CN102527319B - High-efficiency superparamagnetic ferrite nano arsenic adsorbent and preparation process thereof - Google Patents
High-efficiency superparamagnetic ferrite nano arsenic adsorbent and preparation process thereof Download PDFInfo
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- CN102527319B CN102527319B CN 201210004790 CN201210004790A CN102527319B CN 102527319 B CN102527319 B CN 102527319B CN 201210004790 CN201210004790 CN 201210004790 CN 201210004790 A CN201210004790 A CN 201210004790A CN 102527319 B CN102527319 B CN 102527319B
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Abstract
The invention belongs to the field of nano adsorption materials and in particular relates to a high-efficiency superparamagnetic ferrite nano arsenic adsorbent and a preparation process thereof. The prepared nano ferrite can well remove harmful ions (such as arsenic) from water and has strong magnetic recovery capacity, so that the problems of excessive harmful ions in the water and incapability of recovery of the adsorbent at present are solved. The adsorbent consists of superparamagnetic spinel ferrite phase nanoparticles and is nanopowder with the grain size of 3 to 8 nm, wherein the specific surface area is 100 to 500 m<2>/g. According to the process, pure crystallized nano ferrite powder is prepared by using anhydrous metal chloride, absolute ethanol and sodium hydroxide as reaction precursors and performing solvent thermal reaction. The prepared superparamagnetic ferrite nanoparticles are high in purity, small in grain size, high in specific surface area and high in hydrophilicity and more new selectable materials are provided for reducing the harmful ion (such as arsenic) content of water.
Description
Technical field
The invention belongs to the nano adsorption material field, be specially a kind of efficient superparamagnetism ferrite nanometer arsenic adsorbent and preparation technology thereof, the nano-oxide that makes has stronger arsenic adsorption capacity, water body dispersibility and magnetic recovery ability.
Background technology
For a long time, the arsenic in the water body is the focus that people pay close attention to the harm of health always.Studies show that, quote over a long time the generation that the water that contains low arsenic concentration arsenic also can cause a lot of diseases.Regulation in the new drinking water standards (GB5479-2006) of promulgating in 2006, the arsenic concentration standard is 0.01mg/L in the Drinking Water.Therefore, the removal method of arsenic becomes the hot issue of environmental area research in the water, and absorption method is a kind of simple, efficient arsenic processing method.
The efficient adsorption material preparation is the important technical links of processing arsenic-containing water.At present, after deliberation nano-oxide adsorbent has titanium oxide, zirconia and cerium oxide.But, except the arsenic adsorption efficiency low or cost higher, most of adsorbent is far smaller than pentavalent arsenic to arsenious adsorption capacity.Will be through the adjusting of pre-oxidation and pH value as adsorption treatment is last, this processing for the large volume arsenic polluted water body is infeasible.Therefore, developing low-cost, efficient arsenic (trivalent or pentavalent) adsorbent are the focuses of current research.
The influence factor of arsenic absorption has a lot, and topmost influence factor is the Surface Physical Chemistry state of adsorbent own.For example, surface hydroxyl (OH) concentration, specific area, aperture, pore volume etc.Ferrite forms a large amount of surface hydroxyls in water body, they all have extremely strong affinity to trivalent arsenic and pentavalent arsenic species.In order to prepare efficient ferrite trivalent and pentavalent arsenic adsorbent, the ferrite that obtains high-specific surface area and the concentration of surface hydroxyl groups selection that is inevitable.From bibliographical information as can be known, refinement of particle size and element doping are the effective ways that obtain the high surface oxide.Especially, when the size reduction of magnetic nano-particle was following to critical value, it just had superparamagnetism, did not show the magnetization of self under without the effect of externally-applied magnetic field, and it has the loose ability of oversubscription in water body, and this is conducive to improve the absorption property of adsorbent.In order to prepare ultra-fine ferrite nano material, utilize that traditional hydro-thermal method, collosol and gel are sent out, coprecipitation, will inevitably introduce the exhibiting high surface activating agent, cause product surface a large amount of hydrophobic groupings to occur, this is unfavorable for that product is in the application of water treatment field.
In addition, be the difficult problem that the arsenic adsorbent faces when selecting separating of the optimization of arsenic absorption property and adsorbent always.The ferrous acid salt face of spinel structure has the larger intensity of magnetization, and this provides possibility for the magnetic separating adsorbent.Mode by element doping may make a large amount of defective of appearance in the ferrite lattice, so that improve ferritic specific area and arsenic adsorption capacity.In addition, the dispersibility of nano particle in water body also is the important factor in order of its absorption property.
In order to obtain high magnetic nano ferrite arsenic (trivalent and pentavalent) adsorbent, so that the applying nano oxide reaches the purpose of water purification, must the suitable ferritic synthesis technique of ultra-fine hydrophily and an amount of doped chemical of selection of exploitation.
Summary of the invention
The object of the present invention is to provide a kind of high magnetic ferrite nanometer arsenic adsorbent and preparation technology thereof, the nano ferrite of preparing can be well except anhydrating middle harmful ion (take arsenic as example), and show strong magnetic recovery ability, to solve the problem that harmful ion exceeds standard and adsorbent is recycled in the present water.
Technical scheme of the present invention is:
A kind of efficient super-paramagnetism nano ferrite arsenic adsorbent, sorbent material purity is high, specific area is large, crystal grain is tiny, good hydrophilic property, this adsorbent is that single superparamagnetism spinel ferrite phase nano particle forms, and nano ferrite is nano magnesium ferrite, nanometer zinc ferrite, nano ferrous acid copper, nanometer ferrous acid lithium, nanometer Manganese Ferrite, nano-ferrous acid or nano nickel ferrite etc.
Described efficient super-paramagnetism nano ferrite arsenic adsorbent, nano ferrite is the nano-oxide powder of crystallite dimension 3～8nm, its specific area is 100～500m
2/ g.
Described efficient super-paramagnetism nano ferrite arsenic adsorbent, adsorbent has preferably superparamagnetism, has given its strong water body dispersibility and Magnetic Isolation ability, and the adsorbent after the recovery still shows high arsenic adsorption efficiency.
Described efficient super-paramagnetism nano ferrite arsenic adsorbent when this adsorbent once uses, is 100% to the adsorption efficiency of trivalent arsenic (III) or pentavalent arsenic (V); Water sample after the arsenic absorption is carried out magnetic separates and again obtain nano ferrite phase particle, then through alkali cleaning desorption and cycling and reutilization, through 3～5 times recycling after, be 70～80% to the adsorption efficiency of trivalent arsenic (III) or pentavalent arsenic (V).
The preparation technology of described efficient super-paramagnetism nano ferrite arsenic adsorbent may further comprise the steps:
(1) under magnetic agitation, the anhydrous metal chloride joined by different mol ratio be configured to the metal chloride ethanolic solution that cation concn is 0.1mol/L～0.3mol/L in the absolute ethyl alcohol, again NaOH is joined in the metal chloride ethanolic solution room temperature reaction 0.5～2h.The addition of the valence state * metal chloride of the addition=metal ion of NaOH.
(2) will react mixture and import in the reactor of polytetrafluoroethylene (PTFE), carry out solvent thermal reaction, 100～180 ℃ of lower insulations 1～3 hour.
(3) the question response still naturally cools to room temperature, and water and alcohol clean up sample, and drying is ground and obtained pure nano ferrite powder.
The preparation technology of described efficient super-paramagnetism nano ferrite arsenic adsorbent, the anhydrous metal chloride is the anhydrous chloride salt of iron and magnesium, zinc, copper, lithium, manganese, cobalt or nickel etc.
The preparation technology of described efficient super-paramagnetism nano ferrite arsenic adsorbent, raw material is commercial pure anhydrous metal chloride, absolute ethyl alcohol and the commercial pure cerium hydroxide sodium of analyzing analyzed.
The preparation technology of described efficient super-paramagnetism nano ferrite arsenic adsorbent, the specific area of nano-oxide is 100～500m
2/ g, nano-oxide are the nanometer powders of crystallite dimension 3～8nm.
Design principle of the present invention is as follows:
Room temperature reaction generates excessive NaCl salt voluntarily, and it is rapid crystallization in ethanol, is wrapped in the presoma hydroxide particles peripheral.In the solvent heat process, the NaCl salt that is wrapped in the hydroxide periphery continues growing up of restriction nanometer metallic iron silicate nanometer particle.In building-up process, doped chemical enters into ferrite lattice, causes lattice defect, obtains the superparamagnetism ferrite arsenic adsorbent of high-ratio surface.The present invention uses absolute ethyl alcohol as solvent, by a kind of method of simple control nanoparticle size, develops a kind of solvent heat new preparation process of efficient superparamagnetism ferrite nanometer arsenic adsorbent.Take the preparation technology of nano magnesium ferrite as example, use this technical process to prepare to have single cubic spinelle, high-specific surface area, super-paramagnetism nano magnesium ferrite that crystal grain is tiny, and reach the purpose except middle harmful ion (take the arsenic as example) that anhydrates.
At present, in various traditional preparation methods, nanoparticle size is not easy control, and introduces the size that a large amount of organic matters is controlled nano particle in the reaction system, cause product surface a large amount of hydrophobic groupings to occur, this is unfavorable for that product is in the application of water treatment field.In addition, be the difficult problem that the arsenic adsorbent faces when selecting separating of the optimization of arsenic absorption property and adsorbent always.The invention has the advantages that:
1. the cost of material of the present invention's use is low, and reaction temperature is low, energy savings, and technological operation is simple, is easy to control.
2. the present invention utilizes the NaCl salt rapid crystallization that generates voluntarily in the room temperature reaction process, and then be coated on nano grain surface, thereby in the solvent heat process, growing up of control nano particle, obtain ultra-fine hydrophilic magnetic nano ferrite arsenic adsorbent, a kind of method of control particle diameter of excellence is provided for the various high magnetic nano ferrite of solwution method industrial production arsenic adsorbent.
3. the efficient super-paramagnetism nano magnesium ferrite arsenic adsorbent prepared of the present invention, the nano magnesium ferrite powder is the cubic spinel Mg of complete crystallization
0.27Fe
2.49O
4Phase, its specific area can reach 438.2m
2/ g, average grain size is 3.7nm, and it has very strong adsorption capacity, water body dispersibility and Magnetic Isolation ability, directly the sorbing material of harmful ion (take arsenic as example) in the water is removed in conduct, but harmful ion content provides more new material selections in the water in order to reduce.
4. the present invention introduces element doping in ferrite lattice, and playing increases the ferrite lattice defective, the effect that increases the product specific area.
5. process of the present invention can be used for the production of the nano metal ferrite of the magnetic spinel structures commonly used such as nano magnesium ferrite, nanometer zinc ferrite, nano ferrous acid copper, nanometer ferrous acid lithium, nanometer Manganese Ferrite, nano-ferrous acid, nano nickel ferrite.
In a word, the present invention can be used for the efficient super-paramagnetism nano ferrite arsenic adsorbent of drinking water, and adsorbent is high by purity, particle diameter is little, specific area is high, hydrophilic superparamagnetism spinel ferrite nano particle forms.Arsenic-removing adsorption agent of the present invention has the high rate of adsorption and efficient to low concentration arsenic-containing water body, and high concentration arsenic-containing water body is had high adsorption capacity.And this adsorbent has preferably superparamagnetism, is convenient to dispersion and the recovery of adsorbent in water body, and the adsorbent after the recovery still shows high arsenic adsorption efficiency through recycled for multiple times.This technique obtains the nano ferrite particle of crystallization take anhydrous chloride, absolute ethyl alcohol, NaOH as pre-reaction material by solvent thermal reaction, then water and ethanol clean and obtains pure binary metal ferrite powder.The present invention does not use any surfactant, but the NaCl crystal clad nano that utilizes room temperature reaction to become voluntarily is brilliant, thereby limits nanocrystalline growing up in the solvent heat process.Preparation technology of the present invention is simple, and reaction temperature is low, has greatly saved the energy, for the various small size ferrite of industrial production nano particle provides a kind of new approach.That the present invention prepares is high-purity, high-specific surface area, superparamagnetism binary metal ferrite nano particle that crystal grain is tiny, for reducing harmful ion (take arsenic as example) in the water but content provides more new material selections.
Description of drawings:
Fig. 1: the present invention prepares TEM photo (a) and the high-resolution phase (b) of magnesium ferrite Nanoparticles During particle.
Fig. 2 (a)-(b): the BET figure (a) of the nano magnesium ferrite that the present invention prepares and XRD figure (b).Among Fig. 2 (a), P
0The ratio of the saturated vapour pressure of gas and gas balance pressure when/P represents experimental temperature T, illustration represents the pore-size distribution of nano particle.
Fig. 3: the nano magnesium ferrite that the present invention prepares is processed Magnetic Isolation situation and the recovery utilization rate behind the natural environment water sample.(a) before figure is Magnetic Isolation, after (b) figure is Magnetic Isolation.
Fig. 4: Mg
0.27Fe
2.49O
4The graph of a relation of cyclic utilization rate and cycle-index when the nano particle processing contains arsenic (III, V) natural water.
The specific embodiment:
Further specify by the following examples the present invention:
Prepare efficient superparamagnetism magnesium ferrite nanometer arsenic adsorbent with method provided by the invention, its technological process is as follows:
Under magnetic agitation, with anhydrous FeCl
3(1.13g) and MgCl
2(0.075g) be dissolved into and be configured to the chloride ethanolic solution that molar concentration is 0.1M in the absolute ethyl alcohol (80m1), again a certain amount of NaOH is slowly joined (addition of the valence state * metal chloride of the addition=metal ion of NaOH, two metal ion species Mg in the chloride ethanolic solution
2+With Fe
3+Add up to after calculating respectively), under the magnetic agitation effect, fully mix 1h, then import in the reactor of polytetrafluoroethylene (PTFE), carry out solvent thermal reaction, 150 ℃ of the temperature of solvent thermal reaction, solvent heat time 2h.Solution to be mixed is cooled to centrifugal supersound washing after the room temperature., grind and obtain high pure and ultra-fine Mg after 12 hours through 80 ℃ of vacuum drying
0.27Fe
2.49O
4The nano particle product.
Use transmission electron microscope (TEM) to observe nanometer Mg
0.27Fe
2.49O
4Granule-morphology in the preparation process is found:
Have typical black particle through the condensate behind the solvent thermal reaction and be distributed in the dual structure (shown in Fig. 1 (a)) that forms in white " cloud " the shape material, lattice paprmeter determines that " cloud " that the particle periphery is wrapped in is the NaCl crystal after measured.With deionized water NaCl salt is washed, obtain nanometer Mg after the drying
0.27Fe
2.49O
4The high-resolution phase of particle (shown in Fig. 1 (b)) as can be known, finally obtains the Mg of complete crystallization
0.27Fe
2.49O
4Particle, its crystallite dimension is approximately 3.7nm.
Fig. 2 has provided nanometer Mg
0.27Fe
2.49O
4The BET figure (a) of particle and XRD figure (b).This has confirmed that further products obtained therefrom is the cubic spinel Mg of complete crystallization
0.27Fe
2.49O
4Phase; The specific area of testing its particle through BET is 438.2m
2/ g, the aperture is mesopore, and average-size is about 3.9nm.
Fig. 3 has provided under the external magnetic field and has contained Mg
0.27Fe
2.49O
4The situation of change of the water sample of nano particle.Can find out, compare synthetic pure iron oxide, the magnesium ferrite arsenic adsorbent that magnesium obtains after mixing has the higher intensity of magnetization, can separate from water body at short notice under magnetic fields.Therefore, proved that magnetic separates Mg from water body
0.27Fe
2.49O
4The arsenic adsorbent is feasible.This recovery and cycling and reutilization for adsorbent provides possibility.
Fig. 4 is Mg
0.27Fe
2.49O
4The relation of cyclic utilization rate and cycle-index when the nano particle processing contains arsenic (III, V) natural water.Natural Water is taken from Yunnan Yang Zonghai, and the concentration of its arsenic (III) and arsenic (V) is respectively 0.071mg/L and 0.045mg/L.When the adsorbent consumption was 0.02g/L, an arsenic (III) and arsenic (V) adsorption efficiency were 100%.Water sample after the arsenic absorption is carried out the magnetic separation again obtain Mg
0.27Fe
2.49O
4Nano particle is then through alkali cleaning desorption and cycling and reutilization.As seen, four times recycling after, the adsorption efficiency of its arsenic (III) and arsenic (V) is still up to about 70～80%, this is that the cost that reduces the arsenic adsorbent is very favorable.
In addition, less about the simultaneously research of arsenic-adsorbing (III) and arsenic (V) of ferrite in the document, the people such as Gim é nez show the result of study of natural bloodstone arsenic-adsorbing, and bloodstone only is 0.265mg/g to the saturated extent of adsorption of arsenic (III).And the nanometer Mg that technique of the present invention obtains
0.27Fe
2.49O
4To the saturated extent of adsorption of arsenic (III) and arsenic (V) respectively up to 127.4mg/g and 83.2mg/g.This has illustrated the nanometer Mg that this technique obtains
0.27Fe
2.49O
4Have strong arsenic (III) and arsenic (V) absorption property.Nanometer Mg
0.27Fe
2.49O
4High saturated extent of adsorption is owing to nano magnesium ferrite high specific area and concentration of surface hydroxyl groups.Generally speaking, this technique has very large application prospect in efficient nano oxide arsenic absorbent preparation field.
Embodiment result shows, a kind of high magnetic ferrite nanometer arsenic adsorbent and the solvent heat new technique for synthesizing thereof that adopt the present invention to propose prepare that purity is high, specific area is large, crystal grain is tiny, good hydrophilic property, and by single superparamagnetism spinelle Mg
0.27Fe
2.49O
4Nanometer arsenic adsorbent.Take anhydrous ferric chloride, anhydrous magnesium chloride and NaOH as pre-reaction material, by the superparamagnetism Mg of solvent heat synthesizing high specific surface area
0.27Fe
2.49O
4Nano particle not only has very strong ion adsorption capacity, and has extremely strong water body dispersibility and Magnetic Isolation ability, for reducing harmful ion (take arsenic as example) in the water content and magnetic recovery but new material selection is provided.
Difference from Example 1 is, prepares efficient superparamagnetism Manganese Ferrite nanometer arsenic adsorbent with method provided by the invention, and the super-paramagnetism nano Manganese Ferrite powder that makes is the cubic spinel Mn of complete crystallization
0.11Fe
2.52O
4Phase, specific area are 389m
2/ g, particle size is 3～6nm.
When this adsorbent once uses 0.04g/L, the adsorption efficiency of trivalent arsenic or pentavalent arsenic is 100%; Water sample after the arsenic absorption is carried out magnetic separates and again obtain nano ferrite phase particle, then through alkali cleaning desorption and cycling and reutilization, through 3～5 times recycling after, be 70～80% to the adsorption efficiency of trivalent arsenic or pentavalent arsenic.
Difference from Example 1 is, prepares efficient superparamagnetism zinc ferrite nanometer arsenic adsorbent with method provided by the invention, and the super-paramagnetism nano zinc ferrite powder that makes is the cubic spinel Zn of complete crystallization
0.45Fe
2.37O
4Phase, specific area are 330m
2/ g, particle size is 4～8nm.
When this adsorbent once uses 0.05g/L, the adsorption efficiency of trivalent arsenic or pentavalent arsenic is 100%; Water sample after the arsenic absorption is carried out magnetic separates and again obtain nano ferrite phase particle, then through alkali cleaning desorption and cycling and reutilization, through 3～5 times recycling after, be 70～80% to the adsorption efficiency of trivalent arsenic or pentavalent arsenic.
Claims (2)
1. the preparation technology of an efficient superparamagnetism ferrite nanometer arsenic adsorbent, it is characterized in that: this adsorbent is comprised of single superparamagnetism spinel ferrite phase nano particle, nano ferrite is nano magnesium ferrite, nanometer Manganese Ferrite, nanometer zinc ferrite, nano ferrous acid copper, nanometer ferrous acid lithium, nano-ferrous acid or nano nickel ferrite, adsorbent is the nanometer powder of crystallite dimension 3-8nm, and its specific area is 100-500 m2/g;
Its preparation technology may further comprise the steps:
(1) under magnetic agitation, the anhydrous metal chloride joined by different mol ratio be configured to the metal chloride ethanolic solution that cation concn is 0.1mol/L-0.3mol/L in the absolute ethyl alcohol, NaOH is joined in the metal chloride ethanolic solution again, room temperature reaction 0.5-2h, the addition of the valence state * metal chloride of the addition=metal ion of NaOH;
The anhydrous metal chloride is the anhydrous chloride salt of iron and magnesium, manganese, zinc, copper, lithium, cobalt or nickel;
(2) will react mixture and import in the reactor of polytetrafluoroethylene (PTFE), carry out solvent thermal reaction, 100-180 ℃ of lower insulation 1-3 hour;
(3) the question response still naturally cools to room temperature, and water and alcohol clean up sample, and drying is ground and obtained pure nano ferrite powder.
2. according to the preparation technology of efficient superparamagnetism ferrite nanometer arsenic adsorbent claimed in claim 1, it is characterized in that, raw material is commercial pure anhydrous metal chloride, absolute ethyl alcohol and the commercial pure cerium hydroxide sodium of analyzing analyzed.
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| WO2016203038A1 (en) * | 2015-06-19 | 2016-12-22 | Universitat Autonoma De Barcelona | Method for desorption of metal oxyanions from superparamagnetic iron oxide nanoparticles (spion) |
| CN105344332A (en) * | 2015-11-04 | 2016-02-24 | 苏州书瑞环保科技有限公司 | Water treatment arsenic adsorption material and preparation method thereof |
| CN105381780B (en) * | 2015-12-07 | 2017-10-31 | 中国科学院生态环境研究中心 | A kind of magnetic adsorbent for adsorbing superconduction Magneto separate arsenic removal antimony and preparation method thereof |
| CN107362768B (en) * | 2017-07-31 | 2020-04-24 | 浙江工业大学 | Copper foam ferrite, preparation method thereof and application thereof in adsorption removal of arsenic in water body |
| CN108640196A (en) * | 2018-04-20 | 2018-10-12 | 湖南大学 | A kind of method that depth removes arsenic in water removal |
| CN108328629A (en) * | 2018-05-16 | 2018-07-27 | 湖南华佳纳米新材料科技有限公司 | A kind of method and system preparing nano magnesia |
| CN110090615B (en) * | 2019-04-24 | 2022-03-11 | 华东理工大学 | Preparation method and application of high-valence metal ferrite adsorbent |
| CN110479283B (en) * | 2019-08-27 | 2020-09-08 | 华中科技大学 | Catalyst with nickel loaded on surface of copper ferrite spinel, preparation method and application thereof |
| CN111362422B (en) * | 2020-03-17 | 2022-05-10 | 山东普尼奥水处理科技有限公司 | Magnetic complex-cyanide lyase composite nanoparticle, preparation method and application thereof, and method for treating electroplating wastewater by using magnetic complex-cyanide lyase composite nanoparticle |
| CN112588256A (en) * | 2021-01-28 | 2021-04-02 | 华东交通大学 | Magnetic nano bimetal oxide adsorbent and application thereof |
| CN114551812A (en) * | 2022-01-27 | 2022-05-27 | 广东邦普循环科技有限公司 | Lithium ion battery prelithiation agent and preparation method and application thereof |
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