CN104045129B - A kind of preparation method removing the Nanoscale Iron charcoal micro-electrolysis material of nitrate nitrogen - Google Patents
A kind of preparation method removing the Nanoscale Iron charcoal micro-electrolysis material of nitrate nitrogen Download PDFInfo
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- CN104045129B CN104045129B CN201410177681.9A CN201410177681A CN104045129B CN 104045129 B CN104045129 B CN 104045129B CN 201410177681 A CN201410177681 A CN 201410177681A CN 104045129 B CN104045129 B CN 104045129B
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Abstract
The invention discloses a kind of preparation method removing the Nanoscale Iron charcoal micro-electrolysis material of nitrate nitrogen, belong to groundwater pollutant and repair field.The preparation method of this material, for iron trichloride is dissolved in the alcohol solution of 3: 7, constantly stirs, and drips sodium borohydride solution, and then adds gac and polyoxyethylene glycol; Whole process passes into nitrogen, stirs 30 minutes, can obtain nanometer Fe-C micro electrolysis particle.This preparation method is simple to operate, and raw material is easy to get, and utilize the made distribution of material of surfactant polyethylene even, good dispersity, the strong reducing property of combining nano iron and the strong adsorptivity of gac, 100% removes nitrate nitrogen.The present invention, by preparing novel nano Fe-C micro electrolysis material, realizes Nanoscale Iron charcoal micro electrolysis tech to the efficient removal of nitrate nitrogen in underground water, for effective removal of groundwater azotate pollution thing provides technical strategies and method.
Description
Technical field
The invention belongs to groundwater pollution and repair field, particularly relate to the development innovation of sewage treating material in environment protection.
Background technology
Fe-C micro electrolysis refers to: when iron filings and charcoal particle being immersed in acid waste water, due to the difference in Electrode Potential between iron and charcoal, can form numerous micro-galvanic cell in waste water.These trickle batteries become anode with the iron that current potential is low, and the charcoal that current potential is high becomes negative electrode, in containing the aqueous solution of acidic electrolyte bath, electrochemical reaction occurs.In reaction, the Fe of status nascendi of generation
2+with atom H, they have high chemically reactive, can change many organic structure and characteristics in waste water, make the effects such as organism generation chain rupture, open loop.The result of reaction is that iron is corroded the iron ion becoming divalence and enters solution.Because iron ion has coagulation, there is a natural attraction between the sexes for the particulate with faint negative charge in it and pollutent, forms more stable throw out (being also iron mud) and remove.There are some researches show, Fe-C micro electrolysis as coking chemical waste water, waste water from dyestuff, and shows higher efficiency and potentiality in the application of inorganic pollutant nitrate etc. at process organic waste water.
Light electrolysis equipment is all fixed beds both at home and abroad at present, is characterized in that structure is simple, pushes away good fluidity, but there is many practicality problems: one is that efficiency is not high, and speed of response is unhappy; Two is that a body easily hardens, and causes short circuit and dead band.Iron bed is after operation after a while, and filling surface can form passive film, and the suspended particle in waste water also can partly be deposited on filling surface, has so just intercepted filler and has contacted with the effective of waste water, causes iron bed treatment effect to reduce.Hardening except causing the inner waste water fluidised form of iron bed to worsen and causing treatment effect reduction of iron bed fillers, also can make the difficulty of replacement greatly increase.
Nanoscale Iron has great specific surface area, multiple environmental pollutant of not only effectively degrading, and can be retained in suspension for a long time due to their sizes little (generally at 1-100nm), effectively can transmit in groundwater flow.External successful Application permeable reactive barrier (PRB technology) removably being descended to water pollutant technology in recent years, makes to utilize Nanoscale Iron and matrix material thereof to reveal very large potential advantages and application prospect in underground water in-situ immobilization side.
Gac is non-polar adsorbent, energy adsorption selection apolar substance, very little to the adsorptive power of polar material.If carry out oxidation modification to activated carbon granule surface, its adsorptive power to polar material can be strengthened.Function of surface group hydroxyl, hydroxy kind compound, charcoal acyl group etc. can be attached to activated carbon surface and then improve the physico-chemical properties of gac.And the modification of function of surface group can be realized very easily, as surfactant polyethylene etc. by chemical process gac.
In Nanoscale Iron after dopped activated carbon and polyoxyethylene glycol, Nanoscale Iron passivation and easy agglomeration traits can be slowed down to a certain extent.Because the redox potential difference of iron and charcoal is comparatively large, corrosion cell can be formed thus " Inner electrolysis " occurs, produce enough active hydrogens by microelectrode electrolysis and then strengthen its reductibility.The present invention, by preparing novel nano Fe-C micro electrolysis material, realizes Nanoscale Iron charcoal micro electrolysis tech to the efficient removal of nitrate nitrogen in underground water.
Summary of the invention
The object of the invention is for overcoming the deficiencies in the prior art, providing a kind of preparation method of Nanoscale Iron charcoal micro-electrolysis material of efficient removal nitrate nitrogen, the problem effectively can solve the easy passivation of Fe-C micro electrolysis technology, easily hardening.
The present invention is achieved in that a kind of preparation method of Nanoscale Iron charcoal comprises the following steps:
Step one, take 3.5000g iron(ic) chloride with electronic balance, 1.8000g sodium borohydride, 0.4000g sieves 200 object gacs and 0.1000g surfactant polyethylene;
Step 2, measure 140mL deionized water with graduated cylinder, pass into nitrogen, add iron(ic) chloride, be stirred to and dissolve completely, then add 66mL dehydrated alcohol, form alcohol-water mixture, in addition sodium borohydride is dissolved in 10mL deionized water, and regulates pH to equal 10 with dilute solution of sodium hydroxide, for subsequent use;
Step 3, alcohol-water mixture is added in the there-necked flask of 500mL, passes into nitrogen, flask is fixed on electric mixer, start agitator and adjusting rotary speed to 500rpm;
Step 4, peristaltic pump is utilized in there-necked flask, at the uniform velocity to add the sodium borohydride solution of new preparation with 9mL/min speed, reinforced end covers soft rubber ball and prevents air from entering, stir after 10 minutes, in there-necked flask, first add 0.4000g gac, then add surfactant polyethylene;
Step 5, continue stirring after 20 minutes, stop stirring, namely obtained Nanoscale Iron charcoal micro-electrolysis material, collects this material with magnetite, with dehydrated alcohol rinse once, deionized water rinsing three times, then put into vacuum drier, 100 DEG C of dryings were taken out after 1 day.
the advantage that the present invention has and positively effect are:
1, the present invention passes through nanotechnology, change nanometer iron-carbon growing environment in the solution (dripping alkaline sodium borohydride), the growth driving force improving the nucleation probability of nanometer iron-carbon, reduce the critical size of growth cores, improve nanometer iron-carbon, made material particle size little (about 80nm), specific surface area is large, and reductibility is strong;
2, utilize wetting ability and the lipophilicity of surfactant polyethylene, thus improve the dispersiveness of nano particle and must guarantee that the surfactivity of Nanoscale Iron avoids its premature deactivation;
3, after mixing gac, Nanoscale Iron passivation and easy agglomeration traits can be slowed down to a certain extent, because the redox potential difference of iron and charcoal is comparatively large, corrosion cell can be formed thus " Inner electrolysis " occurs, produce enough active hydrogens by microelectrode electrolysis and then strengthen its reductibility;
4, efficiently solve the problem of filling surface passivation in Fe-C micro electrolysis technique, enhance the suspension of filler, improve filler and contact with the effective of nitrate nitrogen;
5, efficiently solve the problem that in Fe-C micro electrolysis technology, filler hardens, improve the processing efficiency to nitrate nitrogen.
Accompanying drawing explanation
Fig. 1 is preparation method's schema of the Nanoscale Iron charcoal that the embodiment of the present invention provides;
Fig. 2 is preparation method's schema of the Nanoscale Iron charcoal micro-electrolysis material removal nitrate nitrogen that the embodiment of the present invention provides;
Fig. 3 is that the Nanoscale Iron charcoal SEM of the preparation that the embodiment of the present invention provides schemes;
Fig. 4 is the Nanoscale Iron charcoal XRD figure of the preparation that the embodiment of the present invention provides;
Nitrate nitrogen graphic representation over time when Fig. 5 is the Nanoscale Iron charcoal of the input different mass that the embodiment of the present invention provides.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Fig. 1 shows preparation method's flow process of Nanoscale Iron charcoal, and as shown in the figure, a kind of preparation method of Nanoscale Iron charcoal comprises the following steps:
S101: take 3.5000g iron trichloride with electronic balance, 1.8000g sodium borohydride, 0.4000g sieves 200 object gacs and 0.1000g surfactant polyethylene;
S102: measure 140mL deionized water with graduated cylinder, pass into nitrogen, add iron trichloride, be stirred to and dissolve completely, then add 66mL dehydrated alcohol, form alcohol-water mixture, in addition sodium borohydride is dissolved in 10mL deionized water, and regulates pH to equal 10 with dilute solution of sodium hydroxide, for subsequent use;
S103: added by alcohol-water mixture in the there-necked flask of 500mL, pass into nitrogen, is fixed on flask on electric mixer, starts agitator adjusting rotary speed to 500rpm;
S104: utilize peristaltic pump at the uniform velocity to add the sodium borohydride solution of new preparation with 9mL/min speed in there-necked flask, reinforced end covers soft rubber ball and prevents air from entering, stir after 10 minutes, in there-necked flask, first add 0.4000g gac, then add surfactant polyethylene;
S105: continue stirring after 20 minutes, stops stirring, and obtained Nanoscale Iron charcoal suspension, collects suspended particle with magnetite, with dehydrated alcohol rinse once, deionized water rinsing three times, then put into vacuum drier, 100 DEG C of dryings were taken out after 1 day.
The step that prepared Nanoscale Iron charcoal micro-electrolysis material removes nitrate nitrogen is as follows:
S201: preparation starting point concentration is the sodium nitrate solution of 60mg/L, respectively getting 200mL joins in 4 anaerobism bottles, 0.1g, 0.2g, 0.5g, 1g, 2g Nanoscale Iron charcoal micro-electrolysis material is added respectively again to anaerobism bottle, deoxygenation seals, put into vibrator vibration, hunting speed is 220rpm, and temperature is 25 DEG C, oscillatory reaction 60min;
S202: from concussion to reaction 2,5,10,15,20,30,40,60min time, get respectively 2mL reaction time sodium nitrate solution, be diluted to 50mL, to be measured;
S203: by the concentration of the sodium nitrate solution of UV-spectrophotometry determination step two, with the quartz colorimetric utensil of 1cm, place measures its absorbancy at 220nm and 275nm wavelength; In different time sampling, detection by quantitative Nanoscale Iron charcoal micro-electrolysis material removes the process of nitrate nitrogen.
The present invention, by preparing novel nano Fe-C micro electrolysis material, realizes Nanoscale Iron charcoal micro electrolysis tech to the efficient removal of nitrate nitrogen in underground water, for effective removal of groundwater azotate pollution thing provides technical strategies and method.
By reference to the accompanying drawings the specific embodiment of the present invention is described although above-mentioned; but not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various amendment or distortion that performing creative labour can make still within protection scope of the present invention.
Claims (2)
1. remove a preparation method for the Nanoscale Iron charcoal micro-electrolysis material of nitrate nitrogen, it is characterized in that, the preparation method of described Nanoscale Iron charcoal micro-electrolysis material comprises the following steps:
Step one, take 3.5000g iron trichloride with electronic balance, 1.8000g sodium borohydride, 0.4000g sieves 200 object gacs and 0.1000g surfactant polyethylene;
Step 2, measure 140mL deionized water with graduated cylinder, pass into nitrogen, add iron trichloride, be stirred to and dissolve completely, then add 66mL dehydrated alcohol, form alcohol-water mixture, in addition sodium borohydride is dissolved in 10mL deionized water, and regulates pH to equal 10 with dilute solution of sodium hydroxide, for subsequent use;
Step 3, alcohol-water mixture is added in the there-necked flask of 500mL, passes into nitrogen, flask is fixed on electric mixer, start agitator and adjusting rotary speed to 500rpm;
Step 4, peristaltic pump is utilized in there-necked flask, at the uniform velocity to add the sodium borohydride solution of new preparation with 9mL/min speed, reinforced end covers soft rubber ball and prevents air from entering, stir after 10 minutes, in there-necked flask, first add 0.4000g gac, then add surfactant polyethylene;
Step 5, continue stirring after 20 minutes, stop stirring, obtained Nanoscale Iron charcoal suspension, collects suspended particle with magnetite, with dehydrated alcohol rinse once, deionized water rinsing three times, then put into vacuum drier, 100 DEG C of dryings were taken out after 1 day.
2. the preparation method of the Nanoscale Iron charcoal micro-electrolysis material of removal nitrate nitrogen according to claim 1, is characterized in that, the experimental procedure removing nitrate nitrogen is as follows:
Step one, preparation starting point concentration are the sodium nitrate solution of 60mg/L, respectively getting 200mL joins in 5 anaerobism bottles, 0.1g, 0.2g, 0.5g, 1g, 2g Nanoscale Iron charcoal micro-electrolysis material is added respectively again to anaerobism bottle, deoxygenation seals, put into vibrator vibration, hunting speed is 220rpm, and temperature is 25 DEG C, oscillatory reaction 60min;
Step 2, from concussion to reaction 2,5,10,15,20,30,40,60min time, get respectively 2mL reaction time sodium nitrate solution, be diluted to 50mL, to be measured;
The concentration of the sodium nitrate solution of step 3, use UV-spectrophotometry determination step two, with the quartz colorimetric utensil of 1cm, at 220nm and 275nm wavelength, place measures its absorbancy; In different time sampling, detection by quantitative Nanoscale Iron charcoal micro-electrolysis material removes the process of nitrate nitrogen.
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| CN105236518B (en) * | 2015-07-02 | 2018-03-23 | 北京农业职业学院 | A kind of method of organic pollution in magnetic field-intensification iron-carbon micro-electrolysis processing percolate |
| CN105399199A (en) * | 2015-12-23 | 2016-03-16 | 成都理工大学 | Preparation method of biosurfactants-modified nano-iron/carbon composite material and application in removing nitrate nitrogen in underground water |
| CN111362396A (en) * | 2020-03-12 | 2020-07-03 | 哈尔滨工业大学 | Preparation method and application of polyurethane composite carrier self-generating functional material for in-situ enhanced biological dehalogenation of underground water |
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