CN105646904B - A kind of preparation method of conduction photon crystal water gel - Google Patents
A kind of preparation method of conduction photon crystal water gel Download PDFInfo
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- CN105646904B CN105646904B CN201610005116.3A CN201610005116A CN105646904B CN 105646904 B CN105646904 B CN 105646904B CN 201610005116 A CN201610005116 A CN 201610005116A CN 105646904 B CN105646904 B CN 105646904B
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
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- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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Abstract
The present invention relates to a kind of preparation method of conductive photon crystal water gel, including：By N N-isopropylacrylamides; N N methylene-bisacrylamides and acrylic acid are dissolved in ultra-pure water, obtain reaction solution, then under stirring, condensing reflux, argon gas protective condition; it is heated to 60 80 DEG C and keeps 15 45min; then add potassium persulfate solution and react 4 6h, obtain lotion, be then cooled to room temperature under argon gas protection; centrifugation; PNIPAM Co AAc colloid micro balls are obtained, is then redispersed in ultra-pure water, obtains colloid micro ball dispersion liquid；The aqueous dispersions of colloid micro ball dispersion liquid and poly- (3,4 ethene dioxythiophene) polystyrolsulfon acid PEDOT/PSS are mixed, then carry out self assembly, to obtain the final product.This method is simple and practicable, and the preparation to conductive photon crystal water gel has important value.
Description
Technical field
The invention belongs to the preparation field of Responsive photonic crystals material, more particularly to a kind of conductive photon crystal water gel
Preparation method.
Background technology
Photonic crystal (Photonic Crystal, PC) be it is a kind of possess special periodic structure, can to photon spread into
A kind of material of row regulation and control.1987, E.Yabnolovitch and S.John were respectively on Physical review letters
The concept of photonic crystal is proposed, over the last couple of decades, many methods are had developed into build different scale scope
Interior photonic crystal.Comparing classical certain methods includes layer-by-layer, electrochemical etching technology, laser beam flying
Learn gas phase deposition technology and holographic lithography.As what photonic crystal was studied gos deep into, researcher gradually has the external world
The photon crystal material of response generates keen interest.By the way that some functional polymers and photon crystal structure are compound,
The photon crystal structure that there is response to environmental stimuli (such as temperature, ion, solvent, mechanical force) has been prepared.These
Response type photon crystal material is shown in color, biology or chemical sensor, ink and pigment and some optical sensibilities
Played an increasingly important role on device.
In recent years, constantly explored always in the preparation field of Responsive photonic crystals material, researcher both domestic and external：Example
It is brilliant that such as Asher is used to prepare the photon for having response to temperature using the n-isopropyl acrylamide (PNIPAM) of Thermo-sensitive
Body, on this working foundation, many researcher's profits are prepared for the photon for having response to a variety of environmental stimulis in this way
Crystal structure.Takeoka and Watanabe further have extensively studied thermo-responsive polymerization on the working foundation of Asher etc.
The synthetic method of thing film, they are template using pre-assembled silica colloidal crystal, are prepared for porous hydrogel,
Then silicon dioxide colloid microballoon is etched using hydrofluoric acid (HF), in the case of no silicon dioxide microsphere, this water-setting
Glue still has reversible optic response to the change of temperature.By the colour developing of hydrogel at different temperatures, we can lead to
Cross the height that color carrys out temperature.Fudouzi and Sawada etc. is by the way that polystyrene (PS) colloidal crystal structure is embedded into
Method on one layer of very thin dimethyl silicone polymer (PDMS) film, which is prepared for a kind of color, can occur reversible adjusting
Flexible silicon film, when this thin slice is stretched in the horizontal direction, the distance in its vertical direction will reduce, this is resulted in
The interplanar distance of its (111) crystal face reduces, while blue shift occurs for diffraction maximum, we can determine this by the change of color
The size of external force suffered by kind film.In addition, Responsive photonic crystals material can also be realized to ion, chemical substance, magnetic
The environmental stimulis such as field realize response.Although these response materials have vast potential for future development in fields such as display, detections,
It is the accurate detection difficult to realize to these environmental stimulis.One of the main reasons for this is that by color come to these environmental stimulis into
There are large error for row monitoring.Since electric signal is more readily detected relative to optical signal, these optical signals are converted into electricity
Signal will be highly effective method.And traditional Responsive photonic crystals do not possess electric conductivity, electric conductivity photon material nearly all
The preparation tool of material is of great significance.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation method of conductive photon crystal water gel, the present invention
Method is simple and practicable, and the preparation to conductive photon crystal water gel has important value.
A kind of preparation method of conductive photon crystal water gel of the present invention, including：
(1) n-isopropyl acrylamide, N-N- methylene-bisacrylamides and acrylic acid are dissolved in ultra-pure water, obtained anti-
Liquid is answered, then under stirring, condensing reflux, argon gas protective condition, 60-80 DEG C is heated to and keeps 15-45min, is then added again
Enter potassium persulfate solution reaction 4-6h, obtain lotion, be then cooled to room temperature under argon gas protection, centrifuge, obtain PNIPAM-
Co-AAc colloid micro balls, are then redispersed in ultra-pure water, obtain colloid micro ball dispersion liquid；
(2) by colloid micro ball dispersion liquid and the moisture of poly- (3,4- ethene dioxythiophenes)-polystyrolsulfon acid PEDOT/PSS
Dispersion liquid mixes, and then carries out self assembly, up to conductive photon hydrogel.
It is n-isopropyl acrylamide in reaction solution in the step (1), N-N- methylene-bisacrylamides, acrylic acid, super
The ratio of pure water is：1.0-3.0g：0.01-0.03g：0.2-0.5g：120-160mL.
The mass percentage concentration of potassium persulfate solution is 5%-10% in the step (1).
The volume ratio of potassium persulfate solution and reaction solution is 8-12mL in the step (1)：120-160mL.
Centrifuging temperature is 25-35 DEG C in the step (1), centrifugation rate 8000-11000rpm.
The mass percentage concentration of colloid micro ball dispersion liquid is 45-75% in the step (1).
Colloid micro ball dispersion liquid, poly- (3,4- ethene dioxythiophenes)-polystyrolsulfon acid PEDOT/ in the step (2)
The volume ratio of the aqueous dispersions of PSS is 2:1-5:6.
The matter of the aqueous dispersions of poly- (3,4- ethene dioxythiophenes)-polystyrolsulfon acid PEDOT/PSS in the step (2)
Amount percentage concentration is 30-50%.
Mixed in the step (2) and be：Magnetic agitation mixes after being mixed under the conditions of 35-45 DEG C.
Self assembly is in the step (2)：It is 25-33 DEG C in temperature, keeps 3-5h.
The present invention by the way that n-isopropyl acrylamide, N-N- methylene-bisacrylamides and acrylic acid are dispersed in water,
Then transfer them to again in three-necked flask, adjust temperature, under argon gas atmosphere protection reaction obtain PNIPAM-Co-AAc and receive
Rice ball, and distribute it in water；Finally by the PEDOT/ of the colloid micro ball lotion of different quality containing and different quality concentration
PSS dispersion liquids are mixed and it is carried out self assembly at a certain temperature, have obtained a kind of conductive photonic crystal
Hydrogel.
Beneficial effect
(1) the method for the present invention is simple and practicable, and the preparation to conductive photon crystal water gel has important value；
(2) conductive photon crystal water gel prepared by the present invention, is to be changed based on photon crystal structure and make its electric conductivity
Change, and the process is reversible；
(3) conductive photon crystal water gel prepared by the present invention, can externally show difference according to its different structure
Electric signal, temperature, atmosphere detect etc. field be with a wide range of applications.
Brief description of the drawings
The SEM pictures of the PNIPAM-Co-AAc colloid micro balls of Fig. 1 embodiments 1；
The digital photograph of conductive photon crystal water gel prepared by Fig. 2 embodiments 1 at different temperatures, wherein (a) is water
Gel reagent bottle is overturn at 25 DEG C after digital photograph, conductive photon crystal water gel is gel state at this time, and (b) is water-setting
Digital photograph of the glue at 35 DEG C, conductive photon crystal water gel is dissolved colloidal state at this time；
PNIPAM-Co-AAc prepared by Fig. 3 embodiments 2：The infrared spectrum of PEDOT/PSS conduction photon crystal water gels
Figure；
The conductive photon crystal water gel resistance variation with temperature of Fig. 4 embodiments 2；
SEM figures after the conductive photon crystal water gel of Fig. 5 embodiments 3 is freeze-dried；
For the conductive photon crystal water gel of Fig. 6 embodiments 3 to the response of thermal stimulus, wherein illustration is hydrogel in temperature
The partial enlarged view of resistance variations under stimulating.
Embodiment
With reference to specific embodiment, the present invention is further explained.It is to be understood that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Scope.
Embodiment 1
At room temperature, 1.0g n-isopropyl acrylamide, 0.01g N-N- methylene-bisacrylamides, 0.2g third are weighed
Olefin(e) acid, is placed in beaker, adds 120mL ultra-pure waters.Low whipping speed is that magnetic agitation fills reactant in 30 minutes under 300rpm
Divide and dissolve and be transferred into the three-necked flask of 250mL.Three-necked flask is placed in oil bath pan, in stirring, condensing reflux, argon
80 DEG C are heated under gas atmosphere protection, continues 25min and is passed through argon gas, achievees the purpose that to remove the oxygen dissolved in ultra-pure water.
Next, adding the potassium persulfate solution that 12mL mass fractions are 5% into three-necked flask, 4h is reacted at 80 DEG C.Reaction
After the completion of, colloid micro ball lotion is cooled to room temperature under argon gas atmosphere protection.Then, by colloid emulsion at 27 DEG C,
Centrifuged under 11000rpm rotating speeds, obtain PNIPAM-Co-AAc colloid micro balls.As shown in Figure 1.
Fig. 1 is the SEM pictures of prepared PNIPAM-Co-AAc colloid micro balls.Then it is dispersed in water, makes its matter
It is 45% to measure fraction.The dispersion liquid of 2mL PNIPAM-Co-AAc colloid micro balls in water is measured, is 50% with 1mL mass concentrations
PEDOT/PSS dispersion liquids be thoroughly mixed at a temperature of 35 DEG C.After the completion of mixing, transfer them in 26 DEG C of environment
Colloid micro ball is set to carry out self assembly, the time of its self assembly is 4h.After being completed, a kind of conductive photonic crystal water has been obtained
Gel.Fig. 2 is digital photograph of the conductive photon crystal water gel in the case where 35 DEG C of 25 DEG C of (a) and (b), at different temperatures, conductive
Photonic crystal hydrogel can occur gel-sol state transformation.
Embodiment 2
At room temperature, 1.5g n-isopropyl acrylamide, 0.02g N-N- methylene-bisacrylamides, 0.3g third are weighed
Olefin(e) acid, is placed in beaker, adds 140mL ultra-pure waters.Low whipping speed is that magnetic agitation fills reactant in 30 minutes under 300rpm
Divide and dissolve and be transferred into the three-necked flask of 250mL.Three-necked flask is placed in oil bath pan, in stirring, condensing reflux, argon
70 DEG C are heated under gas atmosphere protection, continues 35min and is passed through argon gas, achievees the purpose that to remove the oxygen dissolved in ultra-pure water.
Next, adding the potassium persulfate solution that 10mL mass fractions are 8% into three-necked flask, 4h is reacted at 70 DEG C.Reaction
After the completion of, colloid micro ball lotion is cooled to room temperature under argon gas atmosphere protection.Then, by colloid emulsion at 30 DEG C,
Centrifuged under 10000rpm rotating speeds, obtain PNIPAM-Co-AAc colloid micro balls.Then colloid micro ball is dispersed in water, made
Its mass fraction is 50%.The dispersion liquid of 3mL PNIPAM-Co-AAc colloid micro balls in water is measured, is with 4mL mass concentrations
40% PEDOT/PSS dispersion liquids are thoroughly mixed at a temperature of 40 DEG C.After the completion of mixing, 30 DEG C of ring is transferred them to
Colloid micro ball is set to carry out self assembly in border, the time of its self assembly is 5h.After being completed, it is brilliant a kind of conductive photon has been obtained
Body hydrogel.Fig. 3 is conductive photon crystal water gel infrared spectrogram, by infrared spectrogram it can be seen that what is be prepared leads
The photonic crystal hydrogel of electricity has been provided simultaneously with PNIPAM-Co-AAc and PEDOT/PSS characteristic groups.Fig. 4 is this hydrogel
Resistance at different temperatures.
Embodiment 3
At room temperature, 2.5g n-isopropyl acrylamide, 0.03g N-N- methylene-bisacrylamides, 0.4g third are weighed
Olefin(e) acid, is placed in beaker, adds 160mL ultra-pure waters.Low whipping speed is that magnetic agitation fills reactant in 30 minutes under 300rpm
Divide and dissolve and be transferred into the three-necked flask of 250mL.Three-necked flask is placed in oil bath pan, in stirring, condensing reflux, argon
60 DEG C are heated under gas atmosphere protection, continues 40min and is passed through argon gas, achievees the purpose that to remove the oxygen dissolved in ultra-pure water.
Next, adding the potassium persulfate solution that 9mL mass fractions are 10% into three-necked flask, 6h is reacted at 60 DEG C.Reaction
After the completion of, colloid micro ball lotion is cooled to room temperature under argon gas atmosphere protection.Then, by colloid emulsion at 33 DEG C, 8000rpm
Centrifuged under rotating speed, obtain PNIPAM-Co-AAc colloid micro balls, be then dispersed in water, make its mass fraction be
55%.The dispersion liquid of 5mL PNIPAM-Co-AAc colloid micro balls in water is measured, with the PEDOT/ that 6mL mass concentrations are 50%
PSS dispersion liquids are thoroughly mixed at a temperature of 45 DEG C.After the completion of mixing, transferring them in 33 DEG C of environment makes colloid micro-
Ball carries out self assembly, and the time of its self assembly is 6h.After being completed, a kind of conductive photonic crystal hydrogel has been obtained.Fig. 5
The SEM for being this conductive hydrogel after freeze-dried figures, Fig. 6 are signal of the conductive photon crystal water gel under thermal stimulus
Response.
Claims (10)
1. a kind of preparation method of conduction photon crystal water gel, including：
(1) n-isopropyl acrylamide, N, N- methylene-bisacrylamides and acrylic acid are dissolved in ultra-pure water, are reacted
Liquid, then under stirring, condensing reflux, argon gas protective condition, is heated to 60-80 DEG C and keeps 15-45min, then add
Potassium persulfate solution reacts 4-6h, obtains lotion, is then cooled to room temperature under argon gas protection, centrifuges, obtain PNIPAM-Co-
AAc colloid micro balls, are then redispersed in ultra-pure water, obtain colloid micro ball dispersion liquid；
(2) by colloid micro ball dispersion liquid and the aqueous dispersions of poly- (3,4- ethene dioxythiophenes)-polystyrolsulfon acid PEDOT/PSS
Mix, then carry out self assembly, up to conductive photon hydrogel.
A kind of 2. preparation method of conductive photon crystal water gel according to claim 1, it is characterised in that：The step
(1) n-isopropyl acrylamide, N, N- methylene-bisacrylamides, acrylic acid, the ratio of ultra-pure water are in reaction solution in：1.0-
3.0g：0.01-0.03g：0.2-0.5g：120-160mL.
A kind of 3. preparation method of conductive photon crystal water gel according to claim 1, it is characterised in that：The step
(1) mass percentage concentration of potassium persulfate solution is 5%-10% in.
A kind of 4. preparation method of conductive photon crystal water gel according to claim 1, it is characterised in that：The step
(1) volume ratio of potassium persulfate solution and reaction solution is 8-12mL in：120-160mL.
A kind of 5. preparation method of conductive photon crystal water gel according to claim 1, it is characterised in that：The step
(1) centrifuging temperature is 25-35 DEG C in, centrifugation rate 8000-11000rpm.
A kind of 6. preparation method of conductive photon crystal water gel according to claim 1, it is characterised in that：The step
(1) mass percentage concentration of colloid micro ball dispersion liquid is 45-75% in.
A kind of 7. preparation method of conductive photon crystal water gel according to claim 1, it is characterised in that：The step
(2) colloid micro ball dispersion liquid in, poly- (3,4- ethene dioxythiophenes)-polystyrolsulfon acid PEDOT/PSS aqueous dispersions body
Product is than being 2:1-5:6.
A kind of 8. preparation method of conductive photon crystal water gel according to claim 1, it is characterised in that：The step
(2) mass percentage concentration of the aqueous dispersions of (3,4- ethene dioxythiophenes)-polystyrolsulfon acid PEDOT/PSS poly- in is 30-
50%.
A kind of 9. preparation method of conductive photon crystal water gel according to claim 1, it is characterised in that：The step
(2) mixed in and be：Magnetic agitation mixes after being mixed under the conditions of 35-45 DEG C.
A kind of 10. preparation method of conductive photon crystal water gel according to claim 1, it is characterised in that：The step
Suddenly self assembly is in (2)：It is 25-33 DEG C in temperature, keeps 3-5h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103436965A (en) * | 2013-07-13 | 2013-12-11 | 吉林大学 | Preparation method of polymer photonic crystals with adjustable photonic band gap and presenting patterned color display |
| CN103804700A (en) * | 2014-02-19 | 2014-05-21 | 东华大学 | Method for preparing chemically crosslinked photonic crystal hydrogel with adjustable color |
| CN103980670A (en) * | 2014-05-13 | 2014-08-13 | 南京理工大学 | A bacterial cellulose/poly(3,4-ethylenedioxythiophene) nanometer conductive composite material and a preparing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103436965A (en) * | 2013-07-13 | 2013-12-11 | 吉林大学 | Preparation method of polymer photonic crystals with adjustable photonic band gap and presenting patterned color display |
| CN103804700A (en) * | 2014-02-19 | 2014-05-21 | 东华大学 | Method for preparing chemically crosslinked photonic crystal hydrogel with adjustable color |
| CN103980670A (en) * | 2014-05-13 | 2014-08-13 | 南京理工大学 | A bacterial cellulose/poly(3,4-ethylenedioxythiophene) nanometer conductive composite material and a preparing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| "Electro-active hybrid actuators based on freeze-dried bacterial cellulose and PEDOT:PSS";Si-Seup Kim et al.;《Smart Materials and Structures》;20130706;第22卷;第3页第2段 * |
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