CN103044915B - Preparation method of polyaniline/graphene/nano nickel composite material - Google Patents
Preparation method of polyaniline/graphene/nano nickel composite material Download PDFInfo
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- CN103044915B CN103044915B CN201310017501.6A CN201310017501A CN103044915B CN 103044915 B CN103044915 B CN 103044915B CN 201310017501 A CN201310017501 A CN 201310017501A CN 103044915 B CN103044915 B CN 103044915B
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Abstract
The invention provides a preparation method of a polyaniline/graphene/nano nickel composite material, and relates to the preparation method of the polyaniline composite material, in order to solve the problem that the polyaniline has no electrochemical performance. The preparation method comprises the following steps: 1, preparing a graphene oxide solution; 2, preparing composite powder in a graphene carrying nano nickel manner; and 3, preparing the polyaniline/graphene/nano nickel composite material. The method provided by the invention is simple, convenient and easy to implement, low in cost and high in yield, thereby being suitable for mass production. The method is applied to the field of chemical industry.
Description
Technical field
The present invention relates to a kind of preparation method of polyaniline composite material.
Background technology
Polyaniline is with good thermostability, chemical stability and electrochemical reversibility, good absorption of electromagnetic wave ability, potential solution and the doping phenomenon that melt-processable, raw material are easy to get, synthetic method is simple and unique etc. and become one of the fastest conduction high polymer of present progress.But pure polyaniline is isolator, there is some self insurmountable difficult problem in single electrode materials, for example not higher than capacitance, cycle performance is not good, expensive etc.The defect existing in order to make up single component, compound electrode material has become the main research tendency of electrode material for super capacitor development.
Nano-nickel powder is a kind of important magneticmetal material, all has wide practical use in many fields such as magnetic storage, medical diagnosis, conductive coating, sensor, catalysis and rechargeable batteries.Graphene is a kind of carbon two-dimensional nano material of monoatomic layer, has desirable bi-dimensional cellular shape lattice structure.In Graphene plane, carbon atom is arranged with the form of six-ring, and the thickness of Graphene only has 0.335nm, is the thinnest in known materials in the world at present, is also one of the most firm material in history.Graphene has the performances such as unique two-dirnentional structure and excellent mechanics, electricity, optics, and these performances make Graphene all have good development trend in matrix material, microelectronics, optics, the energy, sensor field.
Therefore nano-nickel powder, Graphene and polyaniline are carried out compoundly, can overcome polyaniline is isolator, does not have the shortcoming of electric property.
" Acta PhySico-Chimica Sinica " the 28th 11 phases of volume in 2012, " preparation of different-shape nickel nano particle-graphene composite material and microwave property " that Li Songmei etc. deliver discloses following technical characterictic: by powdered graphite and NaNO
3mixture joins the vitriol oil, under ice bath, by KMnO
4under agitation condition, slowly join in reaction soln, then add water stir and heat up, after reaction finishes, the throw out in centrifugal collection mixture, and repetitive scrubbing to sulfate radical-free ion exists; Prepare graphene oxide solution; By nickel chloride solution and graphene oxide aqueous solution, regulate pH value to 11, add hydrazine hydrate reaction, product washs and is dried, and obtains nickel nano particle-graphene composite material.
Summary of the invention
Although the present invention is the problem that will solve polyaniline and do not have electric property, provide the preparation method of polyaniline/graphene/nanometer nickel composite material.
The preparation method of polyaniline/graphene/nanometer nickel composite material of the present invention, realizes according to the following steps:
One, prepare graphene oxide solution: in the sulfuric acid that is 98% at the quality percentage composition of 40～60ml, add 1.0～1.5g crystalline flake graphite, under 0～4 DEG C of ice-water bath, stir 20～40min, then add 1～2g SODIUMNITRATE and 9～11g potassium permanganate, reaction 1～3h; Then be placed in 35 DEG C of water-baths and react 9～13h, then add 350～450mL distilled water diluting, carry out ultrasonic dispersion, then add the H of 80～100mL quality percentage composition 5%
2o
2, then add 45～55mL dilute hydrochloric acid; Then carry out suction filtration, centrifugal, collect solid formation, be then placed in 350～450ml distilled water and dissolve, then put into semi-permeable membranes dialysis processing until solution is neutral, then be 0.001～0.003g/mL by distilled water diluting to concentration, obtain required graphene oxide solution;
Two, the NaOH solution that the concentration of preparing graphene-supported nano nickel composite granule: a, the preparation 10～30mL protochloride nickel ethylene glycol solution that is 0.1mol/L and 2～4mL concentration are 0.2mol/L; B, graphene oxide solution prepared by protochloride nickel ethylene glycol solution and 50mL step 2 mix ultrasonic 30min, add successively the hydrazine hydrate solution that NaOH solution prepared by step a and 4～6mL quality percentage composition are 80% after taking-up under magnetic agitation; Then pour in hydrothermal reaction kettle and react 3～5h at 120 DEG C, then carry out filtering and washing, at 50 DEG C, dry 20～28h obtains graphene-supported nano nickel composite granule after grinding;
Three, prepare polyaniline/graphene/nanometer nickel composite material: c, add 0.5～1.5ml toluene after graphene-supported 0.1～0.3g nano nickel composite granule is placed in to three-necked bottle, ultrasonic 3～6min, obtains solution A; D, 0.5～1.5ml aniline is dissolved in the hydrochloric acid of 12～16ml1.5mol/L, obtains solution B; E, 1.5～2g Sodium dodecylbenzene sulfonate is dissolved in 20～30ml distilled water, ultrasonic 3～6min makes it to mix, and obtains solution C; F, solution A, solution B and solution C are mixed in the three-necked bottle of step c, ultrasonic 10～20min, obtains mixing solutions; G, 2～3g ammonium persulphate is dissolved in 20～30ml distilled water, under the rotating speed of 300r/m, join in the mixing solutions that step f makes by separating funnel, rate of addition be 5 seconds every, continue again to wash after reaction 3～5h, then dry 20～28h at 50 DEG C obtains polyaniline/graphene/nanometer nickel composite material after grinding.
Of the present invention method is simple, cost is low, productive rate is high, can be used for scale operation.Utilize graphene-supported nano nickel composite granule prepared by this method can be on Graphene load good dispersion, size uniform, the nickel nano particle that particle diameter is less.And it is low, easily synthetic to prepare polyaniline/graphene/nanometer nickel composite material cost by present method, has handiness and higher pseudo-capacitance characteristic.Present method has also strengthened the bonding force of graphene-supported nano nickel composite granule and polyaniline, be beneficial to the performance of Graphene and nano nickel particle good characteristic in mixture, the specific surface area that the special nucleus shell structure forming between graphene-supported nano nickel composite granule and polyaniline and Graphene are larger, these features are all beneficial to the diffusion of electrolyte ion and then improve the electrochemical properties of polyaniline.
Brief description of the drawings
Fig. 1 is the SEM figure of polyaniline/graphene/nanometer nickel composite material of test preparation;
Fig. 2 is the cyclic voltammogram of polyaniline/graphene/nanometer nickel composite material of test preparation; Wherein a is the oxidation peak of polyaniline, and b is the reduction peak of polyaniline;
Fig. 3 is the XRD spectra of polyaniline/graphene/nanometer nickel composite material of test preparation.
Embodiment:
Embodiment one: the preparation method of present embodiment polyaniline/graphene/nanometer nickel composite material, realizes according to the following steps:
One, prepare graphene oxide solution: in the sulfuric acid that is 98% at the quality percentage composition of 40～60ml, add 1.0～1.5g crystalline flake graphite, under 0～4 DEG C of ice-water bath, stir 20～40min, then add 1～2g SODIUMNITRATE and 9～11g potassium permanganate, reaction 1～3h; Then be placed in 35 DEG C of water-baths and react 9～13h, then add 350～450mL distilled water diluting, carry out ultrasonic dispersion, then add the H of 80～100mL quality percentage composition 5%
2o
2, then add 45～55mL dilute hydrochloric acid; Then carry out suction filtration, centrifugal, collect solid formation, be then placed in 350～450ml distilled water and dissolve, then put into semi-permeable membranes dialysis processing until solution is neutral, then be 0.001～0.003g/mL by distilled water diluting to concentration, obtain required graphene oxide solution;
Two, the NaOH solution that the concentration of preparing graphene-supported nano nickel composite granule: a, the preparation 10～30mL protochloride nickel ethylene glycol solution that is 0.1mol/L and 2～4mL concentration are 0.2mol/L; B, graphene oxide solution prepared by protochloride nickel ethylene glycol solution and 50mL step 2 mix ultrasonic 30min, add successively the hydrazine hydrate solution that NaOH solution prepared by step a and 4～6mL quality percentage composition are 80% after taking-up under magnetic agitation; Then pour in hydrothermal reaction kettle and react 3～5h at 120 DEG C, then carry out filtering and washing, at 50 DEG C, dry 20～28h obtains graphene-supported nano nickel composite granule after grinding;
Three, prepare polyaniline/graphene/nanometer nickel composite material: c, add 0.5～1.5ml toluene after graphene-supported 0.1～0.3g nano nickel composite granule is placed in to three-necked bottle, ultrasonic 3～6min, obtains solution A; D, 0.5～1.5ml aniline is dissolved in the hydrochloric acid of 12～16ml1.5mol/L, obtains solution B; E, 1.5～2g Sodium dodecylbenzene sulfonate is dissolved in 20～30ml distilled water, ultrasonic 3～6min makes it to mix, and obtains solution C; F, solution A, solution B and solution C are mixed in the three-necked bottle of step c, ultrasonic 10～20min, obtains mixing solutions; G, 2～3g ammonium persulphate is dissolved in 20～30ml distilled water, under the rotating speed of 300r/m, join in the mixing solutions that step f makes by separating funnel, rate of addition be 5 seconds every, continue again to wash after reaction 3～5h, then dry 20～28h at 50 DEG C obtains polyaniline/graphene/nanometer nickel composite material after grinding.
Method is simple for present embodiment, cost is low, productive rate is high, can be used for scale operation.Utilize graphene-supported nano nickel composite granule prepared by this method can be on Graphene load good dispersion, size uniform, the nickel nano particle that particle diameter is less.And it is low, easily synthetic to prepare polyaniline/graphene/nanometer nickel composite material cost by present method, has handiness and higher pseudo-capacitance characteristic.Present method has also strengthened the bonding force of graphene-supported nano nickel composite granule and polyaniline, be beneficial to the performance of Graphene and nano nickel particle good characteristic in mixture, the specific surface area that the special nucleus shell structure forming between graphene-supported nano nickel composite granule and polyaniline and Graphene are larger, these features are all beneficial to the diffusion of electrolyte ion and then improve the electrochemical properties of polyaniline.
Embodiment two: present embodiment is different from embodiment one: be placed in 35 DEG C of water-baths in step 1 and react 10h.Other is identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one: be placed in 400mL distilled water in step 1 and dissolve.Other is identical with embodiment one.
Embodiment four: present embodiment is different from embodiment one: in step 1, the concentration of graphene oxide solution is 0.002g/mL.Other is identical with embodiment one.
Embodiment five: present embodiment is different from embodiment one: pour in step b in hydrothermal reaction kettle and react 4h at 120 DEG C.Other is identical with embodiment one.
Embodiment six: present embodiment is different from one of embodiment one to five: add 1ml toluene in step c in the graphene-supported nano nickel composite granule of 0.2g.Other is identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to five: in steps d, 1ml aniline is dissolved in the hydrochloric acid of 14ml1.5mol/L.Other is identical with one of embodiment one to five.
Embodiment eight: present embodiment is different from one of embodiment one to five: in step e, 1.75g sodium dodecylbenzenesulfonate is dissolved in 25ml distilled water.Other is identical with one of embodiment one to five.
Embodiment nine: present embodiment is different from one of embodiment one to eight: in step g, 2.45g ammonium persulphate is dissolved in 25ml distilled water.Other is identical with one of embodiment one to eight.
Embodiment ten: present embodiment is different from one of embodiment one to nine: the washing in step g is first to use distilled water filtering and washing 5 times, then uses acetone filtering and washing 1 time, finally uses ethanol filtering and washing 1 time.Other is identical with one of embodiment one to nine.
By following verification experimental verification beneficial effect of the present invention:
The preparation method of test, this test polyaniline/graphene/nanometer nickel composite material, realizes according to the following steps:
One, prepare graphene oxide solution: in the sulfuric acid that is 98% at the quality percentage composition of 50ml, add 1.2g crystalline flake graphite, under 0～4 DEG C of ice-water bath, stir 30min, then slowly add 1.5g SODIUMNITRATE and 10g potassium permanganate, reaction 2h; Then be placed in 35 DEG C of water-baths and react 12h, then add 400mL distilled water diluting, carry out ultrasonic dispersion, then add the H of 90mL quality percentage composition 5%
2o
2, then add 50mL dilute hydrochloric acid; Then carrying out suction filtration, centrifugal, collect solid formation, be then placed in 4000ml distilled water and dissolve, then put into semi-permeable membranes dialysis processing until solution is neutral, is then 0.002g/mL by distilled water diluting to concentration, obtains required graphene oxide solution;
Two, the NaOH solution that the concentration of preparing graphene-supported nano nickel composite granule: a, the preparation 20mL protochloride nickel ethylene glycol solution that is 0.1mol/L and 3mL concentration are 0.2mol/L; B, graphene oxide solution prepared by protochloride nickel ethylene glycol solution and 50mL step 2 mix ultrasonic 30min, add successively the hydrazine hydrate solution that NaOH solution prepared by step a and 5mL quality percentage composition are 80% after taking-up under magnetic agitation; Then pour in hydrothermal reaction kettle and react 4h at 120 DEG C, then carry out filtering and washing, at 50 DEG C, dry 24h obtains graphene-supported nano nickel composite granule after grinding;
Three, prepare polyaniline/graphene/nanometer nickel composite material: c, add 1ml toluene after graphene-supported 0.2g nano nickel composite granule is placed in to three-necked bottle, ultrasonic 5min, obtains solution A; D, 1ml aniline is dissolved in the hydrochloric acid of 14ml1.5mol/L, obtains solution B; E, 1.75g Sodium dodecylbenzene sulfonate is dissolved in 25ml distilled water, ultrasonic 5min makes it to mix, and obtains solution C; F, solution A, solution B and solution C are mixed in the three-necked bottle of step c, ultrasonic 15min, obtains mixing solutions; G, 2.45g ammonium persulphate is dissolved in 25ml distilled water, under the rotating speed of 300r/m, join in the mixing solutions that step f makes by separating funnel, rate of addition be 5 seconds every, continue again after reaction 4h, first use distilled water filtering and washing 5 times, then use acetone filtering and washing 1 time, then use ethanol filtering and washing 1 time.Finally dry 24h at 50 DEG C obtains polyaniline/graphene/nanometer nickel composite material after grinding.
Polyaniline/graphene/nanometer nickel composite material to this test preparation carries out electron-microscope scanning, and result as shown in Figure 1, as shown in Figure 1: graphene-supported nano nickel composite granule is wrapped up by polyaniline, forms nucleocapsid structure.
Polyaniline/graphene/nanometer nickel composite material to this test preparation carries out cyclic voltammetry, and as shown in Figure 2, a is the oxidation peak of polyaniline to result, and b is the reduction peak of polyaniline.As shown in Figure 2: the polyaniline/graphene/nanometer nickel composite material by this test preparation has obvious redox peak.
Polyaniline/graphene/nanometer nickel composite material to this test preparation carries out XRD test, result as shown in Figure 3,2 θ=44.4 °, 51.6 °, 76.5 ° of crystal face diffraction peaks that the peak of locating is nickel, the peak of 2 θ between 15 ° to 30 ° is the diffraction peak of polyaniline.Can significantly see the characteristic peak of polyaniline and nickel from Fig. 3, the characteristic peak of Graphene and the characteristic peak of polyaniline are overlapping, so not obvious.
Claims (10)
1. the preparation method of polyaniline/graphene/nanometer nickel composite material, is characterized in that the preparation method of polyaniline/graphene/nanometer nickel composite material realizes according to the following steps:
One, prepare graphene oxide solution: in the sulfuric acid that is 98% at the quality percentage composition of 40～60ml, add 1.0～1.5g crystalline flake graphite, under 0～4 DEG C of ice-water bath, stir 20～40min, then add 1～2g SODIUMNITRATE and 9～11g potassium permanganate, reaction 1～3h; Then be placed in 35 DEG C of water-baths and react 9～13h, then add 350～450mL distilled water diluting, carry out ultrasonic dispersion, then add the H of 80～100mL quality percentage composition 5%
2o
2, then add 45～55mL dilute hydrochloric acid; Then carry out suction filtration, centrifugal, collect solid formation, be then placed in 350～450ml distilled water and dissolve, then put into semi-permeable membranes dialysis processing until solution is neutral, then be 0.001～0.003g/mL by distilled water diluting to concentration, obtain required graphene oxide solution;
Two, the NaOH solution that the concentration of preparing graphene-supported nano nickel composite granule: a, the preparation 10～30mL protochloride nickel ethylene glycol solution that is 0.1mol/L and 2～4mL concentration are 0.2mol/L; B, graphene oxide solution prepared by protochloride nickel ethylene glycol solution and 50mL step 2 mix ultrasonic 30min, add successively the hydrazine hydrate solution that NaOH solution prepared by step a and 4～6mL quality percentage composition are 80% after taking-up under magnetic agitation; Then pour in hydrothermal reaction kettle and react 3～5h at 120 DEG C, then carry out filtering and washing, at 50 DEG C, dry 20～28h obtains graphene-supported nano nickel composite granule after grinding;
Three, prepare polyaniline/graphene/nanometer nickel composite material: c, add 0.5～1.5ml toluene after graphene-supported 0.1～0.3g nano nickel composite granule is placed in to three-necked bottle, ultrasonic 3～6min, obtains solution A; D, 0.5～1.5ml aniline is dissolved in the hydrochloric acid of 12～16ml 1.5mol/L, obtains solution B; E, 1.5～2g Sodium dodecylbenzene sulfonate is dissolved in 20～30ml distilled water, ultrasonic 3～6min makes it to mix, and obtains solution C; F, solution A, solution B and solution C are mixed in the three-necked bottle of step c, ultrasonic 10～20min, obtains mixing solutions; G, 2～3g ammonium persulphate is dissolved in 20～30ml distilled water, under the rotating speed of 300r/m, join in the mixing solutions that step f makes by separating funnel, rate of addition be 5 seconds every, continue again to wash after reaction 3～5h, then dry 20～28h at 50 DEG C obtains polyaniline/graphene/nanometer nickel composite material after grinding.
2. the preparation method of polyaniline/graphene/nanometer nickel composite material according to claim 1, is characterized in that in step 1, being placed in 35 DEG C of water-baths reacts 10h.
3. the preparation method of polyaniline/graphene/nanometer nickel composite material according to claim 1 and 2, is characterized in that in step 1, being placed in 400mL distilled water dissolves.
4. the preparation method of polyaniline/graphene/nanometer nickel composite material according to claim 3, the concentration that it is characterized in that graphene oxide solution in step 1 is 0.002g/mL.
5. the preparation method of polyaniline/graphene/nanometer nickel composite material according to claim 4, is characterized in that pouring in hydrothermal reaction kettle and react 4h at 120 DEG C in step b.
6. the preparation method of polyaniline/graphene/nanometer nickel composite material according to claim 4, is characterized in that in the graphene-supported nano nickel composite granule of 0.2g, adding 1ml toluene in step c.
7. the preparation method of polyaniline/graphene/nanometer nickel composite material according to claim 4, is characterized in that in steps d, 1ml aniline being dissolved in the hydrochloric acid of 14ml 1.5mol/L.
8. the preparation method of polyaniline/graphene/nanometer nickel composite material according to claim 4, is characterized in that in step e, 1.75g sodium dodecylbenzenesulfonate being dissolved in 25ml distilled water.
9. the preparation method of polyaniline/graphene/nanometer nickel composite material according to claim 4, is characterized in that in step g, 2.45g ammonium persulphate being dissolved in 25ml distilled water.
10. the preparation method of polyaniline/graphene/nanometer nickel composite material according to claim 4, is characterized in that the washing in step g is first to use distilled water filtering and washing 5 times, then uses acetone filtering and washing 1 time, finally uses ethanol filtering and washing 1 time.
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| CN102581295A (en) * | 2012-01-10 | 2012-07-18 | 黑龙江大学 | Method of using liquid-phase reduction method to prepare nano copper powder loaded graphene |
| CN102604085A (en) * | 2012-01-20 | 2012-07-25 | 黑龙江大学 | Preparation method of polyaniline/carbon nano tube/nano-copper composite material |
| CN102850543A (en) * | 2012-09-28 | 2013-01-02 | 中国科学院宁波材料技术与工程研究所 | Graphene/conductive polymer composite material and preparation method thereof |
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