CN101664668A - Preparation method and application of core-shell type Fe3O4/C magnetic nano solid extracting agent - Google Patents
Preparation method and application of core-shell type Fe3O4/C magnetic nano solid extracting agent Download PDFInfo
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- CN101664668A CN101664668A CN200910093406A CN200910093406A CN101664668A CN 101664668 A CN101664668 A CN 101664668A CN 200910093406 A CN200910093406 A CN 200910093406A CN 200910093406 A CN200910093406 A CN 200910093406A CN 101664668 A CN101664668 A CN 101664668A
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Abstract
The invention relates to a Fe3O4/C magnetic nano solid extracting agent coated with a novel carbon material, belonging to the field of chemical analysis and test instruments and equipment. The extracting agent simultaneously has large special surface area of nano material, short disperse path, magnetic separation capacity of magnetic material and strong adsorption capacity of carbon material, thereby being very suitable for pretreating large-scale and large-size water samples in batch. In addition, the solid extracting agent is simple to prepare, low in raw material cost, rapid and convenientto extract and friendly to the environment and only needs using a small amount of organic solvent in the whole process.
Description
Technical field
The invention belongs to chemical analysis test instrument and equipment field, relate to the Fe that a kind of novel material with carbon element coats
3O
4Magnetic nano solid extracting agent as the sample pre-treatments material, comes organic pollution in the enrichment large volume environmental water sample with it.
Background technology
The background in present technique field and current situation are roughly as follows: SPE is present widely used more novel environmental sample pre-treating method.SPE has that extraction time is short, the rate of recovery is high, enrichment times is high and the advantage such as organic reagent consumption is few.Nano material has high specific area and remarkable absorption property, but because the nanoparticle particle diameter is too small, carries out the above-mentioned solid phase extraction and goes up sample and cross post and have difficulties.Fe
3O
4Magnetic Nano material not only has the advantage of nano material, also has paramagnetism.During no externally-applied magnetic field, magnetic Nano Fe
3O
4Well do not have agglomeration in the aqueous dispersion, behind the adding externally-applied magnetic field, magnetic nanoparticle is deposited to beaker bottom faster, and upper sample resistance is than the shortcoming of big and nanometer extractant and mother liquor separation difficulty when having overcome general nano material SPE.Simple magnetic Nano Fe
3O
4Its adsorption capacity is limited, therefore need to carry out on its surface suitable modification to improve absorption property.Material with carbon element comprises ketjenblack EC, porous graphite carbon, and activated carbon, CNT etc. have very strong adsorption capacity, are often used as SPE or are adsorbed with the material [1-6] of organic pollutants.Material with carbon element also has certain shortcoming as the SPE material, is difficult to elute [6] too by force as some object and its binding ability.At Fe
3O
4The magnetic Nano surface coats one deck material with carbon element and can effectively address these problems.The core-shell type Fe of preparation
3O
4/ C nano material has kept strong superparamagnetism, the evolving path that the strong absorption property of material with carbon element, nano particle are short and big specific area.Paramagnetism so that adsorbed under the nano material outside magnetic field effect of object is separated from solution easily, surface coated material with carbon element has guaranteed the absorption to object, and the evolving path that nano particle is short is so that material can be realized quick adsorption and the easier wash-out to object.The Fe of preparation
3O
4/ C nano material has good stability, can be applicable to the preliminary treatment of various environmental water samples.
[1]Y.Q.Cai，G?B.Jiang，J.Y.Liu，Q.X.Zhou.Anal.Chem.75(2003)2517-2521.
[2]M.J.Page，Y.Ma，H.W.Qi，E.Healy，J.Trolinger.J.Agric.Food.Chem.45(1997)3095-3099.
[3]Z.Q.Gong，K.Alef，B.M.Wilke，P.J.Li.J.Hazard.Mater.143(2007)372-378.
[4]M.S.Kim，T.W.Kang，H.Pyo，J.Yoon，K.Choi，J.K.Hong.J.Chromatogr.A.1208(2008)25-33.
[5]W.D.Wang，Y.M.Huang，W.Q.Shu，J.Cao.J?Chromatogr.A.1173(2007)27-36.
[6]M.C.Hennion.J.Chromatogr.A.885(2000)73-95.
Summary of the invention
The core-shell type Fe of the present invention's preparation
3O
4/ C magnetic nano solid extracting agent, the magnetic separating power of the magnetic material that got both, the strong extracting power of material with carbon element, the characteristics of nano material quick adsorption and easy wash-out.At first having prepared particle diameter with coprecipitation is magnetic Nano Fe about 10nm
3O
4, again with the magnetic Nano Fe that makes
3O
4Be distributed in the certain density glucose solution, make glucose molecule at magnetic Nano Fe
3O
4Surface dewatering condensation carbonization, obtain core-shell type Fe
3O
4/ C magnetic Nano material.Because the incomplete carbonization of glucose is that material surface has abundant active group, can be in the aqueous solution stable dispersion.To from water sample, extract object, only need to make core-shell type Fe
3O
4/ C nano material is dispersed in the aqueous solution and stirs, and need not to regulate acidity and adds other additive, also need not equilibration time, and directly the magnetic separation can be finished extraction process.The nano material of separating concentrates laggard liquid chromatogram measuring object concentration with eluent again with a spot of organic solvent wash-out.Whole pretreatment process very fast, facility.Therefore, core-shell type Fe
3O
4Aspect the concentration and separation of/C magnetic nano solid extracting agent organic pollution in the large volume environmental sample good application prospect is arranged.
Compare with existing traditional SPE material sample pre-treating method, this extractant has the following advantages:
1. the extractant consumption is few, the extraction efficiency height.Generally use at present solid extracting agent bigger as particle diameter, its specific area is littler, and loading capacity is lower, and extraction penetration volume and enrichment times are just littler; The Fe of preparation
3O
4/ C magnetic Nano material particle diameter is tens nanometers, and surface area is big, the loading capacity height, and adsorption power is strong.
2. environmental friendliness.In preparation of adsorbent and SPE process, need a spot of organic solvent when having only wash-out, in water sample, do not introduce any poisonous and hazardous material, environmentally friendly.
3. easy and simple to handle, rate of extraction is fast.On the one hand, because the nano material particle diameter is little, the evolving path is short, therefore can realize quick adsorption; On the other hand, make Fe
3O
4/ C magnetic Nano material has good superparamagnetism, uses a strong magnet just can easily realize that extractant and mother liquor are quick and complete and separates.It is bigger to go up the sample resistance when magnetic Nano material has overcome general nano material SPE, and the shortcoming that wastes time and energy is fit to batch preliminary treatment of extensive large volume water sample very much.
4. with low cost, preparation is simple.The primary raw material of using in the preparation process is FeCl
36H
2O, FeCl
24H
2O, glucose, cheap, it is convenient to buy.
5. good stability, renewable and recycling.The object that is adsorbed on the nano material can elute with a small amount of organic solvent easily, and the material with carbon element of coating and magnetic kernel can be not destroyed, can be used for the extraction of next water sample.Therefore, Fe
3O
4/ C magnetic nano solid extracting agent has updatability, has overcome to a certain extent the shortcoming of general solid phase extraction adsorbents weak point in service life and extraction precision difference.
Description of drawings
Fig. 1 is the synthetic schematic diagram of magnetic nano-material extractant of the present invention;
Fig. 2 is the transmission electron microscope photo of magnetic nano-material extractant of the present invention, (a) Fe
3O
4, (b) Fe
3O
4/ C;
Fig. 3 is the energy spectrogram of magnetic nano-material extractant of the present invention;
Fig. 4 is the XRD spectra of magnetic nano-material extractant of the present invention;
Fig. 5 is the hysteresis curve of magnetic nano-material extractant of the present invention;
Fig. 6 is a magnetic Nano material SPE flow chart of the present invention
The specific embodiment
Further set forth the present invention below in conjunction with preferred embodiment, but these embodiment only limit to illustrate the present invention, can not limit the scope of the invention.
Embodiment 1: the preparation method of magnetic nano-material extractant of the present invention
Core-shell type Fe provided by the present invention
3O
4The synthetic schematic diagram of/C magnetic nano-material extractant as shown in Figure 1, its concrete preparation method can be divided into following two steps:
At first, preparation nano-sized iron oxide.At first with 5.2g FeCl
36H
2O and 2.0g FeCl
24H
2O and 0.85mL concentrated hydrochloric acid are dissolved in 25mL in advance through N
2In the aqueous solution of deoxidation; Under violent mechanical agitation, above solution dropwise is added drop-wise in the 250mL 1.5mol/LNaOH aqueous solution, drip the back and continued stirring reaction 0.5 hour; Reaction utilizes externally-applied magnetic field that the magnetic nanoparticle that makes is separated after finishing.
Secondly, preparation core-shell type Fe
3O
4/ C magnetic Nano material.Get the Fe of 1/4th preparations
3O
4Magnetic-particle with washed with de-ionized water three times, cleans twice with ethanol again, is distributed to then in the glucose solution of 0.5M (80mL), behind the ultrasonic 20min, this mixed solution forwarded in the 100mL reactor seals, at 180 ℃ of reactions 4 hours, the Fe that obtains
3O
4/ C nano material is cleaned repeatedly with deionized water and methyl alcohol, remove be distributed in the deionized water behind the responseless impurity stand-by.
Embodiment 2: the structural characterization of magnetic nano-material extractant of the present invention
Present embodiment carries out structural characterization for the magnetic nano-material extractant to embodiment 1 preparation, and is specific as follows:
1. particle diameter and morphology characterization
Adopt transmission electron microscope (TEM) to observe the core-shell type Fe of preparation
3O
4/ C magnetic Nano material, its TEM photo as shown in Figure 2.As can be seen from Figure 2, prepared Fe
3O
4/ C nano particle is spherical substantially, and the darker part of inner layer color is Fe
3O
4Magnetic nuclear, particle diameter is about 10nm, and the more shallow part of outer color is the material with carbon element on coating, and clad is 2-5nm, and whole nano particle presents obvious nucleocapsid structure.
2. elementary analysis
Adopt the X-gamma ray spectrometer to measure the Fe of preparation
3O
4And Fe
3O
4The content of each element of/C magnetic nanoparticle.Result by Fig. 3 can find out nanometer Fe
3O
4Middle essential element is Fe and O, only contains a small amount of carbon, after the carbon coated, and Fe
3O
4The molar percentage of the carbon the in/C nano particle is up to 54.4%, and the content of Fe and O descends greatly, and this shows that material with carbon element has been coated to magnetic Nano Fe by success
3O
4On.
3. crystal formation characterizes
Utilize powder x-ray diffraction instrument (XRD) to characterize Fe
3O
4And Fe
3O
4The crystal type of/C, its XRD spectra as shown in Figure 4.Can find out magnetic Fe with the contrast of X-ray diffraction card
3O
4The crystal structure of nano particle is spinelle, coated material with carbon element after, the quantity of its diffraction maximum does not increase, the position does not change yet, just the intensity of diffraction maximum slightly reduces, and this shows that the material with carbon element in the coating is agraphitic carbon, the process kernel magnetic Nano Fe of coating
3O
4Crystal formation do not change.
4. magnetic characterization
Adopt vibrating specimen magnetometer to characterize Fe
3O
4And Fe
3O
4The magnetic of/C nano particle, its hysteresis curve is seen Fig. 5.Fe
3O
4And Fe
3O
4The remanent magnetism of/C nano particle and coercivity are zero, show typical superparamagnetism, Fe
3O
4The saturated magnetic intensity of nano particle is 59.87emu/g, Fe
3O
4The saturated magnetic intensity of/C nano particle is 43.75emu/g, and after the carbon coated, saturated magnetic intensity is decreased significantly, and this is because the material with carbon element on coating does not have the magnetic response performance.Big saturated magnetic intensity and superparamagnetism have guaranteed can separate faster from solution under the effect of preparation magnetic nanometer adsorbent outside magnetic field, remove external magnetic field after, can be distributed in the solution easily again.
Embodiment 3: the absorption property test of magnetic nano-material extractant of the present invention
Present embodiment is selected induced by alkyl hydroxybenzene pollutant bisphenol-A (BPA), nonyl phenol (4-OP) and octyl phenol (4-NP), phthalate pollutant phthalandione n-propyl (DPP), the positive butyl ester of phthalandione (DBP), phthalandione cyclohexyl (DCP) and phthalandione n-octyl (DOP), polyaromatic hydrocarbon pollutant phenanthrene (PhA), fluoranthene (FluA), pyrene (Pyr), benzo [a] anthracene (BaA), benzo [b] fluoranthene (BbF), benzo [a] pyrene (BaP), benzo [g, h, i] perylene (BghiP), Deng representative, the absorption property of preparation magnetic nano-material extractant among the embodiment 1 is tested as common pollutant.
The operating procedure of test as shown in Figure 6, concrete experimentation is as follows: the standard liquid that adds an amount of each pollutant in water sample, the magnetic Nano material solid phase extraction adsorbents that the back adding that stirs prepares, stir, the container that water sample is housed placed carry out magnetic on the strong magnets and separate, after 30 minutes, the magnetic Nano adsorbent can be separated from solution fully, and the complete clear solutions in upper strata is outwelled; Disposable adding 8mL acetonitrile in the adsorbent of separating, the object of ultrasonic wash-out absorption in 20 seconds relends magnetic assist iron adsorbent is separated from eluent, eluent N
2After drying up residual residue is dissolved in the 1mL acetonitrile, utilizes the concentration of each object in the high-performance liquid chromatogram determination concentrate, calculate the rate of recovery of each pollutant again.For polyaromatic hydrocarbon pollutant, only need to use the Fe of 0.05g in the 1000mL ambient water sample
3O
4/ C magnetic Nano extractant, its rate of recovery all can reach more than 80%; For induced by alkyl hydroxybenzene and phthalate pollutant, the extraction object needs the 0.1g adsorbent from 500mL ambient water sample, and the rate of recovery all can reach more than 80%.The mark-on recovery result who running water, rainwater, river, sewage treatment plant is gone out ambient water samples such as saliva is satisfactory, the reappearance RSD 8% of analysis result.
Claims (6)
1. prepared a kind of nano material with unique physicochemical property--the Fe that material with carbon element coats
3O
4Magnetic nano solid extracting agent.
2. described according to right 1, the magnetic nano solid extracting agent that this technology makes is with Fe
3O
4Be nuclear, material with carbon element is shell.
3. according to the requirement of right 1, generate Fe with the method for co-precipitation
3O
4Magnetic nanoparticle is with the Fe that makes
3O
4Nano particle is ultrasonic to be distributed in the glucose solution, and confined reaction under 180 ℃ high temperature, the product that obtains repeatedly clean with deionized water and methyl alcohol and obtain Fe
3O
4/ C magnetic Nano material.
4. designed a kind of Fe
3O
4/ C magnetic nano solid extracting agent extracts the method for object, and is applied to the enrichment of organic pollution in the large volume ambient water sample.
5. according to right 4 described methods, with Fe
3O
4/ C magnetic nano solid extracting agent is distributed in the 500-1000mL water sample, stirs, and rubidium-iron-boron magnets is placed the container bottom that holds water sample, isolates solid extracting agent, with the 8mL acetonitrile object is eluted from solid extracting agent.
6. according to right 4 described methods, wherein said organic pollution comprises alkylphenol compounds, phthalate compound and polycyclic arene compound.
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