CN103613759B - A kind of MoO 3the preparation method of/polyaniline co-axial nano heterojunction - Google Patents

A kind of MoO 3the preparation method of/polyaniline co-axial nano heterojunction Download PDF

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CN103613759B
CN103613759B CN201310658871.8A CN201310658871A CN103613759B CN 103613759 B CN103613759 B CN 103613759B CN 201310658871 A CN201310658871 A CN 201310658871A CN 103613759 B CN103613759 B CN 103613759B
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moo
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polyaniline
deionized water
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胡俊青
蒋扉然
李文尧
邹儒佳
徐开兵
李博
安磊
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Donghua University
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Abstract

The present invention relates to a kind of MoO 3the preparation method of/polyaniline co-axial nano heterojunction, comprising: (1) is by H 2o 2in the metal molybdenum powder be added drop-wise under ice-water bath condition, after stirring, constant volume obtains precursor solution; (2) in above-mentioned precursor solution, add deionized water, carry out hydro-thermal reaction after stirred at ambient temperature, naturally cool to room temperature after reaction terminates, by the excessive washing with alcohol of product, last centrifugation obtains MoO 3nano belt; (3) at MoO 3add deionized water in nano belt, obtain solution A; While stirring the hydrochloric acid soln of aniline is added drop-wise in solution A, and then adds the deionized water solution of ammonium persulphate, stirring at normal temperature 1 ~ 24h; After reaction terminates, washing, centrifugal, vacuum-drying, obtain MoO 3/ polyaniline co-axial nano heterojunction.Preparation method of the present invention is simple to operate, does not need complex apparatus, and comparison of ingredients easily controls, and can large-scale production, has a extensive future.

Description

A kind of MoO 3the preparation method of/polyaniline co-axial nano heterojunction
Technical field
The invention belongs to polyaniline nano Material Field, particularly a kind of MoO 3the preparation method of/polyaniline co-axial nano heterojunction.
Background technology
Transition metal oxide molybdic oxide has electrochromism, photochromic, the character such as photocatalytic degradation and gas-sensitive property, all has widespread use in fast ion conduction, catalyzer, sensor and electrochemical field.Molybdic oxide has three kinds of common thing phases: orthorhombic phase (α-MoO 3), monoclinic phase (β-MoO 3) and six side's phase (h-MoO 3), the former belongs to thermodynamically stable phase, and rear both belong to thermodynamically metastable phases.Wherein orthorhombic phase MoO 3because of the one dimension laminate structure of its uniqueness, make the electrode materials that it is widely used in electrochemical energy storing device, as lithium ion primary cell, lithium-ion secondary cell, ultracapacitor etc., at present, MoO 3the application in electrochemical field such as nanometer rod, nanometer sheet, nano wire, nano belt has corresponding report.But molybdic oxide ion and electronic conduction rate variance, this is restricted with regard to making its chemical property, thus improves the focus that its electroconductibility just becomes research, adopts the means such as coated, hydridization doping can effectively improve its electroconductibility.Be combined together to form matrix material with conducting polymer and can solve these defects, and obtain more superior performance by the synergy of each several part.
Since American scientist black square (A.J.Heeger), MacDiarmid (A.G.MacDiamid) and Japanese Scientists Hideki Shirakawa (H.Shirakawa) in 1977 find that doped polyacetylene has metallic conductivity, polymkeric substance thoroughly can not be changed as the concept of electro-conductive material, and from then on conductive polymers receives the extensive concern of various countries scientist.Common conductive polymers has Polythiophene, polypyrrole, polyaniline etc., and wherein polyaniline has synthesis simply because of it, can pass through electrochemical oxidation, chemical syntheses; Raw material is easy to get; High temperature resistant and advantages such as good in oxidation resistance, become the conducting polymer composite of most prospect.The performances such as the conduction of polyaniline and catalysis depend on dopant states and the structure of polymkeric substance to a great extent, can by changing the redox state of polyaniline, doping agent or by improving the performance of polyaniline with inorganic compounding, electrically conductive polyaniline/inorganic materials matrix material combines the premium properties of superpolymer and inorganic materials, thus obtains the functional materials with performances such as special optical, electrical, magnetic, catalysis by compound.
At present, aniline monomer is inserted molybdic oxide interlayer by the general intercalation polymeric method that adopts, and obtains MoO 3with the hybrid material of polyaniline, because the oxidisability of molybdic oxide own is very weak and do not have tradable ion, therefore polyaniline is inserted into MoO 3interlayer is very difficult, and method is complicated, complex steps, therefore needs exploitation one simply to prepare polyaniline-coated MoO efficiently 3the preparation method of matrix material.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of MoO 3the preparation method of/polyaniline co-axial nano heterojunction, this preparation method is simple to operate, does not need complex apparatus, obtains the even coated MoO of polyaniline 3nano composite material.
A kind of MoO of the present invention 3the preparation method of/polyaniline co-axial nano heterojunction, comprising:
(1) synthesis of presoma:
By H 2o 2in the metal molybdenum powder be slowly added drop-wise under ice-water bath condition, and constantly stir to avoid overheated, a large amount of heat and gas are released in reaction; After dropwising, continue under normal temperature to stir 2-8 hour, obtain the peroxo-polymolybdic acid colloidal sol (MoO of orange 3pH 2o 2qH 2o), constant volume obtains precursor solution;
(2) MoO 3the synthesis of nano belt:
In above-mentioned precursor solution, add deionized water, carry out hydro-thermal reaction 6-24 hour after stirred at ambient temperature with at 60-180 DEG C, naturally cool to room temperature after reaction terminates, by the excessive washing with alcohol of product, last centrifugation obtains MoO 3nano belt;
(3) polyaniline-coated MoO 3nano belt:
At MoO 3add deionized water in nano belt, then the ultrasonic 0.5 ~ 1h of room temperature, makes MoO 3nano belt is dispersed in water, obtains solution A; According to MoO 3the mol ratio of nano belt and aniline is 1:0.25 ~ 2, is added drop-wise in solution A by the hydrochloric acid soln of aniline while stirring, and then adds the deionized water solution of ammonium persulphate, stirring at normal temperature 1 ~ 24h; After reaction terminates, with excessive washing with alcohol, centrifugation, collecting precipitation thing, last vacuum-drying, obtains MoO 3/ polyaniline co-axial nano heterojunction.
H described in step (1) 2o 2be 40mL:0.05mol with the amount ratio of metal molybdenum powder, wherein H used 2o 2massfraction be 30%; Last constant volume obtains 100mL precursor solution.
MoO in solution A described in step (3) 3the concentration of nano belt is 0.01 ~ 0.03g/mL.
The concentration of the deionized water solution of the ammonium persulphate described in step (3) is 0.01 ~ 0.03g/mL.
Vacuum drying temperature described in step (3) is 60 DEG C.
The present invention directly uses metal molybdenum powder for molybdenum source, and prepares MoO under not adopting any template condition 3nano belt.
Beneficial effect:
The simple experimental installation of the present invention can prepare MoO 3/ polyaniline co-axial nano heterojunction; The advantages such as this reaction has environmental friendliness, required starting material are easy to get, cheap, operating process is easy, and can relatively largely prepare, be preparation MoO 3a kind of new and effective method of/polyaniline co-axial nano heterojunction.
Accompanying drawing explanation
Fig. 1 is the MoO prepared in the present invention 3nano belt and MoO 3the SEM picture of/polyaniline co-axial nano heterojunction; Wherein (a) is MoO 3nano belt, (b) is MoO 3/ polyaniline co-axial nano heterojunction;
Fig. 2 is the MoO prepared in the present invention 3the TEM figure of/polyaniline co-axial nano heterojunction;
Fig. 3 is the MoO prepared in the present invention 3nano belt and MoO 3the FTIR collection of illustrative plates of/polyaniline co-axial nano heterojunction; Wherein (a) is MoO 3nano belt, (b) is MoO 3/ polyaniline co-axial nano heterojunction.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
(1) synthesis of presoma: by 40mL H 2o 2slowly be added drop-wise in the metal molybdenum powder of 0.05mol under ice-water bath condition, and constantly stir to avoid overheated.After dropwising, continue stirring under normal temperature 4 hours, obtain the peroxo-polymolybdic acid colloidal sol (MoO of orange 3pH 2o 2qH 2o), constant volume in 100ml volumetric flask, for subsequent use.
(2) measure 5mL peroxo-polymolybdic acid precursor solution in beaker, add 15mL deionized water, room temperature lower magnetic force goes in autoclave after stirring 1h, and at 180 DEG C, hydro-thermal reaction 12 hours, naturally cools to room temperature.By the white MoO of gained 3precipitate by excessive washing with alcohol, centrifugation, namely obtains MoO 3nano belt.
(3) 0.1g MoO is taken 3nano belt, adds 10mL deionized water deionized water, is made into the aqueous solution that concentration is 0.01g/ml, and the ultrasonic 1h of room temperature, makes MoO 3nano belt is dispersed in water, is solution A; Be added in 10mL deionized water by 0.1g ammonium persulphate, be made into the aqueous solution that concentration is 0.01g/ml, ultrasonic disperse is even, is B solution; According to MoO 3the mol ratio of nano belt and aniline is 1:1, is added drop-wise in solution A while stirring, obtains C solution, then join in C solution by B solution, stirring at normal temperature 4h by the hydrochloric acid soln of aniline.After reaction terminates, with excessive washing with alcohol, centrifugation, collecting precipitation thing, vacuum-drying at temperature is 60 DEG C, obtains MoO 3/ polyaniline co-axial nano heterojunction.
Embodiment 2
(1) synthesis of presoma: by 40mL H 2o 2slowly be added drop-wise in the metal molybdenum powder of 0.05mol under ice-water bath condition, and constantly stir to avoid overheated.After dropwising, continue stirring under normal temperature 4 hours, obtain the peroxo-polymolybdic acid colloidal sol (MoO of orange 3pH 2o 2qH 2o), constant volume in 100ml volumetric flask, for subsequent use.
(2) measure 10mL peroxo-polymolybdic acid precursor solution in beaker, add 10mL deionized water, room temperature lower magnetic force goes in autoclave after stirring 1h, and at 180 DEG C, hydro-thermal reaction 12 hours, naturally cools to room temperature.By the white MoO of gained 3precipitate by excessive washing with alcohol, centrifugation, namely obtains MoO 3nano belt.
(3) 0.1g MoO is taken 3nano belt, adds 10mL deionized water deionized water, is made into the aqueous solution that concentration is 0.01g/ml, and the ultrasonic 1h of room temperature, makes MoO 3nano belt is dispersed in water, is solution A; Be added in 10mL deionized water by 0.1g ammonium persulphate, be made into the aqueous solution that concentration is 0.01g/ml, ultrasonic disperse is even, is B solution; According to MoO 3the mol ratio of nano belt and aniline is 1:1, is added drop-wise in solution A while stirring, obtains C solution, then join in C solution by B solution, stirring at normal temperature 4h by the hydrochloric acid soln of aniline.After reaction terminates, with excessive washing with alcohol, centrifugation, collecting precipitation thing, vacuum-drying at temperature is 60 DEG C, obtains MoO 3/ polyaniline co-axial nano heterojunction.
Embodiment 3
(1) synthesis of presoma: by 40mL H 2o 2slowly be added drop-wise in the metal molybdenum powder of 0.05mol under ice-water bath condition, and constantly stir to avoid overheated.After dropwising, continue stirring under normal temperature 4 hours, obtain the peroxo-polymolybdic acid colloidal sol (MoO of orange 3pH 2o 2qH 2o), constant volume in 100ml volumetric flask, for subsequent use.
(2) measure 20mL peroxo-polymolybdic acid precursor solution in beaker, room temperature lower magnetic force goes in autoclave after stirring 1h, and at 180 DEG C, hydro-thermal reaction 12 hours, naturally cools to room temperature.By the white MoO of gained 3precipitate by excessive washing with alcohol, centrifugation, namely obtains MoO 3nano belt.
(3) 0.1g MoO is taken 3nano belt, adds 10mL deionized water deionized water, is made into the aqueous solution that concentration is 0.01g/ml, and the ultrasonic 1h of room temperature, makes MoO 3nano belt is dispersed in water, is solution A; Be added in 10mL deionized water by 0.1g ammonium persulphate, be made into the aqueous solution that concentration is 0.01g/ml, ultrasonic disperse is even, is B solution; According to MoO 3the mol ratio of nano belt and aniline is 1:1, is added drop-wise in solution A while stirring, obtains C solution, then join in C solution by B solution, stirring at normal temperature 4h by the hydrochloric acid soln of aniline.After reaction terminates, with excessive washing with alcohol, centrifugation, collecting precipitation thing, vacuum-drying at temperature is 60 DEG C, obtains MoO 3/ polyaniline co-axial nano heterojunction.
Embodiment 4
(1) synthesis of presoma: by 40mL H 2o 2slowly be added drop-wise in the metal molybdenum powder of 0.05mol under ice-water bath condition, and constantly stir to avoid overheated.After dropwising, continue stirring under normal temperature 4 hours, obtain the peroxo-polymolybdic acid colloidal sol (MoO of orange 3pH 2o 2qH 2o), constant volume in 100ml volumetric flask, for subsequent use.
(2) measure 10mL peroxo-polymolybdic acid precursor solution in beaker, add 10mL deionized water, room temperature lower magnetic force goes in autoclave after stirring 1h, and at 180 DEG C, hydro-thermal reaction 12 hours, naturally cools to room temperature.By the white MoO of gained 3precipitate by excessive washing with alcohol, centrifugation, namely obtains MoO 3nano belt.
(3) 0.1g MoO is taken 3nano belt, adds 10mL deionized water deionized water, is made into the aqueous solution that concentration is 0.01g/ml, and the ultrasonic 1h of room temperature, makes MoO 3nano belt is dispersed in water, is solution A; Be added in 10mL deionized water by 0.1g ammonium persulphate, be made into the aqueous solution that concentration is 0.01g/ml, ultrasonic disperse is even, is B solution; According to MoO 3the mol ratio of nano belt and aniline is 1:1, is added drop-wise in solution A while stirring, obtains C solution, then join in C solution by B solution, stirring at normal temperature 12h by the hydrochloric acid soln of aniline.After reaction terminates, with excessive washing with alcohol, centrifugation, collecting precipitation thing, vacuum-drying at temperature is 60 DEG C, obtains MoO 3/ polyaniline co-axial nano heterojunction.
Embodiment 5
(1) synthesis of presoma: by 40mL H 2o 2slowly be added drop-wise in the metal molybdenum powder of 0.05mol under ice-water bath condition, and constantly stir to avoid overheated.After dropwising, continue stirring under normal temperature 4 hours, obtain the peroxo-polymolybdic acid colloidal sol (MoO of orange 3pH 2o 2qH 2o), constant volume in 100ml volumetric flask, for subsequent use.
(2) measure 10mL peroxo-polymolybdic acid precursor solution in beaker, add 10mL deionized water, room temperature lower magnetic force goes in autoclave after stirring 1h, and at 180 DEG C, hydro-thermal reaction 12 hours, naturally cools to room temperature.By the white MoO of gained 3precipitate by excessive washing with alcohol, centrifugation, namely obtains MoO 3nano belt.
(3) 0.1g MoO is taken 3nano belt, adds 10mL deionized water deionized water, is made into the aqueous solution that concentration is 0.01g/ml, and the ultrasonic 1h of room temperature, makes MoO 3nano belt is dispersed in water, is solution A; Be added in 10mL deionized water by 0.1g ammonium persulphate, be made into the aqueous solution that concentration is 0.01g/ml, ultrasonic disperse is even, is B solution; According to MoO 3the mol ratio of nano belt and aniline is 1:1, is added drop-wise in solution A while stirring, obtains C solution, then join in C solution by B solution, stirring at normal temperature 24h by the hydrochloric acid soln of aniline.After reaction terminates, with excessive washing with alcohol, centrifugation, collecting precipitation thing, vacuum-drying at temperature is 60 DEG C, obtains MoO 3/ polyaniline co-axial nano heterojunction.
Embodiment 6
(1) synthesis of presoma: by 40mL H 2o 2slowly be added drop-wise in the metal molybdenum powder of 0.05mol under ice-water bath condition, and constantly stir to avoid overheated.After dropwising, continue stirring under normal temperature 4 hours, obtain the peroxo-polymolybdic acid colloidal sol (MoO of orange 3pH 2o 2qH 2o), constant volume in 100ml volumetric flask, for subsequent use.
(2) measure 10mL peroxo-polymolybdic acid precursor solution in beaker, add 10mL deionized water, room temperature lower magnetic force goes in autoclave after stirring 1h, and at 180 DEG C, hydro-thermal reaction 12 hours, naturally cools to room temperature.By the white MoO of gained 3precipitate by excessive washing with alcohol, centrifugation, namely obtains MoO 3nano belt.
(3) 0.2g MoO is taken 3nano belt, adds 10mL deionized water deionized water, is made into the aqueous solution that concentration is 0.02g/ml, and the ultrasonic 1h of room temperature, makes MoO 3nano belt is dispersed in water, is solution A; Be added in 10mL deionized water by 0.2g ammonium persulphate, be made into the aqueous solution that concentration is 0.02g/ml, ultrasonic disperse is even, is B solution; According to MoO 3the mol ratio of nano belt and aniline is 1:0.25, is added drop-wise in solution A while stirring, obtains C solution, then join in C solution by B solution, stirring at normal temperature 8h by the hydrochloric acid soln of aniline.After reaction terminates, with excessive washing with alcohol, centrifugation, collecting precipitation thing, vacuum-drying at temperature is 60 DEG C, obtains MoO 3/ polyaniline co-axial nano heterojunction.
Embodiment 7
(1) synthesis of presoma: by 40mL H 2o 2slowly be added drop-wise in the metal molybdenum powder of 0.05mol under ice-water bath condition, and constantly stir to avoid overheated.After dropwising, continue stirring under normal temperature 4 hours, obtain the peroxo-polymolybdic acid colloidal sol (MoO of orange 3pH 2o 2qH 2o), constant volume in 100ml volumetric flask, for subsequent use.
(2) measure 10mL peroxo-polymolybdic acid precursor solution in beaker, add 10mL deionized water, room temperature lower magnetic force goes in autoclave after stirring 1h, and at 180 DEG C, hydro-thermal reaction 12 hours, naturally cools to room temperature.The just white MoO of gained 3precipitate by excessive washing with alcohol, centrifugation, namely obtains MoO 3nano belt.
(3) 0.3g MoO is taken 3nano belt, adds 10mL deionized water deionized water, is made into the aqueous solution that concentration is 0.03g/ml, and the ultrasonic 1h of room temperature, makes MoO 3nano belt is dispersed in water, is solution A; Be added in 10mL deionized water by 0.3g ammonium persulphate, be made into the aqueous solution that concentration is 0.03g/ml, ultrasonic disperse is even, is B solution; According to MoO 3the mol ratio of nano belt and aniline is 1:2, is added drop-wise in solution A while stirring, obtains C solution, then join in C solution by B solution, stirring at normal temperature 12h by the hydrochloric acid soln of aniline.After reaction terminates, with excessive washing with alcohol, centrifugation, collecting precipitation thing, vacuum-drying at temperature is 60 DEG C, obtains MoO 3/ polyaniline co-axial nano heterojunction.

Claims (4)

1. a MoO 3the preparation method of/polyaniline co-axial nano heterojunction, comprising:
(1) by H 2o 2in the metal molybdenum powder be slowly added drop-wise under ice-water bath condition, after dropwising, continue under normal temperature to stir 2-8 hour, obtain the peroxo-polymolybdic acid colloidal sol of orange, constant volume obtains precursor solution;
(2) in above-mentioned precursor solution, add deionized water, carry out hydro-thermal reaction 6-24 hour after stirred at ambient temperature at 60-180 DEG C, naturally cool to room temperature after reaction terminates, by the excessive washing with alcohol of product, last centrifugation obtains MoO 3nano belt;
(3) at MoO 3add deionized water in nano belt, then the ultrasonic 0.5 ~ 1h of room temperature, obtains solution A; According to MoO 3the mol ratio of nano belt and aniline is 1:0.25 ~ 2, is added drop-wise in solution A by the hydrochloric acid soln of aniline while stirring, and then adds the deionized water solution of ammonium persulphate, stirring at normal temperature 1 ~ 24h; After reaction terminates, with excessive washing with alcohol, centrifugation, collecting precipitation thing, last vacuum-drying, obtains MoO 3/ polyaniline co-axial nano heterojunction; Wherein MoO in solution A 3the concentration of nano belt is 0.01 ~ 0.03g/mL.
2. a kind of MoO according to claim 1 3the preparation method of/polyaniline co-axial nano heterojunction, is characterized in that: the H described in step (1) 2o 2be 40mL:0.05mol with the amount ratio of metal molybdenum powder, wherein H used 2o 2massfraction be 30%; Last constant volume obtains 100mL precursor solution.
3. a kind of MoO according to claim 1 3the preparation method of/polyaniline co-axial nano heterojunction, is characterized in that: the concentration of the deionized water solution of the ammonium persulphate described in step (3) is 0.01 ~ 0.03g/mL.
4. a kind of MoO according to claim 1 3the preparation method of/polyaniline co-axial nano heterojunction, is characterized in that: the vacuum drying temperature described in step (3) is 60 DEG C.
CN201310658871.8A 2013-12-06 2013-12-06 A kind of MoO 3the preparation method of/polyaniline co-axial nano heterojunction Expired - Fee Related CN103613759B (en)

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