CN102784624A - Preparation method and use of carbon coated magnetic adsorption material - Google Patents
Preparation method and use of carbon coated magnetic adsorption material Download PDFInfo
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- CN102784624A CN102784624A CN2012102540842A CN201210254084A CN102784624A CN 102784624 A CN102784624 A CN 102784624A CN 2012102540842 A CN2012102540842 A CN 2012102540842A CN 201210254084 A CN201210254084 A CN 201210254084A CN 102784624 A CN102784624 A CN 102784624A
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Abstract
The invention discloses a preparation method of a carbon coated magnetic adsorption material. The preparation method which adopts a carbon source citric acid and nickel nitrate as raw materials comprises the following steps: dissolving the nickel nitrate and the carbon source in an aqueous ethanol solution at room temperature, wherein the mass ratio of the nickel nitrate to the carbon source is 1:3-10, and the volume ratio of ethanol to water of the aqueous ethanol solution is 1:1-5; uniformly stirring and mixing the solution; evaporating a solvent to obtain a solid mixture; grinding the mixture; and carbonizing through calcining the mixture in an inert gas environment to obtain the magnetic adsorption material having a carbon coating structure. The magnetic adsorption material prepared through the method has the advantages of carbon coating structure, uniform particle dimension distribution, large specific surface area, and realization of the rapid adsorption of pollutive heavy metal ions in sewage within a short period of time. Simultaneously the adsorption material has a magnetic property, so the adsorption material can realize quick separation and recovery under the action of an external magnetic field without the generation of secondary pollution. The method has the advantages of simple and safe operation, low cost, no environmental pollution, and according with practical production needs.
Description
One, technical field
The present invention relates to a kind of preparation method of functional material.Specifically, be a kind of preparation method of charcoal coated magnetic sorbing material and the application of this sorbing material polluted heavy metals ions in administering sewage.
Two, background technology
Because human exploitation, smelting, processing and commercial manufacturing activities to heavy metal is increasing, causes heavy metal pollution of water body to increase the weight of, and ecological environment and human health have been caused certain harm.Can produce the waste water of precious metals such as containing gold and silver in addition in industries such as chemical industry, plating, manufacturings.Along with improving constantly of living standard, people are to environment, health, food-safety problem growing interest.Therefore, from healthy with economic angle, optionally removal, some precious metal of recovery and reuse are very important.
In the existing technology, there is several different methods can realize the removal of heavy metal ion, like chemical precipitation method, ion floatation method, electrodeposit method, ion-exchange, electroosmose process, evaporation etc.These methods are at cost, efficient, complexity and cause the secondary pollution aspect to exist certain limitation.And as a kind of simple, method that economy can efficiently be removed polluted heavy metals ion in the water, absorption method receives widely in recent years and pays close attention to, studies and use.Had by the adsorbent of development and utilization multiple, like active carbon, silica gel, activated alumina, synthetic polymer and zeolite molecular sieve etc.But because these adsorbents are in stability, adsorption capacity, the adsorptive selectivity aspect is the deficiency of various degrees also, and especially operating process such as their complicated and loaded down with trivial details separation, recovery make it on the popularity of using, receive certain restriction.
Therefore; Select a kind of simple and effective method for preparing new material; Make it have spheric granules micro-/ nanoization, porous, bigger specific area, bigger good characteristics such as saturation magnetization; Under the effect of externally-applied magnetic field, can separate fast, and realize recovery and recycle sorbing material and precious metal ion.Can not only overcome the deficiency in the polluted heavy metals ion traditional treatment method, and highlight remarkable advantages in the recovery that solves sorbing material, heavy metal with aspect utilizing.
Three, summary of the invention
The object of the present invention is to provide a kind of preparation method and application thereof of charcoal coated magnetic sorbing material.This charcoal coated magnetic sorbing material has adsorption effect preferably to the polluted heavy metals ion in the polluted-water, and can realize the recovery of precious metal ion and sorbing material.
Realize technical scheme of the present invention:
Thinking of the present invention is fully to mix in solvent with nickel source and carbon source, and is dry after grinding obtains solid mixture, solid mixture calcined in inert atmosphere obtained charcoal coated magnetic sorbing material.
A kind of preparation method of charcoal coated magnetic sorbing material is characterized in that operating as follows:
1), nickel nitrate and carbon source are pressed mass ratio 1:3 ~ 10 weighings, join in the ethanol water that volume ratio is 1:1 ~ 5, at room temperature stirring and dissolving forms homogeneous phase solution;
2), homogeneous phase solution that step 1) is obtained places 80～120 ℃ baking oven to carry out drying, and is dry after grind and obtain solid mixture;
3), with step 2) solid mixture that obtains places tube furnace, under atmosphere of inert gases, in 550 ~ 850 ℃ of calcining 2 ~ 10h, obtains charcoal coated magnetic sorbing material.
Described carbon source is selected from a kind of in citric acid, glucose, oxalic acid, shitosan or the urea or several.
Described atmosphere of inert gases is by argon gas or nitrogen or nitrogen-argon mixture gas formation.
600 ~ 800 ℃ of preferred calcination temperature.
The purposes of the charcoal coated magnetic sorbing material of this method preparation is as the application that separates, reclaims adsorbent for heavy metal in waste water control.
The present invention adopts cheap carbon compounds such as citric acid as carbon source, is magnetic source with the nickel nitrate.Both are sneaked into evenly stirring in the ethanol water, after solvent evaporated is ground, carry out gentle calcination process again and just can a step obtain charcoal coated magnetic composite.This magnetic adsorptive material of preparing with charcoal clad structure is as a kind of novel surrounding purifying functional material; Can adsorb the polluted heavy metals ion in the sewage within a short period of time; Can realize the recycle of sorbing material and the recovery of precious metal simultaneously; Reduce cost, economical and effective and do not produce secondary pollution is for the production application that enlarges industrial scale provides certain research basis.
Effect of the present invention and advantage:
1, the magnetic adsorptive material that obtains of the inventive method has the charcoal clad structure, Stability Analysis of Structures, and specific area reaches 200m
2G
-1More than.
2, this sorbing material has magnetic, thereby externally just can realize quick separation under the effect in magnetic field, and does not produce secondary pollution.
3, compare with existing synthesizing magnetic material technology, whole technical process preparation method is simple and safe, and cost is low, and productive rate is high, non-environmental-pollution.And absorption polluted heavy metals ion just can reach adsorption equilibrium in 30 ~ 50min.
Four, description of drawings
Figure l is the XRD figure of embodiment 3 prepared samples;
Fig. 2, Fig. 3 are respectively the SEM figure and the TEM figure of embodiment 3 products therefroms; Wherein Fig. 2 is the overall picture of gained magnetic adsorptive material, from figure, can find out that the magnetic adsorptive material that makes has equally distributed microballoon pattern; Fig. 3 is respectively the high resolution structure characteristic of gained sorbing material, can know that from the gained picture magnetic adsorptive material that makes has tangible charcoal clad structure, coating thickness 2-3nm.
Fig. 4 is the N of embodiment 3 gained magnetic adsorptive materials
2Adsorb a desorption curve and a graph of pore diameter distribution; Can get average pore size by pore size distribution curve figure and be about 20nm.
Fig. 5 is that the magnetic material of embodiment 3 gained is to different heavy metal ion (Pb
2+And Cu
2+) adsorption curve figure; From curve map, can obtain adsorption process and in 30 ~ 50min, just can reach adsorption equilibrium, explain that the speed of the magnetic adsorbent adsorbing metal ions that makes is fast, effect is obvious.
Five, the specific embodiment
Further the present invention will be described below in conjunction with accompanying drawing and embodiment.
Embodiment 1
The preparation of charcoal coated magnetic sorbing material
Preparation process is following successively:
1), 3.0g glucose and 1.0g nickel nitrate are joined in the ethanol water that the 80mL volume ratio is 1:1, under magnetic agitation, forms homogeneous phase solution;
2), homogeneous phase solution that step 1) is obtained be heated to 105 ℃ make its dry solid mixture, in mortar, fully grind then.
3), with step 2) solid mixture after grinding, 700 ℃ of argon atmospheres calcining 2h down in tube furnace obtain to have the magnetic adsorptive material of charcoal clad structure.
Embodiment 2
The charcoal coated magnetic sorbing material that is prepared into by embodiment 1 adsorbs lead ion and copper ion experiment in the sewage
1), takes by weighing 3.197g plumbi nitras Pb (NO
3)
2In the volumetric flask of 1000mL, be mixed with concentration is 2gL to solid with dissolved in distilled water
-1Pb
2+Standard liquid:
Take by weighing 7.6039g Gerhardite Cu (NO
3)
23H
2In the volumetric flask of 1000mL, be mixed with concentration is 2gL to the O solid with dissolved in distilled water
-1Cu
2+Standard liquid.
2), the standard liquid that makes of removing step 1 is diluted to 20.0mgL respectively
-1Each 500mL of simulated sewage with subsequent use:
3), lead ion and copper ion experiment in the absorption sewage, experiment is carried out at ambient temperature, need not regulate the pH value of sewage, adding the concentration that is prepared into magnetic adsorptive material by embodiment 1 is 0.8gL
-1, picking up counting after adsorbent evenly spread in the sewage, whole adsorption process keeps stabilizing mechanical to stir, and takes a sample under the time period in different adsorption, and institute's liquid of take a sample gets supernatant fluid filtrate after filtering, filtrates and analyzes with atomic absorption spectrum.Analysis result is depicted as adsorption curve figure.
Embodiment 3
The preparation of charcoal coated magnetic sorbing material
Preparation process is following successively:
1), 5.0g citric acid and 1.0g nickel nitrate are joined in the ethanol water that the 80mL volume ratio is 1:3, under magnetic agitation, forms homogeneous phase solution;
2), homogeneous phase solution that step 1) is obtained be heated to 105 ℃ make its dry solid mixture, in mortar, fully grind then.
3), with step 2) solid mixture after grinding, 600 ℃ of argon atmospheres calcining 2h down in tube furnace obtain to have the magnetic adsorptive material of charcoal clad structure.
Embodiment 4
The charcoal coated magnetic sorbing material that is prepared into by embodiment 3 adsorbs lead ion and copper ion experiment in the sewage
1), takes by weighing 3.197g plumbi nitras Pb (NO
3)
2In the volumetric flask of 1000mL, be mixed with concentration is 2gL to solid with dissolved in distilled water
-1Pb
2+Standard liquid:
Take by weighing 7.6039g Gerhardite Cu (NO
3)
23H
2In the volumetric flask of 1000mL, be mixed with concentration is 2gL to the O solid with dissolved in distilled water
-1Cu
2+Standard liquid.
2), the standard liquid that makes of removing step 1 is diluted to 40.0mgL respectively
-1Each 500mL of simulated sewage with subsequent use:
3), lead ion and copper ion experiment in the absorption sewage, experiment is carried out at ambient temperature, need not regulate the pH value of sewage, adding the concentration that is prepared into magnetic adsorptive material by embodiment 7 is 0.8gL
-1, picking up counting after adsorbent evenly spread in the sewage, whole adsorption process keeps stabilizing mechanical to stir, and takes a sample under the time period in different adsorption, and institute's liquid of take a sample gets supernatant fluid filtrate after filtering, filtrates and analyzes with atomic absorption spectrum.Analysis result is depicted as adsorption curve figure.
Embodiment 5
The preparation of charcoal coated magnetic sorbing material
Preparation process is following successively:
1), 7.5g oxalic acid and 1.0g nickel nitrate are joined in the ethanol water that the 100mL volume ratio is 1:4, under magnetic agitation, forms homogeneous phase solution;
2), homogeneous phase solution that step 1) is obtained be heated to 110 ℃ make its dry solid mixture, in mortar, fully grind then.
3), with step 2) solid mixture after grinding, 650 ℃ of argon atmospheres calcining 3h down in tube furnace obtain to have the magnetic adsorptive material of charcoal clad structure.
Embodiment 6
The charcoal coated magnetic sorbing material that is prepared into by embodiment 5 adsorbs lead ion and copper ion experiment in the sewage
1), takes by weighing 3.197g plumbi nitras Pb (NO
3)
2In the volumetric flask of 1000mL, be mixed with concentration is 2gL to solid with dissolved in distilled water
-1Pb
2+Standard liquid:
Take by weighing 7.6039g Gerhardite Cu (NO
3)
23H
2In the volumetric flask of 1000mL, be mixed with concentration is 2gL to the O solid with dissolved in distilled water
-1Cu
2+Standard liquid.
2), the standard liquid that makes of removing step 1 is diluted to 50.0mgL respectively
-1Each 500mL of simulated sewage with subsequent use:
3), lead ion and copper ion experiment in the absorption sewage, experiment is carried out at ambient temperature, need not regulate the pH value of sewage, adding the concentration that is prepared into magnetic adsorptive material by embodiment 5 is 1.0gL
-1, picking up counting after adsorbent evenly spread in the sewage, whole adsorption process keeps stabilizing mechanical to stir, and takes a sample under the time period in different adsorption, and institute's liquid of take a sample gets supernatant fluid filtrate after filtering, filtrates and analyzes with atomic absorption spectrum.Analysis result is depicted as adsorption curve figure.
Embodiment 7
The preparation of charcoal coated magnetic sorbing material
Preparation process is following successively:
1), 10.0g urea and 1.0g nickel nitrate are joined in the ethanol water that the 100mL volume ratio is 1:5, under magnetic agitation, forms homogeneous phase solution;
2), homogeneous phase solution that step 1) is obtained be heated to 110 ℃ make its dry solid mixture, in mortar, fully grind then.
3), with step 2) solid mixture after grinding, 800 ℃ of argon atmospheres calcining 4h down in tube furnace obtain to have the magnetic adsorptive material of charcoal clad structure.
Embodiment 8
The charcoal coated magnetic sorbing material that is prepared into by embodiment 7 adsorbs lead ion and copper ion experiment in the sewage
1), takes by weighing 3.197g plumbi nitras Pb (NO
3)
2In the volumetric flask of 1000mL, be mixed with concentration is 2gL to solid with dissolved in distilled water
-1Pb
2+Standard liquid:
Take by weighing 7.6039g Gerhardite Cu (NO
3)
23H
2In the volumetric flask of 1000mL, be mixed with concentration is 2gL to the O solid with dissolved in distilled water
-1Cu
2+Standard liquid.
2), the standard liquid that makes of removing step 1 is diluted to 40.0mgL respectively
-1Each 500mL of simulated sewage with subsequent use:
3), lead ion and copper ion experiment in the absorption sewage, experiment is carried out at ambient temperature, need not regulate the pH value of sewage, adding the concentration that is prepared into magnetic adsorptive material by embodiment 7 is 1.0gL
-1, picking up counting after adsorbent evenly spread in the sewage, whole adsorption process keeps stabilizing mechanical to stir, and takes a sample under the time period in different adsorption, and institute's liquid of take a sample gets supernatant fluid filtrate after filtering, filtrates and analyzes with atomic absorption spectrum.Analysis result is depicted as adsorption curve figure.
Claims (5)
1. the preparation method of a charcoal coated magnetic sorbing material is characterized in that operating as follows:
1), nickel nitrate and carbon source are pressed mass ratio 1:3 ~ 10 weighings, joins in the ethanol water that volume ratio is 1:1 ~ 5, at room temperature stir and form homogeneous phase solution;
2), homogeneous phase solution that step 1) is obtained places 80 ~ 120 ℃ baking oven to carry out drying, and is dry after grind and obtain solid mixture;
3), with step 2) solid mixture that obtains places tube furnace, under atmosphere of inert gases, in 550-850 ℃ of calcining 2 ~ 10h, obtains charcoal coated magnetic sorbing material.
2. preparation method according to claim 1 is characterized in that: described carbon source is selected from a kind of in citric acid, glucose, oxalic acid, shitosan or the urea or several.
3. preparation method according to claim 1 is characterized in that: described atmosphere of inert gases is by argon gas or nitrogen or nitrogen-argon mixture gas formation.
4. preparation method according to claim 1 is characterized in that: described preferred calcination temperature is 600 ~ 800 ℃.
5. the purposes of a charcoal coated magnetic sorbing material is characterized in that: in the improvement of polluted heavy metals ion, as the adsorbent that separates, reclaims heavy metal ion.
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| CN103632793A (en) * | 2013-12-03 | 2014-03-12 | 南昌航空大学 | Preparation method for carbon-coated Ni-Zn-Fe magnetic nanometer material taking chitosan as carbon source |
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Patent Citations (2)
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| WO2003060035A1 (en) * | 2001-12-20 | 2003-07-24 | Cognitek Management Systems, Inc. | Composition for enhancing thermal conductivity of a heat transfer medium and method of use thereof |
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