CN102702520A - Preparation method for composite material of sulfonated graphene/polypyrrole - Google Patents
Preparation method for composite material of sulfonated graphene/polypyrrole Download PDFInfo
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- CN102702520A CN102702520A CN2012101880137A CN201210188013A CN102702520A CN 102702520 A CN102702520 A CN 102702520A CN 2012101880137 A CN2012101880137 A CN 2012101880137A CN 201210188013 A CN201210188013 A CN 201210188013A CN 102702520 A CN102702520 A CN 102702520A
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Abstract
The invention relates to a preparation method of a silver-ion absorbent, and an application of the silver-ion absorbent, belonging to the field of industrial waste water treatment. The preparation method for composite material of sulfonated graphene/polypyrrole comprises the following steps that 1) sulfonated grapheme is prepared via a chemical oxidization method by utilizing natural graphite; 2) the sulfonated grapheme is dispersed and dissolved in water, and pyrrol is added to obtain solution A, wherein the concentration of the sulfonated grapheme is 0.5-1.5mg/mL, and the concentration of the pyrrol is 0.05-0.2mol/L; 3) ammonium peroxydisulfate is dissolved in water, a mole ratio of the ammonium peroxydisulfate to the pyrrol is 0.5:1 to 2:1, and aqueous solution of the ammonium peroxydisulfate is obtained; 4) the aqueous solution of the ammonium peroxydisulfate is added into the solution A, and is mixed for a reaction for 12-36 hours; and 5) the obtained product in the step 4) is filtered and washed until the filter liquor is colorless, and the composite material of the sulfonated graphene/polypyrrole is obtained after the filter liquor is dried by vacuum baking. The composite material of the sulfonated graphene/polypyrrole has a remarkable absorbing and recycling performance for silver ions.
Description
Technical field
The present invention relates to the preparation method of a kind of silver ion adsorbant (sulfonated graphene/Pt/Polypyrrole composite material), and the application of this silver ion adsorbant, the Industrial Wastewater Treatment field belonged to.
Background technology
Along with the sustained and rapid development of Chinese society economy, sanitary wastewater and trade effluent are more and more serious for the influence of environment.If these waste water are not handled, the objectionable impurities in the waste water just might be participated in food chain and circulated in enrichment in the human body so, and harm humans is healthy, causes many environmental problems.In wastewater treatment, heavy metal wastewater thereby is one of the most reluctant waste water.The method of handling heavy metal wastewater thereby at present mainly contains absorption method, ion precipitation method, exchange resin method etc.But the ion precipitation method causes the water quality sclerosis easily, causes shortcomings such as secondary pollution.What the exchange resin method was difficult to realize the heavy metal ion of adsorbing and resin separates shortcomings such as subsequent technique complicacy.Inorganic or organic materials more and more receives people's concern as the absorption method of adsorbent for heavy metal with gac, zeolite, chitosan etc. in recent years.These traditional sorbent material ubiquities shortcomings such as loading capacity to silver ions is low, adsorption effect is not good.
Therefore develop the simple stable performance of a kind of technology, and in absorption, can to reduce silver ions be that the efficient silver ion adsorbant of simple substance silver is one of present argentiferous ion waste water processing aspect problem demanding prompt solution.
Summary of the invention
The object of the present invention is to provide a kind of silver ions to be had the preparation method of the sulfonated graphene/Pt/Polypyrrole composite material (silver ion adsorbant) of favourable absorption recyclability, and the application of this sulfonated graphene/Pt/Polypyrrole composite material.
To achieve these goals, the technical scheme that the present invention taked is that the preparation method of sulfonated graphene/Pt/Polypyrrole composite material is characterized in that it comprises the steps:
1) utilizes natural graphite, prepare sulfonated graphene through chemical oxidation method;
2) with the sulfonated graphene dispersing and dissolving in water, add the pyrroles again and obtain solution A, wherein the concentration of sulfonated graphene is 0.5-1.5mg/mL, pyrroles's concentration is 0.05-0.2mol/L;
3) soluble in water (concentration to ammonium persulphate does not require with ammonium persulphate; Only need the final mol ratio of assurance ammonium persulphate and pyrroles just); Making ammonium persulphate and pyrroles's mol ratio is 0.5:1-2:1 [i.e. (0.5～2): 1], obtains the aqueous solution of ammonium persulphate;
4) aqueous solution with ammonium persulphate adds in the solution A stirring reaction 12-36 hour;
5) the step 4) products therefrom filters, and washing for colourless, behind the vacuum drying, obtains sulfonated graphene/Pt/Polypyrrole composite material up to filtrating.
The application of above-mentioned sulfonated graphene/Pt/Polypyrrole composite material; It is characterized in that: as silver ion adsorbant; The argentiferous ion waste water is carried out adsorption treatment, add sulfonated graphene/Pt/Polypyrrole composite material 20-60mg, in the argentiferous ion waste water, add sulfonated graphene/Pt/Polypyrrole composite material by every 20mL argentiferous ion waste water (argentiferous ionic water); Sonic oscillation 30-60 minute, restir absorption 24-72 hour; Initial concentration of silver ions in the said argentiferous ion waste water is 5-20mg/L.
Distinguishing feature of the present invention is: 1) on Graphene, introduce sulfonic acid group, improved the solubility property of Graphene in water, and utilized sulfonated graphene as doping agent, can be doped in the molecular chain of polypyrrole, realize combining closely with polypyrrole is intermolecular; 2) composite copolymerization of sulfonated graphene and polypyrrole; Both provided Graphene great specific surface area; Let the sulfonic group introduced on the Graphene and the common performance of the nitrogen-containing group on the polypyrrole molecular chain adsorptive power simultaneously for silver ions; And in absorption, most of silver ions is reduced to argent, helps direct recovery.
The invention has the beneficial effects as follows: silver ions is had the favourable absorption recyclability.
Embodiment
For a better understanding of the present invention, further illustrate content of the present invention, but content of the present invention not only is confined to following embodiment below in conjunction with embodiment.
In following examples; The silver ions adsorption experiment is sulfonated graphene/Pt/Polypyrrole composite material to be added 20mL contain in the water (argentiferous ion waste water) of silver ions; Sonic oscillation 30-60 minute, restir absorption certain hour filtered; Remaining concentration of silver ions in the filtrating is adopted the Fo Erhadefa titration, calculate the silver ions adsorption rate according to (1) formula.
Adsorption rate=(C
0– C)/C
0* 100%
(1)
C wherein
0Be initial concentration of silver ions, C is an absorption back residue concentration of silver ions.
Embodiment 1:
The preparation method of sulfonated graphene/Pt/Polypyrrole composite material, it comprises the steps:
1) according to the method for bibliographical information prepare sulfonated graphene (Nano Letts 2008,8,1679-1682.);
2) with the sulfonated graphene dispersing and dissolving in water, add the pyrroles again and obtain solution A, wherein the concentration of sulfonated graphene is 0.5mg/mL, pyrroles's concentration is 0.1mol/L;
3) ammonium persulphate is soluble in water, making ammonium persulphate and pyrroles's mol ratio is 1:1, obtains the aqueous solution of ammonium persulphate;
4) aqueous solution with ammonium persulphate adds in the solution A stirring reaction 12 hours;
5) the step 4) products therefrom filters, and washing for colourless, obtains sulfonated graphene/Pt/Polypyrrole composite material up to filtrating behind the vacuum drying.
20mg sulfonated graphene/Pt/Polypyrrole composite material is added 20mL to be contained in the water of 10mg/L silver ions; Sonic oscillation 30 minutes; Restir absorption 48 hours; Filter the back with silver ion content in the Fo Erhadefa titration filtrating, the result shows that the silver ions adsorption rate is 86.3% in such cases, explains that the present invention has the favourable absorption recyclability to silver ions.
Embodiment 2:
The preparation method of sulfonated graphene/Pt/Polypyrrole composite material, it comprises the steps:
1) according to the method for bibliographical information prepare sulfonated graphene (Nano Letts 2008,8,1679-1682.);
2) with the sulfonated graphene dispersing and dissolving in water, add the pyrroles again and obtain solution A, wherein the concentration of sulfonated graphene is 1mg/mL, pyrroles's concentration is 0.1mol/L;
3) ammonium persulphate is soluble in water, making ammonium persulphate and pyrroles's mol ratio is 0.5:1, obtains the aqueous solution of ammonium persulphate;
4) aqueous solution with ammonium persulphate adds in the solution A stirring reaction 24 hours;
5) the step 4) products therefrom filters, and washing for colourless, obtains sulfonated graphene/Pt/Polypyrrole composite material up to filtrating behind the vacuum drying.
30mg sulfonated graphene/Pt/Polypyrrole composite material is added 20mL to be contained in the water of 20mg/L silver ions; Sonic oscillation 60 minutes; Restir absorption 72 hours; Filter the back with silver ion content in the Fo Erhadefa titration filtrating, the result shows that the silver ions adsorption rate is 75.2% in such cases, explains that the present invention has the favourable absorption recyclability to silver ions.
Embodiment 3:
The preparation method of sulfonated graphene/Pt/Polypyrrole composite material, it comprises the steps:
1) according to the method for bibliographical information prepare sulfonated graphene (Nano Letts 2008,8,1679-1682.);
2) with the sulfonated graphene dispersing and dissolving in water, add the pyrroles again and obtain solution A, wherein the concentration of sulfonated graphene is 1.5mg/mL, pyrroles's concentration is 0.2mol/L;
3) ammonium persulphate is soluble in water, making ammonium persulphate and pyrroles's mol ratio is 2:1, obtains the aqueous solution of ammonium persulphate;
4) aqueous solution with ammonium persulphate adds in the solution A stirring reaction 36 hours;
5) the step 4) products therefrom filters, and washing for colourless, obtains sulfonated graphene/Pt/Polypyrrole composite material up to filtrating behind the vacuum drying.
40mg sulfonated graphene/Pt/Polypyrrole composite material is added 20mL to be contained in the water of 5mg/L silver ions; Sonic oscillation 45 minutes; Restir absorption 24 hours; Filter the back with silver ion content in the Fo Erhadefa titration filtrating, the result shows that the silver ions adsorption rate is 98.5% in such cases, explains that the present invention has the favourable absorption recyclability to silver ions.
Embodiment 4:
The preparation method of sulfonated graphene/Pt/Polypyrrole composite material, it comprises the steps:
1) according to the method for bibliographical information prepare sulfonated graphene (Nano Letts 2008,8,1679-1682.);
2) with the sulfonated graphene dispersing and dissolving in water, add the pyrroles again and obtain solution A, wherein the concentration of sulfonated graphene is 1mg/mL, pyrroles's concentration is 0.1mol/L;
3) ammonium persulphate is soluble in water, making ammonium persulphate and pyrroles's mol ratio is 2:1, obtains the aqueous solution of ammonium persulphate;
4) aqueous solution with ammonium persulphate adds in the solution A stirring reaction 24 hours;
5) the step 4) products therefrom filters, and washing for colourless, obtains sulfonated graphene/Pt/Polypyrrole composite material up to filtrating behind the vacuum drying.
60mg sulfonated graphene/Pt/Polypyrrole composite material is added 20mL to be contained in the water of 10mg/L silver ions; Sonic oscillation 60 minutes; Restir absorption 72 hours; Filter the back with silver ion content in the Fo Erhadefa titration filtrating, the result shows that the silver ions adsorption rate is 93.1% in such cases, explains that the present invention has the favourable absorption recyclability to silver ions.
Embodiment 5:
The preparation method of sulfonated graphene/Pt/Polypyrrole composite material, it comprises the steps:
1) according to the method for bibliographical information prepare sulfonated graphene (Nano Letts 2008,8,1679-1682.);
2) with the sulfonated graphene dispersing and dissolving in water, add the pyrroles again and obtain solution A, wherein the concentration of sulfonated graphene is 0.5mg/mL, pyrroles's concentration is 0.05mol/L;
3) ammonium persulphate is soluble in water, making ammonium persulphate and pyrroles's mol ratio is 1:1, obtains the aqueous solution of ammonium persulphate;
4) aqueous solution with ammonium persulphate adds in the solution A stirring reaction 36 hours;
5) the step 4) products therefrom filters, and washing for colourless, obtains sulfonated graphene/Pt/Polypyrrole composite material up to filtrating behind the vacuum drying.
30mg sulfonated graphene/Pt/Polypyrrole composite material is added 20mL to be contained in the water of 5mg/L silver ions; Sonic oscillation 30 minutes; Restir absorption 72 hours; Filter the back with silver ion content in the Fo Erhadefa titration filtrating, the result shows that the silver ions adsorption rate is 99.1% in such cases, explains that the present invention has the favourable absorption recyclability to silver ions.
Embodiment 6:
The preparation method of sulfonated graphene/Pt/Polypyrrole composite material, it comprises the steps:
1) according to the method for bibliographical information prepare sulfonated graphene (Nano Letts 2008,8,1679-1682.);
2) with the sulfonated graphene dispersing and dissolving in water, add the pyrroles again and obtain solution A, wherein the concentration of sulfonated graphene is 1.5mg/mL, pyrroles's concentration is 0.1mol/L;
3) ammonium persulphate is soluble in water, making ammonium persulphate and pyrroles's mol ratio is 0.5:1, obtains the aqueous solution of ammonium persulphate;
4) aqueous solution with ammonium persulphate adds in the solution A stirring reaction 18 hours;
5) the step 4) products therefrom filters, and washing for colourless, obtains sulfonated graphene/Pt/Polypyrrole composite material up to filtrating behind the vacuum drying.
50mg sulfonated graphene/Pt/Polypyrrole composite material is added 20mL to be contained in the water of 5mg/L silver ions; Sonic oscillation 30 minutes; Restir absorption 48 hours; Filter the back with silver ion content in the Fo Erhadefa titration filtrating, the result shows that the silver ions adsorption rate is 98.8% in such cases, explains that the present invention has the favourable absorption recyclability to silver ions.
Embodiment 7:
The preparation method of sulfonated graphene/Pt/Polypyrrole composite material, it comprises the steps:
1) according to the method for bibliographical information prepare sulfonated graphene (Nano Letts 2008,8,1679-1682.);
2) with the sulfonated graphene dispersing and dissolving in water, add the pyrroles again and obtain solution A, wherein the concentration of sulfonated graphene is 0.5mg/mL, pyrroles's concentration is 0.15mol/L;
3) ammonium persulphate is soluble in water, making ammonium persulphate and pyrroles's mol ratio is 1:1, obtains the aqueous solution of ammonium persulphate;
4) aqueous solution with ammonium persulphate adds in the solution A stirring reaction 36 hours;
5) the step 4) products therefrom filters, and washing for colourless, obtains sulfonated graphene/Pt/Polypyrrole composite material up to filtrating behind the vacuum drying.
40mg sulfonated graphene/Pt/Polypyrrole composite material is added 20mL to be contained in the water of 10mg/L silver ions; Sonic oscillation 45 minutes; Restir absorption 48 hours; Filter the back with silver ion content in the Fo Erhadefa titration filtrating, the result shows that the silver ions adsorption rate is 88.2% in such cases, explains that the present invention has the favourable absorption recyclability to silver ions.
Embodiment 8:
The preparation method of sulfonated graphene/Pt/Polypyrrole composite material, it comprises the steps:
1) according to the method for bibliographical information prepare sulfonated graphene (Nano Letts 2008,8,1679-1682.);
2) with the sulfonated graphene dispersing and dissolving in water, add the pyrroles again and obtain solution A, wherein the concentration of sulfonated graphene is 1.5mg/mL, pyrroles's concentration is 0.15mol/L;
3) ammonium persulphate is soluble in water, making ammonium persulphate and pyrroles's mol ratio is 1:1, obtains the aqueous solution of ammonium persulphate;
4) aqueous solution with ammonium persulphate adds in the solution A stirring reaction 24 hours;
5) the step 4) products therefrom filters, and washing for colourless, obtains sulfonated graphene/Pt/Polypyrrole composite material up to filtrating behind the vacuum drying.
50mg sulfonated graphene/Pt/Polypyrrole composite material is added 20mL to be contained in the water of 5mg/L silver ions; Sonic oscillation 60 minutes; Restir absorption 72 hours; Filter the back with silver ion content in the Fo Erhadefa titration filtrating, the result shows that the silver ions adsorption rate is 99.2% in such cases, explains that the present invention has the favourable absorption recyclability to silver ions.
Each cited raw material of the present invention can both be realized the present invention, and the bound value of each raw material, interval value can both realize the present invention; Do not enumerate embodiment one by one at this.Bound value, the interval value of processing parameter of the present invention can both be realized the present invention, do not enumerate embodiment one by one at this.
Claims (2)
1. the preparation method of sulfonated graphene/Pt/Polypyrrole composite material is characterized in that it comprises the steps:
1) utilizes natural graphite, prepare sulfonated graphene through chemical oxidation method;
2) with the sulfonated graphene dispersing and dissolving in water, add the pyrroles again and obtain solution A, wherein the concentration of sulfonated graphene is 0.5-1.5mg/mL, pyrroles's concentration is 0.05-0.2mol/L;
3) ammonium persulphate is soluble in water, making ammonium persulphate and pyrroles's mol ratio is 0.5:1-2:1, obtains the aqueous solution of ammonium persulphate;
4) aqueous solution with ammonium persulphate adds in the solution A stirring reaction 12-36 hour;
5) the step 4) products therefrom filters, and washing for colourless, behind the vacuum drying, obtains sulfonated graphene/Pt/Polypyrrole composite material up to filtrating.
2. the application of the resulting sulfonated graphene/Pt/Polypyrrole composite material of claim 1; It is characterized in that: as silver ion adsorbant; The argentiferous ion waste water is carried out adsorption treatment, add sulfonated graphene/Pt/Polypyrrole composite material 20-60mg, in the argentiferous ion waste water, add sulfonated graphene/Pt/Polypyrrole composite material by every 20mL argentiferous ion waste water; Sonic oscillation 30-60 minute, restir absorption 24-72 hour; Initial concentration of silver ions in the said argentiferous ion waste water is 5-20mg/L.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103390511A (en) * | 2013-07-30 | 2013-11-13 | 河海大学 | Preparation method for graphene oxide/polypyrrole composite material of lamellar microstructure |
| CN103421188A (en) * | 2013-08-01 | 2013-12-04 | 河海大学 | Method for preparing sheet polypyrrole with high conductivity |
| CN104190385A (en) * | 2014-08-29 | 2014-12-10 | 湖南大学 | Polypyrrole/Fe3O4/graphene composite material, and preparation method and application thereof |
| WO2016090523A1 (en) * | 2014-11-13 | 2016-06-16 | 上海工程技术大学 | Graphene-containing composite material and preparation method and use thereof |
| CN106876156A (en) * | 2013-12-02 | 2017-06-20 | 天津大学 | Polyaniline-sulfonated graphene composite material and its application |
| CN106876154A (en) * | 2013-12-02 | 2017-06-20 | 天津大学 | The preparation method of polyaniline-sulfonated graphene combination electrode material |
| CN107118554A (en) * | 2016-11-28 | 2017-09-01 | 江南大学 | A kind of preparation method of sulfonated graphene/polypyrrole conducing composite material |
| CN107519846A (en) * | 2017-07-31 | 2017-12-29 | 华南理工大学 | A kind of graphene/silicon dioxide Pt/Polypyrrole composite material and preparation method and application |
| CN108091761A (en) * | 2017-12-25 | 2018-05-29 | 武汉工程大学 | Memory device based on sulfonated graphene/polypyrrole/gold nano particle composite material and preparation method thereof |
| CN108409963A (en) * | 2018-04-19 | 2018-08-17 | 太仓美克斯机械设备有限公司 | A kind of preparation method of anti-oxidant Polypyrrole Conducting Materials |
| CN108675284A (en) * | 2018-05-14 | 2018-10-19 | 江苏大学 | Polypyrrole/Ni (OH)2The preparation method and application of/sulfonated graphene ternary composite electrode material |
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| CN103390511A (en) * | 2013-07-30 | 2013-11-13 | 河海大学 | Preparation method for graphene oxide/polypyrrole composite material of lamellar microstructure |
| CN103421188A (en) * | 2013-08-01 | 2013-12-04 | 河海大学 | Method for preparing sheet polypyrrole with high conductivity |
| CN103421188B (en) * | 2013-08-01 | 2015-07-29 | 河海大学 | A kind of preparation method of sheet polypyrrole with high conductivity |
| CN106876156B (en) * | 2013-12-02 | 2018-12-14 | 天津大学 | Polyaniline-sulfonated graphene composite material and its application |
| CN106876156A (en) * | 2013-12-02 | 2017-06-20 | 天津大学 | Polyaniline-sulfonated graphene composite material and its application |
| CN106876154A (en) * | 2013-12-02 | 2017-06-20 | 天津大学 | The preparation method of polyaniline-sulfonated graphene combination electrode material |
| CN104190385A (en) * | 2014-08-29 | 2014-12-10 | 湖南大学 | Polypyrrole/Fe3O4/graphene composite material, and preparation method and application thereof |
| WO2016090523A1 (en) * | 2014-11-13 | 2016-06-16 | 上海工程技术大学 | Graphene-containing composite material and preparation method and use thereof |
| CN107118554A (en) * | 2016-11-28 | 2017-09-01 | 江南大学 | A kind of preparation method of sulfonated graphene/polypyrrole conducing composite material |
| CN107519846A (en) * | 2017-07-31 | 2017-12-29 | 华南理工大学 | A kind of graphene/silicon dioxide Pt/Polypyrrole composite material and preparation method and application |
| CN108091761A (en) * | 2017-12-25 | 2018-05-29 | 武汉工程大学 | Memory device based on sulfonated graphene/polypyrrole/gold nano particle composite material and preparation method thereof |
| CN108091761B (en) * | 2017-12-25 | 2021-03-30 | 武汉工程大学 | Storage device based on sulfonated graphene/polypyrrole/gold nanoparticle composite material and preparation method thereof |
| CN108409963A (en) * | 2018-04-19 | 2018-08-17 | 太仓美克斯机械设备有限公司 | A kind of preparation method of anti-oxidant Polypyrrole Conducting Materials |
| CN108675284A (en) * | 2018-05-14 | 2018-10-19 | 江苏大学 | Polypyrrole/Ni (OH)2The preparation method and application of/sulfonated graphene ternary composite electrode material |
| CN113713782A (en) * | 2021-08-16 | 2021-11-30 | 中化学朗正环保科技有限公司 | Silver @ polypyrrole composite material for wastewater adsorption and preparation method and application thereof |
| CN113713782B (en) * | 2021-08-16 | 2024-02-06 | 中化学朗正环保科技有限公司 | Silver@polypyrrole composite material for wastewater adsorption and preparation method and application thereof |
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Application publication date: 20121003 |