 is the nanosphere FE-SEM be obtained by reacting.
(2) carbon fiber is positioned over successively 90% ethanolic solution, 90% acetone soln, resistivity is 18.2M Ω cm
-1ultra-pure water in carry out each 25min of ultrasonic cleaning, finally dry.
(3) by the centrifugal nanosphere emulsion dispersion obtained in ultra-pure water, and dispersion liquid is placed in toroidal container, the carbon fiber of cleaning, drying is placed in toroidal container central authorities, at applied voltage 2.5V, electro-deposition is carried out under the condition of sedimentation time 180s, after deposition terminates, carbon fiber is pulled out from toroidal container, dry 1h at normal temperatures, prepare the schemochrome carbon fiber of P (NIPAAm-co-HEAC) nanosphere assembling, Fig. 2 is the optical microscope photograph of obtained schemochrome carbon fiber, obviously can find out it is green schemochrome carbon fiber from way.
Embodiment 2
(1) 1g NIPA, 0.1gN is taken, the there-necked flask magnetic agitation rotating speed that N '-methylene-bisacrylamide, 0.15g hydroxy-ethyl acrylate, 0.1g dodecyl sodium sulfate, 120ml ultra-pure water put into 250ml is 500rpm, obtains reaction solution.Keep flow velocity to pass into nitrogen, heat 1h when 70 DEG C, potassium peroxydisulfate (KPS) 0.10g adding prior wiring solution-forming carries out emulsion polymerization 4h, and adding speed is 10ml/40s, is cooled to room temperature, and the emulsion obtained is carried out centrifuge washing.Centrifuge speed is set as 9000rpm, obtains P (NIPAAm-co-HEAC) nanosphere.
(2) carbon fiber is positioned over successively 90% ethanolic solution, 90% acetone soln, resistivity is 18.2M Ω cm
-1ultra-pure water in carry out each 28min of ultrasonic cleaning, finally dry.
(3) by the centrifugal nanosphere emulsion dispersion obtained in ultra-pure water, and dispersion liquid is placed in toroidal container, the carbon fiber of cleaning, drying is placed in toroidal container central authorities, at applied voltage 2.5V, electro-deposition is carried out under the condition of sedimentation time 200s, after deposition terminates, carbon fiber is pulled out from toroidal container, dry 70min at normal temperatures, prepare the schemochrome carbon fiber of P (NIPAAm-co-HEAC) nanosphere assembling, Fig. 3 is the optical microscope photograph of obtained schemochrome carbon fiber.
Embodiment 3
(1) 2g NIPA, 0.1gN is taken, the there-necked flask magnetic agitation rotating speed that N '-methylene-bisacrylamide, 0.25g hydroxy-ethyl acrylate, 0.1g dodecyl sodium sulfate, 120ml ultra-pure water put into 250ml is 800rpm, obtains reaction solution.Keep flow velocity to pass into nitrogen, heat 1h when 70 DEG C, potassium peroxydisulfate (KPS) 0.1g adding prior wiring solution-forming carries out emulsion polymerization 5h, and adding speed is 10ml/60s, is cooled to room temperature, and the emulsion obtained is carried out centrifuge washing.Centrifuge speed is set as 8500rpm, obtains P (NIPAAm-co-HEAC) nanosphere.
(2) carbon fiber is positioned over successively 90% ethanolic solution, 90% acetone soln, resistivity is 18.2M Ω cm
-1ultra-pure water in carry out each 30min of ultrasonic cleaning, finally dry.
(3) by the centrifugal nanosphere emulsion dispersion obtained in ultra-pure water, and dispersion liquid is placed in toroidal container, the carbon fiber of cleaning, drying is placed in toroidal container central authorities, at applied voltage 2.8V, electro-deposition is carried out under the condition of sedimentation time 250s, after deposition terminates, carbon fiber is pulled out from toroidal container, dry 80min at normal temperatures, prepare the schemochrome carbon fiber of P (NIPAAm-co-HEAC) nanosphere assembling.Fig. 4 is the reflectance spectrum of obtained schemochrome carbon fiber.
Claims (9)
1. prepare a method for schemochrome carbon fiber based on P (NIPAAm-co-HEAC) nanosphere, comprising:
(1) NIPA, N, N is taken under room temperature '-methylene-bisacrylamide, hydroxy-ethyl acrylate, dodecyl sodium sulfate and ultra-pure water, stirring and dissolving obtains reaction solution; Pass into nitrogen, heating, adds initator and carries out emulsion polymerization 1-6h, be cooled to room temperature, the emulsion obtained is carried out centrifuge washing, obtain P (NIPAAm-co-HEAC) nanosphere; Wherein the mass ratio of NIPA and hydroxy-ethyl acrylate is 5:1-40:1; NIPA, N, N ' mass ratio of-methylene-bisacrylamide and dodecyl sodium sulfate is 10:1:1-25:1:1;
(2) carbon fiber is positioned in ethanolic solution, acetone soln, ultra-pure water successively carries out ultrasonic cleaning, finally dry;
(3) P (NIPAAm-co-HEAC) nanosphere in step (1) and ultra-pure water are mixed to get dispersion liquid, and dispersion liquid is placed in endless metal container, carbon fiber in step (2) is placed in container center place, by extra electric field electrophoretic deposition, then fiber is at the uniform velocity pulled out from container, dry under normal temperature, obtain the schemochrome fiber of P (NIPAAm-co-HEAC) nanosphere assembling.
2. one according to claim 1 prepares the method for schemochrome carbon fiber based on P (NIPAAm-co-HEAC) nanosphere, it is characterized in that: the stirring in described step (1) is magnetic agitation, and mixing speed is 400-900rpm.
3. one according to claim 1 prepares the method for schemochrome carbon fiber based on P (NIPAAm-co-HEAC) nanosphere, it is characterized in that: the centrifugal rotational speed in described step (1) is 8500-9500rpm.
4. one according to claim 1 prepares the method for schemochrome carbon fiber based on P (NIPAAm-co-HEAC) nanosphere, it is characterized in that: the initator in described step (1) is the one in ammonium persulfate, potassium peroxydisulfate, adding speed is 10ml/30s-10ml/60s, and the mass ratio of NIPA and initator is 15:1-25:1.
5. one according to claim 1 prepares the method for schemochrome carbon fiber based on P (NIPAAm-co-HEAC) nanosphere, it is characterized in that: the heating-up temperature in described step (1) is 65-75 DEG C, and heat time heating time is 50-70min.
6. one according to claim 1 prepares the method for schemochrome carbon fiber based on P (NIPAAm-co-HEAC) nanosphere, it is characterized in that: the concentration of the ethanolic solution in described step (2) is 90%-99%, the concentration of acetone soln is 90%-99%, and ultrapure resistivity of water is 18.2M Ω cm
-1.
7. one according to claim 1 prepares the method for schemochrome carbon fiber based on P (NIPAAm-co-HEAC) nanosphere, it is characterized in that: the ultrasonic cleaning time in described step (2) is respectively 25 ~ 30min.
8. one according to claim 1 prepares the method for schemochrome carbon fiber based on P (NIPAAm-co-HEAC) nanosphere, it is characterized in that: the electrophoretic deposition parameter in described step (3) is: electrophoretic voltage 1.6-3.0V, sedimentation time 20s-300s.
9. one according to claim 1 prepares the method for schemochrome carbon fiber based on P (NIPAAm-co-HEAC) nanosphere, it is characterized in that: the drying time in described step (3) is 0.5-1.5h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108084334A (en) * | 2017-12-19 | 2018-05-29 | 苏州中科纳福材料科技有限公司 | The preparation method of polyisopropyl acrylamide-acrylic acid photonic crystal |
| CN116657289A (en) * | 2023-08-01 | 2023-08-29 | 江苏恒力化纤股份有限公司 | Preparation method of thermosensitive polyester yarns |
Citations (2)
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| JP2001261845A (en) * | 2000-03-14 | 2001-09-26 | Mitsubishi Chemicals Corp | Hydrogel particulate |
| JP2002102331A (en) * | 2000-09-21 | 2002-04-09 | Kwangju Inst Of Science & Technol | Liquid phase polymeric vascular occlusion material which gives rise to sol-gel phase transition and its application |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001261845A (en) * | 2000-03-14 | 2001-09-26 | Mitsubishi Chemicals Corp | Hydrogel particulate |
| JP2002102331A (en) * | 2000-09-21 | 2002-04-09 | Kwangju Inst Of Science & Technol | Liquid phase polymeric vascular occlusion material which gives rise to sol-gel phase transition and its application |
Non-Patent Citations (1)
| Title |
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| 张骜: "电泳沉积法制备结构色纤维", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108084334A (en) * | 2017-12-19 | 2018-05-29 | 苏州中科纳福材料科技有限公司 | The preparation method of polyisopropyl acrylamide-acrylic acid photonic crystal |
| CN116657289A (en) * | 2023-08-01 | 2023-08-29 | 江苏恒力化纤股份有限公司 | Preparation method of thermosensitive polyester yarns |
| CN116657289B (en) * | 2023-08-01 | 2023-11-24 | 江苏恒力化纤股份有限公司 | Preparation method of thermosensitive polyester yarns |
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