CN108359092A - A kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material - Google Patents
A kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material Download PDFInfo
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Abstract
A kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material, is related to a kind of preparation method of nanocomposite, includes the preparation of three-dimensional grapheme：Graphene oxide is mixed with deionized water, graphene oxide dispersion is obtained after ultrasonic disperse；The graphene oxide dispersion is placed in hydro-thermal reaction in ptfe autoclave and obtains three-dimensional grapheme；The preparation of three-dimensional meso-hole graphene：Three-dimensional grapheme is soaked in alkaline solution, after vacuum freeze drying, the priming reaction under nitrogen or argon gas atmosphere is dried to obtain three-dimensional meso-hole graphene through pickling and deionized water washing；The preparation of three-dimensional meso-hole grapheme/polyaniline composite material：By three-dimensional meso-hole graphene dispersion in acid solution, and aniline and ammonium persulfate is added, under the conditions of ice salt bath, in-situ polymerization obtains three-dimensional meso-hole grapheme/polyaniline composite material.The material is applied to the fields such as electrode material for super capacitor, energy storage material and Heat Conduction Material.
Description
Technical field
The present invention relates to a kind of preparation method of nanocomposite, more particularly to a kind of three-dimensional meso-hole graphene/poly-
The preparation method of aniline composite material.
Background technology
The reunion of graphene and stacking always affect its application in terms of capacitor, and many researchers are prepared for having
The three-dimensional grapheme of big specific surface area and porous structure, and three-dimensional grapheme and polyaniline progress is compound, formation foam-like,
Nano thin-film and reticular structure etc. improve application of the graphene in terms of energy storage.Three-dimensional grapheme/polyaniline composite material system
Preparation Method is different, and there is also differences for obtained composite structure and performance.Currently, the method prepared mainly has in-situ polymerization
Method, electrochemical polymerization method and self-assembly method etc..Both situ aggregation method is being distributed to graphene uniform in aniline solution, make
Polymerisation occurs, covers polyaniline on the surface of graphene, the structure of graphene is made not change.Prepare composite material at present
Situ aggregation method is mostly used greatly, is the preparation method of comparative maturity.
" a kind of three-dimensional redox graphene/polyaniline is compound for the Chinese patent application that notification number is CN104559176A
The preparation method of material " through hydrothermal reduction by obtaining three-dimensional porous graphite again by graphene oxide and polyaniline In-situ reaction
Alkene/polyaniline composite material." a kind of three-dimensional grapheme/polyaniline is multiple for the Chinese patent application that notification number is CN105254877A
The preparation method of condensation material " is the three-dimensional structure of graphene to be built by poly furfuryl alcohol template, then prepare three-dimensional by hydro-thermal method
Grapheme/polyaniline composite material." porous graphene/polyaniline is multiple for the Chinese patent application that notification number is CN104558597A
The preparation method of condensation material " is by introducing carbonate deposition in graphene oxide solution, under alkaline condition through chemical water
After heat-treating and removing carbonate, in-situ polymerization obtains porous graphene/polyaniline composite material.
Tang Wei（Tang Wei, the preparation of three-dimensional grapheme/polyaniline composite material and its south research [D] of chemical property
Capital:Nanjing Univ. of Posts and Telecommunications 2015）Using three-dimensional grapheme/polyaniline composite material that calcium carbonate is prepared as template, have mutual
The pore structure of perforation, cyclical stability is high under low voltage condition.Xu Jianjun（Perhaps strong monarch graphenes and polyaniline composite sponge
Preparation and the Harbin performance study [D]:Harbin University of Science and Technology 2015）It is prepared using in-situ polymerization and freeze-drying
Graphene/polyaniline composite sponge specific capacitance it is high and there is three-dimensional porous reticular structure, with the increase of polyphenyl amine content,
The specific capacitance of composite material also gradually increases, and can reach 487 F/g, can be applied to ultracapacitor field.Luo Jianping etc.
People（The such as Luo Jianping polymer material sciences and engineering, 2017,33 (03):84-88）Also use in-situ polymerization and freezing dry
Dry method has synthesized three-dimensional porous structure grapheme/polyaniline composite material, when current density is 0.5 A/g, composite material
Specific capacitance is 321.91 F/g, than being higher by 81.53 F/g before reduction.
The three-dimensional porous grapheme/polyaniline composite material that above-mentioned published method is prepared is mostly macroporous structure, multiple
The specific surface area of condensation material and hole appearance raising are limited, prepare three-dimensional there has been no the method using the activation of hydrothermal reduction combination alkali at present
It is prepared the relevant report of three-dimensional meso-hole grapheme/polyaniline composite material by mesoporous graphene with aniline in-situ polymerization again.This
Outside, it is uniform on three-dimensional grapheme matrix to effectively increase alkali for the method for vacuum freeze drying after the alkali that the application proposes impregnates
Distribution, it is ensured that three-dimensional grapheme integrally etches highly uniform.
Invention content
The purpose of the present invention is to provide a kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material, this hairs
It is bright to prepare three-dimensional meso-hole graphene and make aniline for in-situ polymerization at polyaniline, preparation method is simple on three-dimensional meso-hole graphene,
Obtained composite material chemical property is good.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material, the method includes following preparation processes：
A. the preparation of three-dimensional grapheme：Graphene oxide is mixed with deionized water, graphene oxide point is obtained after ultrasonic disperse
Dispersion liquid；The graphene oxide dispersion is placed in hydro-thermal reaction in ptfe autoclave, and for a period of time, vacuum is taken out after cooling
Filter, is washed, vacuum freeze drying, obtains three-dimensional grapheme later repeatedly with deionized water；
B. the preparation of three-dimensional meso-hole graphene：The three-dimensional grapheme of step a is soaked in alkaline solution, it is dry through vacuum refrigeration
After dry, the priming reaction under nitrogen or argon gas atmosphere is dried to obtain three-dimensional meso-hole graphene through pickling and deionized water washing；
C. the preparation of three-dimensional meso-hole grapheme/polyaniline composite material：By the three-dimensional meso-hole graphene dispersion of step b in acidity
In solution, and aniline and ammonium persulfate is added, under the conditions of ice salt bath, in-situ polymerization obtains three-dimensional meso-hole graphene/polyaniline
Composite material.
A kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material, the graphite oxide of the step a
A concentration of 0.2 ~ 5 mg/ml of alkene dispersion liquid, the reaction temperature that the hydro-thermal reaction obtains three-dimensional grapheme are 160 ~ 200
DEG C, the reaction time is 12 ~ 48 hours.
A kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material, the three-dimensional graphite of the step b
The mass ratio of alkene and potassium hydroxide is 1：（0.5~15）, soaking time is 12 ~ 48 hours, and activation temperature is 400 ~ 800 DEG C, living
It is 1 ~ 5 hour to change the time.
A kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material, step b pickling examination used
Agent is one kind in hydrochloric acid or acetic acid.
A kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material, the acid solution of the step c
For any one in hydrochloric acid, sulfuric acid, phosphoric acid, perchloric acid, a concentration of 1 ~ 2 mol/L of acid solution.
A kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material, the three-dimensional meso-hole of the step c
The mass ratio of graphene and aniline is（0.1~10）:1, the molar ratio of aniline and ammonium persulfate is（0.25~4）:1.
The cryosel of a kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material, the step c is chlorine
Change any one in sodium, calcium chloride, sodium nitrate.
A kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material, the polymerisation of the step c
Temperature is 0 ~ 5 DEG C, and the reaction time is 2 ~ 12 hours.
Advantages of the present invention is with effect：
The present invention constructs three-dimensional grapheme using the method for hydrothermal reduction, avoids using toxic chemical reducing agent, green ring
It protects；The three-dimensional meso-hole graphene obtained by alkali activation has higher specific surface area and high conductivity；The three-dimensional prepared
Mesoporous grapheme/polyaniline composite material be conducive to electrolyte come into full contact with and electron-transport, show good electrification
Performance is learned, the fields such as electrode material for super capacitor, energy storage material and Heat Conduction Material are can be applied to.
Description of the drawings
Fig. 1 is the SEM figures of the three-dimensional meso-hole graphene in embodiment 1.
Specific implementation mode
The following describes the present invention in detail with reference to examples.
Embodiment 1
A kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material, includes the following steps：
Step a：Graphene oxide is mixed, ultrasonic disperse 1 hour with deionized water, obtains a concentration of 2 mg/ml oxidation
Graphene dispersing solution；The graphene oxide dispersion is placed in ptfe autoclave small in 180 DEG C of hydro-thermal reactions 12
When, it is filtered by vacuum, is washed repeatedly with deionized water, vacuum freeze drying, obtains three-dimensional grapheme later after cooling.
Step b：The obtained three-dimensional graphemes of step a are soaked in potassium hydroxide solution（Three-dimensional grapheme and hydroxide
The mass ratio of potassium is 1：3）, ultrasonic disperse 1 hour, standing 24 hours, after vacuum freeze drying, in a nitrogen atmosphere in pipe
It activates 3 hours for 500 DEG C in formula stove, after cooling, is successively washed to neutrality, vacuum with 36% acetic acid solution and deionized water
Freeze-drying, obtains three-dimensional meso-hole graphene.
Step c：Aniline monomer is substantially soluble in 100 milliliters of the hydrochloric acid solution of 1 mol/L, then step b is obtained
Three-dimensional meso-hole graphene be substantially soluble in the hydrochloric acid solution of the aniline（The mass ratio of three-dimensional grapheme and aniline is 0.2:1）,
Under the conditions of ice salt bath, 100 milliliters of the hydrochloric acid solution dissolved with 1 mol/L of ammonium persulfate is slowly added dropwise into above-mentioned mixed liquor
（The molar ratio of aniline and ammonium persulfate is 1:1）, controlling reaction temperature is at 0 ~ 5 DEG C, reaction 8 hours；After reaction, it will precipitate
It filters, washing to neutrality, is dried at 60 DEG C, obtain three-dimensional meso-hole grapheme/polyaniline composite material.
According to the method described above, three-dimensional meso-hole graphene is subjected to SEM scanning electron microscope analysis, as shown in Figure 1, can obviously see
Go out the hole that a large amount of mesoporous ranks are formd in three-dimensional grapheme structure.
Embodiment 2
A kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material, includes the following steps：
Step a：Graphene oxide is mixed, ultrasonic disperse 1 hour with deionized water, obtains a concentration of 1 mg/ml and aoxidize stone
Black alkene dispersion liquid；The graphene oxide dispersion is placed in ptfe autoclave in 180 DEG C of hydro-thermal reactions 24 hours, it is cold
But it is filtered by vacuum, is washed repeatedly with deionized water, vacuum freeze drying, obtains three-dimensional grapheme later afterwards.
Step b：The obtained three-dimensional graphemes of step a are soaked in potassium hydroxide solution（Three-dimensional grapheme and hydroxide
The mass ratio of potassium is 1：2.5）, ultrasonic disperse 1 hour, stand 48 hours, after vacuum freeze drying, in a nitrogen atmosphere in
It activates 5 hours for 500 DEG C in tube furnace, after cooling, is successively washed to neutrality, very with 36% acetic acid solution and deionized water
Vacuum freecing-dry obtains three-dimensional meso-hole graphene.
Step c：Aniline monomer is substantially soluble in 100 milliliters of the hydrochloric acid solution of 1 mol/L, then step b is obtained
Three-dimensional meso-hole graphene be substantially soluble in the hydrochloric acid solution of the aniline（The mass ratio of three-dimensional grapheme and aniline is 0.333:
1）, under the conditions of ice salt bath, the hydrochloric acid solution 100 of 1 mol/L dissolved with ammonium persulfate is slowly added dropwise into above-mentioned mixed liquor
Milliliter（I.e. the molar ratio of aniline and ammonium persulfate is 2:1）, controlling reaction temperature is at 0 ~ 5 DEG C, reaction 12 hours；After reaction,
Precipitation is filtered, washed to neutrality, is dried at 60 DEG C, three-dimensional meso-hole grapheme/polyaniline composite material is obtained.
Embodiment 3
A kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material, includes the following steps：
Step a：Graphene oxide is mixed, ultrasonic disperse 1 hour with deionized water, obtains a concentration of 0.5 mg/ml oxygen
Graphite alkene dispersion liquid；The graphene oxide dispersion is placed in ptfe autoclave in 180 DEG C of hydro-thermal reactions 24
Hour, it is filtered by vacuum, is washed repeatedly with deionized water, vacuum freeze drying, obtains three-dimensional grapheme later after cooling.
Step b：The obtained three-dimensional graphemes of step a are soaked in potassium hydroxide solution（Three-dimensional grapheme and hydroxide
The mass ratio of potassium is 1：4）, ultrasonic disperse 1 hour, standing 24 hours, after vacuum freeze drying, in a nitrogen atmosphere in pipe
It activates 2 hours for 500 DEG C in formula stove, after cooling, is successively washed to neutrality, vacuum with 36% acetic acid solution and deionized water
Freeze-drying, obtains three-dimensional meso-hole graphene.
Step c：Aniline monomer is substantially soluble in 100 milliliters of the hydrochloric acid solution of 1 mol/L, then step b is obtained
Three-dimensional meso-hole graphene be substantially soluble in the hydrochloric acid solution of the aniline（The mass ratio of three-dimensional grapheme and aniline is 0.167:
1）, under the conditions of ice salt bath, the hydrochloric acid solution 100 of 1 mol/L dissolved with ammonium persulfate is slowly added dropwise into above-mentioned mixed liquor
Milliliter（I.e. the molar ratio of aniline and ammonium persulfate is 1:1）, controlling reaction temperature is at 0 ~ 5 DEG C, reaction 8 hours；It, will after reaction
Precipitation is filtered, washed to neutrality, is dried at 60 DEG C, is obtained three-dimensional meso-hole grapheme/polyaniline composite material.
Embodiment 4
A kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material, includes the following steps：
Step a：Graphene oxide is mixed, ultrasonic disperse 1 hour with deionized water, obtains a concentration of 2 mg/ml oxidation
Graphene dispersing solution；The graphene oxide dispersion is placed in ptfe autoclave small in 180 DEG C of hydro-thermal reactions 24
When, it is filtered by vacuum, is washed repeatedly with deionized water, vacuum freeze drying, obtains three-dimensional grapheme later after cooling.
Step b：The obtained three-dimensional graphemes of step a are soaked in potassium hydroxide solution, ultrasonic disperse 1 hour, are stood
48 hours, after vacuum freeze drying, in a nitrogen atmosphere in tube furnace 500 DEG C activate 3 hours, after cooling, successively
It is washed to neutrality, vacuum freeze drying with 36% acetic acid solution and deionized water, obtains three-dimensional meso-hole graphene.
Step c：Aniline monomer is substantially soluble in 100 milliliters of the hydrochloric acid solution of 1 mol/L, then step b is obtained
Three-dimensional meso-hole graphene be substantially soluble in the hydrochloric acid solution of the aniline（The mass ratio of three-dimensional grapheme and aniline is 0.167:
1）, under the conditions of ice salt bath, the hydrochloric acid solution 100 of 1 mol/L dissolved with ammonium persulfate is slowly added dropwise into above-mentioned mixed liquor
Milliliter（I.e. the molar ratio of aniline and ammonium persulfate is 4:1）, controlling reaction temperature is at 0 ~ 5 DEG C, reaction 12 hours；After reaction,
Precipitation is filtered, washed to neutrality, is dried at 60 DEG C, three-dimensional meso-hole grapheme/polyaniline composite material is obtained.
Claims (8)
1. a kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material, which is characterized in that the method includes following
Preparation process：
The preparation of three-dimensional grapheme：Graphene oxide is mixed with deionized water, graphene oxide dispersion is obtained after ultrasonic disperse
Liquid；The graphene oxide dispersion is placed in hydro-thermal reaction in ptfe autoclave for a period of time, to be filtered by vacuum after cooling,
It is washed repeatedly with deionized water, vacuum freeze drying, obtains three-dimensional grapheme later；
The preparation of three-dimensional meso-hole graphene：The three-dimensional grapheme of step a is soaked in alkaline solution, through vacuum freeze drying
Afterwards, the priming reaction under nitrogen or argon gas atmosphere is dried to obtain three-dimensional meso-hole graphene through pickling and deionized water washing；
The preparation of three-dimensional meso-hole grapheme/polyaniline composite material：By the three-dimensional meso-hole graphene dispersion of step b in acid solution
In, and aniline and ammonium persulfate is added, under the conditions of ice salt bath, it is compound that in-situ polymerization obtains three-dimensional meso-hole graphene/polyaniline
Material.
2. a kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material according to claim 1, feature exist
In：A concentration of 0.2 ~ 5 mg/ml of the graphene oxide dispersion of the step a, the hydro-thermal reaction obtain three-dimensional stone
The reaction temperature of black alkene is 160 ~ 200 DEG C, and the reaction time is 12 ~ 48 hours.
3. a kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material according to claim 1, feature exist
In：The three-dimensional grapheme of the step b and the mass ratio of potassium hydroxide are 1：（0.5~15）, soaking time is 12 ~ 48 hours,
Activation temperature is 400 ~ 800 DEG C, and soak time is 1 ~ 5 hour.
4. a kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material according to claim 1, feature exist
In：The step b pickling agents useful for same is one kind in hydrochloric acid or acetic acid.
5. a kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material according to claim 1, feature exist
In：The acid solution of the step c is any one in hydrochloric acid, sulfuric acid, phosphoric acid, perchloric acid, and acid solution a concentration of 1 ~ 2 rubs
You/liter.
6. a kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material according to claim 1, feature exist
In：The three-dimensional meso-hole graphene of the step c and the mass ratio of aniline are（0.1~10）:1, the molar ratio of aniline and ammonium persulfate
For（0.25~4）:1.
7. a kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material according to claim 1, feature exist
In：The cryosel of the step c is any one in sodium chloride, calcium chloride, sodium nitrate.
8. a kind of preparation method of three-dimensional meso-hole grapheme/polyaniline composite material according to claim 1, feature exist
In：The polymeric reaction temperature of the step c is 0 ~ 5 DEG C, and the reaction time is 2 ~ 12 hours.
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Cited By (7)
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| CN109233273A (en) * | 2018-09-20 | 2019-01-18 | 王景硕 | A kind of preparation method of graphene-polyaniline composite sponge |
| CN109329304A (en) * | 2018-11-27 | 2019-02-15 | 辽宁大学 | Mesoporous graphene-supported silver nano particle composite material of one kind and its preparation method and application |
| CN109444250A (en) * | 2018-09-30 | 2019-03-08 | 中国科学院山西煤炭化学研究所 | A kind of preparation of graphene/porous carbon complex and mass spectral analysis application of double heteroatoms doping |
| CN111029544A (en) * | 2019-11-29 | 2020-04-17 | 合肥国轩高科动力能源有限公司 | Preparation method of modified three-dimensional graphene coated sulfur positive electrode for lithium-sulfur battery |
| CN113410061A (en) * | 2021-04-30 | 2021-09-17 | 上海交通大学 | Nitrogen-fluorine co-doped porous graphene/polyaniline supercapacitor electrode material and preparation method and application thereof |
| CN114171325A (en) * | 2021-11-17 | 2022-03-11 | 中北大学南通智能光机电研究院 | Preparation method of three-dimensional graphene/polyaniline loaded conductive fabric composite electrode material |
| CN114775090A (en) * | 2022-05-17 | 2022-07-22 | 凯盛家纺股份有限公司 | Preparation method of graphene modified anti-static fabric |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109233273A (en) * | 2018-09-20 | 2019-01-18 | 王景硕 | A kind of preparation method of graphene-polyaniline composite sponge |
| CN109444250A (en) * | 2018-09-30 | 2019-03-08 | 中国科学院山西煤炭化学研究所 | A kind of preparation of graphene/porous carbon complex and mass spectral analysis application of double heteroatoms doping |
| CN109329304A (en) * | 2018-11-27 | 2019-02-15 | 辽宁大学 | Mesoporous graphene-supported silver nano particle composite material of one kind and its preparation method and application |
| CN111029544A (en) * | 2019-11-29 | 2020-04-17 | 合肥国轩高科动力能源有限公司 | Preparation method of modified three-dimensional graphene coated sulfur positive electrode for lithium-sulfur battery |
| CN113410061A (en) * | 2021-04-30 | 2021-09-17 | 上海交通大学 | Nitrogen-fluorine co-doped porous graphene/polyaniline supercapacitor electrode material and preparation method and application thereof |
| CN114171325A (en) * | 2021-11-17 | 2022-03-11 | 中北大学南通智能光机电研究院 | Preparation method of three-dimensional graphene/polyaniline loaded conductive fabric composite electrode material |
| CN114775090A (en) * | 2022-05-17 | 2022-07-22 | 凯盛家纺股份有限公司 | Preparation method of graphene modified anti-static fabric |
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