CN101966445A - Magnetism-based nanocomposite for simultaneously removing arsenic and fluorine and application method thereof - Google Patents
Magnetism-based nanocomposite for simultaneously removing arsenic and fluorine and application method thereof Download PDFInfo
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- CN101966445A CN101966445A CN 201010266711 CN201010266711A CN101966445A CN 101966445 A CN101966445 A CN 101966445A CN 201010266711 CN201010266711 CN 201010266711 CN 201010266711 A CN201010266711 A CN 201010266711A CN 101966445 A CN101966445 A CN 101966445A
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Abstract
The invention relates to a magnetism-based nanocomposite for simultaneously removing arsenic and fluorine. A preparation method comprises the following steps of: adding 80 to 120mL of deionized water under the protection of nitrogen; putting the mixture into a constant temperature water-bath pot at the temperature of between 85 and 95 DEG C under the condition of mechanical agitation; dropwise adding 1 to 3 mol/L NaOH until the solution turns into bright black; continuously stirring the solution to react for 2 to 3 hours; performing additional magnetic field separation to obtain magnetic Fe3O4; depositing the magnetic Fe3O4 in 100 to 200mL of deionized water in a sealing way; mixing 10 to 30mL of magnetic Fe3O4 suspension solution and 100 to 200mL of 1 to 2mol/L ZrOCl2.8H2O; dropwise adding 1 to 3 mol/L NaOH until the solution turns from the black to dark yellow; continuously stirring the solution to react for 2 to 3 hours; and performing the additional magnetic field separation to obtain the magnetic nanocomposite which is represented by Fe3O4@ZrO(OH)2. The preparation method has the advantages of achieving continuous reaction and continuous water outlet, reusing desorbed adsorbing materials and saving cost and time by operating cycle. The desorbed adsorbing materials can be recycled from a recycling outlet in a regeneration tank when the adsorbing performance is too low.
Description
Technical field
The present invention relates to a kind of based on magnetic nanometer composite material and processing method thereof, relate in particular to a kind of remove simultaneously arsenic and fluorine based on magnetic nanometer composite material and application process thereof.
Background technology
Drinking water arsenic fluoride pollution is the water quality safety problem that the whole world generally faces.The report of relevant arsenic fluorine poisoning incident emerges in an endless stream especially in recent years.Fluorine poisoning is a kind of systemic disease, especially tooth and bone is had bigger harm, and arsenic then is carcinogenic, teratogenesis, mutagenic arch-criminal.May raise greatly because of the two collaborative poisonous effect makes the arsenic fluorine poisoning incidence of disease when reporting the coexistence of arsenic fluorine.The phenomenon that coexistence of High Concentration of Arsenic fluorine water and arsenic fluorine are united poisoning all has report in areas such as Xinjiang of China, Shanxi, the Inner Mongol, Guizhou, high-fluorine water mainly is distributed in North China, northwest, northeast and area, the Yellow River and Huai He River sea plain, some villages and small towns arsenic fluorine concentration even respectively up to 0.2mg/L with more than the 3.5mg/L.The content of arsenic fluorine can not be lower than 0.01mg/L and 1mg/L respectively in China's drinking water sanitary standard (GB 5749-2006) regulation drinking water.Therefore, imperative to the removal of arsenic fluorine in the drinking water.
Arsenic fluorine removal method is that the emphasis of whole world research also is a difficult point in the drinking water.The effective ways of also not removing simultaneously about the arsenic fluorine are both at home and abroad reported at present.Removal method to single arsenic or fluorine in the solution is then similar, mainly contains: coagulant sedimentation, ion-exchange, membrane separation process, bioanalysis and absorption method etc.Wherein absorption method since its have simple to operate, economic environmental protection, advantage such as of a great variety enjoys people to pay close attention to.Use more arsenic removal defluorination absorbing material in recent years and mainly contain rare earth element (laterite, imvite, clay material etc.), iron aluminium and compound (Zero-valent Iron, iron oxide, aluminium hydroxide etc.) thereof, active material (active carbon, activated zeolite, activated aluminum etc.), material modified (modified manganese dioxide, changed red mud etc.), composite (ferrimanganic composite, iron compound and aluminium compound compound etc.) etc.Although above-mentioned sorbing material has advantages such as synthetic easy, with low cost, it causes the expensive energy and time of domestic and international researcher to remove to seek the bigger adsorbent of adsorption capacity because of the low shortcoming of ubiquity adsorption capacity.Nano material (nano titanium oxide, nano zirconium dioxide, nano silicon etc.) is exactly to enter the people visual field in this case, because of it has the very characteristics of bigger serface, so its adsorption capacity is also much larger than other traditional adsorbent.Blemish in an otherwise perfect thing be that it also has simultaneously separable programming complexity, recycling difficulty, is difficult to reach to As in the water (III), As (V) and fluorine shortcoming such as removal effect simultaneously.More up to the present, have simultaneously that adsorption capacity is big, separating rate is fast, the recycling number of times is good and the adsorbent report at home and abroad that can be simultaneously can both remove arsenic in the water and fluorine does not almost have.In addition, in the water treatment technology of reality, mainly contain with adsorption particle and fill out the fixed bed device of post and utilize liquid to continue to flow the momentum that movable property gives birth to and make adsorption particle be in the fluidized bed plant of suspended motion state.Unfortunately these two kinds all have a bigger shortcoming, and that is to reach saturated adsorption particle recycling complicated operation, and cost is also higher relatively, and reach the process of changing post after saturated in absorption and waste time and energy, and can't allow reaction process carry out continuously.
Summary of the invention
The object of the present invention is to provide a kind of remove simultaneously arsenic and fluorine based on magnetic nanometer composite material and processing method thereof, this magnetic nanometer composite material is a carrier with the magnetic Nano adsorbent, and at the hydroxide of its surperficial embedding one deck transition metal, the synthetic composite that has magnetic and nanometer performance simultaneously; With this magnetic nanometer composite material underground water such as the high arsenic of high fluorine, the low fluorine of high arsenic, the low high fluorine of arsenic are handled absorption.
The present invention be achieved in that a kind of remove simultaneously arsenic and fluorine based on magnetic nanometer composite material, its preparation method is: the FeCl that takes by weighing mol ratio Fe (III): Fe (II)=2: 1
36H
2O and FeSO
47H
2O adds the 80-120mL deionized water under protection of nitrogen gas, put it under churned mechanically condition in 85-95 ℃ the thermostat water bath; the NaOH that dropwise adds 1-3mol/L; till solution becomes bright black, continued stirring reaction 2-3 hour, utilize externally-applied magnetic field to separate and can obtain magnetic Fe
3O
4, sealing is deposited in the 100-200mL deionized water, with magnetic Fe
3O
4The ZrOCl of aaerosol solution 10-30mL and 1-2mol/L
28H
2O 100-200mL mixes, and dropwise adds the NaOH of 1-3mol/L, till solution becomes buff by black, continues stirring reaction 2-3 hour, utilizes externally-applied magnetic field to separate and can obtain magnetic nanometer composite material, uses Fe
3O
4@ZrO (OH)
2Expression.
Based on the synthetic magnetic composite of the hydroxide of magnetic nanometer composite material surface embedding one deck transition elements (as: cerium, iron, manganese, titanium etc.), also has efficient, easily separated, as to remove arsenic and fluorine simultaneously performance.
Transition elements is cerium, iron, manganese or titanium.
A kind of application process step based on magnetic nanometer composite material of removing arsenic and fluorine simultaneously is:
1) contain arsenic fluorine underground water and regulate pH5-7 by regulating reservoir earlier, temperature 23-28 ℃ is that the speed of 1-3L/min enters reaction tank i then with the flow velocity, adds magnetic nanometer composite material Fe
3O
4@ZrO (OH)
2Arsenic fluorine waste water is carried out adsorption treatment;
2) close the into valve of reaction tank i behind the adsorption reaction 5-15min, open alternating magnetic field, waste water is fully contacted with magnetic nanometer composite material, reaction 20-40min reaches adsorption equilibrium, and changing into alternating magnetic field in the same way after the balance, electromagnetic field carries out Magnetic Isolation 4-6min;
3) then with the speed inflow sterilization pool of liquid with 0.6-0.8L/min, after liquid has flowed, solid then is transported to regenerated reactor and carries out desorption and regeneration, about 5-15min of shipping time, regenerated liquid is selected the NaOH of 1-3mol/L, Vltrasonic device and the alternating magnetic field established in opening in the regenerated reactor during regeneration, the recovery time is 30-50min;
4) magnetic nanometer composite material that regeneration is good is stored in the different dividing plates of regenerated reactor with the form of suspension, then be extracted in the reaction tank when needing and react with pump, required time is about 5-10min, after opening reaction tank i valve 20-40min, open reaction tank ii valve, carry out in the identical operations mode, like this, when liquid is about to drain in the reaction tank i, reached solid-liquid in the reaction tank ii and thoroughly separated, the valve of opening between reaction tank ii and the sterilization pool just can be realized continuous effluent, and this moment, also carrying out adsorption reaction in the reaction tank i, also can control carrying out continuously of reaction by the valve between conditioned reaction pond and the sterilization pool;
5) finally record behind sterilization pool, contain arsenic and fluorine in the water outlet content respectively less than 0.01mg/L and 1mg/L, reached China's drinking water sanitary standard (GB 5749-2006), can be used as safe drinking water.
Advantage of the present invention is: this operation cycle is reciprocal, not only realizes the successive reaction continuous effluent, and the sorbing material after the desorb also realized utilizing again, and has saved cost and has also saved the time; When absorption property after the desorbed of adsorbed materials is too low, by reclaiming the outlet recycling in the regenerated reactor.
The specific embodiment
Embodiment 1:
Preparation water inlet As (III), each 10mg/L of As (V), F-are the mixing arsenic fluorine solution 20L of the 20mg/L regulating reservoir of flowing through, and with HCl and the NaOH of 0.5mol/L pH value of solution are adjusted to 7.With the arsenic fluorine solution that mixes up is in the speed feeding reaction tank i of 2L/min with the flow velocity, closes the valve between regulating reservoir and the reaction tank i behind the 10min.Adding 40mL concentration is the magnetic Nano Fe of 10g/mL
3O
4@ZrO (OH)
2Aaerosol solution is opened the alternating electromagnetic field reaction, and temperature is adjusted to 25 ℃, and changing into alternating magnetic field 1 in the same way behind the reaction 30min, electromagnetic field carries out Magnetic Isolation 5min.Liquid flows into sterilization pool with the speed of 0.68L/min then, and after liquid exhausted, solid then was transported to regenerated reactor and carries out desorption and regeneration, shipping time 10min.NaOH with 2mol/L in the regenerated reactor carries out desorption and regeneration to reaching the saturated adsorbent of absorption, opens automatic stirrer and ultrasonic facility simultaneously, fully reacts (10+10) min, and externally-applied magnetic field is washed till neutrality with ultra-pure water again with Separation of Solid and Liquid 10min.Adsorbent after regenerated reactor regeneration still is stored in to 10g/mL in the dividing plate of regenerated reactor with the ultra-pure water constant volume, is evacuated in the reaction tank required time 8min when needing with pump.After opening reaction tank i valve 30min, open valve that regulating reservoir and reaction tank ii connect and carry out adsorption reaction (condition and reaction tank i interior identical).Liquid behind sterilization pool is measured the content of remaining total arsenic and fluorine in the solution respectively with atomic fluorescence spectrophotometer and fluoride ion selective electrode, the content that records in the solution total arsenic and fluorine is lower than 0.008mg/L and 0.76mg/L respectively, and clearance is respectively 99.96% and 96.2%.Be lower than the relevant regulations of China's drinking water sanitary standard (GB5749-2006).Carry out adsorption reaction in the sorbing material suction reaction tank after the regeneration, the result shows that the adsorbent after regeneration is handled still can be reduced to 0.01mg/L to the content of total arsenic and fluorine in the solution respectively and below the 1mg/L.This adsorbent recycling performance can reach 4-5 time.
Embodiment 2:
Preparation water inlet As (III), each 10mg/L of As (V) respectively, F-are the low fluorine solution 20L of the high arsenic of the mixing of the 3mg/L sterilization pool of flowing through, and with HCl and the NaOH of 0.5mol/L pH value of solution are adjusted to 7.With the arsenic fluorine solution that mixes up is in the speed feeding reaction tank i of 2L/min with the flow velocity, closes the valve between regulating reservoir and the reaction tank i behind the 10min.Adding 40mL concentration is the magnetic Nano Fe of 10g/mL
3O
4@ZrO (OH)
2Aaerosol solution is opened the alternating electromagnetic field reaction, and temperature is adjusted to 25 ℃, and changing into alternating magnetic field 1 in the same way behind the reaction 30min, electromagnetic field carries out Magnetic Isolation 5min.Liquid flows into sterilization pool with the speed of 0.68L/min then, and after liquid exhausted, solid then was transported to regenerated reactor and carries out desorption and regeneration, shipping time 10min.NaOH with 2mol/L in the regenerated reactor carries out desorption and regeneration to reaching the saturated adsorbent of absorption, opens automatic stirrer and ultrasonic facility simultaneously, fully reacts (10+10) min, and externally-applied magnetic field is washed till neutrality with ultra-pure water again with Separation of Solid and Liquid 10min.Adsorbent after regenerated reactor regeneration still is stored in to 10g/mL in the dividing plate of regenerated reactor with the ultra-pure water constant volume, is evacuated in the reaction tank required time 8min when needing with pump.After opening reaction tank i valve 30min, open valve that regulating reservoir and reaction tank ii connect and carry out adsorption reaction (condition and reaction tank i interior identical).Liquid behind sterilization pool is measured the content of remaining total arsenic and fluorine in the solution respectively with atomic fluorescence spectrophotometer and fluoride ion selective electrode, the content that records in the solution total arsenic and fluorine is lower than 0.0073mg/L and 0.54mg/L respectively, and clearance is respectively 99.96% and 82%.Be lower than the relevant regulations of China's drinking water sanitary standard (GB 5749-2006).Carry out adsorption reaction in the sorbing material suction reaction tank after the regeneration, the result shows that the adsorbent after regeneration is handled still can be reduced to 0.01mg/L to the content of total arsenic and fluorine in the solution respectively and below the 1mg/L.
Embodiment 3:
Preparation water inlet As (III), each 1mg/L of As (V) respectively, F-are the mixing arsenic fluorine solution 20L of the 20mg/L regulating reservoir of flowing through, and with HCl and the NaOH of 0.5mol/L pH value of solution are adjusted to 7.With the arsenic fluorine solution that mixes up is in the speed feeding reaction tank i of 2L/min with the flow velocity, closes the valve between regulating reservoir and the reaction tank i behind the 10min.Adding 40mL concentration is the magnetic Nano Fe of 10g/mL
3O
4@ZrO (OH)
2Aaerosol solution is opened the alternating electromagnetic field reaction, and temperature is adjusted to 25 ℃, and changing into alternating magnetic field 1 in the same way behind the reaction 30min, electromagnetic field carries out Magnetic Isolation 5min.Liquid flows into sterilization pool with the speed of 0.68L/min then, and after liquid exhausted, solid then was transported to regenerated reactor and carries out desorption and regeneration, shipping time 10min.NaOH with 2mol/L in the regenerated reactor carries out desorption and regeneration to reaching the saturated adsorbent of absorption, opens automatic stirrer and ultrasonic facility simultaneously, fully reacts (10+10) min, and externally-applied magnetic field is washed till neutrality with ultra-pure water again with Separation of Solid and Liquid 10min.Adsorbent after regenerated reactor regeneration still is stored in to 10g/mL in the dividing plate of regenerated reactor with the ultra-pure water constant volume, is evacuated in the reaction tank required time 8min when needing with pump.After opening reaction tank i valve 30min, open valve that regulating reservoir and reaction tank ii connect and carry out adsorption reaction (condition and reaction tank i interior identical).Liquid behind sterilization pool is measured the content of remaining total arsenic and fluorine in the solution respectively with atomic fluorescence spectrophotometer and fluoride ion selective electrode, the content that records in the solution total arsenic and fluorine is lower than 0.056mg/L and 0.72mg/L respectively, and clearance is respectively 99.72% and 96.4%.Be lower than the relevant regulations of China's drinking water sanitary standard (GB 5749-2006).Carry out adsorption reaction in the sorbing material suction reaction tank after the regeneration, the result shows that the adsorbent after regeneration is handled still can be reduced to 0.01mg/L to the content of total arsenic and fluorine in the solution respectively and below the 1mg/L.
Claims (4)
- One kind remove simultaneously arsenic and fluorine based on magnetic nanometer composite material, it is characterized in that the preparation method is: the FeCl that takes by weighing mol ratio Fe (III): Fe (II)=2: 1 36H 2O and FeSO 47H 2O adds the 80-120mL deionized water under protection of nitrogen gas, put it under churned mechanically condition in 85-95 ℃ the thermostat water bath; the NaOH that dropwise adds 1-3mol/L; till solution becomes bright black, continued stirring reaction 2-3 hour, utilize externally-applied magnetic field to separate and can obtain magnetic Fe 3O 4, sealing is deposited in the 100-200mL deionized water, with magnetic Fe 3O 4The ZrOCl of aaerosol solution 10-30mL and 1-2mol/L 28H 2O100-200mL mixes, and dropwise adds the NaOH of 1-3mol/L, till solution becomes buff by black, continues stirring reaction 2-3 hour, utilizes externally-applied magnetic field to separate and can obtain magnetic nanometer composite material, uses Fe 3O 4@ZrO (OH) 2Expression.
- 2. according to claim 1 remove simultaneously arsenic and fluorine based on magnetic nanometer composite material, it is characterized in that also having efficient, easily separated, as to remove arsenic and fluorine simultaneously performance at the synthetic magnetic composite of hydroxide based on magnetic nanometer composite material surface embedding one deck transition elements.
- 3. according to claim 2 remove simultaneously arsenic and fluorine based on magnetic nanometer composite material, it is characterized in that transition elements is cerium, iron, manganese or titanium.
- 4. described a kind of application process based on magnetic nanometer composite material of removing arsenic and fluorine simultaneously of claim 1 is characterized in that step is:1) contain arsenic fluorine underground water and regulate pH5-7 by regulating reservoir earlier, temperature 23-28 ℃ is that the speed of 1-3L/min enters reaction tank i then with the flow velocity, adds magnetic nanometer composite material Fe 3O 4@ZrO (OH) 2Arsenic fluorine waste water is carried out adsorption treatment;2) close the into valve of reaction tank i behind the adsorption reaction 5-15min, open alternating magnetic field, waste water is fully contacted with magnetic nanometer composite material, reaction 20-40min reaches adsorption equilibrium, and changing into alternating magnetic field in the same way after the balance, electromagnetic field carries out Magnetic Isolation 4-6min;3) then with the speed inflow sterilization pool of liquid with 0.6-0.8L/min, after liquid has flowed, solid then is transported to regenerated reactor and carries out desorption and regeneration, about 5-15min of shipping time, regenerated liquid is selected the NaOH of 1-3mol/L, Vltrasonic device and the alternating magnetic field established in opening in the regenerated reactor during regeneration, the recovery time is 30-50min;4) magnetic nanometer composite material that regeneration is good is stored in the different dividing plates of regenerated reactor with the form of suspension, then be extracted in the reaction tank when needing and react with pump, required time is about 5-10min, after opening reaction tank i valve 20-40min, open reaction tank ii valve, carry out in the identical operations mode, like this, when liquid is about to drain in the reaction tank i, reached solid-liquid in the reaction tank ii and thoroughly separated, the valve of opening between reaction tank ii and the sterilization pool just can be realized continuous effluent, and this moment, also carrying out adsorption reaction in the reaction tank i, also can control carrying out continuously of reaction by the valve between conditioned reaction pond and the sterilization pool;5) finally record behind sterilization pool, contain arsenic and fluorine in the water outlet content respectively less than 0.01mg/L and 1mg/L, reached China's drinking water sanitary standard (GB 5749-2006), can be used as safe drinking water.
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| CN103601862B (en) * | 2013-11-18 | 2016-01-13 | 南昌航空大学 | Method using macrocyclic polyether class alkene as function monomer surface aggregate legal system for magnetic lithium ion trace microballoon |
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| CN104148004B (en) * | 2014-09-01 | 2016-08-17 | 南昌航空大学 | A kind of magnetic fluorine ion absorber and preparation method thereof |
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