CN103506065B - A kind of Magnetic heavy metal adsorbent with casing-core structure and preparation method thereof - Google Patents
A kind of Magnetic heavy metal adsorbent with casing-core structure and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to water treatment applications, specifically a kind of Magnetic heavy metal adsorbent with casing-core structure and preparation method thereof.With magnetic Nano ferrimanganic compound Mn
xfe
3-xo
4(x=0 ~ 1) is kernel, and Mn oxide is the Magnetic heavy metal adsorbent with casing-core structure of shell.Magnetic heavy metal adsorbent with casing-core structure prepared by the present invention is the aggregation of nano particle, and particle size range is 10nm ~ 250nm, and specific area is 70 ~ 120m
2/ g, 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, when heavy metal concentration is lower, also has good removal effect; And have good magnetic, saturation magnetization is 35 ~ 55Am
2kg
-1, can carry out Magnetic Isolation, separating rate is fast, and simple to operate, efficiency is high, and energy consumption is low, and can not cause secondary pollution.
Description
Technical field
The present invention relates to water treatment applications, specifically a kind of Magnetic heavy metal adsorbent with casing-core structure and preparation method thereof.
Background technology
Heavy metal has enriching, is difficult to degrade in the environment.In the exploitation of heavy metal, smelting, process, cause many heavy metals as lead, mercury, cadmium, cobalt etc. enter air, water, soil causes serious environmental pollution.With the heavy metal that waste water is discharged, even if concentration is little, also can accumulate in algae and bed mud, be adsorbed by fish and shellfish body surface, produce food chain and concentrate, thus cause public hazards.Such as, 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 the absorption of microorganism or plant, accumulation, enrichment to remove the method for heavy metal in waste water, comprise the methods such as biological adsorption, bioflocculation, phytoremediation, current many places are in developing stage.(2) chemical method, comprises chemical precipitation method, oxidation-reduction method, electrochemical process etc., and be mainly applicable to the process containing higher concentration effluent containing heavy metal ions, 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, thus reach the object removing heavy metal in water, this method is simple, and applicable system is many, and secondary pollution is little and cost is low, be applied in heavy metal containing wastewater treatment, be particularly useful for the water treatment that content of beary metal is lower.
At present, sorbing material for heavy metal has bentonite, zeolite, red mud, cocoanut shell, coated sand, activated alumina, the metal oxide of active carbon and natural or synthesis and hydrous oxide etc. thereof, 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, can effective heavy metal contaminants in Adsorption water, but its particle diameter is less, the separation method of traditional filtering is adopted then to there is easy loss, separation difficulty, inefficient problem in actual applications.And Magneto separate utilizes the effect of externally-applied magnetic field to make magnetic-particle and namagnetic substance separate, the application in water treatment more and more receives publicity.Compared with traditional filtering separation method, magnetic separation technique is simply efficient, can realize Separation of Solid and Liquid quickly and easily.
Summary of the invention
The object of the invention is to provide a kind of Magnetic heavy metal adsorbent with casing-core structure and preparation method thereof.
For achieving the above object, the present invention adopts technical scheme to be:
A kind of Magnetic heavy metal adsorbent with casing-core structure: magnetic Nano ferrimanganic compound Mn
xfe
3-xo
4(x=0 ~ 1) is kernel, and Mn oxide is the Magnetic heavy metal adsorbent with casing-core structure of shell.
Described kernel is soluble ferric iron salt, one or more in soluble ferrite and soluble manganese salt are raw material reaction gained magnetic Nano ferrimanganic compound.
Described shell is solubility permanganate and soluble manganese salt is 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 the mixing of one or more in manganese chloride, manganese nitrate, manganese sulfate, manganese carbonate.
Described solubility permanganate is potassium permanganate and/or sodium permanganate; Described soluble manganese salt is the mixing of one or more in manganese chloride, manganese nitrate, manganese sulfate, manganese carbonate.
A kind of preparation method of Magnetic heavy metal adsorbent with casing-core structure:
1) preparation of kernel magnetic Nano ferrimanganic compound: with one or more in soluble ferric iron salt, soluble ferrite and soluble manganese salt for raw material is made into mixed solution, pH of mixed is adjusted to 6 ~ 12, and DEG C reaction in room temperature ~ 100, then ageing, be separated, wash 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, PEG solution final concentration is made to be 0.1 ~ 15%, mix with soluble manganese salting liquid and solubility permanganate solution again after mixing, reaction at room temperature ~ 100 DEG C, 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, drying, namely obtains Magnetic heavy metal adsorbent with casing-core structure.
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) in the pH value of mixed liquor.
Described step 2) in the mol ratio of soluble manganese salt and solubility permanganate be (5: 1) ~ (3: 2).
The quality of Magnetic heavy metal adsorbent with casing-core structure housing accounts for 0 ~ 60% of adsorbent gross mass.
An application for Magnetic heavy metal adsorbent with casing-core structure, the application of heavy metal ion in described Magnetic heavy metal adsorbent with casing-core structure adsorbent solution.
Described heavy metal ion is one or more in lead, cadmium, mercury, copper, nickel, zinc and cobalt.
The advantage that the present invention has:
1. the present invention is by magnetic-particle and Mn oxide compound, form magnetic heavy metal adsorbent, have the heavy metal adsorption characteristic of Mn oxide concurrently, there is the Magneto separate performance of magnetic-particle simultaneously, conveniently realize Separation of Solid and Liquid, reduce processing cost, metal water of attaching most importance to process provides efficient, economical and practical technology.
2. preparation technology is simple, and relative inexpensiveness, the Magnetic heavy metal adsorbent with casing-core structure prepared by the present invention is the aggregation of nano particle, has larger surface area.
3. the Magnetic heavy metal adsorbent with casing-core structure prepared by the present invention has good magnetic, can carry out Magnetic Isolation, simple to operate, and speed is fast, and efficiency is high, and energy consumption is low, and can not cause secondary pollution.
4. the Magnetic heavy metal adsorbent with casing-core structure prepared by 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 if when heavy metal concentration is lower, also there is good removal effect.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of Magnetic heavy metal adsorbent with casing-core structure of the present invention.
Fig. 2 is that Magnetic heavy metal adsorbent with casing-core structure of the present invention is to Pb
2+adsorption isothermal curve figure.
Fig. 3 is that Magnetic heavy metal adsorbent with casing-core structure of the present invention is to Cu
2+adsorption isothermal curve figure.
Detailed description of the invention
Embodiment 1
With iron chloride and frerrous chloride for raw material, preparation Fe
3+and Fe
2+mol ratio is the mixed solution 500mL of 2:1, slowly adds the sodium hydroxide solution of 2mol/L in mixed solution, stirs, until the pH of mixed liquor is 11.Mixed solution is at 60 DEG C of reaction 2h, and ageing 30min under room temperature, carries out Separation of Solid and Liquid, spend deionized water 3-4 time under magnetic fields, 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%, mix with the manganese chloride solution of 120mL0.036mol/L after mixing, be heated to 60 DEG C, slowly drip the liquor potassic permanganate of 80mL0.036mol/L again, 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 obtain material Magneto separate from solution, spend deionized water 3-4 time, dry at 80 DEG C, obtain with magnetic Nano ferrimanganic compound Mn
xfe
3-xo
4(x=0) being kernel, take manganese dioxide as the Magnetic heavy metal adsorbent with casing-core structure (see Fig. 1) of shell.
Embodiment 2
With ferric sulfate, ferrous sulfate and manganese sulfate for raw material, preparation Fe
3+, Fe
2+with Mn
2+mol ratio is the molten 500mL of mixing of 2:0.5:0.5, slowly adds the potassium hydroxide solution of 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, spend deionized water 3-4 time under magnetic fields, 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%, mix with the manganese chloride solution of 120mL0.036mol/L after mixing, be heated to 60 DEG C, slowly drip the sodium permanganate solution of 80mL0.036mol/L again, 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 obtain material Magneto separate from solution, spend deionized water 3-4 time, dry at 80 DEG C, obtain with magnetic Nano ferrimanganic compound Mn
xfe
3-xo
4(x=0.5) being kernel, take manganese dioxide as the Magnetic heavy metal adsorbent with casing-core structure of shell.
Embodiment 3
With ferric nitrate and manganese nitrate for raw material, preparation Fe
3+with Mn
2+mol ratio is the mixed solution 500mL of 2:1, slowly adds the sodium hydroxide solution of 2mol/L in mixed solution, stirs, until the pH of mixed liquor is 11.Mixed solution is at 60 DEG C of reaction 2h, and ageing 30min under room temperature, carries out Separation of Solid and Liquid, spend deionized water 3-4 time under magnetic fields, namely 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%, mix with the manganese nitrate solution of 200mL0.036mol/L after mixing, be heated to 60 DEG C, slowly drip the sodium permanganate solution of 40mL0.036mol/L again, 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 obtain material Magneto separate from solution, spend deionized water 3-4 time, dry at 80 DEG C, obtain with magnetic Nano ferrimanganic compound Mn
xfe
3-xo
4(x=1) being kernel, take manganese sesquioxide managnic oxide as the Magnetic heavy metal adsorbent with casing-core structure of shell.
Magnetic heavy metal adsorbent with casing-core structure prepared by above embodiment there is nanostructured, particle size range is 10nm ~ 250nm, and specific area is 70 ~ 120m
2/ g, saturation magnetization is 35 ~ 55Am
2kg
-1, can Magneto separate be carried out under the effect of externally-applied magnetic field.
Application examples 1
Application in the treatment of waste water.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 and prepare gained Magnetic heavy metal adsorbent with casing-core structure, 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 the treatment of waste water.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 and prepare gained Magnetic heavy metal adsorbent with casing-core structure, 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 the treatment of waste water.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 and prepare gained Magnetic heavy metal adsorbent with casing-core structure, 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 the treatment of waste water.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 and prepare gained Magnetic heavy metal adsorbent with casing-core structure, 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 (7)
1. a Magnetic heavy metal adsorbent with casing-core structure, is characterized in that: magnetic Nano ferrimanganic compound Mn
xfe
3-xo
4for kernel, wherein 0 < x≤1, Mn oxide is the Magnetic heavy metal adsorbent with casing-core structure of shell;
Described kernel is several for raw material reaction gained magnetic Nano ferrimanganic compound in soluble ferric iron salt, soluble ferrite and soluble manganese salt;
Described shell is solubility permanganate and soluble manganese salt is raw material reaction gained Mn oxide.
2., by Magnetic heavy metal adsorbent with casing-core structure according to claim 1, 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 the mixing of one or more in manganese chloride, manganese nitrate, manganese sulfate, manganese carbonate.
3., by Magnetic heavy metal adsorbent with casing-core structure according to claim 1, it is characterized in that: described solubility permanganate is potassium permanganate and/or sodium permanganate; Described soluble manganese salt is the mixing of one or more in manganese chloride, manganese nitrate, manganese sulfate, manganese carbonate.
4. a preparation method for Magnetic heavy metal adsorbent with casing-core structure according to claim 1, is characterized in that:
1) preparation of kernel magnetic Nano ferrimanganic compound: be made into mixed solution for raw material with several in soluble ferric iron salt, soluble ferrite and soluble manganese salt, pH of mixed is adjusted to 6 ~ 12, and DEG C reaction in room temperature ~ 100, then ageing, be separated, wash to obtain kernel magnetic Nano ferrimanganic compound Mn
xfe
3-xo
4, wherein 0 < x≤1;
2) above-mentioned gained kernel magnetic Nano ferrimanganic compound is mixed with PEG solution, mix with soluble manganese salting liquid and solubility permanganate solution again after mixing, reaction at room temperature ~ 100 DEG C, 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, namely obtain Magnetic heavy metal adsorbent with casing-core structure.
5., by the preparation method of Magnetic heavy metal adsorbent with casing-core structure according to claim 4, it is characterized in that: described step 1) mol ratio of Raw soluble ferric iron salt, soluble ferrite and soluble manganese salt is 2: (1 ~ 0.5): (0.5 ~ 1).
6., by the preparation method of Magnetic heavy metal adsorbent with casing-core structure according to claim 4, it is characterized in that: described step 2) in soluble manganese salt be (5: 1) ~ (3: 2) with the mol ratio of solubility permanganate.
7., by the preparation method of Magnetic heavy metal adsorbent with casing-core structure according to claim 4, it is characterized in that: the quality of Magnetic heavy metal adsorbent with casing-core structure housing accounts for 38.5 ~ 60% of adsorbent gross mass.
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