CN106147204A - A kind of preparation method of graphene/polyaniline/conductive polyurethane laminated film - Google Patents
A kind of preparation method of graphene/polyaniline/conductive polyurethane laminated film Download PDFInfo
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- CN106147204A CN106147204A CN201610761653.0A CN201610761653A CN106147204A CN 106147204 A CN106147204 A CN 106147204A CN 201610761653 A CN201610761653 A CN 201610761653A CN 106147204 A CN106147204 A CN 106147204A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
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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
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
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Abstract
The present invention relates to the preparation method of a kind of graphene/polyaniline/conductive polyurethane laminated film, use Ammonium persulfate. as oxidant, hydrochloric acid is as adulterant, aniline monomer in-situ polymerization is used to generate graphene oxide/polyaniline modification polyurethane film, then thermal reduction is used to process graphene oxide obtained above/polyaniline/polyurethane laminated film, obtain the graphene/polyaniline/conductive polyurethane laminated film of the present invention, finally carry out conducting performance test.The method is quick, easy, and energy expenditure is low, it is adaptable to large-scale production, and prepared conductive polyurethane Thin film conductive performance is excellent.
Description
Technical field
The present invention relates to the preparation method of a kind of functional material, particularly relate to graphene/polyaniline/polyurethane guide and reply by cable
Close method for manufacturing thin film.
Background technology
Polyurethane is a kind of not only to have the high rigidity of plastics but also have the elastomeric high molecular synthetic material of rubber.With other
Material is compared, on soft or hard section chain numerous functional groups and labyrinth make polyurethane have abrasion performance, oil resistant, resistance to chemical attack,
The characteristics such as resistance to x radiation x, are widely used as plastics, rubber, adhesive, coating, leather, but owing to it is heat-resisting, water-fast and anti-
The poor performance such as electrostatic, limit it and further apply.The development maked rapid progress along with science and technology, conductive polyurethane functionalization becomes
One new study hotspot of polyurethane field, conductivity type polyurethane has the widest application prospect because of it, thus closes in recent years
Research in conductive polyurethane causes people more and more to pay close attention to.These many researcheres are used organosilicons, acrylic resin,
Epoxy resin, natural product and with the method such as plastic blend, chopped fiber filling, it is modified, with satisfied different departments pair
The requirement of polyurethane material performance, but these method of modifying exist, and cost is the highest or the shortcoming of poor effect.
Polyaniline is a kind of very important conducting polymer, this is because compared to other structural conductive macromoleculars,
Polyaniline self has high conductivity and high environmental stability, and aniline monomer is relatively cheap, and polymerization technique is simple and produces
Amount height.Therefore, just it has been widely studied since polyaniline occurs, and is considered as the conducting polymer having most application prospect.But
It is that for common high molecular materials, the machine-shaping of polyaniline is the most difficult, and it can not melt, because polyaniline exists
It softens or just decomposes under melt temperature.To this end, common by polyaniline and the excellent performance being prone to processing and forming
Functional type material is prepared in macromolecule combination, becomes the first-selected approach improving Polyaniline Processability energy, and conductivity type polyurethane is just
Cater to this demand.At present, had some reports about polyurethane/polyaniline composite material, but obtain compound
The performance of material is the most poor, and most of limting concentration ratio is relatively low, which limits the range of application of this composite.
Graphene is that it is permissible by the carbonaceous new material of the bi-dimensional cellular shape lattice structure of the tightly packed one-tenth of monolayer carbon atom
Being warped into the fullerene of zero dimension, be rolled into one-dimensional CNT or be stacked to the graphite of three-dimensional, therefore Graphene is to constitute other
The elementary cell of material with carbon element, is described as " mother of material with carbon element ".With electricity, mechanics and the thermal property of its excellence, become energy storage material
The focus of material area research.Modified by surface that graphene-based material can be made to have good power characteristic, higher energy is close
Degree and good electrochemical stability, have good application prospect in terms of preparing conductive material.
Therefore, the present invention combines the addition of novel conductive material Graphene, in-situ polymerization polyaniline, and modified polyurethane is thin
Film, is prepared for a kind of novel graphene/polyaniline/conductive polyurethane laminated film.This invention is simple to operate, low cost, easily
Amplify in technique.
Summary of the invention
It is an object of the invention to provide the preparation method of the excellent polyurethane film of a kind of conducting function, the method quickly,
Easy, low cost, it is adaptable to large-scale production.
The preparation method of a kind of graphene/polyaniline/conductive polyurethane laminated film of the present invention, comprises the following steps:
(1) appropriate monomer aniline is joined in the hydrochloric acid solution of certain molar concentration, obtain the monomer solution of reaction；
(2) graphene oxide and the Ammonium persulfate. of certain mass are dissolved in the hydrochloric acid solution of certain molar concentration, stirring,
To initiator solution；
(3) in the solution of step (2), add certain mass and the polyurethane film of size, in above-mentioned solution, then add step
Suddenly the aniline monomer solution of (1), rapid mix homogeneously, stand 10-30 minute；
(4) take out polyurethane film, be washed with deionized water clean, put in baking oven and dry, i.e. obtain the Graphene/polyphenyl of the present invention
Amine/polyurethane guide conductive film.
The consumption of the aniline of described step (1) is 30 ~ 180 μ L.
The molar concentration of the hydrochloric acid of described step (1) is 0.5-2.5 mol/L.
The volume of described step (1) hydrochloric acid is 5 ~ 15 mL.
The quality of the graphene oxide of described step (2) is 1.0-100 mg.
The consumption of the Ammonium persulfate. of described step (2) is 0.15 ~ 0.3g.
The volume of described step (2) hydrochloric acid is 5 ~ 15mL.
The quality of the polyurethane of described step (3) is 200 ~ 1000 mg.
The size of the polyurethane of described step (3) is 2cmx2cm.
The thickness of the polyurethane of described step (3) is 2-10 m.
The quick mixing time of described step (3) is 1-5 minute.
The oven temperature of described step (4) is 100-250 DEG C.
The drying time of described step (4) is: 1.0 ~ 2.0 hours.
Beneficial effects of the present invention:
(1) method of the present invention is simple to operate, the most less, product excellent electric conductivity；
(2) raw material sources are convenient, it is simple to large-scale industrial production；
(3) production process does not the most produce pollutant, it is to avoid environmental pollution.
Accompanying drawing explanation
Fig. 1 is the different Graphene consumption impacts on laminated film electrical conductivity.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate the present invention
Rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, people in the art
The present invention can be made various changes or modifications by member, and these equivalent form of values fall within the application appended claims equally and limited
Scope.
Embodiment 1
The preparation of polyaniline/polyurethane conductive composite film, comprises the steps:
Step (1): 150 μ L aniline are joined 10 ml, and molar concentration is in the hydrochloric acid solution of 1.0 mol/L；
Step (2): the Ammonium persulfate. of 0.2g is dissolved in 10 ml, molar concentration is in the hydrochloric acid solution of 1.0 mol/L, and adds
Entering quality is 500 mg, and size is 2cmx2cm, and thickness is the polyurethane film of 5um；
Step (3): the solution of step (1) is poured into rapidly the solution of step (2), rocks 3 minutes, mix homogeneously up and down, stands
20 minutes, obtain polyaniline/polyurethane conductive composite film, obtain the sample 1# of the present invention.
Embodiment 2
The preparation of the graphene/polyaniline/conductive polyurethane laminated film of different Graphene content, comprises the steps:
Step (1): 150 μ L aniline are joined 10 ml, and molar concentration is in the hydrochloric acid solution of 1.0 mol/L；
Step (2): the Ammonium persulfate. of 0.2g is dissolved in 10 ml, molar concentration is in the hydrochloric acid solution of 1.0 mol/L, treats molten
Xie Hou, adds the graphene oxide of 2.0 mg, stirs；
Step (3): adding quality in the solution of step (2) is 500 mg, and size is 2cmx2cm, and thickness is the polyurethane of 5um
Thin film；
Step (4): the solution of step (1) is poured into rapidly in the solution of step (3), rock up and down 3 minutes, mix homogeneously, quiet
Put 20 minutes, obtain graphene oxide/polyaniline/polyurethane conductive composite film；
Step (5): graphene oxide obtained above/layer/polyaniline conductive bafta is placed in baking oven reduction, dries, and temperature is
200 DEG C, 1.5 hours time, obtain the sample 2# of the present invention.
Embodiment 3
The preparation of the graphene/polyaniline/conductive polyurethane laminated film of different Graphene content, comprises the steps:
Step (1): 150 μ L aniline are joined 10 ml, and molar concentration is in the hydrochloric acid solution of 1.0 mol/L；
Step (2): the Ammonium persulfate. of 0.2g is dissolved in 10 ml, molar concentration is in the hydrochloric acid solution of 1.0 mol/L, treats molten
Xie Hou, adds the graphene oxide of 5.0 mg, stirs；
Step (3): adding quality in the solution of step (2) is 500 mg, and size is 2cmx2cm, and thickness is the polyurethane of 5um
Thin film；
Step (4): the solution of step (1) is poured into rapidly in the solution of step (3), rock up and down 3 minutes, mix homogeneously, quiet
Put 20 minutes, obtain graphene oxide/polyaniline/polyurethane conductive composite film；
Step (5): graphene oxide obtained above/layer/polyaniline conductive bafta is placed in baking oven reduction, dries, and temperature is
200 DEG C, 1.5 hours time, obtain the sample 3# of the present invention.
Embodiment 4
The preparation of the graphene/polyaniline/conductive polyurethane laminated film of different Graphene content, comprises the steps:
Step (1): 150 μ L aniline are joined 10 ml, and molar concentration is in the hydrochloric acid solution of 1.0 mol/L；
Step (2): the Ammonium persulfate. of 0.2g is dissolved in 10 ml, molar concentration is in the hydrochloric acid solution of 1.0 mol/L, treats molten
Xie Hou, adds the graphene oxide of 10.0 mg, stirs；
Step (3): adding quality in the solution of step (2) is 500 mg, and size is 2cmx2cm, and thickness is the polyurethane of 5um
Thin film；
Step (4): the solution of step (1) is poured into rapidly in the solution of step (3), rock up and down 3 minutes, mix homogeneously, quiet
Put 20 minutes, obtain graphene oxide/polyaniline/polyurethane conductive composite film；
Step (5): graphene oxide obtained above/layer/polyaniline conductive bafta is placed in baking oven reduction, dries, and temperature is
200 DEG C, 1.5 hours time, obtain the sample 4# of the present invention.
Embodiment 5
The preparation of the graphene/polyaniline/conductive polyurethane laminated film of different Graphene content, comprises the steps:
Step (1): 150 μ L aniline are joined 10 ml, and molar concentration is in the hydrochloric acid solution of 1.0 mol/L；
Step (2): the Ammonium persulfate. of 0.2g is dissolved in 10 ml, molar concentration is in the hydrochloric acid solution of 1.0 mol/L, treats molten
Xie Hou, adds the graphene oxide of 20.0 mg, stirs；
Step (3): adding quality in the solution of step (2) is 500 mg, and size is 2cmx2cm, and thickness is the polyurethane of 5um
Thin film；
Step (4): the solution of step (1) is poured into rapidly in the solution of step (3), rock up and down 3 minutes, mix homogeneously, quiet
Put 20 minutes, obtain graphene oxide/polyaniline/polyurethane conductive composite film；
Step (5): graphene oxide obtained above/layer/polyaniline conductive bafta is placed in baking oven reduction, dries, and temperature is
200 DEG C, 1.5 hours time, obtain the sample 5# of the present invention.
Embodiment 6
The preparation of the graphene/polyaniline/conductive polyurethane laminated film of different Graphene content, comprises the steps:
Step (1): 150 μ L aniline are joined 10 ml, and molar concentration is in the hydrochloric acid solution of 1.0 mol/L；
Step (2): the Ammonium persulfate. of 0.2g is dissolved in 10 ml, molar concentration is in the hydrochloric acid solution of 1.0 mol/L, treats molten
Xie Hou, adds the graphene oxide of 50.0 mg, stirs；
Step (3): adding quality in the solution of step (2) is 500 mg, and size is 2cmx2cm, and thickness is the polyurethane of 5um
Thin film；
Step (4): the solution of step (1) is poured into rapidly in the solution of step (3), rock up and down 3 minutes, mix homogeneously, quiet
Put 20 minutes, obtain graphene oxide/polyaniline/polyurethane conductive composite film；
Step (5): graphene oxide obtained above/layer/polyaniline conductive bafta is placed in baking oven reduction, dries, and temperature is
200 DEG C, 1.5 hours time, obtain the sample 6# of the present invention.
Embodiment 7
The test of the conductivity of graphene/polyaniline/conductive polyurethane laminated film, comprises the steps:
Sample 1#, 2#, 3#, 4#, 5# and 6# of the present invention are dried at 60 DEG C in vacuum drying oven, takes appropriate amount of sample, utilize four
Test instrument probe (QJ36C type) is tested, and test result is shown in Fig. 1.Experiment of Electrical Conductivity shows the conductance of blank polyurethane film
Rate is respectively less than 1.0 × 10-10 S/cm, the polyaniline/polyurethane conductive composite film obtained when in-situ polymerization is polyaniline-modified
(1#), electric conductivity is greatly improved, and reaches 10 × 10-5S/cm, after adding a small amount of Graphene, obtains sample 2#,
Its conductivity is significantly improved, and reaches 588 × 10-5 S/cm, along with the increase of Graphene content, electrical conductivity gradually steps up,
The sample 6# that Graphene content is the highest, conductivity reaches 1350 × 10-5S/cm, therefore, Graphene/polyphenyl prepared by the present invention
Amine/conductive polyurethane laminated film has good electric conductivity.
Claims (6)
1. a preparation method for graphene/polyaniline/conductive polyurethane laminated film, comprises the following steps:
(1) appropriate monomer aniline is joined in the hydrochloric acid solution of certain molar concentration, obtain the monomer solution of reaction；
(2) graphene oxide and the Ammonium persulfate. of certain mass are dissolved in the hydrochloric acid solution of certain molar concentration, are drawn
Send out agent solution；
(3) in the solution of step (2), add certain mass and the polyurethane film of size, in above-mentioned solution, then add step
Suddenly the aniline monomer solution of (1), rapid mix homogeneously, stand 10-30 minute；
(4) take out polyurethane film, be washed with deionized water clean, put into and baking oven is dried and reduces, i.e. obtain the graphite of the present invention
Alkene/polyaniline/polyurethane conductive composite film.
2. according to the preparation method of a kind of graphene/polyaniline/polyurethane guide conductive film described in claim 1 step (1), its
Being characterised by: the consumption of described aniline is 30 ~ 180 μ L, the molar concentration of hydrochloric acid is 0.5-2.5 mol/L, the volume of hydrochloric acid
It is 5 ~ 15 mL.
3. according to the preparation method of a kind of graphene/polyaniline/polyurethane guide conductive film described in claim 1 step (2), its
Being characterised by: the quality of described graphene oxide is 1.0-100 mg, the consumption of Ammonium persulfate. is 0.15 ~ 0.3g, hydrochloric acid
Volume is 5 ~ 15 mL.
4. according to the preparation method of a kind of graphene/polyaniline/polyurethane guide conductive film described in claim 1 step (3), its
Being characterised by: the quality of described polyurethane film is 200 ~ 1000 mg, size is 2cmx2cm, and thickness is 2-10 m.
5. according to the preparation method of a kind of graphene/polyaniline/polyurethane guide conductive film described in claim 1 step (3), its
It is characterised by: described rapid mix homogeneously, for manually acutely rocking 1-5 minute.
6. according to the preparation method of a kind of graphene/polyaniline/polyurethane guide conductive film described in claim 1 step (4), its
Being characterised by, described oven temperature is 100-250 DEG C, and drying time is: 1.0 ~ 2.0 hours.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106674989A (en) * | 2017-01-10 | 2017-05-17 | 福州大学 | RGO-PPDA (reduction graphene oxide-polyp phenylenediamine)/TPU (thermoplastic polyurethane) composite thin film |
| CN108899498A (en) * | 2018-06-26 | 2018-11-27 | 宁波革创新材料科技有限公司 | The preparation method of environmental protection flexible lithium ion cell positive framework material |
| CN109776830A (en) * | 2019-03-05 | 2019-05-21 | 中原工学院 | A kind of polyurethane/carboxymethyl chitosan/PAn conducting membrane preparation method |
| CN112927836A (en) * | 2021-01-26 | 2021-06-08 | 中国科学院兰州化学物理研究所 | Sponge composite conductive elastic material, preparation method thereof and application thereof in antistatic field |
| CN113337114A (en) * | 2021-06-10 | 2021-09-03 | 深圳市亮一方光电有限公司 | Conductive polyaniline composite material and application thereof in preparing printable thin film electrode |
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| CN112927836A (en) * | 2021-01-26 | 2021-06-08 | 中国科学院兰州化学物理研究所 | Sponge composite conductive elastic material, preparation method thereof and application thereof in antistatic field |
| CN113337114A (en) * | 2021-06-10 | 2021-09-03 | 深圳市亮一方光电有限公司 | Conductive polyaniline composite material and application thereof in preparing printable thin film electrode |
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