CN106065180A - A kind of preparation method of molybdenum trioxide polypyrrole polyaniline trielement composite material - Google Patents
A kind of preparation method of molybdenum trioxide polypyrrole polyaniline trielement composite material Download PDFInfo
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Abstract
The invention provides the preparation method of a kind of molybdenum trioxide polypyrrole polyaniline trielement composite material, it is characterised in that including: step 1: prepare molybdenum trioxide nano band by hydro-thermal method；Step 2: growth in situ polypyrrole obtains molybdenum trioxide polypyrrole binary composite on molybdenum trioxide nano band；Step 3: obtain molybdenum trioxide polypyrrole polyaniline trielement composite material for template at its surface in situ growth polyaniline with molybdenum trioxide polypyrrole binary composite.Molybdenum trioxide polypyrrole polyaniline trielement composite material prepared by the present invention can be used as the ideal electrode material of high-performance super capacitor and the novel energy such as lithium ion battery, solaode.
Description
Technical field
The invention belongs to transition metal oxide-conducting polymer composite technical field, be specifically related to a kind of molybdenum trioxide-
The preparation method of polypyrrole-polyaniline trielement composite material.
Background technology
Day by day serious along with energy crisis and environmental problem, exploitation cleaning, the continuable energy becomes the world today
Hot research field and problem.Polyaniline has, good can processing forming, excellent electric conductivity, quickly adulterate-go
Doping ability, storage volume is high it is considered to be as one of most promising conducting polymer of electrode material.But polyaniline exists
Repeatedly adulterate/go and be susceptible to during adulterating expand and shrink, cause stable circulation performance to decline, constrain it in reality
In application.Polypyrrole is convieniently synthesized because of it, morphology controllable, and doping/dedoping is reversible, environmental friendliness, and is that a kind of ratio is poly-
Aniline elasticity and the more preferable conducting polymer of mechanical performance, but polypyrrole stability in cyclic process is the most poor.Therefore will be poly-
Aniline is compound with polypyrrole to be expected to improve its specific capacity further, and in order to solve the problem of its cyclical stability further, logical
Often by polyaniline, polypyrrole is combined.
Transistion metal compound molybdenum trioxide nano band good stability, specific surface area is big, and electro-chemical activity is high.But, single
Pure molybdenum trioxide electron transfer rate is the most weak.Therefore its application process is also restrained.By molybdenum trioxide and polyaniline
Conjunction polypyrrole is combined, and is expected to play the synergism of three, improves its capacity circulating stability further.
Summary of the invention
It is an object of the invention to provide that a kind of preparation cost is cheap, the molybdenum trioxide-polypyrrole of electrochemical performance-
The preparation method of polyaniline trielement composite material.
In order to achieve the above object, the invention provides a kind of molybdenum trioxide-polypyrrole-polyaniline trielement composite material
Preparation method, it is characterised in that including:
Step 1: prepare molybdenum trioxide nano band by hydro-thermal method；
Step 2: growth in situ polypyrrole obtains molybdenum trioxide-polypyrrole binary composite wood on molybdenum trioxide nano band
Material；
Step 3: obtain three for template at its surface in situ growth polyaniline with molybdenum trioxide-polypyrrole binary composite
Molybdenum oxide-polypyrrole-polyaniline trielement composite material.
Preferably, the concrete steps " preparing molybdenum trioxide nano band by hydro-thermal method " in described step 1 include: by molybdenum
Acid sodium is added to the water with sodium chloride, and stirring obtains dispersion liquid, adds hydrochloric acid solution regulation pH, carries out hydro-thermal reaction, by institute's score
Dissipate liquid sucking filtration, gained solid deionized water is cleaned, is dried, obtains molybdenum trioxide nano band.
It is highly preferred that in described " sodium molybdate and sodium chloride are dissolved in water and obtain solution ", sodium molybdate and sodium chloride
Mass ratio be 10: 1-1: 20, preferably 2: 1-1: 2, in gained dispersion liquid, the concentration of sodium molybdate is 0.01-0.1g/mL, preferably
For 0.02-0.05g/mL.
It is highly preferred that described addition hydrochloric acid solution regulation pH is 0-2, preferably pH=0.5-1.5.
It is highly preferred that the reaction temperature of described hydro-thermal reaction is 160-220 DEG C, preferably 180-200 DEG C, the response time is
10-48h, preferably 18-30h.
Preferably, in described step 2, " on molybdenum trioxide nano band, growth in situ polypyrrole obtains molybdenum trioxide-poly-
Pyrroles's binary composite " concrete steps include: molybdenum trioxide nano band dispersed with stirring is obtained dispersion liquid in water, add
Pyrroles and initiator, grow polypyrrole by home position polymerization reaction on molybdenum trioxide, after reaction terminates, and sucking filtration, gained is solid
Body washs and is dried, and obtains molybdenum trioxide-polypyrrole binary composite.
It is highly preferred that described initiator is Ammonium persulfate., potassium peroxydisulfate, ferric chloride, initiator and pyrroles mole
Ratio is 1: 8-4: 1, preferably 1: 4-1: 1.
It is highly preferred that the mass ratio of described molybdenum trioxide and pyrroles is 1: 1-1: 20, preferably 1: 10.
It is highly preferred that the reaction temperature of described home position polymerization reaction is 0 ± 10 DEG C, preferably 0 ± 2 DEG C, the response time is,
6-48h, preferably 12-24h.
Preferably, " with molybdenum trioxide-polypyrrole binary composite for template at its surface in situ in described step 3
Growth polyaniline obtains molybdenum trioxide-polypyrrole-polyaniline trielement composite material " concrete steps include: by molybdenum trioxide-poly-
Pyrroles's binary composite is distributed in sulfuric acid solution obtain dispersion liquid, adds aniline and initiator, at a certain temperature three
Molybdenum oxide-polypyrrole binary composite surface grows polyaniline by home position polymerization reaction, and after reaction terminates, sucking filtration, by institute
Obtain solid to wash and be dried, obtain molybdenum trioxide-polypyrrole-polyaniline trielement composite material.
It is highly preferred that the concentration of described sulfuric acid solution is 1g/mL-10g/mL, molybdenum trioxide-polypyrrole binary composite wood
Material is 40: 1-10: 1 with the mass ratio of sulfuric acid solution.
It is highly preferred that described initiator is Ammonium persulfate. or potassium peroxydisulfate, initiator is 1: 8-4 with the mol ratio of aniline
: 1, preferably 1: 4-1: 1.
It is highly preferred that the mass ratio of described molybdenum trioxide-polypyrrole binary composite and aniline is 1: 5-1: 50, excellent
Select 1: 10-1: 30.
It is highly preferred that the reaction temperature of described home position polymerization reaction is 0 ± 10 DEG C, preferably 0 ± 2 DEG C, the response time is
6-48h, preferably 12-24h.
Molybdenum trioxide-polypyrrole-polyaniline the trielement composite material of the present invention, this trielement composite material can be used as super electricity
The high-performance ideal electrode material of container and the novel energy such as lithium ion battery, solaode.
Compared with prior art, the invention has the beneficial effects as follows:
1, the present invention uses molybdenum trioxide nano band to be combined with conductive polymer polyanilinc and polypyrrole so that have preferably
The molybdenum trioxide nano band of draw ratio can load more polypyrrole and polyaniline, has effectively constructed multilevel hierarchy, it is simple to electricity
Solve infiltration and the migration of matter ion, it is possible to give full play to the synergism of three, and polyaniline shows as nano whiskers, effectively
Inhibit the reunion of polyaniline, it is achieved that effective dispersion of polyaniline, further increase the chemical property of composite.Separately
Outward, molybdenum trioxide nano band has preferably draw ratio, it is possible to loads more polypyrrole and polyaniline, thus fully improves multiple
The capacity of condensation material；The excellent electric conductivity of polypyrrole is conducive to electric transmission, thus improves the electric conductivity of composite；Three oxidations
The micro-nano multi-level structure of molybdenum-polypyrrole-polyaniline trielement composite material uniqueness is conducive to the dispersion of polypyrrole and polyaniline, thus
Improve its cyclical stability.
2, the molybdenum trioxide-polypyrrole-polyaniline trielement composite material prepared by the present invention has stable chemical nature, electricity
The advantages such as chemical property is excellent.Trielement composite material prepared by the present invention has the feature of morphology controllable, polypyrrole layer structure
Being coated on molybdenum trioxide nano band, it is multiple that polyaniline is coated on molybdenum trioxide-polypyrrole binary with the form of nanoneedle further
On condensation material, restrained effectively the reunion of polypyrrole and polyaniline, take full advantage of the specific surface that molybdenum trioxide nano band is high
Long-pending, given full play to the synergism of three further increase when trielement composite material uses as electrode material electrolyte from
The infiltration of son and migration.
3, the present invention prepares composite by the method for simple in-situ polymerization, and reaction condition is gentle, simple to operate.
Preparation process of the present invention is simple, environmental protection, it is easy to operation, is a kind of preparation method the most efficiently.
4, molybdenum trioxide-polypyrrole-polyaniline trielement composite material prepared by the present invention, can be used as high-performance super capacitor
The ideal electrode material of device and the novel energy such as lithium ion battery, solaode.
Accompanying drawing explanation
Fig. 1 is the TEM figure of molybdenum trioxide-polypyrrole-polyaniline trielement composite material in the present invention
Fig. 2 is the XRD figure of molybdenum trioxide-polypyrrole-polyaniline trielement composite material in the present invention.
The constant current charge-discharge curve of molybdenum trioxide-polypyrrole-polyaniline trielement composite material in present invention during Fig. 3.
3000 circle stability diagrams of molybdenum trioxide-polypyrrole-polyaniline trielement composite material in present invention during Fig. 4.
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 method of a kind of molybdenum trioxide-polypyrrole-polyaniline trielement composite material, concretely comprises the following steps:
1, molybdenum trioxide nano band is prepared by hydro-thermal method:
1.21g sodium molybdate and 0.6g sodium chloride are joined 60mL deionized water obtains solution, continuously stirred 10 minutes,
Obtain uniform dispersion, add 3mol/L hydrochloric acid solution regulation pH to 1, be transferred in water heating kettle in baking oven, carry out hydro-thermal anti-
Should, reaction temperature is 180 DEG C, and the response time is 24h, and question response still cools down up to room temperature, gained dispersion liquid is carried out sucking filtration and divides
From light blue precipitation therein, being cleaned by gained solid deionized water, in baking oven, 60 DEG C of dry 24h, obtain molybdenum trioxide
Nano belt.
2, on molybdenum trioxide nano band, growth in situ polypyrrole obtains molybdenum trioxide-polypyrrole binary composite:
In 250ml flask, add 40mg above-mentioned gained molybdenum trioxide nano band, add the stirring of 80ml deionized water and make three
Molybdenum oxide is dispersed in water and obtains dispersion liquid, measures 200 μ L pyrroles (0.00288mol) with pipet and adds above-mentioned flask
In, after stirring 10 minutes, it is added dropwise over the initiator ammonium persulfate solution (16.5mg/ml) of 20ml, controls pyrroles and persulfuric acid
The mol ratio of ammonium is 2: 1, is put into by flask in freezing circulating pump, and arranging reaction temperature is 0 ± 2 DEG C, stirring reaction 12h,
Molybdenum trioxide grows polypyrrole by home position polymerization reaction, after reaction terminates, by dispersion liquid sucking filtration, gained solid is spent
Ionized water washs several times, and 60 DEG C of dry 24h under vacuum obtain molybdenum trioxide-polypyrrole binary composite.
3, three oxidations are obtained for template at its surface in situ growth polyaniline with molybdenum trioxide-polypyrrole binary composite
Molybdenum-polypyrrole-polyaniline trielement composite material:
In 250ml flask, add 20mg above-mentioned gained molybdenum trioxide-polypyrrole binary composite, add 80ml
The stirring of 0.5mol/L sulfuric acid solution makes molybdenum trioxide-polypyrrole binary composite be uniformly dispersed therein and obtain dispersion liquid.With
Pipet measures 80 μ L aniline (0.00087mol) and adds in above-mentioned flask, after stirring 10 minutes, is added dropwise over the initiation of 20ml
Agent ammonium persulfate solution (16.5mg/ml), the mol ratio controlling aniline and Ammonium persulfate. is 2: 1.Flask is put into freezing
Circulating pump grows polyaniline on molybdenum trioxide-polypyrrole binary composite surface by home position polymerization reaction, reaction is set
Temperature is 0 ± 2 DEG C, stirring reaction 24h, after reaction terminates, by dispersion liquid sucking filtration, gained solid ethanol and deionization is washed
Wash several times, products therefrom 60 DEG C of dry 24h under vacuum, obtain molybdenum trioxide-polypyrrole-polyaniline tri compound material
Material.
Using transmission electron microscope (TEM), X-ray diffractometer (XRD), the constant current charge-discharge at electrochemical workstation is surveyed
Examination and loop test characterize the structure and morphology of molybdenum trioxide-polypyrrole-polyaniline trielement composite material that the present invention is obtained
And chemical property, its result is as follows:
(1) TEM test result shows: as it is shown in figure 1, molybdenum trioxide-polypyrrole-polyaniline three prepared in the present invention
Unit's composite is by molybdenum trioxide nano band and to be coated with polypyrrole further, and finally cladding polyaniline forms.Molybdenum trioxide
Having higher draw ratio, polypyrrole is relatively good with the associativity of polyaniline and molybdenum trioxide such that it is able to give full play to three
The synergism of person, increases specific surface area, largely on improve the capacity of composite.Receive additionally, polyaniline presents
The structure of rice needle-like further suppress the reunion of polyaniline.Thus improve the cyclical stability of composite.
(2) XRD test result further demonstrates that as in figure 2 it is shown, the XRD diffraction maximum of pure molybdenum trioxide is narrow and high, baseline
Steadily, MoO3Belonging to rhombic system, cell parameter is a=0.396nm, b=1.386nm, c=0.370nm, and (020) (040)
(060) crystal face has the strongest diffracted intensity, consistent with the card index value of JCPDS-05-0508.Pure polypyrrole 2 θ=
The peak of 25 °, corresponding to its (002) crystal face.At 2 θ, pure polyaniline is that the peak at 20 ° and 25 ° shows that polyaniline is in doped.
The XRD diffraction maximum of molybdenum trioxide-polypyrrole-polyaniline trielement composite material prepared in the present invention and pure molybdenum trioxide
Peak shows similar characteristic, also occurs in that the characteristic peak of polyaniline and polypyrrole simultaneously, shows that polypyrrole and polyaniline are successfully answered
Being combined on molybdenum trioxide, polypyrrole does not produce impact to the crystallinity of molybdenum trioxide with the cladding of polyaniline simultaneously.
(3) constant current charge-discharge test result shows: Fig. 3 is molybdenum trioxide-polypyrrole-polyaniline composite material and relevant sample
Product are at 1Ag-1Charging and discharging curve, it can be seen that charging and discharging curve is the isosceles triangle of approximation, and this is typical capacitor
Figure, being calculated in electric current density according to charging and discharging curve is 1Ag-1Time, molybdenum trioxide-polypyrrole-polyaniline, poly-pyrrole
Coughing up, polyaniline, molybdenum trioxide electric capacity is respectively 1200, and 111.2,476.1 and 151.2Fg-1, show trielement composite material capacity
Height, has the chemical property of excellence.
(4) loop test result shows: as shown in Figure 4, and test condition is electric current density 2Ag-1Lower voltage range be 0～
Carry out constant current charge-discharge 3000 under 1.0V to enclose.As seen from the figure, the cyclical stability of molybdenum trioxide-polypyrrole-polyaniline is best,
After circulating 3000 times, capability retention is 87%, is better than polyaniline (45%) and polypyrrole (47%), and polyaniline (45%)
With molybdenum trioxide (50%), demonstrate good application prospect.
Claims (10)
1. the preparation method of molybdenum trioxide-polypyrrole-polyaniline trielement composite material, it is characterised in that including:
Step 1: prepare molybdenum trioxide nano band by hydro-thermal method；
Step 2: growth in situ polypyrrole obtains molybdenum trioxide-polypyrrole binary composite on molybdenum trioxide nano band；
Step 3: obtain three oxidations for template at its surface in situ growth polyaniline with molybdenum trioxide-polypyrrole binary composite
Molybdenum-polypyrrole-polyaniline trielement composite material.
2. the preparation method of molybdenum trioxide-polypyrrole-polyaniline trielement composite material as claimed in claim 1, its feature exists
In, the concrete steps " preparing molybdenum trioxide nano band by hydro-thermal method " in described step 1 include: by sodium molybdate and sodium chloride
Being added to the water, stirring obtains dispersion liquid, adds hydrochloric acid solution regulation pH, carries out hydro-thermal reaction, by gained dispersion liquid sucking filtration, by institute
Obtain solid deionized water to clean, be dried, obtain molybdenum trioxide nano band.
3. the preparation method of molybdenum trioxide-polypyrrole-polyaniline trielement composite material as claimed in claim 2, its feature exists
In, in described " sodium molybdate and sodium chloride are dissolved in water and obtain solution ", sodium aluminate is 10: 1-with the mass ratio of sodium chloride
1: 20, in gained dispersion liquid, the concentration of sodium molybdate is 0.01-0.1g/mL.
4. the preparation method of molybdenum trioxide-polypyrrole-polyaniline trielement composite material as claimed in claim 2, its feature exists
In, the reaction temperature of described hydro-thermal reaction is 160-220 DEG C, and the response time is 10-48h.
5. the preparation method of molybdenum trioxide-polypyrrole-polyaniline trielement composite material as claimed in claim 1, its feature exists
In, in described step 2 " on molybdenum trioxide nano band growth in situ polypyrrole obtain molybdenum trioxide-polypyrrole binary be combined
Material " concrete steps include: molybdenum trioxide nano band dispersed with stirring is obtained in water dispersion liquid, adds pyrroles and initiation
Agent, grows polypyrrole by home position polymerization reaction on molybdenum trioxide, after reaction terminates, sucking filtration, washs gained solid and does
Dry, obtain molybdenum trioxide-polypyrrole binary composite.
6. the preparation method of molybdenum trioxide-polypyrrole-polyaniline trielement composite material as claimed in claim 5, its feature exists
In, described initiator is Ammonium persulfate., potassium peroxydisulfate, ferric chloride, and initiator is 1: 8-4: 1 with the mol ratio of pyrroles, excellent
Select 1: 4-1: 1.
7. the preparation method of molybdenum trioxide-polypyrrole-polyaniline trielement composite material as claimed in claim 5, its feature exists
In, described molybdenum trioxide is 1: 1-1: 20 with the mass ratio of pyrroles.
8. the preparation method of molybdenum trioxide-polypyrrole-polyaniline trielement composite material as claimed in claim 5, its feature exists
In, the reaction temperature of described home position polymerization reaction is 0 ± 10 DEG C, and the response time is 6-48h.
9. the preparation method of molybdenum trioxide-polypyrrole-polyaniline trielement composite material as claimed in claim 1, its feature exists
In, described step 3 " obtains at its surface in situ growth polyaniline with molybdenum trioxide-polypyrrole binary composite for template
To molybdenum trioxide-polypyrrole-polyaniline trielement composite material " concrete steps include: molybdenum trioxide-polypyrrole binary is combined
Material is distributed in sulfuric acid solution obtain dispersion liquid, adds aniline and initiator, at a certain temperature at molybdenum trioxide-polypyrrole
Binary composite surface grows polyaniline by home position polymerization reaction, after reaction terminates, sucking filtration, washs gained solid and does
Dry, obtain molybdenum trioxide-polypyrrole-polyaniline trielement composite material.
10. the preparation method of molybdenum trioxide-polypyrrole-polyaniline trielement composite material as claimed in claim 9, its feature exists
In, the reaction temperature of described home position polymerization reaction is 0 ± 10 DEG C, and the response time is 6-48h.
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| CN110767459A (en) * | 2019-10-30 | 2020-02-07 | 东华大学 | High-voltage water system symmetrical super capacitor and preparation method thereof |
| CN113173570A (en) * | 2021-04-21 | 2021-07-27 | 国网黑龙江省电力有限公司电力科学研究院 | Preparation method and application of graphene-like sheet nitrogen-doped porous carbon material |
| CN115160564A (en) * | 2022-07-19 | 2022-10-11 | 湖北大学 | Molybdenum oxide composite polyaniline nanofiber paper and preparation method thereof |
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| WO2003027203A2 (en) * | 2001-09-27 | 2003-04-03 | The Board Of Governors For Higher Education, State Of Rhode Island And Providence Plantations | Conducting polymer for pretreatment of metallic and non-metallic surfaces |
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| WO2003027203A2 (en) * | 2001-09-27 | 2003-04-03 | The Board Of Governors For Higher Education, State Of Rhode Island And Providence Plantations | Conducting polymer for pretreatment of metallic and non-metallic surfaces |
| CN101977985A (en) * | 2008-03-19 | 2011-02-16 | E.I.内穆尔杜邦公司 | Electrically conductive polymer compositions and films made therefrom |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107892330A (en) * | 2017-12-01 | 2018-04-10 | 东华大学 | A kind of preparation method of piece heap molybdenum disulfide nano tube |
| CN107892330B (en) * | 2017-12-01 | 2019-06-25 | 东华大学 | A kind of preparation method of piece heap molybdenum disulfide nano tube |
| CN109731617A (en) * | 2018-12-13 | 2019-05-10 | 东莞理工学院 | A kind of Fe3O4/ polypyrrole/polyaniline/TiO2The preparation method of/ZnO composite material |
| CN110767459A (en) * | 2019-10-30 | 2020-02-07 | 东华大学 | High-voltage water system symmetrical super capacitor and preparation method thereof |
| CN113173570A (en) * | 2021-04-21 | 2021-07-27 | 国网黑龙江省电力有限公司电力科学研究院 | Preparation method and application of graphene-like sheet nitrogen-doped porous carbon material |
| CN115160564A (en) * | 2022-07-19 | 2022-10-11 | 湖北大学 | Molybdenum oxide composite polyaniline nanofiber paper and preparation method thereof |
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