CN104264445B - A kind of method preparing schemochrome carbon fiber based on P (NIPAAm-co-AAc) nanosphere - Google Patents
A kind of method preparing schemochrome carbon fiber based on P (NIPAAm-co-AAc) nanosphere Download PDFInfo
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- CN104264445B CN104264445B CN201410455979.1A CN201410455979A CN104264445B CN 104264445 B CN104264445 B CN 104264445B CN 201410455979 A CN201410455979 A CN 201410455979A CN 104264445 B CN104264445 B CN 104264445B
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Abstract
The present invention relates to a kind of method preparing schemochrome carbon fiber based on P (NIPAAm co AAc) nanosphere, including: with N N-isopropylacrylamide, N, N methylene-bisacrylamide, dodecyl sodium sulfate is initiation material, emulsion polymerization is used to prepare P (NIPAAm co AAc) nanosphere, P (NIPAAm co AAc) nanosphere and ultra-pure water are mixed to get dispersion liquid, dispersion liquid is placed in endless metal container, individual carbon fibers is placed at container center, by extra electric field electrophoretic deposition, then fiber is the most at the uniform velocity pulled out, it is dried under room temperature, prepare the schemochrome fiber that P (NIPAAm co AAc) nanosphere assembles.Schemochrome fiber prepared by the present invention has good optical property, and the present invention is without toxic chemical dyestuff, and method is simple, and the environmental pollution to reducing dyeing and finishing industry has important reference value.
Description
Technical field
The invention belongs to stock-dye field, prepare schemochrome carbon particularly to one based on P (NIPAAm-co-AAc) nanosphere fine
The method of dimension.
Background technology
It is known that traditional dyeing course is to utilize organic or inorganic dyestuff and fiber that chemically or physically chemical bond occurs, or
Fiber generates insoluble coloring matter, during this, there is substantial amounts of heavy metal ion and poisonous intermediate, these
Harmful substance is drained into rivers,lakes and seas, and the mankind and environment are caused serious negative effect.And structure dyeing can solve well
Contradiction between traditional dyeing and environmental pollution.Schemochrome be make light wave and fiber surface micro structure scatter, diffraction or interference
And the physical process of the shades of colour produced, it is derived from butterfly's wing in nature, the biomimetic concept of opal structural colour developing.As
Fruit can form a Rotating fields color on the surface of fiber, it is possible to the effective defect overcome during traditional dyeing also brings up intelligence
Structure coloring fiber.
In schemochrome fiber research field, researcher both domestic and external is all constantly being explored, and actively seeks simple to operate, effective
Give the route of fiber color.H.Z.Wang etc. are at Chemical Communications Vol.47 (2011) pp.12801-12803
In report at one layer of opal structural of fiberglass surfacing self assembly, thus realize the target of fiberglass surfacing schemochrome, but
It is the SiO used2Adhesion between nanosphere and fiber is not strong, and the macromolecular fibre with certain schemochrome is the most urgently opened
Send out.The preparation in Optics Express, Vol.16 (2008) pp.15677-15693 such as M.Skorobogatiy seminar of Canada is poly-
Compound photonic crystal fiber (PBG Bragg Fiber) have also discovered the effect of schemochrome, due to refractive index between multiple structure
Difference, when incident illumination is propagated in the optical fiber of the PMMA/PS multiple structure that it is prepared when, part light appears from optical fiber,
Macroscopically can also be observed that bright color, this for utilize two-dimensional photon crystal structure to prepare schemochrome fiber provides must
The theoretical foundation wanted and experiment condition, but premise has been intended to external light source.J.J.Baumberg is at Optics
PS ball is scattered in polymer by Express, Vol.19 (2011) pp.3144-3154 utilize spinning-drawing machine prepared a kind of based on
The schemochrome fiber of opal structural, but its color developing needs to be improved further.
Summary of the invention
The technical problem to be solved is to provide one and prepares schemochrome carbon fibre based on P (NIPAAm-co-AAc) nanosphere
The method of dimension, the schemochrome fiber prepared by the present invention has good optical property, and the present invention is without toxic chemical dyestuff, side
Method is simple, and the environmental pollution to reducing dyeing and finishing industry has important reference value.
The method that the one of the present invention prepares schemochrome carbon fiber based on P (NIPAAm-co-AAc) nanosphere, including:
(1) carbon fiber is sequentially placed in ethanol solution, acetone soln, ultra-pure water, carries out ultrasonic cleaning each 25～30min,
Post-drying；
(2) NIPA, N are weighed under room temperature, N '-methylene-bisacrylamide, acrylic acid, dodecyl sodium sulfonate
Sodium and ultra-pure water magnetic agitation are dissolved and are obtained reaction solution；It is passed through nitrogen, heating, add initiator and carry out emulsion polymerization；
Reaction 4-6h, is cooled to room temperature, the emulsion obtained is centrifuged washing, obtains P (NIPAAm-co-AAc) nanosphere；Its
Middle NIPA and acrylic acid mass ratio are 5: 1-40: 1；NIPA and N, N '-methylene bisacrylamide
The mass ratio of amide and dodecyl sodium sulfate three is 15: 1: 1-25: 1: 1.
(3) P (NIPAAm-co-AAc) nanosphere and ultra-pure water are mixed to get dispersion liquid, and dispersion liquid is placed in endless metal appearance
In device, the carbon fiber in (1) is placed at container center, by extra electric field electrophoretic deposition, then that fiber is the evenest
Speed pull-out, is dried under room temperature, i.e. can get the schemochrome fiber that P (NIPAAm-co-AAc) nanosphere assembles.
In described step (1), ethanol solution concentration is 90%-99%, and acetone soln concentration is 90%-99%, the resistance of ultra-pure water
Rate is 18.2M Ω cm-1。
Magnetic agitation speed in described step (2) is 300-800rpm.
Centrifugal rotational speed in described step (2) is 8500-9000rpm.
Initiator injection rate in described step (2) is 10ml/30s-10ml/60s, and initiator is potassium peroxydisulfate, Ammonium persulfate.
In one.
In described step (2), heating-up temperature is 70 DEG C, and heat time heating time is 1h.
Described in described step (3), electrophoretic voltage is 1.6-3.0V, and sedimentation time is 20s-300s, electrophoretic deposition terminate after often
Temperature is lower is dried 0.5-1h.
The present invention is with NIPA, N, and N '-methylene-bisacrylamide, acrylic acid, dodecyl sodium sulfate are initial
Raw material, use emulsion polymerization prepare P (NIPAAm-co-AAc) nanosphere, by P (NIPAAm-co-AAc) nanosphere with
Ultra-pure water is mixed to get dispersion liquid, is placed in by dispersion liquid in endless metal container, individual carbon fibers is placed at container center, logical
Cross extra electric field electrophoretic deposition, then fiber is the most at the uniform velocity pulled out, be dried under room temperature, prepare
The schemochrome fiber that P (NIPAAm-co-AAc) nanosphere assembles.
Beneficial effect
(1) present invention is simple to operate, effective, has industrial applications potentiality；
(2) the schemochrome fiber prepared by the present invention has the optical property of excellence；
(3) present invention has important reference value without chemical dye, the environmental pollution to reducing Dyeing & Finishing Industry.
Accompanying drawing explanation
The FE-SEM picture of P (NIPAAm-co-AAc) nanosphere that the polymerization of Fig. 1 emulsion obtains；
The schemochrome fiber FE-SEM picture that Fig. 2 electrophoretic deposition obtains；Wherein, a is the Flied emission Electronic Speculum of single structure color carbon fiber
Figure, b are the Flied emission Electronic Speculum figure of two root architecture color carbon fibers；
The green schemochrome fibre optics microphotograph that Fig. 3 electrophoretic deposition obtains；
Fig. 4 green schemochrome fiber reflectance spectrum figure.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments be merely to illustrate the present invention and not
For limiting the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, those skilled in the art can
To make various changes or modifications the present invention, these equivalent form of values fall within the application appended claims limited range equally.
Embodiment 1
Weigh 2g NIPA, 0.1gN, N '-methylene-bisacrylamide, 0.05g acrylic acid, 0.1g dodecyl
Sodium sulfonate, it is 300rpm that ultra-pure water puts into magnetic agitation rotating speed in the there-necked flask of 250ml, obtains reaction solution.Keep certain
Flow velocity is passed through nitrogen, heats 1h, initiator potassium persulfate (KPS) 0.05g adding prior wiring solution-forming and carry out emulsion when 70 DEG C
Polyreaction.Reaction 4h, is cooled to room temperature, and the emulsion obtained is centrifuged washing.Centrifuge speed is set as 9000rpm,
Obtain P (NIPAAm-co-AAc) nanosphere.Fig. 1 is the nanosphere FE-SEM that reaction obtains.By the centrifugal nanosphere obtained breast
Liquid is dispersed in ultra-pure water, and is placed in toroidal container by dispersion liquid, and the carbon fiber of cleaning, drying is placed in toroidal container central authorities,
Carrying out electro-deposition under conditions of applied voltage 2V, sedimentation time 120s, carbon fiber is drawn after terminating from toroidal container by deposition
Going out, be dried 1h at normal temperatures, prepare the schemochrome carbon fiber that P (NIPAAm-co-AAc) nanosphere assembles, Fig. 2 is system
The FE-SEM of the schemochrome carbon fiber obtained.Fig. 3 and Fig. 4 is respectively schemochrome fibre optics microphotograph and the reflection of preparation
Spectrum.This it appears that be green schemochrome carbon fiber from way.Reflectance spectrum also can be in correspondence.
Embodiment 2
Weigh 2g NIPA, 0.1gN, N '-methylene-bisacrylamide, 0.15g acrylic acid, 0.1g dodecyl
It is 500rpm that sodium sulfonate, 120ml ultra-pure water put into magnetic agitation rotating speed in the there-necked flask of 250ml, obtains reaction solution.Protect
Hold certain flow rate and be passed through nitrogen, heat 1h when 70 DEG C, add initiator potassium persulfate (KPS) 0.10g of prior wiring solution-forming
Carry out emulsion polymerization.Reaction 5h, is cooled to room temperature, and the emulsion obtained is centrifuged washing.Centrifuge speed is set as
9000rpm, obtains P (NIPAAm-co-AAc) nanosphere.By the centrifugal nanosphere emulsion dispersion obtained in ultra-pure water, and will
Dispersion liquid is placed in toroidal container, the carbon fiber of cleaning, drying is placed in toroidal container central authorities, at applied voltage 2.2V, during deposition
Between carry out electro-deposition under conditions of 180s, carbon fiber is pulled out from toroidal container after terminating, is dried 40min at normal temperatures by deposition,
Prepare the schemochrome carbon fiber that P (NIPAAm-co-AAc) nanosphere assembles.
Embodiment 3
Weigh 2g NIPA, 0.1gN, N '-methylene-bisacrylamide, 0.25g acrylic acid, 0.1g dodecyl
It is 800rpm that sodium sulfonate, 120ml ultra-pure water put into magnetic agitation rotating speed in the there-necked flask of 250ml, obtains reaction solution.Protect
Hold certain flow rate and be passed through nitrogen, heat 1h when 70 DEG C, add initiator potassium persulfate (KPS) 0.15g of prior wiring solution-forming
Carry out emulsion polymerization.Reaction 6h, is cooled to room temperature, and the emulsion obtained is centrifuged washing.Centrifuge speed is set as
8500rpm, obtains P (NIPAAm-co-AAc) nanosphere.By the centrifugal nanosphere emulsion dispersion obtained in ultra-pure water, and will
Dispersion liquid is placed in toroidal container, the carbon fiber of cleaning, drying is placed in toroidal container central authorities, at applied voltage 2.4V, during deposition
Between carry out electro-deposition under conditions of 250s, carbon fiber is pulled out from toroidal container after terminating, is dried 0.5h at normal temperatures by deposition,
Prepare the schemochrome carbon fiber that P (NIPAAm-co-AAc) nanosphere assembles.
Claims (7)
1. the method preparing schemochrome carbon fiber based on P (NIPAAm-co-AAc) nanosphere, including:
(1) carbon fiber is sequentially placed in ethanol solution, acetone soln, ultra-pure water, carries out ultrasonic cleaning each 25～30min,
Post-drying；
(2) NIPA, N are weighed under room temperature, N '-methylene-bisacrylamide, acrylic acid, dodecyl sodium sulfonate
Sodium and ultra-pure water magnetic agitation are dissolved and are obtained reaction solution；It is passed through nitrogen, heating, add initiator and carry out emulsion polymerization instead
Should；Reaction 4-6h, is cooled to room temperature, the emulsion obtained is centrifuged washing, obtains P (NIPAAm-co-AAc) nanometer
Ball；Wherein NIPA and acrylic acid mass ratio are 5:1-40:1；NIPA and N, N '-
The mass ratio of methylene-bisacrylamide and dodecyl sodium sulfate three is 15:1:1-25:1:1；Initiator be potassium peroxydisulfate,
One in Ammonium persulfate.；
(3) P (NIPAAm-co-AAc) nanosphere and ultra-pure water are mixed to get dispersion liquid, and dispersion liquid is placed in endless metal
In container, the carbon fiber in (1) is placed at container center, by extra electric field electrophoretic deposition, then that fiber is calm
Device at the uniform velocity pulls out, is dried under room temperature, i.e. can get the schemochrome fiber that P (NIPAAm-co-AAc) nanosphere assembles.
The method that one the most according to claim 1 prepares schemochrome carbon fiber based on P (NIPAAm-co-AAc) nanosphere, its
Being characterised by: in described step (1), ethanol solution concentration is 90%-99%, acetone soln concentration is 90%-99%, super
Pure resistivity of water is 18.2M Ω cm.
The method that one the most according to claim 1 prepares schemochrome carbon fiber based on P (NIPAAm-co-AAc) nanosphere, its
It is characterised by: the magnetic agitation speed in described step (2) is 300-800rpm.
The method that one the most according to claim 1 prepares schemochrome carbon fiber based on P (NIPAAm-co-AAc) nanosphere, its
It is characterised by: the centrifugal rotational speed in described step (2) is 8500-9000rpm.
The method that one the most according to claim 1 prepares schemochrome carbon fiber based on P (NIPAAm-co-AAc) nanosphere, its
It is characterised by: the initiator injection rate in described step (2) is 10ml/30s-10ml/60s.
The method that one the most according to claim 1 prepares schemochrome carbon fiber based on P (NIPAAm-co-AAc) nanosphere, its
Being characterised by: in described step (2), heating-up temperature is 70 DEG C, heat time heating time is 1h.
The method that one the most according to claim 1 prepares schemochrome carbon fiber based on P (NIPAAm-co-AAc) nanosphere, its
Being characterised by: described in described step (3), electrophoretic voltage is 1.6-3.0V, sedimentation time is 20s-300s, electrophoretic deposition
0.5-1h it is dried at normal temperatures after end.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102517801A (en) * | 2011-12-07 | 2012-06-27 | 苏州大学 | Method for preparing fiber film with structural color |
| CN103074757A (en) * | 2013-01-21 | 2013-05-01 | 东华大学 | Method for preparing structural color fibers by electrophoretic deposition |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102517801A (en) * | 2011-12-07 | 2012-06-27 | 苏州大学 | Method for preparing fiber film with structural color |
| CN103074757A (en) * | 2013-01-21 | 2013-05-01 | 东华大学 | Method for preparing structural color fibers by electrophoretic deposition |
Non-Patent Citations (1)
| Title |
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| 电泳沉积法制备结构色纤维;张骜;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20121015(第10期);第27，28，30，32页 * |
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