CN102266782B - Method for producing nano Fe(O)/CeO2 composite material and application in removing chlorophenol pollutant thereof - Google Patents

Method for producing nano Fe(O)/CeO2 composite material and application in removing chlorophenol pollutant thereof Download PDF

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CN102266782B
CN102266782B CN 201110158197 CN201110158197A CN102266782B CN 102266782 B CN102266782 B CN 102266782B CN 201110158197 CN201110158197 CN 201110158197 CN 201110158197 A CN201110158197 A CN 201110158197A CN 102266782 B CN102266782 B CN 102266782B
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王建龙
徐乐瑾
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Tsinghua University
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Abstract

The invention discloses a method for producing a nano Fe(O)/CeO2 composite material, which belongs to the field of material preparation and environment technology, and application in removing chlorophenol pollutant thereof. The producing method comprises the following steps of producing nano CeO2 particles by means of liquid precipitation, and then using the nano CeO2 particles as a carrier, synthesizing nano Fe(O)/CeO2 composite material by means of coprecipitation. The application method of the nano Fe(O)/CeO2 composite material is as follows: using the nano Fe(O)/CeO2 composite material asa catalyst, reacting with chlorophenol organic matter under the presence of O2, and then removing the chlorophenol organic matter. The producing method provided by the invention has advantages of simple technology, low requirement for equipment, low cost, high efficiency and speediness for processing waste water containing chlorophenol organic matter, economical feasibility and no secondary pollution. The method also has broad application prospect in ground water remediation and soil bioremediation and processing field of waste water containing chlorinated organic matter.

Description

Nanometer Fe (0)/CeO 2Composite manufacture and the application in removing chlorophenol pollutant thereof
Technical field
The invention belongs to material preparation and Environmental Technology field, be specifically related to a kind of nanometer Fe (0)/CeO 2Composite manufacture method, and nanometer Fe (0)/CeO 2Composite is in the application of removing chlorophenol pollutant.
Background technology
The chlorophenols organic pollution is the intermediate product of many industrial links (such as papermaking, printing and dyeing, weaving etc.), and is widely used as pesticide, anticorrisive agent, herbicide, also is prevalent in the city tap-water.The chlorophenols similar performance, toxicity is large, is very difficult to biodegradation, and wherein major part is classified as priority pollutant by EPA and European Union environmental protection administration.At present, the improvement of chloride phenols wastewater has been subject to increasing attention.Wherein, zero-valent metal reduction is processed this pollutant because it has cheapness, the advantage such as effective, is subject to extensive concern.
The material that is applied to deoxidization, degradation chlorophenols organic pollution mainly contains zero-valent metal and bimetallic system thereof, and they have good dechlorination effect, can effectively reduce the bio-toxicity of compound, strengthens biodegradability.Studies show that the zero-valent metals such as Zero-valent Iron, zinc, magnesium, copper are applied to the chlorinatedorganic reduction dechlorination, but dechlorination rate is slower, required time is long.The metal that nickel, copper, palladium isoreactivity is not high and iron, zinc etc. form the bimetallic system to be used, and can obviously accelerate the degradation rate of pollutant.In recent years, utilize nano zero valence iron dechlorination organic chloride to be subject to paying close attention to widely, but because the specific area of Nanoscale Iron is larger, be exposed to very easily oxidation in the air, form passivation layer on the surface, thereby reactivity is reduced.At present, adopted multiple bimetallic nano system to overcome this shortcoming, comprising nanometer Pd/Fe, nanometer Ni/Fe, nanometer Cu/Fe etc.But, with cerium oxide (CeO 2) dopen Nano Zero-valent Iron and be used for dechlorination and remove the chlorophenols organic pollution and have no report.
Zero-valent Iron (is used Fe 0Or Fe (0) represents) have certain specific area, electronegativity is very large, electrode potential E 0(Fe 2+/ Fe)=-0.44 V has reducing power, can will arrange in the metal activity series table in thereafter metal replacement out and be deposited on the surface of iron, ion that also can oxidisability is stronger or compound and the reduction of some organic matter thereof.Fe 2+Has reproducibility, E 0(Fe 3+/ Fe 2+)=0.771 V, thereby when having oxidant to exist in the water, Fe 2+Can further be oxidized to Fe 3+, and under certain pH condition, can form the hydroxide of iron, it has the effect of Adsorption and flocculation to the pollutant in the solution.Extraction and nanometer iron metal has the microstructures such as crystal shape and dot matrix arrangement, has larger specific area, higher reactivity and stronger adsorptivity than common Zero-valent Iron, can more effectively remove water pollutant.Cerium oxide (CeO 2) storage oxygen and the function of putting oxygen are arranged, can improve the efficient of catalyst.With CeO 2As catalyst Fe 0Auxiliary agent or the additive of catalyst carrier, can by and transition metal between synergy so that improve catalyst activity, improve that it is selective and increase stability.This novel nanometer Fe 0/ CeO 2Catalyst is the Disciplinary Frontiers of current research, has broad application prospects in underground water and soil remediation and sewage chlorinatedorganic process field.
Summary of the invention
The purpose of this invention is to provide that a kind of catalytic efficiency is high, with low cost, non-secondary pollution, and can remove the organic nanometer Fe of chlorophenols 0/ CeO 2Catalyst.
In order to reach the object of the invention, technical scheme of the present invention is:
Nanometer Fe 0/ CeO 2Composite manufacture method, the method comprise the steps: to adopt liquid-phase precipitation method to prepare nano Ce O 2Particle is then with nano Ce O 2Particle is carrier, adopts coprecipitation synthesis of nano Fe 0/ CeO 2Composite.
Described liquid-phase precipitation method prepares nano Ce O 2The step of particle is as follows: with (NH 4) 2CO 3H 2O solution joins Ce (NO fast as precipitating reagent 3) 36H 2In the O solution, (NH 4) 2CO 3H 2O and Ce (NO 3) 36H 2The molar ratio of O is 3:2, and its reaction principle is 2Ce (NO 3) 36H 2O+3 (NH 4) 2CO 3H 2O → Ce 2(CO 3) 3H 2O+6NH 4NO 3+ 14H 2O; Add simultaneously surfactant polyethylene, the reaction time is 10 ~ 50 min, and reaction temperature is 30 ~ 70 ℃, stirs, and reaction generates presoma; Wash with removal of impurities with deionized water after precursor sol filters, and the presoma that is filtered dry is put into the reaction vessel that absolute ethyl alcohol is housed, disperse to reduce " water bridge " between granular precursor with ultrasonic wave; Filter again, namely obtain nano Ce O after vacuum drying and the roasting 2Particle.
Described coprecipitation prepares nanometer Fe 0/ CeO 2The step of composite is as follows: take by weighing a certain amount of nano Ce O 2Particle places reaction vessel, in order to prepare certain mass than the (Fe of 1:3 ~ 3:1) 0/ CeO 2Composite; In reaction vessel, add certain density FeSO 47H 2O solution stirs and passes into argon gas and makes it to be in anaerobic state; With certain density KBH 4Solution splashes in the reaction vessel, makes its reaction generate nano-iron particle, KBH 4Solution and FeSO 47H 2The volume ratio scope of O solution is 1:1 ~ 2.5:1, and the molar concentration rate scope is 5:1 ~ 8:1, guarantees BH 4 -Excessive, reaction principle is Fe (H 2O) 6 2++ 2BH 4 -→ Fe 0↓+2B (OH) 3+ 7H 2↑; Blast argon gas in the course of reaction and keep reaction to carry out under anaerobic state, the micro-bubble that aeration produces is as the reunion of examining and preventing nano particle of adhering to of iron atom, and maintenance is stirred and made solution be in even admixture, behind reaction 1 ~ 2 h, with synthetic nanometer Fe 0/ CeO 2The particle precipitation namely makes nanometer Fe after washing and the vacuum drying 0/ CeO 2Composite.Above-mentioned reaction vessel can be the four-hole round-bottomed flask.
The nanometer Fe of said method preparation 0/ CeO 2The application of composite in removing chlorophenol pollutant is as follows: with nanometer Fe 0/ CeO 2Composite is catalyst, at O 2Exist lower and the reaction of chlorophenols organic wastewater, with the chlorophenols organic matter removal.
When chlorophenols organic wastewater initial concentration is 50 ~ 100 mg/L, nanometer Fe 0/ CeO 2The optimization consumption of composite is 1.0 ~ 2.0 g/L.
Its key reaction principle is: nano zero valence iron is easy to corrosion in water, and formula 1 is seen in reaction, when having dissolved oxygen in the water, reacts 2, thereby causes the rapid corrosion of iron, and the overall reaction equation is seen formula 3; Nano zero valence iron can directly be transferred to electronics and be adsorbed on ironing surface chlorinated organics (RCl), sees formula 4; Ferrous ion with the chlorinated organics reduction dechlorination, is seen formula 5 as reducing agent; The H that produces in the iron rot process 2Perhaps atom state hydrogen is seen formula 6 and 7 with the chlorinated organics reduction dechlorination; Iron also can produce cotton-shaped Fe (OH) in the corrosion oxidation process 2And Fe (OH) 3Precipitations etc., they all have very strong Coagulation and Adsorption effect, can Adsorption part pollutant.CeO in the catalyst 2Ce 4+Be easy to trapped electrons and form Ce 3+(formula 8), and Ce 4+/ Ce 3+The potential energy level that reduction reaction has is 1.84 eV, can promote Fe 3+Be reduced to Fe 2+(formula 9), thus the catalytic activity of nano zero valence iron improved.
Fe+2H 2O→Fe 2++H 2+2OH - (1)
O 2+2H 2O+4e -→4OH - (2)
2Fe+O 2+2H 2O→2Fe 2++4OH - (3)
Fe 0+RCl+H +→Fe 2++RH+Cl - (4)
2Fe 2++RCl+H +→2Fe 3++RH+Cl - (5)
H 2+RCl→RH+H ++Cl - (6)
[H]+RCl+e -→RH+Cl - (7)
Ce 4++e -→Ce 3+ (8)
Ce 3++Fe 3+→Ce 4++Fe 2+ (9)
Beneficial effect of the present invention is mainly reflected in: the material synthesis technique is simple, equipment requirement is low, cost is low; It is efficiently quick to contain chlorophenols organic wastewater in order to processing, and economically feasible, and non-secondary pollution have broad application prospects in underground water and soil remediation and sewage chlorinatedorganic process field.
The specific embodiment
The invention will be further described below in conjunction with specific embodiment, but protection scope of the present invention is not limited in this:
The present invention is with 2,4-Dichlorophenol, 2,4, and 6-trichlorophenol and pentachlorophenol are representative pollutant, carry out nanometer Fe 0/ CeO 2Remove chlorophenols organic wastewater.
Embodiment 1
Adopt first liquid-phase precipitation method to prepare nano Ce O 2Particle, step is as follows: be (the NH of 0.1 mol/L with concentration 4) 2CO 3H 2O joins the Ce (NO that concentration is 0.1 mol/L fast as precipitating reagent 3) 36H 2O, (NH 4) 2CO 3H 2O solution and Ce (NO 3) 36H 2The volume ratio of O solution is 3:2, adds simultaneously the surfactant polyethylene 4000(PEG 4000 of 4 g/L), the reaction time is 10 min, and reaction temperature is 40 ℃, stirs, and reaction generates presoma; Use the deionized water washed twice with removal of impurities after precursor sol filters, and the presoma that is filtered dry is put into the beaker that absolute ethyl alcohol is housed, disperse 10 min to reduce between granular precursor " water bridge " with ultrasonic wave; Filter again, after the vacuum drying in 300 ℃ air roasting 1 h, obtain nano Ce O 2Particle.
Then with nano Ce O 2Particle is carrier, adopts the synthetic Fe of coprecipitation 0/ CeO 2Catalyst, step is as follows: the nano Ce O that takes by weighing 22 mg 2Particle places the four-hole round-bottomed flask, in order to prepare Fe 0And CeO 2Mass ratio is the Fe of 1:1 0/ CeO 2Composite; Adding concentration in the four-hole round-bottomed flask is the FeSO of 4 mM 47H 2O solution 100 mL stir and pass into argon gas and make it to be in anaerobic state; Be the KBH of 20 mM with concentration 4Solution 100 mL splash in the four-hole round-bottomed flask by control valve, make its reaction generate nano-iron particle; Blast argon gas in the course of reaction and keep reaction to carry out under anaerobic state, the micro-bubble that aeration produces is as the reunion of examining and preventing nano particle of adhering to of iron atom, and maintenance is stirred and made solution be in even admixture.After reacting 1.5 h, with synthetic nanometer Fe 0/ CeO 2The particle precipitation, deionized water and absolute ethyl alcohol respectively wash one time, namely make Fe after the vacuum drying 0And CeO 2Mass ratio is the nanometer Fe of 1:1 0/ CeO 2Composite.
Adopt nanometer Fe 0/ CeO 2Composite is catalyst treatment 2,4-Dichlorophenol waste water, and take conical flask as reactor, the waste water initial concentration is 50 mg/L, pH uncomfortable (pH 6.2) adds 1.0 g/L nanometer Fe 0/ CeO 2Composite, the oxygen content in the uncovered assurance solution of conical flask is saturated, and reactor is placed the water-bath oscillator, and rotating speed is 150 rpm, and temperature is 30 ℃.Result sees Table 1.
Detection method: 2,4-Dichlorophenol adopts high performance liquid chromatograph (Agilent 1200 Series, Agilent, USA) to measure; Chlorion adopts ion chromatograph (DX-100, Dionex, Germany) to measure; The TOC value adopts total organic carbon/total blood urea/nitrogen analyzer (MultiN/C2100TOC/TN, Jena, Germany) to measure.
Table 1 is the result show, adopts nanometer Fe 0/ CeO 2Process 2,4-Dichlorophenol waste water, react 24 h after, the conversion ratio of 2,4-Dichlorophenol, dechlorination rate and TOC clearance are respectively 43.1%, 41.5% and 30.2%.PH increases in the course of reaction, and this is the effect owing to reaction equation 1 ~ 3, and the increase of pH value is conducive to the generation of ferric hydroxide precipitate.
Table 1 nanometer Fe 0/ CeO 2Process 2,4-Dichlorophenol waste water
Figure BDA0000210686071
Embodiment 2
Adopt first liquid-phase precipitation method to prepare nano Ce O 2Particle, step is as follows: be (the NH of 0.1 mol/L with concentration 4) 2CO 3H 2O joins the Ce (NO that concentration is 0.2mol/L fast as precipitating reagent 3) 36H 2O, (NH 4) 2CO 3H 2O solution and Ce (NO 3) 36H 2The volume ratio of O solution is 3:1, adds simultaneously the surfactant polyethylene 4000(PEG 4000 of 4 g/L), the reaction time is 25 min, and reaction temperature is 60 ℃, stirs, and reaction generates presoma; Use the deionized water washed twice with removal of impurities after precursor sol filters, and the presoma that is filtered dry is put into the beaker that absolute ethyl alcohol is housed, disperse 10 min to reduce between granular precursor " water bridge " with ultrasonic wave; Filter again, after the vacuum drying in 300 ℃ air roasting 1 h, obtain nano Ce O 2Particle.
Then with nano Ce O 2Particle is carrier, adopts the synthetic Fe of coprecipitation 0/ CeO 2Catalyst, step is as follows: the nano Ce O that takes by weighing 33.6 mg 2Particle places the four-hole round-bottomed flask, in order to prepare Fe 0And CeO 2Mass ratio is the Fe of 1:2 0/ CeO 2Composite; Adding concentration in the four-hole round-bottomed flask is the FeSO of 3mM 47H 2O solution 100 mL stir and pass into argon gas and make it to be in anaerobic state; Be the KBH of 20mM with concentration 4Solution 200 mL splash in the four-hole round-bottomed flask by control valve, make its reaction generate nano-iron particle; Blast argon gas in the course of reaction and keep reaction to carry out under anaerobic state, the micro-bubble that aeration produces is as the reunion of examining and preventing nano particle of adhering to of iron atom, and maintenance is stirred and made solution be in even admixture.After reacting 2 h, with synthetic nanometer Fe 0/ CeO 2The particle precipitation, deionized water and absolute ethyl alcohol respectively wash one time, namely make nanometer Fe after the vacuum drying 0/ CeO 2Composite.
Adopt above-mentioned nanometer Fe 0/ CeO 2Composite is catalyst treatment pentachlorophenol waste water, and the waste water initial concentration is 100 mg/L, and pH uncomfortable (pH 6.7) adds 2.0 g/L nanometer Fe 0/ CeO 2Compound, the oxygen content in the uncovered assurance solution of conical flask is saturated, and reactor is placed the water-bath oscillator, and rotating speed is 150 rpm, and temperature is 30 ℃.After reacting 30 min, the conversion ratio of pentachlorophenol is 99.1%, dechlorination rate 45.6%, and detection method is with embodiment 1.
Embodiment 3
Nanometer Fe 0/ CeO 2The composite manufacture method is with embodiment 1.
Adopt nanometer Fe 0/ CeO 2Composite is catalyst treatment 2,4, and 6-trichlorophenol waste water, waste water initial concentration are 50 mg/L, and pH uncomfortable (pH 5.9) adds 1.0 g/L nanometer Fe 0/ CeO 2Compound, conical flask is uncovered, and reactor is placed the water-bath oscillator, and rotating speed is 150 rpm, and temperature is 30 ℃.Result sees Table 2:
Table 2 nanometer Fe 0/ CeO 2Process 2,4,6-trichlorophenol waste water
Figure BDA0000210686072
Detection method: with embodiment 1.
Table 2 is the result show, adopts nanometer Fe 0/ CeO 2Process 2,4,6-trichlorophenol waste water, react 24 h after, the conversion ratio of 2,4,6-trichlorophenol, dechlorination rate and TOC clearance are respectively 51.9%, 39.8% and 35.8%.PH increases in the course of reaction, reaches 7.0.
Embodiment 4
Nanometer Fe 0/ CeO 2The composite manufacture method is with embodiment 1.
Adopt nanometer Fe 0/ CeO 2Composite is catalyst treatment pentachlorophenol waste water, and the waste water initial concentration is 50 mg/L, and pH uncomfortable (pH 6.7) adds 1.0 g/L nanometer Fe 0/ CeO 2Compound, conical flask is uncovered, and reactor is placed the water-bath oscillator, and rotating speed is 150 rpm, and temperature is 30 ℃.Result sees Table 3:
Table 3 nanometer Fe 0/ CeO 2Process pentachlorophenol waste water
Figure BDA0000210686073
Detection method: with embodiment 1.
As can be seen from Table 3, nanometer Fe 0/ CeO 2Composite can effectively be removed the pentachlorophenol in the waste water fast, react 24 h after, the conversion ratio of pentachlorophenol is up to 100%, dechlorination rate and TOC clearance are respectively 60.0% and 48.2%.Reaction equation 1 ~ 3 has caused pH increase in the course of reaction, is conducive to generate ferric hydroxide precipitate.
Above-described embodiment shows the nanometer Fe that the present invention prepares 0/ CeO 2Composite can dechlorination be removed the chlorophenols organic matter, need not to add other reagent, has reduced energy consumption, and the wide prospect of marketing is arranged.
The above; only for the better specific embodiment of the present invention, but protection scope of the present invention is not limited to this, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.

Claims (6)

1. nanometer Fe 0/ CeO 2The composite manufacture method is characterized in that:
(1) adopt liquid-phase precipitation method to prepare nano Ce O 2Particle:
With (NH 4) 2CO 3H 2O solution joins Ce (NO 3) 36H 2In the O solution, (NH 4) 2CO 3H 2O and Ce (NO 3) 36H 2The molar ratio of O is 3:2, adds simultaneously surfactant polyethylene, and the reaction time is 10 ~ 50 min, and reaction temperature is 30 ~ 70 ℃, stirs, and reaction generates presoma; Wash with deionized water after precursor sol filters, and the presoma that is filtered dry is put into the reaction vessel that absolute ethyl alcohol is housed, disperse with ultrasonic wave; Filter again, namely obtain nano Ce O after vacuum drying and the roasting 2Particle;
(2) adopt coprecipitation synthesis of nano Fe 0/ CeO 2Composite:
Take by weighing the nano Ce O of step (1) preparation 2Particle places reaction vessel, and adds FeSO in reaction vessel 47H 2O solution stirs and passes into argon gas; With KBH 4Solution splashes in the reaction vessel, makes its reaction generate nano-iron particle, KBH 4Solution and FeSO 47H 2The volume ratio scope of O solution is 1:1 ~ 2.5:1, and the molar concentration rate scope is 5:1 ~ 8:1; Blast argon gas in the course of reaction, and keep stirring, behind reaction 1 ~ 2h, with synthetic nanometer Fe 0/ CeO 2The particle precipitation namely makes nanometer Fe after washing and the vacuum drying 0/ CeO 2Composite.
2. method according to claim 1, it is characterized in that: reaction vessel is the four-hole round-bottomed flask.
3. method according to claim 1 is characterized in that: nanometer Fe 0/ CeO 2Fe in the composite 0And CeO 2Mass ratio be: 1:3 ~ 3:1.
4. the nanometer Fe that makes of the described method of the arbitrary claim of claim 1 to 3 0/ CeO 2The application of composite in removing chlorophenol pollutant is characterized in that: with nanometer Fe 0/ CeO 2Composite is catalyst, at O 2Exist lower and the reaction of chlorophenols organic wastewater, with the chlorophenols organic matter removal.
5. application according to claim 4 is characterized in that: the initial concentration of chlorophenols organic wastewater is 50 ~ 100 mg/L.
6. application according to claim 5 is characterized in that: nanometer Fe 0/ CeO 2The consumption of composite is 1.0 ~ 2.0 g/L.
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