CN106166474B - A kind of specific regulatory control nano zero valence iron corrosion product and the method for reinforcing nano zero valence iron adsorption of Low Concentration arsenic - Google Patents
A kind of specific regulatory control nano zero valence iron corrosion product and the method for reinforcing nano zero valence iron adsorption of Low Concentration arsenic Download PDFInfo
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- CN106166474B CN106166474B CN201610678897.2A CN201610678897A CN106166474B CN 106166474 B CN106166474 B CN 106166474B CN 201610678897 A CN201610678897 A CN 201610678897A CN 106166474 B CN106166474 B CN 106166474B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
Abstract
The invention discloses a kind of specific regulatory control nano zero valence iron corrosion product and reinforce the method for nano zero valence iron adsorption of Low Concentration arsenic.NZVI@Mg (OH) is made by the way that nano zero valence iron is carried on magnesium hydroxide surface in this method2Composite material, reaches the regulation of nano zero valence iron corrosion product, while enhancing absorption of the nano zero valence iron to low-concentration arsenic.The method of the present invention is simple to operation, and raw material sources are extensive, low in cost.NZVI@Mg (OH) obtained2Composite material sufficiently amplifies single nZVI or Mg (OH)2As in water body (V) concentration effectively can be down to drinking water standard, also have higher adsorption capacity to As (V) by the advantages of material.
Description
Technical field
The invention belongs to the arsenic adsorption technology field in wastewater treatment, it is related to through load nano zero valence iron to magnesium hydroxide
Surface generates and enhances the method that nano zero valence iron adsorbs low-concentration arsenic to control nano zero valence iron corrosion product.
Background technique
Arsenic is that a kind of element being widely present, inorganic compound have severe toxicity in nature.Arsenic acid is because of and phosphoric acid molecules
Model is similar, can inhibit phosphatic oxidation, to block the main energy metabolism system of life entity.Long Term Contact or
It is exposed to cause the multiple organs of human body and lesion tissue or carcinogenic in containing the exceeded environment of arsenic.Drinking water is asked containing arsenic is exceeded
Topic worldwide influences extensively, Bangladesh, Chile, China, Hungary, India, Mexico, Rome Leah, Vietnam, beauty
Successively there is the different degrees of drinking water report exceeded containing arsenic in the countries and regions such as state.In addition, it is worth noting that, underground water
The pollution of arsenic is a kind of typical low concentration pollution problem, and most countries underground water arsenic concentration is all in 0 ~ 5200 μ g/L range
It is interior.In order to reduce harm of the arsenic to human health, in 1993, drinking water standard was lowered to containing arsenic concentration by 50 μ g/L by WHO
10 μg/L。
Currently, the removal most common method of arsenic in water body is absorption method.Nano zero valence iron (nZVI) because its bigger serface,
High reaction activity, to arsenic high-adsorption-capacity and easy Magnetic Isolation the features such as and by pro-gaze, become wide in removing arsenic in water research
For the material of concern.Stable nZVI specific grain surface product can reach 40m2/ g or more, reaction rate is than micron Zero-valent Iron ZVI high
1000 times or more, maximum adsorption capacity is that 3.5mg/g(initial concentration is 1mg/L-1).However nZVI because it is easy to reunite, unstable with
And intensity difference and be subject to certain restrictions its adsorption capacity.In order to overcome these limitations, nZVI is loaded to other porous materials
Material, such as active carbon, chitosan-carboxymethyl β-cyclodextrin, chitosan nano microballoon and montmorillonite.So
And the research about NZVI composite material arsenic removal performance, the adsorption capacity for improving composite material is had focused largely on, is often but ignored
Water quality requirement after actual environmental problem or processing.Processing water body is significantly larger than actual concentrations in environment containing arsenic concentration,
WHO drinking water standard is not achieved in adsorption equilibrium concentration.In addition, nZVI is easily corroded in aerobic environment, corrosion product
Including magnetic iron ore/maghemite and lepidocrocite.Studies have shown that it is red that As (V) is preferentially adsorbed on magnetic iron ore/magnetic compared with lepidocrocite
Iron ore surface.If can change the reaction condition of nZVI, control its corrosion product for reaching specificity is changed into the red iron of magnetic iron ore/magnetic
Mine can then enhance nZVI to the adsorption capacity of As (V).However but have no the research report of this respect.
Summary of the invention
It is an object of that present invention to provide a kind of specific regulatory control nano zero valence iron corrosion product and reinforce nano zero valence iron suction
The method of attached low-concentration arsenic.The present invention is by being loaded to magnesium hydroxide surface for nano zero valence iron to regulate and control nano zero-valence iron rot
The generation of product, while enhancing absorption of the nano zero valence iron to low-concentration arsenic above-mentioned is asked with solve in the presence of the prior art
Topic.
For achieving the above object, the technical solution adopted by the present invention is as follows.
A kind of specific regulatory control nano zero valence iron corrosion product and the method for reinforcing nano zero valence iron adsorption of Low Concentration arsenic, packet
Include following steps:
(1) Mg (OH) is configured2Suspension: by Mg (OH)2It is dissolved in dehydrated alcohol, ultrasonic disperse obtains Mg (OH)2Suspension；
(2) Fe is configured2SO4Solution: by Fe2SO4∙7H2O is dissolved in deionized water, obtains Fe2SO4Solution；
(3) NaBH is configured4Solution: by NaBH4Solid is dissolved in deionized water, obtains NaBH4Solution；
(4) Mg (OH) is taken2Suspension is placed in three-necked flask, keeps mechanical stirring, is passed through inert gas insulation blocking, is added
Fe2SO4Solution, and NaBH is added dropwise with the speed of 3mL/min immediately4Solution；
(5) after being added dropwise to complete, it is centrifugally separating to obtain black solid, is washed, is dried to get nZVI@Mg (OH) is arrived2It is compound
Material；
(6) it takes As (V) solution in vial at room temperature, adjusts PH with HCl solution and NaOH solution, be added step (5)
NZVI@Mg (OH) obtained2Composite material is placed in constant temperature oscillator and at the uniform velocity vibrates, and solid-liquid sample, test are separated after oscillation
As (V) content in solution.
Further, in step (1), the time of the ultrasonic disperse is 5min.
Further, the Mg (OH)2The concentration of suspension is 0.1mol/L.
Further, the Fe2SO4The concentration of solution is 0.1mol/L.
Further, the NaBH4The concentration of solution is 0.25mol/L.
Further, churned mechanically rate described in step (4) is 300 r/min, and mechanical stirring is kept to NaBH4It is molten
Liquid completion of dropwise addition.
Further, inert gas described in step (4) includes nitrogen or argon gas.
Further, in step (4), the molar ratio of reactant additive amount is Mg (OH)2: Fe2SO4: NaBH4 =1:1:2。
Further, in step (5), the washing refers to successively is cleaned 3 times with dehydrated alcohol and deionized water.
Further, in step (5), the drying is the lower 45 DEG C of dryings of vacuum.
Further, in step (6), the concentration of As (V) solution is 1 ~ 8 mg/L.
Further, in step (6), the concentration of the HCl solution and NaOH solution is 0.1 mol/L.
Further, in step (6), the value of the pH is 7.0 ± 0.25.
Further, in step (6), the nZVI@Mg (OH)2The additive amount of composite material is 0.1 g/L.
Further, in step (6), hunting speed is 200 r/min, and duration of oscillation is 6 h.
Mechanism of the invention is: nZVI is loaded to Mg (OH)2Process use liquid phase reduction, nZVI is in aerobic environment
In be easily corroded, corrosion product includes magnetic iron ore/maghemite and lepidocrocite.Studies have shown that compared with lepidocrocite, As (V)
It is preferentially adsorbed on magnetic iron ore/maghemite surface.The corrosion product of nano zero valence iron in the solution is mainly lepidocrocite, is also contained
A small amount of magnetic iron ore/maghemite.And after nano zero valence iron is loaded to magnesium hydroxide surface, since magnesium hydroxide is slightly soluble in water,
In nano zero valence iron corrosion process, magnesium hydroxide releases OH as a kind of solid base, continuous dissolution-, to make nanometer
Magnetic iron ore/maghemite content increases in the corrosion product of Zero-valent Iron, and the content of lepidocrocite is reduced.And magnetic iron ore/magnetic is red
Iron ore is better than lepidocrocite to the adsorption capacity of arsenic, so that nano zero valence iron enhances the adsorption capacity of arsenic.If can change
The reaction condition of nZVI and As (V) solution, control its corrosion product for reaching specificity are changed into magnetic iron ore/maghemite, from
And enhance nZVI to the adsorption capacity of As (V).
It is shown experimentally that, Mg (OH)2As in water body (V) concentration can be down to drinking water standard, but adsorption capacity is small；
NZVI is big to As (V) adsorption capacity, but the As (V) in solution can not be effectively reduced in low concentration；Prepared by nZVI@
Mg(OH)2Composite material then combines the advantages of the two, As in water body (V) concentration effectively can be down to drinking water standard, right
As (V) also has higher adsorption capacity.
Compared with prior art, the invention has the advantages that and technical effect:
(1) the method for the present invention is simple, easy to operate, easily controllable under room temperature；
(2) raw material sources of the present invention are extensive, low in cost；
(3) the advantages of sufficiently amplifying homogenous material, makes to make the best use of everything, obtained nZVI@Mg (OH)2Composite material can be both
As in water body (V) concentration effectively can be down to drinking water standard, also have higher adsorption capacity to As (V).
Detailed description of the invention
Fig. 1 is nZVI@Mg (OH) obtained2Equilibrium concentration compares after composite material and homogenous material processing low-concentration arsenic.
Specific embodiment
The invention will be further described combined with specific embodiments below, but protection scope of the present invention is not only limited to reality
Apply example.
Mg(OH)2It is synthesized by chemical precipitation method: under room temperature, the NaOH aqueous solution of 1M being added dropwise in equal volume dropwise
0.5M MgSO4In solution, it is added dropwise and is vigorously stirred simultaneously with the speed of 300 r/min, wherein MgSO4Solution passes through dissolution
MgSO4∙7H2It is obtained in the glycerol aqueous solvent of O to 85wt%.After being added dropwise to complete, continuing to stir 6h, standing is centrifugated afterwards for 24 hours,
It is successively cleaned 3 times with deionized water and dehydrated alcohol, 45 DEG C of dryings are spare.
Arsenic removal experiment carries out in 25ml vial: take As (V) solution that 20ml concentration is 1 ~ 8 mg/L in vial,
PH to 7.0 ± 0.25 is adjusted with 0.1 M HCl solution and 0.1M NaOH solution, nZVI@Mg made from 0.1 g/L is added
(OH)2Composite material is placed in constant temperature oscillator and is at the uniform velocity vibrated with 200 r/min, taken out after 6h, by supernatant liquor through 0.45 μm of mistake
Membrane filtration measures As content.
Embodiment 1
(1) Mg (OH) of 0.1 mol/L is configured2Suspension: by Mg (OH)2It is dissolved in dehydrated alcohol, ultrasonic disperse 5min is obtained
To the Mg (OH) of 0.1 mol/L2Suspension；
(2) Fe of 0.1 mol/L is configured2SO4Solution: by Fe2SO4∙7H2O is dissolved in deionized water, obtains 0.1mol/L's
Fe2SO4Solution；
(3) NaBH of 0.25 mol/L is configured4Solution: by NaBH4Solid is dissolved in deionized water, obtains 0.25mol/L's
NaBH4Solution；
(4) Mg (OH) of 75 ml0.1 mol/L is taken2Suspension liquid is placed in 500ml three-necked flask, keeps mechanical stirring
300 r/min are passed through nitrogen insulation blocking, and the Fe of 75 ml, 0.1 mol/L is added2SO4Solution, and immediately with 3 mL/min's
The NaBH of 0.25 mol/L is added dropwise in speed4Solution 60ml；
(5) after being added dropwise to complete, centrifuge separation gained black solid, dehydrated alcohol and deionized water successively clean 3 times, and 45
DEG C vacuum drying to get arrive nZVI@Mg (OH)2Composite material；
(6) at normal temperature, take As (V) solution that 20ml concentration is 1mg/L in vial, it is molten with the HCl of 0.1mol/L
Liquid and 0.1mol/L NaOH solution adjust PH to 7.0, and nZVI@Mg (OH) made from 0.1g/L is added2Composite material is placed in perseverance
Warm oscillator is at the uniform velocity vibrated with 200 r/min, and As (V) concentration is down to 3 μ g/L in solution after 6h；It is more unsupported than nZVI to Mg
(OH)2When residual concentration (18.7 μ g/L) it is low；nZVI@Mg(OH)2Composite material is 0.996 mg/g to the adsorption capacity of arsenic, and
Nano zero valence iron adsorption capacity is then 0.981 mg/g, and adsorption of magnesium hydroxide capacity is then 0.992 mg/g.
Embodiment 2
Step (1)-(5) are same as Example 1；
Arsenic removal experiment:
At normal temperature, take As (V) solution that 20 ml concentration are 5 mg/L in vial, with the HCl solution of 0.1 mol/L
PH to 7.0 is adjusted with 0.1mol/L NaOH solution, nZVI@Mg (OH) made from 0.1 g/L is added2Composite material is placed in constant temperature
Oscillator is at the uniform velocity vibrated with 200 r/min, nZVI@Mg (OH) after 6 h2Composite material is 4.94 to the adsorption capacity of As (V)
mg/g；And nano zero valence iron adsorption capacity is then 4.57 mg/g, and adsorption of magnesium hydroxide capacity is then 3.04 mg/g.
Embodiment 3
Step (1)-(5) are same as Example 1；
Arsenic removal experiment:
At normal temperature, take As (V) solution that 20 ml concentration are 8 mg/L in vial, with the HCl solution of 0.1 mol/L
PH to 7.0 is adjusted with 0.1mol/L NaOH solution, nZVI@Mg (OH) made from 0.1 g/L is added2Composite material is placed in constant temperature
Oscillator is at the uniform velocity vibrated with 200 r/min, nZVI@Mg (OH) after 6 h2Composite material is 6.75 to the adsorption capacity of As (V)
mg/g；And Zero-valent Iron adsorption capacity is then 6.68 mg/g, and adsorption of magnesium hydroxide capacity is then 3.50 mg/g.
Fig. 1 is nZVI@Mg (OH) obtained2Composite material and single nZVI or Mg (OH)2Material processing low concentration water body
In As (V) afterwards equilibrium concentration compare.As shown in Figure 1, when As (V) initial concentration is gradually lowered to 1 mg/L by 8 mg/L,
Equilibrium concentration gradually decreases.Relative to nZVI and Mg (OH)2Individually effect when absorption, nZVI@Mg (OH)2Composite material beginning table
Reveal best arsenic-adsorbing ability.In addition as shown in black arrow on the way, when As (V) initial concentration is 1 mg/L, nZVI@Mg
(OH)2Equilibrium concentration corresponding to composite material is 3.60 μ g/L, is lower than 10 μ g/L of World Health Organization's drinking water standard.Show multiple
As in water body (V) content effectively can be reduced to drinking water standard by condensation material.
Be it is necessary to described herein finally: above embodiments are served only for making technical solution of the present invention further detailed
Ground explanation, should not be understood as limiting the scope of the invention, those skilled in the art's above content according to the present invention
The some nonessential modifications and adaptations made all belong to the scope of protection of the present invention.
Claims (9)
1. a kind of specific regulatory control nano zero valence iron corrosion product and the method for reinforcing nano zero valence iron adsorption of Low Concentration arsenic, special
Sign is, includes the following steps:
(1) Mg (OH) is configured2Suspension: by Mg (OH)2It is dissolved in dehydrated alcohol, ultrasonic disperse obtains Mg (OH)2Suspension；
(2) FeSO is configured4Solution: by FeSO4∙7H2O is dissolved in deionized water, obtains FeSO4Solution；
(3) NaBH is configured4Solution: by NaBH4Solid is dissolved in deionized water, obtains NaBH4Solution；
(4) Mg (OH) is taken2Suspension is placed in three-necked flask, keeps mechanical stirring, is passed through inert gas insulation blocking, and FeSO is added4
Solution, and NaBH is added dropwise with the speed of 3mL/min immediately4Solution；
(5) after being added dropwise to complete, it is centrifugally separating to obtain black solid, is washed, is dried to get nZVI@Mg (OH) is arrived2Composite material；
(6) take As (V) solution in vial at room temperature, the concentration of As (V) solution is 1 ~ 8 mg/L, with HCl solution and
NaOH solution adjusts pH, and nZVI@Mg (OH) made from step (5) is added2Composite material is placed in constant temperature oscillator and at the uniform velocity vibrates,
Solid-liquid sample is separated after oscillation, tests As (V) content in solution.
2. a kind of specific regulatory control nano zero valence iron corrosion product according to claim 1 simultaneously reinforces nano zero valence iron absorption
The method of low-concentration arsenic, which is characterized in that the time of ultrasonic disperse described in step (1) is 5min.
3. a kind of specific regulatory control nano zero valence iron corrosion product according to claim 1 simultaneously reinforces nano zero valence iron absorption
The method of low-concentration arsenic, which is characterized in that the Mg (OH)2The concentration of suspension is 0.1mol/L；The FeSO4Solution it is dense
Degree is 0.1mol/L；The NaBH4The concentration of solution is 0.25mol/L.
4. a kind of specific regulatory control nano zero valence iron corrosion product according to claim 1 simultaneously reinforces nano zero valence iron absorption
The method of low-concentration arsenic, which is characterized in that churned mechanically rate described in step (4) is 300 r/min, and mechanical stirring is kept
To NaBH4Solution completion of dropwise addition；The inert gas includes nitrogen or argon gas.
5. a kind of specific regulatory control nano zero valence iron corrosion product according to claim 1 simultaneously reinforces nano zero valence iron absorption
The method of low-concentration arsenic, which is characterized in that in step (4), the molar ratio of reactant additive amount is Mg (OH)2: FeSO4: NaBH4
=1:1:2。
6. a kind of specific regulatory control nano zero valence iron corrosion product according to claim 1 simultaneously reinforces nano zero valence iron absorption
The method of low-concentration arsenic, which is characterized in that in step (5), the washing, which refers to, successively cleans 3 with dehydrated alcohol and deionized water
It is secondary；The drying is the lower 45 DEG C of dryings of vacuum.
7. a kind of specific regulatory control nano zero valence iron corrosion product according to claim 1 simultaneously reinforces nano zero valence iron absorption
The method of low-concentration arsenic, which is characterized in that in step (6), the concentration of the HCl solution and NaOH solution is 0.1 mol/L；
The value of the pH is 7.0 ± 0.25.
8. a kind of specific regulatory control nano zero valence iron corrosion product according to claim 1 simultaneously reinforces nano zero valence iron absorption
The method of low-concentration arsenic, which is characterized in that in step (6), the nZVI@Mg (OH)2The additive amount of composite material is 0.1 g/
L。
9. a kind of specific regulatory control nano zero valence iron corrosion product according to claim 1 simultaneously reinforces nano zero valence iron absorption
The method of low-concentration arsenic, which is characterized in that in step (6), the speed of the oscillation is 200 r/min, and the time of oscillation is 6
h。
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| CN111362390B (en) * | 2020-03-26 | 2021-06-29 | 中国科学院生态环境研究中心 | Method for enhancing arsenic removal effect of nano zero-valent iron by regulating oxygen content |
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| CN103157451A (en) * | 2013-04-11 | 2013-06-19 | 福州大学 | Zero-valent iron and nano magnesium hydroxide supported reductive spherical cellulose adsorbent |
| CN104759635A (en) * | 2015-03-12 | 2015-07-08 | 中国科学院福建物质结构研究所 | Preparation method of load type nanometer zero-valent iron composite material |
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| CN103157451A (en) * | 2013-04-11 | 2013-06-19 | 福州大学 | Zero-valent iron and nano magnesium hydroxide supported reductive spherical cellulose adsorbent |
| CN104759635A (en) * | 2015-03-12 | 2015-07-08 | 中国科学院福建物质结构研究所 | Preparation method of load type nanometer zero-valent iron composite material |
Non-Patent Citations (2)
| Title |
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| "Montmorillonite-supported nanoscale zero-valent iron for removal of arsenic from aqueous solution: Kinetics and mechanism";Subhamoy Bhowmick et al;《Chemical Engineering Journal》;20131228;第243卷(第243期);实施例1和说明书第2-3段 |
| "沉淀法制备氢氧化镁及其对砷溶液的吸附特性";柴多里等;《硅酸盐学报》;20100130;第38卷(第1期);第1.2节 |
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