CN101973620A - Method for removing heavy metal ions in water by using graphene oxide sheet - Google Patents
Method for removing heavy metal ions in water by using graphene oxide sheet Download PDFInfo
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Abstract
The invention relates to a method for removing heavy metal ions in water by using a graphene oxide sheet, which belongs to the technical fields of water purification and environmental protection. In the invention, the graphene oxide sheet is used as an adsorbent of the heavy metal ions, wherein the graphene oxide sheet is of a monatomic layer two-dimensional structure and has a huge specific surface while ensuring no obvious toxicity. In the purification process of the method, the operations are simple without pollution, and the copper ion adsorption efficiency is 10 times that of the active carbon. In the invention, the graphene oxide sheet adsorbing the metal ions can be recovered to the single sheet structure by a centrifugal separation or dialysis method and can be recycled.
Description
Technical field
The present invention relates to a kind of method of utilizing the graphene oxide sheet to remove heavy metal ion in the water, belong to purification of water quality and environmental protection technical field.
Background technology
In recent years, China is faced with the environmental problem that water pollution etc. is on the rise.Heavy metal is because its high toxicity, non-degradable and easy characteristics such as enrichment in vivo become pollutent important in the water pollution.Purification of heavy metal ionic soil water body has several different methods, for example chemical precipitation method, ion exchange method, electroosmose process, absorption method etc.In these methods, the adsorbents adsorb method is a kind of method of simple, efficient, removal heavy metal ion that expense is cheap.That the key that improves this method is to develop is more efficient, environmental protection, inexpensive sorbent material.
At present, there are many materials to be in the news with the heavy metal ion that removes in the water body, for example gac, flyash, chitin etc.Nano material has great specific surface area, thereby is considered to existing higher efficient aspect heavy metal absorption.For example, carbon nanotube is proved to be a kind of very effective novel heavy metal absorbent, and the common acticarbon of efficiency ratio exceeds 5～7 times.But carbon nanotube costs an arm and a leg, has certain toxicity, and be difficult for to remove in water body, thereby is easy to generate secondary pollution, and the harm that human health is caused.At this problem, need develop efficient more, economical and nontoxic nano adsorber.
Since 2004 were found, because its particular structure and physico-chemical property, Graphene had evoked scientific worker's research enthusiasm greatly.It all has potential to use at aspects such as storage hydrogen, medicine carrier band, exchange membrane and electrodes.Grapheme material yet there are no report aspect the heavy metal contamination processing.Through peroxidation, the Graphene surface can produce a large amount of hydroxyls, carboxyl and epoxide group, and these oxy radicals have great avidity to metal ion.Based on this phenomenon, we have developed a kind of novel nano sorbent material of environmental protection and economy, can remove the heavy metal ion in the water simply, efficiently, greenly.
Summary of the invention
The purpose of this invention is to provide a kind of simple, green, remove the method for heavy metal ion in the water efficiently.
A kind of method of utilizing the graphene oxide sheet to remove heavy metal ion in the water of the present invention is characterized in that having following process and step:
A. be raw material with natural graphite powder, add a certain amount of vitriol oil, Potassium Persulphate and Vanadium Pentoxide in FLAKES,, make its reaction 4.5 hours at 80 ℃ of following uniform mixing; Mixture is cooled to room temperature, releases the back standing over night with deionized water alkene, use the cellulose acetate membrane filtering separation in 0.2 micron hole then, and use a large amount of deionized water wash, product is standing over night at room temperature; With above-mentioned product is that stir on the graphite limit of preoxidation, the limit adds in the mixing solutions of the cold vitriol oil and potassium permanganate, stirs the back down at 35 ℃ and is releasing with deionized water alkene, continues stirring, adds a certain amount of superoxol again; Then above-mentioned solution is filtered, and remove metal ion, remove unnecessary acid with deionized water wash again, and repeatedly be washed with water to neutrality, get graphite oxide with the dilute hydrochloric acid solution washing; The graphite oxide of gained is mixed with the aqueous solution of 1.0mg/ml concentration, and in ultrasonic machine, carries out supersound process, obtain filemot homogeneous dispersive mono-layer graphite oxide alkene sheet solution; Graphene oxide is preserved standby with gel or solid form;
B. the graphene oxide sheet solution that to get the above-mentioned concentration that makes be 0.5～2.0 mg/ml join concentration be 100～200 mmoles/liter cupric chloride or lead nitrate or cadmium nitrate solution in, mix mutually with equal-volume; Shake up, leave standstill, make to reach adsorption equilibrium; This moment, agglomeration appearred in graphene oxide sheet solution, and solution becomes suspension; Can be observed and confirm that by the atomic force microscope photo graphene oxide sheet has adsorbed heavy metal ion.
(1) used nano adsorber is the graphene oxide sheet, has the two-dirnentional structure of monoatomic layer, and surface-area is huge.Graphene oxide sheet good biocompatibility can not cause intensive toxicity even be discharged in the environment yet.
(2) the raw materials used inorganic chemistry material that is inexpensive, low toxicity commonly used is compared with other sorbent material, and with low cost, operating process is simple, and is pollution-free.
(3) to the adsorption efficiency of cupric ion than other carbon material height, be more than 10 times of gac.In Adsorption of Heavy Metal Ions, certain variation appears in its structure arranges, and can remove easily by filtration or sedimentation.
(4) this adsorption process is a kind of reversible behavior, can return to single chip architecture by centrifugal or dialysis behind the graphene oxide sheet adsorbing metal ions, can reuse.
Description of drawings
Fig. 1 is atomic force microscope (AFM) the photo figure of the mono-layer graphite oxide alkene sheet of gained of the present invention.
Fig. 2 is the graphene oxide sheet solution of gained of the present invention and the photo figure of graphene oxide sheet/cupric ion aggregate
Fig. 3 is the graphene oxide sheet Adsorption of Cu of gained of the present invention
2+After atomic force microscope (AFM) photo figure.
Fig. 4 for the graphene oxide sheet of gained of the present invention to Cu
2+The adsorption isotherm line chart.
Fig. 5 is the photo figure of dispersive graphene oxide sheet solution again after the recovery of gained of the present invention.
Embodiment
After now specific embodiments of the invention being discussed in.
Embodiment 1: concrete steps are as follows:
(1), mono-layer graphite oxide alkene sheet formulations prepared from solutions: with natural graphite powder is raw material, get the natural graphite powder of 3 grams, 325 order fineness, add 12 milliliters of vitriol oils, 2.5 gram Potassium Persulphates and 2.5 gram Vanadium Pentoxide in FLAKESs,, make its reaction 4.5 hours at 80 ℃ of following uniform mixing; Mixture is cooled to room temperature, releases the back standing over night with deionized water alkene, use the cellulose acetate membrane filtering separation in 0.2 micron hole then, and use a large amount of deionized water wash, product is standing over night at room temperature; With above-mentioned product is that the graphite limit stirring of preoxidation, 120 milliliters of the vitriol oils and the potassium permanganate 15 that the limit slowly adds 0 ℃ of refrigerative restrain in the mixing solutions of forming, after stirring 2 hours under 35 ℃, release with 250 ml deionized water alkene, continue stirring and add 700 ml deionized water again after 2 hours, after stirring, add 20 milliliters of superoxols again; Then above-mentioned solution is filtered, and wash with 1: 10 dilute hydrochloric acid solution and to remove metal ion, remove unnecessary acid with deionized water wash again, and repeatedly be washed with water to neutrality and obtain graphite oxide; The graphite oxide of gained is mixed with the aqueous solution of 1.0 mg/ml concentration, and in ultrasonic machine, carries out supersound process, obtain filemot homogeneous dispersive mono-layer graphite oxide alkene sheet solution.The visible Fig. 1 of gained result.
(2), to Cu
2+Absorption: get the graphene oxide sheet solution of 2 milliliter of 1.0 mg/ml, add again 2 milliliter of 100 mmole/liter Cupric Chloride Solution, mixing shakes up.Agglomeration appears in graphene oxide sheet solution at once, and solution becomes suspension.The visible Fig. 2 of gained result, Fig. 3.The common filter paper filtering of suspension, filtrate water white transparency, oxygen-free Graphene.
Embodiment 2: the preparation process of the graphene oxide sheet solution in the present embodiment and step and the foregoing description 1 are identical.
Get the graphene oxide sheet solution of 2 milliliter of 1.0 mg/ml, add again 2 milliliter of 100 mmole/liter lead nitrate solution, mixing shakes up.Agglomeration appears in graphene oxide sheet solution at once, and solution becomes suspension.
Get the graphene oxide sheet solution of 2 milliliter of 1.0 mg/ml, add again 2 milliliter of 100 mmole/liter cadmium nitrate solution, mixing shakes up.Agglomeration appears in graphene oxide sheet solution at once, and solution becomes suspension.
This explanation graphene oxide has ubiquity to the absorption of heavy metal ion.
Embodiment 3: the preparation process of the graphene oxide sheet solution in the present embodiment and step and the foregoing description 1 are identical.Different is: with sodium hydroxide solution and hydrogen chloride solution the initial pH value of graphene oxide sheet solution and Cupric Chloride Solution is transferred to 5.0, both are mixed, make the ultimate density of graphene oxide sheet be 0.5 mg/ml, the ultimate density of cupric chloride is respectively 50,75, and 100,200,300,400,500,600,700,1000 micromoles per liter mix, and suspension liquid was at room temperature left standstill 12 hours, afterwards 14000 rev/mins centrifugal 30 minutes, measure the concentration of cupric ion in the supernatant.Cupric ion equilibrium concentration (the C that obtains
e) and equilibrium adsorption ability (q
e) data fit Langmuir's adsorption isotherm model.Adsorption isothermal line is seen Fig. 4.The graphene oxide sheet is 46.6 milligrams of copper/gram graphene oxide to the maximum adsorption ability of cupric ion, this value is higher than the maximum adsorption ability (28.5 milligram copper/gram carbon nanotube) of carbon nanotube to cupric ion, is 10 times of maximum adsorption ability (4～5 milligrams of copper/gram gacs) of gac.
The recycling of graphene oxide sheet: the suspension of the graphene oxide sheet/heavy metal ion aggregate of above-mentioned gained is carried out centrifugation; 14000 rev/mins of following centrifugations 30 minutes, use deionized water wash again 5 times; Perhaps use dialysis process, using and staying molecular weight is 3500 dialysis tubing, changes a deionized water in per 12 hours; The graphene oxide sheet that obtains is disperseed with deionized water again, can obtain tawny graphene oxide sheet solution again.The gained result is referring to Fig. 5.
Claims (1)
1. method of utilizing the graphene oxide sheet to remove heavy metal ion in the water is characterized in that having following process and step:
A. be raw material with natural graphite powder, add a certain amount of vitriol oil, Potassium Persulphate and Vanadium Pentoxide in FLAKES,, make its reaction 4.5 hours at 80 ℃ of following uniform mixing; Mixture is cooled to room temperature, releases the back standing over night with deionized water alkene, use the cellulose acetate membrane filtering separation in 0.2 micron hole then, and use a large amount of deionized water wash, product is standing over night at room temperature; With above-mentioned product is that stir on the graphite limit of preoxidation, the limit adds in the mixing solutions of the cold vitriol oil and potassium permanganate, stirs the back down at 35 ℃ and is releasing with deionized water alkene, continues stirring, adds a certain amount of superoxol again; Then above-mentioned solution is filtered, and remove metal ion, remove unnecessary acid with deionized water wash again, and repeatedly be washed with water to neutrality, get graphite oxide with the dilute hydrochloric acid solution washing; The graphite oxide of gained is mixed with the aqueous solution of 1.0mg/ml concentration, and in ultrasonic machine, carries out supersound process, obtain filemot homogeneous dispersive mono-layer graphite oxide alkene sheet solution; Graphene oxide is preserved standby with gel or solid form;
B. the graphene oxide sheet solution that to get the above-mentioned concentration that makes be 0.5～2.0 mg/ml join concentration be 100～200 mmoles/liter cupric chloride or lead nitrate or cadmium nitrate solution in, mix mutually with equal-volume; Shake up, leave standstill, make to reach adsorption equilibrium; This moment, agglomeration appearred in graphene oxide sheet solution, and solution becomes suspension; Can be observed and confirm that by the atomic force microscope photo graphene oxide sheet has adsorbed heavy metal ion.
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