CN105967287A - Method for removing manganese ions in water through S element decorated graphene electrode - Google Patents
Method for removing manganese ions in water through S element decorated graphene electrode Download PDFInfo
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- CN105967287A CN105967287A CN201610517023.9A CN201610517023A CN105967287A CN 105967287 A CN105967287 A CN 105967287A CN 201610517023 A CN201610517023 A CN 201610517023A CN 105967287 A CN105967287 A CN 105967287A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/206—Manganese or manganese compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2201/00—Apparatus for treatment of water, waste water or sewage
- C02F2201/46—Apparatus for electrochemical processes
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Abstract
The invention relates to a method for removing manganese ions in water through an S element modified graphene electrode. The method comprises the following steps of preparing sulphur-doped graphene aerogel, preparing a sulphur-doped graphene aerogel paper electrode and absorbing different manganese ions through the paper electrode in a three-electrode system. The method has the advantages that a preparation method of the sulphur-doped graphene aerogel is convenient and easy; pollution in a preparation process is avoided, and environment is protected; the electrode modified by the materials is high in absorbing efficiency for the manganese ions in water, quick in speed and convenient to operate; the manganese ions in the water can be effectively removed.
Description
Technical field
The present invention relates to a kind of grapheme modified electrode of S element and remove the method for manganese ion in water, belong to water and process and materials synthesis
Field.
Technical background
Manganese is one of more rich element in nature, is also one of trace element necessary to organism.If but water containing
The manganese of amount, it will make water for industrial use and Drinking Water utilizes Quality Down.The main source of Mn-bearing waste water is: iron and steel enterprise
Efflux wastewater, electrolytic manganese production enterprise wastewater, manganese ore mine contaminant water, ferrous metal mine, metallurgy, chemical industry emission
Waste water etc..China " drinking water sanitary standard " (GB5749-2006) specifies: in water, Fe content is less than 0.1mg/L the most not
Health can be produced harm.When in former water, the content of manganese exceedes above-mentioned standard it is necessary to process.
The processing method of manganese ion in water is had a variety of: electro-adsorption, reverse osmosis, chemical precipitation method etc..Electro-adsorption is relative to it
His method for treating water, has that non-secondary pollution, energy consumption be low, small investment, length in service life and an easy advantage such as regeneration, is a kind of
Economical and effective method.Therefore, electro-adsorption technology is a kind of water technology with development prospect.
Graphene aerogel, as a kind of emerging superior adsorbent, has specific surface area big, and adsorption rate is fast, and adsorption capacity is big,
The advantages such as acid-fast alkali-proof, main is that its regeneration is convenient, meets manganese ion and processes requirement, is widely used in water purification and processes.
The present invention utilizes the bigger serface of graphene aerogel and high electron transfer rate for the manganese ion removing in water.
Summary of the invention
It is an object of the invention to grapheme modified for S element application of electrode in a new field electro-adsorption water in manganese ion.
The manganese ion that can effectively adsorb in water after adsorption electrode made by sulfur graphite alkene aeroge will be mixed.
The present invention relates to a kind of grapheme modified electrode of S element and remove the method for manganese ion in water, comprise the following steps:
Sulfur graphite alkene aeroge is mixed in a, preparation: by graphene oxide ultrasonic disperse in deionized water, ultrasonic 10～30min make it
It is uniformly dispersed.Adding dithiothreitol, DTT after it is uniformly dispersed, stirring makes it be uniformly dispersed.Then by mixed liquor at the bar of 95 DEG C
Heating in water bath 2h is carried out under part.After reaction terminates, product is placed in distilled water and immerses 2～3 days, then lyophilization,
To mixing sulfur graphite alkene aerogel material；
Sulfur graphite alkene Aerogel paper electrode is mixed in b, preparation: step a prepared mixes sulfur graphite alkene aeroge and the poly-second prepared in advance
Enolate solution mixes, and forms the dispersion liquid of pasty state, pipettes the homogeneous dispersion of 0.1～0.4mL and is applied on hard paper, freezing dry
Dry, obtain mixing sulfur graphite alkene Aerogel paper electrode；
C, electrochemical process remove manganese ion in water: prepare manganese ion solution, measure manganese ion solution and be placed in electro-adsorption container, will
The sulfur graphite alkene Aerogel paper electrode of mixing prepared in step b carries out electro-adsorption experiment to manganese ion.The experiment of electro-adsorption manganese ion uses
Three-electrode system, with paper electrode as working electrode, platinum plate electrode is to electrode, and calomel electrode is reference electrode.Make electricity consumption simultaneously
Electrical conductivity instrument monitors the change of electrical conductivity of solution in real time, and when electrical conductivity keeps constant, the absorption of the most each paper electrode reaches balance.
Further, in step a, dithiothreitol, DTT is 3:1 with the mass ratio of graphene oxide, and reaction temperature is 95 DEG C, during reaction
Between be 2～4h.
Further, in step c, the ion in electro-adsorption water is Mn2+。
The invention has the beneficial effects as follows: the preparation method mixing sulfur graphite alkene aeroge is simple and easy to do, and preparation process is environment friendly and pollution-free,
The electrode modified with these materials in water, the adsorption efficiency of manganese ion is higher, the time is short, easy and simple to handle, the electro-adsorption of material
Performance there has also been compared with conventional material and significantly promotes.
Accompanying drawing explanation
The present invention is further described below in conjunction with the accompanying drawings.
Fig. 1 is the infrared spectrum (FT-IR figure) mixing sulfur graphite alkene aeroge of preparation in embodiment one；
Fig. 2 is Mn in solution in embodiment two2+Initial concentration is to Mn2+The impact of clearance；
Fig. 3 is the absorption property mixing sulfur graphite alkene Aerogel paper electrode in embodiment three change with regeneration times.
Detailed description of the invention
Presently in connection with specific embodiment, the present invention will be further described, and following example are intended to illustrate rather than this
Bright further restriction.
Describe in detail in the present invention and measure as follows with the manganese ion clearance shown in examples of implementation:In formula, %R, C0、CeRepresent Mn respectively2+Clearance, initial concentration, equilibrium concentration.
Embodiment one:
Preparation is mixed sulfur graphite alkene aerogel material paper electrode and is included following step:
(1) by graphene oxide (GO) ultrasonic disperse of 0.15g in 100mL distilled water, the two sulfur Soviet Unions of 0.45g are added
Sugar alcohol, mechanical agitation makes it be sufficiently mixed, and then mixed liquor carries out under conditions of 95 DEG C heating in water bath 2h.After reaction terminates,
Being immersed in by the product of generation in distilled water 2～3 days, final sample, at-52 DEG C of lyophilization 24h, must mix sulfur graphite alkene aeroge.
(2) 90mg step (1) prepared mixes the poly-vinyl alcohol solution that sulfur graphite alkene aerogel material adds 2mL 4wt%,
Ultrasonic composite is made to be uniformly dispersed in solution.Take the above-mentioned homogeneous dispersion of 0.16mL and be applied in the cardboard of 35mm × 8mm
On sheet (thick 400 μm), in-52 DEG C of lyophilization 12h, make and mix sulfur graphite alkene Aerogel paper electrode.
Embodiment two:
The preparation process mixing sulfur graphite alkene Aerogel paper electrode is identical with embodiment one.
Nitrogen-doped graphene Aerogel paper electrode by preparation is respectively used to the Mn of 0.25,0.4,0.8,1,3 and 6mM2+Solution
Electrochemical treatments, applying voltage is 0.3V, and the process time is 2min, Mn2+Clearance see Fig. 2, it is seen that nitrating graphite
The alkene aerogel material Mn to low concentration2+Solution has preferable adsorption effect..
Embodiment three:
The preparation process mixing sulfur graphite alkene Aerogel paper electrode is identical with embodiment one.
It is circulated electro-adsorption test to mixing sulfur graphite alkene Aerogel paper electrode.Sulfur graphite alkene Aerogel paper electrode will be mixed and be placed in 80mL
Concentration is the Mn of 0.25mmol/L2+In solution, apply current potential-0.3V, and recording solution electrical conductivity, again record molten after 2min
The electrical conductivity of liquid, calculates clearance.Removing current potential subsequently to be desorbed by it, circulation is repeatedly continuously.Experimental result is as shown in Figure 3.
Adsorb Mn first2+Clearance is 78.7%, at the recycling rear electrode through 30 times to Mn2+Clearance is 77.3%, only
There is decline slightly, but electro-adsorption clearance has significantly decline when proceeding circulation experiment, goes after recycling for 80 times
Except rate is 72.3%.
Claims (3)
1. the grapheme modified electrode of S element removes the method for manganese ion in water, it is characterised in that: step is as follows:
Sulfur graphite alkene aeroge is mixed in a, preparation: by graphene oxide ultrasonic disperse in deionized water, ultrasonic 10～30min make it
It is uniformly dispersed.Adding dithiothreitol, DTT after it is uniformly dispersed, stirring makes it be uniformly dispersed, then by mixed liquor at the bar of 95 DEG C
Heating in water bath 2h is carried out under part.After reaction terminates, product is placed in distilled water and immerses 2～3 days, then lyophilization,
To mixing sulfur graphite alkene aerogel material；
Sulfur graphite alkene Aerogel paper electrode is mixed in b, preparation: step a prepared mixes sulfur graphite alkene aeroge and the poly-second prepared in advance
Enolate solution mixes, and forms the dispersion liquid of pasty state, pipettes the homogeneous dispersion of 0.1～0.4mL and is applied on hard paper, freezing dry
Dry, obtain mixing sulfur graphite alkene Aerogel paper electrode；
C, electrochemical process remove manganese ion in water: prepare manganese ion solution, measure manganese ion solution and be placed in electro-adsorption container, will
The sulfur graphite alkene Aerogel paper electrode of mixing prepared in step b carries out electro-adsorption experiment to manganese ion.The experiment of electro-adsorption manganese ion uses
Three-electrode system, with paper electrode as working electrode, platinum plate electrode is to electrode, and calomel electrode is reference electrode.Make electricity consumption simultaneously
Electrical conductivity instrument monitors the change of electrical conductivity of solution in real time, when electrical conductivity keeps constant, i.e. mixes sulfur graphite alkene Aerogel paper electrode adsorption
Reach balance；
D, desorption and regeneration use after electrode: saturated mix sulfur graphite alkene Aerogel paper electrode for reaching to adsorb, remove on electrode
Voltage after, the electrical conductivity of solution is recovered to close to initial value, it is achieved the desorption and regeneration of electrode.
A kind of grapheme modified electrode of S element removes the method for manganese ion in water, it is characterized in that:
In described step a, dithiothreitol, DTT is 3:1 with the mass ratio of graphene oxide, and reaction temperature is 95 DEG C, and the response time is 2～4h.
A kind of grapheme modified electrode of S element removes the method for manganese ion in water, it is characterized in that:
In described step c, the ion in electro-adsorption water is Mn2+。
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20130134964A (en) * | 2012-05-31 | 2013-12-10 | 에스케이이노베이션 주식회사 | Flowable electrode for energy storage |
| CN103996830A (en) * | 2014-05-12 | 2014-08-20 | 上海大学 | A preparation method of a sulfur-supported graphene aerogel composite material |
| CN105478074A (en) * | 2015-12-23 | 2016-04-13 | 中国科学院烟台海岸带研究所 | Preparation method and application of heavy metal ion remover |
| CN105692818A (en) * | 2016-03-18 | 2016-06-22 | 常州大学 | Sulfur-doped graphene aerogel synthesized by one-step method and electric adsorption removal of sulfur-doped graphene aerogel on various heavy metal ions |
-
2016
- 2016-07-04 CN CN201610517023.9A patent/CN105967287A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20130134964A (en) * | 2012-05-31 | 2013-12-10 | 에스케이이노베이션 주식회사 | Flowable electrode for energy storage |
| CN103996830A (en) * | 2014-05-12 | 2014-08-20 | 上海大学 | A preparation method of a sulfur-supported graphene aerogel composite material |
| CN105478074A (en) * | 2015-12-23 | 2016-04-13 | 中国科学院烟台海岸带研究所 | Preparation method and application of heavy metal ion remover |
| CN105692818A (en) * | 2016-03-18 | 2016-06-22 | 常州大学 | Sulfur-doped graphene aerogel synthesized by one-step method and electric adsorption removal of sulfur-doped graphene aerogel on various heavy metal ions |
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