CN106916325A - A kind of method for preparing free patterned surface film of poly pyrrole - Google Patents
A kind of method for preparing free patterned surface film of poly pyrrole Download PDFInfo
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- CN106916325A CN106916325A CN201710173422.2A CN201710173422A CN106916325A CN 106916325 A CN106916325 A CN 106916325A CN 201710173422 A CN201710173422 A CN 201710173422A CN 106916325 A CN106916325 A CN 106916325A
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- pdms
- pva
- film
- ppy
- poly pyrrole
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0605—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0611—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring, e.g. polypyrroles
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
Abstract
The invention discloses a kind of method for preparing free patterned surface film of poly pyrrole, its preparation process includes：Certain thickness film of poly pyrrole is deposited on elastic substrates PDMS first, the film of poly pyrrole washing drying that will be obtained can obtain the PPy films with patterned surface；Then, the PVA of 10wt% is cast in PDMS/PPy surfaces, obtains three layers of compound system PDMS/PPy/PVA, wherein the thickness of PVA is at 30 μm or so.Then, carefully PPy/PVA bilayer systems are taken off from PDMS substrates, is put in tank and dissolves PVA, so as to the free PPy films for obtaining independently being supported with wrinkle pattern.The present invention is successfully prepared freely independent patterned surface film of poly pyrrole using simple and efficient mode of operation, so as to avoid complicated cumbersome operating procedure, the loss of preparation time with high equipment and experiment consumptive material more long.
Description
Technical field
It is thin the present invention relates to a kind of preparation of patterned surface film of poly pyrrole, more particularly to a kind of free independent polymers
The preparation of film.
Background technology
The independent film of poly pyrrole material of freedom with patterned surface caused the extensive concern of people and
It is widely used in the life of people, such as super hydrophobic material and flexible electronic device.Poly- pyrrole prepared by traditional method
Coughing up its free independence of film and picture on surface can not typically get both, but, if it is possible to the distinct faces that gain freedom pattern
The film of poly pyrrole of change, just can effectively increase the specific surface area of film of poly pyrrole, recycle its free independence to shift
Onto any target substrate, and then its application field can be expanded.In recent years, by from corrugation produce pattern, and using turn
Shifting technology prepares free patterned surface film of poly pyrrole and gradually attracts attention, because its is easy to operate and with one
Fixed controllability and more and more paid attention to.But in existing research, this method is not also especially ripe, so system
The film of poly pyrrole material of standby free patterned surface also turns into a trend and focus of future technical advances.
The content of the invention
For above-mentioned prior art, the invention provides the polypyrrole that free patterned surface is prepared in a kind of short time
The method of film.By the simple control reaction time, the free film of poly pyrrole with different surface morphology can be prepared, had
The features such as having simple, quick, reproducible, it is to avoid preparation process complexity, apparatus expensive, the low shortcoming of efficiency, dredges on surface
There is potential application prospect in water material, the field such as construct of microcircuit.
In order to solve the above-mentioned technical problem, it is proposed by the present invention a kind of to prepare free patterned surface film of poly pyrrole
Method, comprises the following steps：
Step one, according to mass ratio it is 20 by PDMS performed polymers and crosslinking agent:After 1 mixing, pour into centrifuge tube, use glass
Rod stirs to form uniform mixture；
Step 2, the mixture for obtaining step one pour into culture dish after Fruit storage 1h being uniformly distributed；
Step 3, the mixture that will be poured into culture dish carry out Fruit storage 30min, are put into baking oven, at 70 DEG C
Under be heating and curing 4h, obtain PDMS substrates
Step 4, according to mass volume ratio for be dissolved in pyrrole monomer in hydrochloric acid by 6.5~7.0mg/ml, ultrasound is mixed
To solution A, according to mass volume ratio for be dissolved in iron chloride in hydrochloric acid by 30~35mg/ml, ultrasound is uniformly mixed so as to obtain solution B；
Step 5, solution A obtained in step 4 is transferred to it is contained with the culture dish of PDMS substrates, is subsequently adding step
Solution B obtained in four, wherein, solution A is 1 with the volume ratio of solution B:1, it is put into the refrigerator that temperature is 2~5 DEG C after uniform mixing
Interior reaction 3min to 7h；
Step 6, reaction take out culture dish after terminating from refrigerator, remove supernatant liquid, and the reactant in culture dish is used
Distilled water flushing is totally dried up afterwards, obtains PDMS/PPy films；
Step 7：The PVA solution that mass concentration is 10% is cast in the PDMS/PPy film surfaces that step 6 is obtained,
The height of PVA solution is 25~35 μm on PDMS/PPy film surfaces, and tri- layers of compound systems of PDMS/PPy/PVA are obtained；
Step 8：PPy/PVA bilayer systems are taken off from PDMS substrates, are then transferred in tank, dissolve PVA,
So as to the film of poly pyrrole for obtaining that freely there is wrinkle topographical surface patterning.
In the method for preparing free picture on surface polymer film proposed by the present invention, by regulating step five
Reaction time, obtain the free film of poly pyrrole with different surface morphology, the amplitude and frequency of surface topography with reaction
Time is directly proportional.
Compared with prior art, the beneficial effects of the invention are as follows：
The present invention is substrate from elastomeric material PDMS, and certain thickness film of poly pyrrole is deposited on its surface, and PVA is poured
Note in PDMS/PVA surfaces, tri- layers of compound systems of PDMS/PPy/PVA are obtained, PPy/PVA bilayer systems are taken off from PDMS substrates
Under, it is put in tank and is dissolved PVA, so as to obtains with the freely independent PPy films of wrinkle pattern.Finally, by target
A part for substrate is dipped in water, and substrate is pulled out from water, while PPy films are transferred to target substrate surface.By regulation
In the reaction time, the free film of poly pyrrole material with different surface morphology can be obtained.The present invention utilizes simple and efficient operation
Mode prepares free patterned surface film of poly pyrrole in being successfully realized the short time, so as to avoid complicated cumbersome operation
Step, the loss of preparation time more long and high equipment and experiment consumptive material.
Brief description of the drawings
Fig. 1 is the optical microscope picture of the film of poly pyrrole that the embodiment of the present invention 1 is obtained；
Fig. 2 is the optical photograph of the free film of poly pyrrole that the embodiment of the present invention 1 is obtained；
Fig. 3 is the optical microscope picture of the free film of poly pyrrole that the embodiment of the present invention 1 is obtained；
Fig. 4 is the optical microscope picture of the film of poly pyrrole that the embodiment of the present invention 2 is obtained；
Fig. 5 is the optical photograph of the free film of poly pyrrole that the embodiment of the present invention 2 is obtained；
Fig. 6 is the optical microscope picture of the free film of poly pyrrole that the embodiment of the present invention 2 is obtained.
Specific embodiment
Technical solution of the present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings, described is specific
Embodiment is only explained to the present invention, is not intended to limit the invention.
Embodiment 1：
A kind of method of the film of poly pyrrole material for preparing free patterned surface, comprises the following steps：
Step one：It is 20 according to mass ratio by PDMS performed polymers and crosslinking agent:After 1 mixing, pour into centrifuge tube, use glass
Rod stirs to form uniform mixture；
Step 2：Square culture dish is poured into after the mixture of PDMS performed polymers and crosslinking agent is carried out into Fruit storage 1h
In, and be allowed to be evenly distributed in culture dish；
Step 3：The performed polymer that will be poured into culture dish carries out Fruit storage 30min with the mixture of crosslinking agent, so
After be put into baking oven, be heating and curing 4h at 70 DEG C, obtains PDMS substrates；
Step 4：Ultrasound is uniformly mixed so as to obtain chromium solution during 0.2013g pyrrole monomers are dissolved in into the hydrochloric acid of 30ml, stand-by；
Ultrasound is uniformly mixed so as to obtain ferric chloride solution during the iron chloride of 0.9732g is dissolved in into the hydrochloric acid of 30ml, stand-by；
Step 5：The chromium solution that will first prepare is transferred to and is contained with the culture dish of PDMS substrates, is subsequently adding and matches somebody with somebody
The ferric chloride solution for making, makes its uniform mixing, is put into refrigerator (temperature is at 2~5 DEG C), reacts 1h；
Step 6：Reaction takes out culture dish after terminating from refrigerator, removes supernatant liquid, and the reactant in culture dish is used
Distilled water flushing is clean, after dried up with ear washing bulb, the material for obtaining is PDMS/PPy films, as shown in Figure 1；
Step 7：The PVA solution of 10wt% is cast in PDMS/PPy film surfaces, the amount for pouring into a mould PVA solution is liquid
Thickness on film surface is 30 μm or so, and tri- layers of compound systems of PDMS/PPy/PVA are obtained；
Step 8：The PPy/PVA bilayer systems of 1cm × 1cm are cut, is carefully taken it off from PDMS substrates, then
It is transferred in tank, dissolves PVA, so as to the film of poly pyrrole for obtaining that freely there is wrinkle topographical surface patterning, such as Fig. 2
It is shown.Free film of poly pyrrole finally is pulled out to observe its surface topography with the PDMS substrates of blank, as shown in Figure 3.
Embodiment 2：
A kind of method of the film of poly pyrrole material for preparing free patterned surface, in embodiment 2, except step 5 with
Step in embodiment 1 is different, other step all sames.In step 5, the reaction time 2h will be adjusted to, the PDMS/ for obtaining
PPy films are as shown in Figure 4；Free the film of poly pyrrole such as Fig. 5 and Fig. 6 with wrinkle topographical surface patterning for finally giving
It is shown.
To sum up, if the present invention deposits film of poly pyrrole in PDMS substrates, using the phase interaction between PVA and polypyrrole
With, film of poly pyrrole is peeled off from PDMS substrates, PVA is then dissolved in the sink, finally obtain free picture on surface
The film of poly pyrrole of change.The free film of poly pyrrole of different surface morphology, surface are can obtain by adjusting the different reaction time
The amplitude and frequency of pattern are directly proportional to the reaction time.The inventive method preparation process is simple, and process control is stronger.
Although above in conjunction with accompanying drawing, invention has been described, the invention is not limited in above-mentioned specific implementation
Mode, above-mentioned specific embodiment is only schematical, and rather than restricted, one of ordinary skill in the art is at this
Under the enlightenment of invention, without deviating from the spirit of the invention, many variations can also be made, these belong to of the invention
Within protection.
Claims (2)
1. a kind of method for preparing free patterned surface film of poly pyrrole, it is characterised in that comprise the following steps：
Step one, according to mass ratio it is 20 by PDMS performed polymers and crosslinking agent:After 1 mixing, pour into centrifuge tube, stirred with glass bar
Mix to form uniform mixture；
Step 2, the mixture for obtaining step one pour into culture dish after Fruit storage 1h being uniformly distributed；
Step 3, the mixture that will be poured into culture dish carry out Fruit storage 30min, are put into baking oven, add at 70 DEG C
Heat cure 4h, obtains PDMS substrates
Step 4, according to mass volume ratio for be dissolved in pyrrole monomer in hydrochloric acid by 6.5~7.0mg/ml, ultrasound is uniformly mixed so as to obtain molten
Liquid A, according to mass volume ratio for be dissolved in iron chloride in hydrochloric acid by 30~35mg/ml, ultrasound is uniformly mixed so as to obtain solution B；
Step 5, solution A obtained in step 4 is transferred to it is contained with the culture dish of PDMS substrates, is subsequently adding step 4 system
The solution B for obtaining, wherein, solution A is 1 with the volume ratio of solution B:1, it is put into the refrigerator that temperature is 2~5 DEG C after uniform mixing anti-
Answer 3min to 7h；
Step 6, reaction take out culture dish after terminating from refrigerator, remove supernatant liquid, by the reactant distillation in culture dish
Water is dried up after rinsing well, obtains PDMS/PPy films；
Step 7：The PVA solution that mass concentration is 10% is cast in the PDMS/PPy film surfaces that step 6 is obtained, PDMS/
The height of PVA solution is 25~35 μm on PPy film surfaces, and tri- layers of compound systems of PDMS/PPy/PVA are obtained；
Step 8：PPy/PVA bilayer systems are taken off from PDMS substrates, is then transferred in tank, dissolve PVA, so that
Obtain the film of poly pyrrole freely with wrinkle topographical surface patterning.
2. the method for preparing free picture on surface polymer film according to claim 1, it is characterised in that by adjusting
In reaction time in section step 5, obtain the free film of poly pyrrole with different surface morphology, the amplitude and frequency of surface topography
Rate is directly proportional to the reaction time.
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| CN201710173422.2A CN106916325A (en) | 2017-03-22 | 2017-03-22 | A kind of method for preparing free patterned surface film of poly pyrrole |
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| CN201710173422.2A CN106916325A (en) | 2017-03-22 | 2017-03-22 | A kind of method for preparing free patterned surface film of poly pyrrole |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108641106A (en) * | 2018-06-11 | 2018-10-12 | 天津大学 | A method of based on film of poly pyrrole of the PS templates structure with hierarchical morphology |
| CN108659246A (en) * | 2018-06-11 | 2018-10-16 | 天津大学 | A method of based on film of poly pyrrole of the silicon template structure with hierarchical morphology |
| CN108943676A (en) * | 2018-06-11 | 2018-12-07 | 天津大学 | A method of it is write using laser processing on film of poly pyrrole surface |
| CN108978220A (en) * | 2018-07-09 | 2018-12-11 | 天津大学 | A method of preparing the conductive polyurethane fiber with polypyrrole crepe structure |
| CN109161038A (en) * | 2018-07-09 | 2019-01-08 | 天津大学 | A method of regulating and controlling film of poly pyrrole surface topography by changing substrate modulus |
| CN109251335A (en) * | 2018-07-09 | 2019-01-22 | 天津大学 | Regulate and control the method for its surface topography based on polypyrrole polymerization reaction time is changed |
| CN110423368A (en) * | 2019-06-27 | 2019-11-08 | 天津大学 | A method of there is the film of poly pyrrole of hierarchical morphology using the preparation of doped hydrochloride swelling effect |
| CN110628074A (en) * | 2019-09-30 | 2019-12-31 | 天津大学 | Method for preparing internal structure based on porous PDMS |
| CN110696459A (en) * | 2019-09-30 | 2020-01-17 | 天津大学 | Preparation method of polypyrrole-BOPP (biaxially-oriented Polypropylene) -based actuator |
-
2017
- 2017-03-22 CN CN201710173422.2A patent/CN106916325A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108641106A (en) * | 2018-06-11 | 2018-10-12 | 天津大学 | A method of based on film of poly pyrrole of the PS templates structure with hierarchical morphology |
| CN108659246A (en) * | 2018-06-11 | 2018-10-16 | 天津大学 | A method of based on film of poly pyrrole of the silicon template structure with hierarchical morphology |
| CN108943676A (en) * | 2018-06-11 | 2018-12-07 | 天津大学 | A method of it is write using laser processing on film of poly pyrrole surface |
| CN108978220A (en) * | 2018-07-09 | 2018-12-11 | 天津大学 | A method of preparing the conductive polyurethane fiber with polypyrrole crepe structure |
| CN109161038A (en) * | 2018-07-09 | 2019-01-08 | 天津大学 | A method of regulating and controlling film of poly pyrrole surface topography by changing substrate modulus |
| CN109251335A (en) * | 2018-07-09 | 2019-01-22 | 天津大学 | Regulate and control the method for its surface topography based on polypyrrole polymerization reaction time is changed |
| CN110423368A (en) * | 2019-06-27 | 2019-11-08 | 天津大学 | A method of there is the film of poly pyrrole of hierarchical morphology using the preparation of doped hydrochloride swelling effect |
| CN110628074A (en) * | 2019-09-30 | 2019-12-31 | 天津大学 | Method for preparing internal structure based on porous PDMS |
| CN110696459A (en) * | 2019-09-30 | 2020-01-17 | 天津大学 | Preparation method of polypyrrole-BOPP (biaxially-oriented Polypropylene) -based actuator |
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Application publication date: 20170704 |