CN104085964A - Electrochemical treatment method for removing lead ions from water by adopting polyaniline/attapulgite paper electrode - Google Patents

Electrochemical treatment method for removing lead ions from water by adopting polyaniline/attapulgite paper electrode Download PDF

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Publication number
CN104085964A
CN104085964A CN201410319905.5A CN201410319905A CN104085964A CN 104085964 A CN104085964 A CN 104085964A CN 201410319905 A CN201410319905 A CN 201410319905A CN 104085964 A CN104085964 A CN 104085964A
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attapulgite
polyaniline
solution
water
paper electrode
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CN201410319905.5A
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黎珊
孔泳
魏永
陶永新
秦勇
周荣华
张炜
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Changzhou University
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Changzhou University
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Abstract

The invention relates to an electrochemical treatment method for removing lead ions from water by adopting a polyaniline/attapulgite paper electrode. The method comprises the following steps: preparing a polyaniline/attapulgite composite material; preparing a polyaniline/attapulgite paper electrode; removing lead ions from water by adopting an electrochemical process; and desorbing and regenerating the used electrode. The electrochemical treatment method has the beneficial effects that the polyaniline/attapulgite paper electrode is short in preparation cycle, low in cost, simple and convenient to operate when being used for adsorbing lead ions, short in adsorption time, and free of secondary pollution, and can be recycled.

Description

A kind of electrochemical process for treating that adopts polyaniline/attapulgite paper electrode to remove lead ion in water
Technical field
The invention belongs to water and pollute process field, relate to a kind of electrochemical process for treating that adopts polyaniline/attapulgite paper electrode to remove lead ion in water.
Background technology
Lead in water body is one of high-risk pollutent of environment.Lead is widely used in the industries such as battery manufacture, metal processing, petroleum refining, printed electronic, mineral smelting.The waste water of therefore, discharging from these processes also in various degree environment and public health have been caused to adverse influence.Lead and compound thereof can enter human organ by food chain, and bone, heart, enteron aisle, kidney, regeneration system rapidly and neural system are produced to toxic effect.Plumbous especially very large to children's toxicity, because the plumbous development that can disturb nervous system in children.It is 1.0mg/L that China's " integrated wastewater discharge standard " (GB8978-1996) strictly limits total the highest plumbous permission emission concentration in waste water.Therefore, how effectively removing lead ion in water is the important topic that is related to environment and human health.
At present, the method for removing Lead contamination both at home and abroad mainly contains chemical precipitation, reverse osmosis, ion-exchange, solvent extraction, liquid film transmission and absorption.But these technology, owing to there being the higher or secondary pollution problems of method complexity, cost, have limited its application in actual production.And a kind of new technique that electrochemical treatment technology is new development in recent years gets up can be used for removing the solvability inorganic pollutant in the aqueous solution, as metal ion, negatively charged ion etc.Chinese patent CN102267745A has reported a kind of electrochemical process for treating that adopts polyaniline electrode to remove fluorion in water, and this invention, taking polyaniline film cathode as anode, under certain voltage, has special adsorption effect to fluorion.Chinese patent CN102923825A provides a kind of novel method of poly m-phenylene diamine as electrode adsorption material that adopt, in order to the heavy metal ion in adsorbent solution, as Cu 2+and Pb 2+, its maximum adsorption capacity is 876mgg -1, total clearance is 81%.Above two sections of patents are all to adopt conductive polymers as electro-adsorption material, conductive polymers have be easy to synthesize, the feature such as environmental stability is good, conduct electricity very well, environmental protection, but its price is higher, specific surface area is less, during for electro-adsorption process, mainly taking chemisorption as main (comprising sequestering action and electrostatic adsorption), and physical adsorption is little, and its adsorption effect is restricted.Therefore, in order to reduce as far as possible the cost of material, further improve the absorption property of material, prepare polyaniline/attapulgite mixture as electro-adsorption material, can make full use of specific surface area and surperficial negative charge thereof that recessed soil is larger, can utilize again the efficient adsorption ability of polyaniline, in removal lead ion, there is potential application prospect.In addition, utilize polyaniline/attapulgite mixture to there is not yet report as electro-adsorption material for the method for removing water lead ion.
Summary of the invention
The technical problem to be solved in the present invention is: based on the problems referred to above, the invention provides a kind of electrochemical process for treating that adopts polyaniline/attapulgite paper electrode to remove lead ion in water.
The present invention solves the technical scheme that its technical problem adopts: a kind of electrochemical process for treating that adopts polyaniline/attapulgite paper electrode to remove lead ion in water, comprises the following steps:
A, prepare polyaniline/attapulgite matrix material: attapulgite and aniline are dissolved in distilled water, mix and blend 20～60min, in mixed solution, splash into initiator solution while stirring, in ice-water bath, react 3～5h, splash into for the second time the initiator solution of same amount, in ice-water bath, continue reaction 3～5h; After reaction finishes, stop stirring mixture hold over night; Suction filtration, with absolute ethanol washing filter cake three times, then with distilled water rinse to the colourless sample that obtains of filtrate, be dried, obtain polyaniline/attapulgite matrix material.
B, prepare polyaniline/attapulgite paper electrode: the polyaniline/attapulgite matrix material that step a is made adds in polyvinyl alcohol solution, ultrasonic agitation 5～15min, furnishing pasty state dispersion liquid; Dispersion liquid is evenly coated on hard paper, dry, obtain polyaniline/attapulgite paper electrode.
C, electrochemical process are removed lead ion in water: preparation Pb (NO 3) 2solution, measures Pb (NO 3) 2solution is placed in electro-adsorption container, the polyaniline/attapulgite paper electrode that step b is made is put into electro-adsorption container, and paper electrode is connected with electrochemical workstation with wire, carries out electro-adsorption test, use the variation of conductivitimeter Real-Time Monitoring electrical conductivity of solution, until electro-adsorption balance.
Electrode after d, desorption and regeneration use: when the lead ion adsorbing on polyaniline/attapulgite paper electrode reaches capacity, remove applied voltage in electro-adsorption container, treat that the specific conductivity in solution approaches initial value, realize the desorption and regeneration of electrode.
Further, in step a, the reaction of aniline and attapulgite is home position polymerization reaction, wherein attapulgite is as matrix in reaction, and polyaniline nano fiber shape organic layer covers attapulgite particle surface, forms doped polyaniline/attapulgite fibre composite.The mass ratio of aniline and attapulgite is (1～4): 1, and wherein taking 2:1 as good.Initiator is persulfuric acid salt initiator, and the concentration of initiator is 0.3～0.5M, and the speed that splashes into of initiator solution is that 2～5s/ drips.
Further, in step b, the concentration of polyvinyl alcohol solution is 3～5wt%, and hard sheet paper size is 35mm × 8mm × 400 μ m.
Further, Pb (NO in step c 3) 2strength of solution is 0.1～2.5mM, wherein taking 0.1～0.5mM as good.The on load voltage of electro-adsorption test is-0.1～-0.6V, wherein taking-0.3V is as good, the time of on load voltage is about 3～10min.
The invention has the beneficial effects as follows: polyaniline/attapulgite paper electrode fabrication cycle is short, and cost is low, recyclable regenerative; Electrode is easy and simple to handle for adsorpting lead ion, and adsorption time is short, non-secondary pollution.
Brief description of the drawings
Below in conjunction with accompanying drawing, the present invention is further described.
Fig. 1 is the electron scanning micrograph (SEM figure) of the polyaniline/attapulgite matrix material of preparation in embodiment mono-;
Fig. 2 is Pb 2+relation curve between concentration and electrical conductivity of solution;
Fig. 3 is solution Pb in embodiment bis- 2+starting point concentration to Pb 2+the impact of clearance;
Fig. 4 be in embodiment tri-adsorption time to Pb 2+the impact of clearance;
Fig. 5 is that the absorption property of polyaniline/attapulgite paper electrode in embodiment tetra-is with the variation of regeneration times;
Fig. 6 adopts polyaniline paper electrode to process Pb in comparative example one 2+time adsorption time to Pb 2+the impact of clearance.
Embodiment
The invention will be further described in conjunction with specific embodiments now, and following examples are intended to illustrate the present invention instead of limitation of the invention further.
Describe in detail and the lead ion (Pb shown in embodiment in the present invention 2+) clearance measures as follows:
% R = C 0 - C e C 0 × 100
In formula, %R, C 0and C erepresent respectively Pb 2+clearance, starting point concentration (m xl -1) and equilibrium concentration (mgL -1).
Pb 2+relation curve between concentration and electrical conductivity of solution as shown in Figure 2.
Embodiment mono-:
Prepare polyaniline/attapulgite paper electrode, comprise the following steps:
(1) 3.7g attapulgite and 7.3mL aniline are dissolved in 100mL distilled water, mix and blend 30min, under whipped state to the ammonium persulfate solution (3s/ drips) that splashes into 100mL0.4M in mixed solution, in ice-water bath, react 4h, again splash into the ammonium persulfate solution of same amount, in ice-water bath, continue reaction 4h.After reaction finishes, stop stirring mixture hold over night.Suction filtration, with absolute ethanol washing filter cake three times, then with distilled water rinse to the colourless sample that obtains of filtrate, sample, at 60 DEG C of dry 24h, obtains polyaniline/attapulgite matrix material, as Fig. 1 shows.
(2) polyaniline/attapulgite matrix material 1g step (1) being made adds in the polyvinyl alcohol solution of 4mL4wt%, ultrasonic agitation 5min, furnishing pasty state.Above-mentioned 50mg dispersion liquid is evenly coated on to the hard paper of 35mm × 8mm, and (thick 400 μ are m) upper, in 60 DEG C of dry 6h, make polyaniline/attapulgite paper electrode.
The polyaniline/attapulgite paper electrode of preparation is for the Pb (NO of 0.2mM 3) 2the electrochemical treatment of solution, applying voltage is-0.3V that the treatment time is 5min, Pb 2+clearance be 58.26%.
Embodiment bis-:
First prepare polyaniline/attapulgite paper electrode, preparation process is identical with embodiment mono-.
The polyaniline/attapulgite paper electrode of preparation is respectively used to 0.1,0.25,0.5,1.0 and Pb (the NO of 2.5mM 3) 2the electrochemical treatment of solution, applying voltage is-0.3V that the treatment time is 5min, Pb 2+clearance see Fig. 3.Visible, polyaniline/attapulgite paper electrode is applicable to processing the Pb that contains of low concentration 2+waste water.
Embodiment tri-:
First prepare polyaniline/attapulgite paper electrode, preparation process is identical with embodiment mono-.
The polyaniline/attapulgite paper electrode of preparation is for the Pb (NO of 0.1mM 3) 2the electrochemical treatment of solution, applies voltage for-0.3V, and the treatment time is respectively 0.1,0.5,1,2,3,5 and 10min, Pb 2+clearance see Fig. 4, visible, the Pb in electro-adsorption container 2+about 3min reaches adsorption equilibrium, and adsorption rate is very fast.
Embodiment tetra-:
First prepare polyaniline/attapulgite paper electrode, preparation process is identical with embodiment mono-.
According to above test-results, the electro-adsorption/electric desorption test that circulates of p-poly-phenyl amine/attapulgite composite material.Polyaniline/attapulgite paper electrode is placed in to the Pb (NO that 80mL concentration is 0.1mM 3) 2in solution, apply voltage for-0.3V, recording solution specific conductivity, the specific conductivity of recording solution again after 10min, calculates Pb 2+clearance; Remove subsequently current potential by its desorption 10min, the simultaneously variation of recording solution specific conductivity, calculates the velocity of variation of specific conductivity; Continuous circulation 10 times, the results are shown in Figure 5.Visible, polyaniline/attapulgite paper electrode after 10 continuous electro-adsorption/electric desorptions circulation, Pb 2+clearance be down to 64.2% from 66.5%, still to Pb 2+there is good adsorption effect, illustrate that this electrode has fabulous regeneration effect.
Comparative example one:
First prepare polyaniline paper electrode, preparation process is identical with embodiment mono-, just in preparation process, does not add attapulgite.
Be used for the Pb (NO of 0.1mM with the polyaniline paper electrode of preparation 3) 2the electrochemical treatment of solution, applies voltage for-0.3V, and the treatment time is 1,2,3,5 and 10min, Pb 2+clearance see Fig. 6.Visible, the Pb in electro-adsorption container 2+about 10min reaches adsorption equilibrium, now Pb 2+clearance be 61.9%.
The present invention, taking attapulgite as matrix, adopts situ aggregation method to prepare polyaniline/attapulgite matrix material, and the matrix material making is made to paper electrode, has improved the specific surface area of electrode, has reduced the production cost of electrode.Electrochemical treatment by this electrode for lead ion, its absorption property, apparently higher than polyaniline paper electrode, brings up to 66.5% to the clearance of lead ion from 61.9%.In the present invention, the polyaniline/attapulgite paper electrode making is to Pb 2+carry out in the process of electrochemical treatment, its adsorption mechanism mainly comprises three aspects: attapulgite is to Pb 2+physical adsorption, negative voltage lower electrode and Pb 2+between electrostatic adhesion and amino, imido grpup and the Pb on polyaniline molecule chain 2+between sequestering action.Wherein electrostatic adsorption and sequestering action are better than physisorption, and this three's synergy makes polyaniline/attapulgite paper electrode to Pb 2+carry out in the process of electrochemical treatment, absorption property will obviously be better than other sorbing materials.
Adsorption rate is fast, adopts polyaniline/attapulgite paper electrode, and about 3min can reach adsorption equilibrium, and adopts polyaniline paper electrode, need to just can reach adsorption equilibrium by about 10min, and its adsorption time shortens greatly, and adsorption efficiency obviously improves.
Electrode recyclable regenerative, polyaniline/attapulgite paper electrode, after 10 continuous lead ion electro-adsorption of experience/electric desorption circulation, only has slightly and declines the clearance of lead ion, drops to 64.2% from 66.5%.
Taking above-mentioned foundation desirable embodiment of the present invention as enlightenment, by above-mentioned description, relevant staff can, not departing from the scope of this invention technological thought, carry out various change and amendment completely.The technical scope of this invention is not limited to the content on specification sheets, must determine its technical scope according to claim scope.

Claims (4)

1. adopt polyaniline/attapulgite paper electrode to remove an electrochemical process for treating for lead ion in water, it is characterized in that: comprise the following steps:
A, prepare polyaniline/attapulgite matrix material: attapulgite and aniline are dissolved in distilled water, mix and blend 20～60min, in mixed solution, splash into initiator solution while stirring, in ice-water bath, react 3～5h, splash into for the second time the initiator solution of same amount, in ice-water bath, continue reaction 3～5h; After reaction finishes, stop stirring mixture hold over night; Suction filtration, with absolute ethanol washing filter cake three times, then with distilled water rinse to the colourless sample that obtains of filtrate, be dried, obtain polyaniline/attapulgite matrix material;
B, prepare polyaniline/attapulgite paper electrode: the polyaniline/attapulgite matrix material that step a is made adds in polyvinyl alcohol solution, ultrasonic agitation 5～15min, furnishing pasty state dispersion liquid; Dispersion liquid is evenly coated on hard paper, dry, obtain polyaniline/attapulgite paper electrode;
C, electrochemical process are removed lead ion in water: preparation Pb (NO 3) 2solution, measures Pb (NO 3) 2solution is placed in electro-adsorption container, the polyaniline/attapulgite paper electrode making in step b is put into electro-adsorption container, and paper electrode is connected with electrochemical workstation with wire, carries out electro-adsorption test, use the variation of conductivitimeter Real-Time Monitoring electrical conductivity of solution, until electro-adsorption balance;
Electrode after d, desorption and regeneration use: when the lead ion adsorbing on polyaniline/attapulgite paper electrode reaches capacity, remove applied voltage in electro-adsorption container, treat that the specific conductivity in solution approaches initial value, realize the desorption and regeneration of electrode.
2. a kind of electrochemical process for treating that adopts polyaniline/attapulgite paper electrode to remove lead ion in water according to claim 1, it is characterized in that: in described step a, the mass ratio of aniline and attapulgite is (1～4): 1, initiator is persulfuric acid salt initiator, the concentration of initiator is 0.3～0.5M, and the speed that splashes into of initiator solution is that 2～5s/ drips.
3. a kind of electrochemical process for treating that adopts polyaniline/attapulgite paper electrode to remove lead ion in water according to claim 1, it is characterized in that: in described step b, the concentration of polyvinyl alcohol solution is 3～5wt%, hard sheet paper size is 35mm × 8mm × 400 μ m.
4. a kind of electrochemical process for treating that adopts polyaniline/attapulgite paper electrode to remove lead ion in water according to claim 1, is characterized in that: Pb (NO in described step c 3) 2strength of solution is 0.1～2.5mM, and the on load voltage of electro-adsorption test is-0.1～-0.6V, and the time of on load voltage is about 3～10min.
CN201410319905.5A 2014-07-07 2014-07-07 Electrochemical treatment method for removing lead ions from water by adopting polyaniline/attapulgite paper electrode Pending CN104085964A (en)

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CN107417911A (en) * 2017-07-16 2017-12-01 常州大学 A kind of attapulgite rod crystalline substance beam dissociation and its conducing composite material integral preparation process
CN110642335A (en) * 2019-09-29 2020-01-03 南昌航空大学 Method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater

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* Cited by examiner, † Cited by third party
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CN107417911A (en) * 2017-07-16 2017-12-01 常州大学 A kind of attapulgite rod crystalline substance beam dissociation and its conducing composite material integral preparation process
CN110642335A (en) * 2019-09-29 2020-01-03 南昌航空大学 Method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater
CN110642335B (en) * 2019-09-29 2021-12-07 南昌航空大学 Method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater

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