CN103506065A - Magnetic heavy metal adsorbent with casing-core structure and preparation method thereof - Google Patents
Magnetic heavy metal adsorbent with casing-core structure and preparation method thereof Download PDFInfo
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Abstract
The invention relates to application of water treatment, in particular to a magnetic heavy metal adsorbent with a casing-core structure and a preparation method thereof. The magnetic heavy metal adsorbent with the casing-core structure uses a magnetic nano Fe-Mn compound MnxFe3-xO4(x=0-1) as a core, and uses a manganese oxide as a casing. The prepared magnetic heavy metal adsorbent is aggregate of nano particles, is 10-250 nm in particle size range and 70-120m<2>/g in specific area, has excellent performance of adsorbing ions of heavy metals including lead, cadmium, mercury, copper, nickel, zinc, cobalt and the like in a water body, is high in adsorption speed and adsorption capacity, still has a good removing effect when the heavy metals are lower in density, has good magnetism, is 35-55 A.m<2>/kg<-1> in saturatation magnetization, meanwhile magnetic separation can be performed, the separation speed is high, the operation is simple, the efficiency is high, the energy consumption is low and secondary pollution cannot be caused.
Description
Technical field
The present invention relates to water treatment applications, specifically a kind of shell-core structure magnetic heavy metal absorbent and preparation method thereof.
Background technology
Heavy metal has enriching, is difficult to degrade in environment.In the exploitation of heavy metal, smelting, process, cause many heavy metals to cause serious environmental pollution as lead, mercury, cadmium, cobalt etc. enter atmosphere, water, soil.The heavy metal of discharging with waste water even if concentration is little, also can accumulate in algae and bed mud, by fish and shellfish body surface, is adsorbed, and produces food chain concentrated, thus the public hazards of causing.For example, the nuisance diseases such as the minamata disease (mercury pollution) that Japan occurs and Itai-itai diseases (cadmium pollution), are all caused by heavy metal pollution.
At present, the method of heavy metal containing wastewater treatment roughly can be divided into three major types: (1) bioanalysis, utilize the effects such as absorption, accumulation, enrichment of microorganism or plant to remove the method for heavy metal in waste water, comprise the methods such as biological adsorption, bioflocculation, phytoremediation, many places are in developing stage at present.(2) chemical method, comprises chemical precipitation method, oxidation-reduction method, electrochemical process etc., is mainly applicable to the processing containing higher concentration effluent containing heavy metal ions, and efficiency is high, but energy consumption is large, easily produces secondary pollution.(3) Physical, mainly comprise solvent extraction and separation, ion-exchange, membrane separation technique, absorption method etc., wherein absorption method is by heavy metal ion adsorbed at adsorbent surface in water by effects such as absorption or ion-exchanges, thereby reach the object of removing heavy metal in water, this method is simple, and applicable system is many, and secondary pollution is little and cost is low, in heavy metal containing wastewater treatment, be applied, be particularly useful for the water treatment that content of beary metal is lower.
At present, for the sorbing material of heavy metal, there are bentonite, zeolite, red mud, cocoanut shell, coated sand, activated alumina, active carbon and natural or synthetic metal oxide and hydrous oxide thereof etc., wherein Mn oxide has the features such as isoelectric point is low, specific area is large, surface hydroxyl is abundant, there is stronger heavy metal adsorption characteristic, effective heavy metal contaminants in Adsorption water, but its particle diameter is less, adopt in actual applications the separation method of traditional filtering to have easy loss, separation difficulty, inefficient problem.And magnetic separation is to utilize the effect of externally-applied magnetic field that magnetic-particle and namagnetic substance are separated, the application in water treatment more and more receives publicity.Compare with traditional filtering separation method, magnetic separation technique is simply efficient, can realize quickly and easily Separation of Solid and Liquid.
Summary of the invention
The object of the invention is to provide a kind of shell-core structure magnetic heavy metal absorbent and preparation method thereof.
For achieving the above object, the present invention adopts technical scheme to be:
A kind of shell-core structure magnetic heavy metal absorbent: magnetic Nano ferrimanganic compound Mn
xfe
3-xo
4(x=0～1) is kernel, the shell-core structure magnetic heavy metal absorbent that Mn oxide is shell.
Described kernel is that one or more in soluble ferric iron salt, soluble ferrite and soluble manganese salt are raw material reaction gained magnetic Nano ferrimanganic compound.
Described shell is that solubility permanganate and soluble manganese salt are raw material reaction gained Mn oxide.
Described soluble ferric iron salt is iron chloride, ferric nitrate, ferric sulfate or their mixture; Described soluble ferrite is frerrous chloride and/or ferrous sulfate; Described soluble manganese salt is one or more the mixing in manganese chloride, manganese nitrate, manganese sulfate, manganese carbonate.
Described solubility permanganate is potassium permanganate and/or sodium permanganate; Described soluble manganese salt is one or more the mixing in manganese chloride, manganese nitrate, manganese sulfate, manganese carbonate.
A kind of preparation method of shell-core structure magnetic heavy metal absorbent:
1) preparation of kernel magnetic Nano ferrimanganic compound: one or more of take in soluble ferric iron salt, soluble ferrite and soluble manganese salt are made into mixed solution as raw material, pH of mixed is adjusted to 6～12, and ℃ reaction in room temperature～100, then ageing, separation, washes to obtain kernel magnetic Nano ferrimanganic compound Mn
xfe
3-xo
4(x=0～1);
2) above-mentioned gained kernel magnetic Nano ferrimanganic compound is mixed with PEG solution, making PEG solution final concentration is 0.1～15%, after mixing, mix with soluble manganese salting liquid and solubility permanganate solution again, reaction at room temperature～100 ℃, the surface that reaction gained Mn oxide is directly coated on kernel magnetic Nano ferrimanganic compound forms shell, then by gained separating substances, and washing, dry, obtain shell-core structure magnetic heavy metal absorbent.
The mol ratio of described step 1) Raw soluble ferric iron salt, soluble ferrite and soluble manganese salt is 2: (1～0): (0～1).
With one or more in NaOH, potassium hydroxide, ammoniacal liquor, sodium carbonate and potash for regulating step 1) the pH value of mixed liquor.
Described step 2) in, the mol ratio of soluble manganese salt and solubility permanganate is (5: 1)～(3: 2).
The quality of shell-core structure magnetic heavy metal absorbent housing accounts for 0～60% of adsorbent gross mass.
An application for shell-core structure magnetic heavy metal absorbent, the application of heavy metal ion in described shell-core structure magnetic heavy metal absorbent adsorbent solution.
Described heavy metal ion is one or more in lead, cadmium, mercury, copper, nickel, zinc and cobalt.
The present invention has advantages of:
1. the present invention is compound by magnetic-particle and Mn oxide, form magnetic heavy metal absorbent, have the heavy metal adsorption characteristic of Mn oxide concurrently, the magnetic separating property simultaneously with magnetic-particle, conveniently realize Separation of Solid and Liquid, reduce processing cost, the metal water of attaching most importance to is provided by efficient, the economical and practical technology that provides.
2. preparation technology is simple, and cost is relatively cheap, and the prepared shell-core structure magnetic heavy metal absorbent of the present invention is the aggregation of nano particle, has larger surface area.
3. the prepared shell-core structure magnetic heavy metal absorbent of the present invention has good magnetic, can carry out Magnetic Isolation, and simple to operate, speed is fast, and efficiency is high, and energy consumption is low, and can not cause secondary pollution.
4. the prepared shell-core structure magnetic heavy metal absorbent of the present invention all has excellent absorption property to heavy metal ion such as lead, cadmium, mercury, copper, nickel, zinc, cobalts in water body, and adsorption rate is fast, and adsorption capacity is high.Even when heavy metal concentration is lower, also there is good removal effect.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of shell-core structure magnetic heavy metal absorbent of the present invention.
Fig. 2 is that shell-core structure magnetic heavy metal absorbent of the present invention is to Pb
2+adsorption isothermal curve figure.
Fig. 3 is that shell-core structure magnetic heavy metal absorbent of the present invention is to Cu
2+adsorption isothermal curve figure.
The specific embodiment
Take iron chloride and frerrous chloride as raw material, preparation Fe
3+and Fe
2+mol ratio is the mixed solution 500mL of 2:1, to the sodium hydroxide solution that slowly adds 2mol/L in mixed solution, stirs, until the pH of mixed liquor is 11.Mixed solution is at 60 ℃ of reaction 2h, and ageing 30min under room temperature carries out Separation of Solid and Liquid under magnetic fields, with deionized water washing 3-4 time, obtains kernel magnetic Nano ferrimanganic compound Mn
xfe
3-xo
4(x=0).Take kernel Mn prepared by 1.0g
xfe
3-xo
4(x=0), mix with the PEG solution of 100mL2%, after mixing, mix with the manganese chloride solution of 120mL0.036mol/L, be heated to 60 ℃, slowly drip again the liquor potassic permanganate of 80mL0.036mol/L, vigorous stirring is to being added dropwise to complete, and room temperature reaction, reacts gained manganese dioxide and be directly coated on core surface formation shell, then will make material magnetic from solution separated, with deionized water washing 3-4 time, oven dry at 80 ℃, obtains with magnetic Nano ferrimanganic compound Mn
xfe
3-xo
4(x=0) be kernel, the shell-core structure magnetic heavy metal absorbent (referring to Fig. 1) that the manganese dioxide of take is shell.
Embodiment 2
Take ferric sulfate, ferrous sulfate and manganese sulfate as raw material, preparation Fe
3+, Fe
2+with Mn
2+mol ratio is the molten 500mL of the mixing of 2:0.5:0.5, to the potassium hydroxide solution that slowly adds 2mol/L in mixed solution, stirs, until the pH of mixed liquor is 11.Mixed solution is at room temperature reaction 2h, and ageing 30min under room temperature carries out Separation of Solid and Liquid under magnetic fields, with deionized water washing 3-4 time, obtains kernel magnetic Nano ferrimanganic compound Mn
xfe
3-xo
4(x=0.5).Take kernel Mn prepared by 1.0g
xfe
3-xo
4(x=0.5), mix with the PEG solution of 50mL5%, after mixing, mix with the manganese chloride solution of 120mL0.036mol/L, be heated to 60 ℃, slowly drip again the sodium permanganate solution of 80mL0.036mol/L, vigorous stirring is to being added dropwise to complete, and room temperature reaction, reacts gained manganese dioxide and be directly coated on core surface formation shell, then will make material magnetic from solution separated, with deionized water washing 3-4 time, oven dry at 80 ℃, obtains with magnetic Nano ferrimanganic compound Mn
xfe
3-xo
4(x=0.5) be kernel, the shell-core structure magnetic heavy metal absorbent that the manganese dioxide of take is shell.
Embodiment 3
Take ferric nitrate and manganese nitrate as raw material, preparation Fe
3+with Mn
2+mol ratio is the mixed solution 500mL of 2:1, to the sodium hydroxide solution that slowly adds 2mol/L in mixed solution, stirs, until the pH of mixed liquor is 11.Mixed solution is at 60 ℃ of reaction 2h, and ageing 30min under room temperature carries out Separation of Solid and Liquid under magnetic fields, with deionized water washing 3-4 time, obtains kernel magnetic Nano ferrimanganic compound Mn
xfe
3-xo
4(x=1).Take kernel Mn prepared by 1.0g
xfe
3-xo
4(x=1), mix with the PEG solution of 20mL10%, after mixing, mix with the manganese nitrate solution of 200mL0.036mol/L, be heated to 60 ℃, slowly drip again the sodium permanganate solution of 40mL0.036mol/L, vigorous stirring is to being added dropwise to complete, and room temperature reaction, reacts gained manganese sesquioxide managnic oxide and be directly coated on core surface formation shell, then will make material magnetic from solution separated, with deionized water washing 3-4 time, oven dry at 80 ℃, obtains with magnetic Nano ferrimanganic compound Mn
xfe
3-xo
4(x=1) be kernel, the shell-core structure magnetic heavy metal absorbent that the manganese sesquioxide managnic oxide of take is shell.
Shell-core structure magnetic heavy metal absorbent prepared by above embodiment there is nanostructured, particle size range is 10nm～250nm, specific area is 70～120m
2/ g, saturation magnetization is 35～55Am
2kg
-1, under the effect of externally-applied magnetic field, can carry out magnetic separation.
Application examples 1
Application in wastewater treatment.Certain lead waste water, Pb
2+concentration is 100mg/L, wastewater pH 5.0.Get 1 liter of waste water, add 0.5g above-described embodiment to prepare gained shell-core structure magnetic heavy metal absorbent, carry out Separation of Solid and Liquid after being uniformly mixed 1 hour, record water outlet Pb
2+concentration be less than 0.5mg/L, Pb
2+clearance is higher than 99.5%.
Application examples 2
Application in wastewater treatment.Certain lead waste water, Pb
2+concentration is 1.0mg/L, wastewater pH 5.0.Get 1 liter of waste water, add 0.1g above-described embodiment to prepare gained shell-core structure magnetic heavy metal absorbent, carry out Separation of Solid and Liquid after being uniformly mixed 1 hour, record water outlet Pb
2+concentration be less than 0.01mg/L, Pb
2+clearance is higher than 99%.
Application examples 3
Application in wastewater treatment.Certain lead waste water, Cu
2+concentration is 10mg/L, wastewater pH 5.0.Get 1 liter of waste water, add 0.5g above-described embodiment to prepare gained shell-core structure magnetic heavy metal absorbent, carry out Separation of Solid and Liquid after being uniformly mixed 1 hour, record water outlet Cu
2+concentration be less than 0.2mg/L, Cu
2+clearance is higher than 98%.
Application examples 4
Application in wastewater treatment.Certain lead waste water, Cu
2+concentration is 2mg/L, wastewater pH 5.0.Get 1 liter of waste water, add 0.2g above-described embodiment to prepare gained shell-core structure magnetic heavy metal absorbent, carry out Separation of Solid and Liquid after being uniformly mixed 1 hour, record water outlet Cu
2+concentration be less than 0.05mg/L, Cu
2+clearance is higher than 97.5%.
Claims (10)
1. a shell-core structure magnetic heavy metal absorbent, is characterized in that: magnetic Nano ferrimanganic compound Mn
xfe
3-xo
4(x=0～1) is kernel, the shell-core structure magnetic heavy metal absorbent that Mn oxide is shell.
2. by shell-core structure magnetic heavy metal absorbent claimed in claim 1, it is characterized in that: described kernel is that one or more in soluble ferric iron salt, soluble ferrite and soluble manganese salt are raw material reaction gained magnetic Nano ferrimanganic compound.
3. by shell-core structure magnetic heavy metal absorbent claimed in claim 1, it is characterized in that: described shell is that solubility permanganate and soluble manganese salt are raw material reaction gained Mn oxide.
4. by shell-core structure magnetic heavy metal absorbent claimed in claim 2, it is characterized in that: described soluble ferric iron salt is iron chloride, ferric nitrate, ferric sulfate or their mixture; Described soluble ferrite is frerrous chloride and/or ferrous sulfate; Described soluble manganese salt is one or more the mixing in manganese chloride, manganese nitrate, manganese sulfate, manganese carbonate.
5. by shell-core structure magnetic heavy metal absorbent claimed in claim 3, it is characterized in that: described solubility permanganate is potassium permanganate and/or sodium permanganate; Described soluble manganese salt is one or more the mixing in manganese chloride, manganese nitrate, manganese sulfate, manganese carbonate.
6. a preparation method for shell-core structure magnetic heavy metal absorbent claimed in claim 1, is characterized in that:
1) preparation of kernel magnetic Nano ferrimanganic compound: one or more of take in soluble ferric iron salt, soluble ferrite and soluble manganese salt are made into mixed solution as raw material, pH of mixed is adjusted to 6～12, and ℃ reaction in room temperature～100, then ageing, separation, washes to obtain kernel magnetic Nano ferrimanganic compound Mn
xfe
3-xo
4(x=0～1);
2) above-mentioned gained kernel magnetic Nano ferrimanganic compound is mixed with PEG solution, after mixing, mix with soluble manganese salting liquid and solubility permanganate solution again, reaction at room temperature～100 ℃, the surface that reaction gained Mn oxide is directly coated on kernel magnetic Nano ferrimanganic compound forms shell, then by gained separating substances, washing, dry, obtain shell-core structure magnetic heavy metal absorbent.
7. by the preparation method of shell-core structure magnetic heavy metal absorbent claimed in claim 6, it is characterized in that: the mol ratio of described step 1) Raw soluble ferric iron salt, soluble ferrite and soluble manganese salt is 2: (1～0): (0～1).
8. by the preparation method of shell-core structure magnetic heavy metal absorbent claimed in claim 6, it is characterized in that: described step 2), the mol ratio of soluble manganese salt and solubility permanganate is (5: 1)～(3: 2).
9. by the preparation method of shell-core structure magnetic heavy metal absorbent claimed in claim 6, it is characterized in that: the quality of shell-core structure magnetic heavy metal absorbent housing accounts for 0～60% of adsorbent gross mass.
10. an application for shell-core structure magnetic heavy metal absorbent claimed in claim 1, is characterized in that: the application of heavy metal ion in described shell-core structure magnetic heavy metal absorbent adsorbent solution.
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| CN104142355A (en) * | 2014-05-08 | 2014-11-12 | 上海师范大学 | Nuclear magnetic resonance sensor for detecting Cd<2+> ions based on magnetic nanoparticles and preparation method of sensor |
| CN106215948A (en) * | 2016-07-06 | 2016-12-14 | 重庆大学 | A kind of preparation method of manganese dioxide composite magnetic catalyst |
| CN106669614A (en) * | 2017-01-18 | 2017-05-17 | 湖南大学 | Preparation and application of CTAB (cetyl trimethyl ammonium bromide) surface-activated clay mineral-loaded nano metal oxide |
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