CN104525156B - A kind of magnetic nanometer adsorbent of organic-capping and its preparation method and application - Google Patents
A kind of magnetic nanometer adsorbent of organic-capping and its preparation method and application Download PDFInfo
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- CN104525156B CN104525156B CN201510000987.1A CN201510000987A CN104525156B CN 104525156 B CN104525156 B CN 104525156B CN 201510000987 A CN201510000987 A CN 201510000987A CN 104525156 B CN104525156 B CN 104525156B
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
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- C08F290/00—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups
- C08F290/02—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups on to polymers modified by introduction of unsaturated end groups
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses magnetic nanometer adsorbent of a kind of organic-capping and its preparation method and application, belong to sorbing material preparation field.Use dispersion polymerization processes, with polyethylene glycol methacrylate-styrene polymer and 4 vinylpyridines as monomer, ferroso-ferric oxide is magnetic core, functional group is introduced under the effect of crosslinking agent pentaerythritol triacrylate, a kind of SPE material of synthesis, its even particle size distribution, crystal structure is good, and there is fine absorption property, bonding is firm, stable in properties, favorable reproducibility, and enrichment times is bigger, can use in the range of wider pH, it is adaptable to the enrichment pretreatment of trace Cu (II) in environmental water sample.
Description
Technical field
The invention belongs to sorbing material preparation field, be specifically related to magnetic nanometer adsorbent of a kind of organic-capping and its preparation method and application.
Background technology
With industrial expansion, a large amount of industrial wastewaters containing heavy metal ion produce therewith.But, substantial amounts of sewage is not through necessary process, but is directly discharged in waters, can produce significant damage to ecological environment.At present flame atomic absorption spectrometry, ICP-AES and graphite furnace atomic absorption spectrometry etc. are had to the detection method of metallic copper.FAAS is widely used due to advantages such as simple to operate in analysis, analysis fast, the applied ranges of speed.But, in practical operation, the existence concentration of the cadmium metal in environmental sample is extremely low and composition is complicated, is difficult to directly measure with FAAS, needs to use suitable pretreatment to ensure to obtain analysis result accurately and reliably in sample.SPE becomes the preconditioning technique of current high efficient and reliable due to the character of its uniqueness.And Magnetic solid phases fiber material can be separated by externally-applied magnetic field easily and collect, simple to operate, obtain concern widely.
Number of ways perhaps is had preparing magnetic microsphere, to generally include polymer overmold and remove solvent, metal ion chemistry precipitation in polymer, improve suspension polymerisation, emulsion polymerization, dispersin polymerization etc. at present.Compared with other methods, dispersin polymerization can synthesize the particle being evenly distributed, simple to operate and do not have wider particle diameter distribution, is kind of a good alternative.And, nano material also has Micro-environmental effects, and under same volume, particle diameter is less, and specific surface area is bigger, the effect of absorption can more preferably, become apparent from.
Dispersin polymerization is commonly used to prepare monodisperse particle due to its simplicity.Cao L. Q. (The
Journal of Supercritical Fluids, 2011,58 (2): 233-238) etc. at supercritical carbon dioxide (scCO2) under environment, using the copolymerzation with cross-linking method of microgel, methylene-bisacrylamide makees crosslinking agent, is prepared for 4-vinylpridine cross-linked methyl propionic acid olefin(e) acid (4VP-co-MAA) adsorbent, and for the absorption of Cu (II).Nikita T. T. (Talanta, 2013,116:670-677) etc. has synthesized the 4-vinylpridine microballoon of magnetic, and for the absorption of Cr (VI).At present, there is no the relevant report of the magnetic adsorbent using dispersion copolymerization method synthesizing polyethylene glycol methacrylate and 4-vinylpridine copolymerization.
Content of the invention
It is an object of the invention to provide magnetic nanometer adsorbent of a kind of organic-capping and its preparation method and application, its even particle size distribution, crystal structure is good, and there is fine absorption property, bonding is firm, stable in properties, favorable reproducibility, and enrichment times is bigger, can use in the range of wider pH, it is adaptable to the enrichment pretreatment of trace Cu (II) in environmental water sample.
For achieving the above object, the present invention adopts the following technical scheme that
The preparation method of the magnetic nanometer adsorbent of a kind of organic-capping comprises the following steps:
(1) preparation of magnetic nano-particle；
(2) preparation of the magnetic nano-particle of organic-capping.
Specifically comprise the following steps that
(1) 2.0 ~ 2.5 g FeCl are quick and precisely weighed3·6H2O, and be dissolved in 60 ~ 70 mL ethylene glycol, adding 5.0 ~ 6.0 g anhydrous sodium acetates, magnetic agitation is uniform, in 50 ~ 60 DEG C of water bath, continue strong stirring 20 ~ 30 min, until solute is completely dissolved, 190 ~ 210 DEG C of reaction 6 ~ 10 h, it is cooled to room temperature, wash for several times respectively by absolute ethyl alcohol and deionized water, 50 DEG C of drying 24 h, prepare magnetic nano-particle；
(2) 0.2 ~ 0.3 g magnetic nano-particle is scattered in 15 ~ 20 mL ethanol, adds 1 ~ 2 mL 4-vinylpridine and 1 ~ 2 mL polyethylene glycol methacrylate-styrene polymer, sonic oscillation 20 ~ 30 min；
It is dissolved in 0.3 ~ 0.5g polyvinylpyrrolidone-K30 in 10 ~ 20 mL ethanol, is heated to 70 ~ 80 DEG C, add ultrasonic good mixed monomer solution, 0.5 ~ 1.0 g pentaerythritol triacrylate and 0.1 ~ 0.2
G AIBN, stirs reaction 10 ~ 12 h under nitrogen protection, analyses separation cleaning, 50 DEG C of vacuum drying 12 h by ethanol and deionization hydromagnetic, obtains the magnetic nano-particle of organic-capping, the magnetic nanometer adsorbent of i.e. described organic-capping.
The particle diameter of adsorbent is 270 ~ 290 nm.
Described adsorbent is for the enrichment pretreatment of trace Cu (II) in environmental water sample.
The remarkable advantage of the present invention is:
(1) the organic-capping magnetic nanometer adsorbent of present invention synthesis, with monodispersed ferroso-ferric oxide for magnetic core, dispersin polymerization synthesizes.Particle diameter distribution is homogeneous, and product has good stability, and can use in the range of wider pH.
(2) the organic-capping magnetic nanometer adsorbent of present invention synthesis, with polyethylene glycol methacrylate-styrene polymer and 4-vinylpridine as monomer, reaction introduces functional group, can improve its adsorption capacity and selectivity.
(3) the organic-capping magnetic nanometer adsorbent of present invention synthesis, has enrichment times relatively big, favorable reproducibility, repeatable utilization, the good advantage of reproducibility.
Brief description
Fig. 1 is the scanning electron microscope (SEM) photograph of organic-capping magnetic nanometer adsorbent.
The XRD spectrum of Fig. 2 organic-capping magnetic nanometer adsorbent.
Fig. 3 is the impact on organic-capping magnetic nanometer adsorbent Adsorption of Cu (II) performance for the pH.
Detailed description of the invention
Embodiment 1
The preparation of organic-capping magnetic nanometer adsorbent
(1) preparation of magnetic core: quick and precisely weigh 2.0 g
FeCl3·6H2O is dissolved in 60 mL ethylene glycol, adds 5.0g anhydrous sodium acetate to mix in beaker.Mixed liquor magnetic stirring apparatus is stirred, and move in 50 DEG C of water bath, continue strong stirring 20min, until solute is completely dissolved the homogeneous orange solution of formation, this solution is sealed in 100 mL polytetrafluoroethylene (PTFE) reactors, it with stainless steel outer sleeve locking, is placed in 190 DEG C of reacting furnaces heating reaction 6h.It is cooled to room temperature after taking-up in atmosphere, remove product, and wash for several times respectively by absolute ethyl alcohol and deionized water, to remove residuals.It is dried 24 h in 50 DEG C of vacuum drying chambers, obtain magnetic nano-particle.
(2) organic-capping magnetic particle: by 0.2g Fe3O4It is scattered in 15mL ethanol, add 1 mL 4-VP and 1 mL PEGMA, sonic oscillation 20min.The 10 mL ethanol solutions dissolved with 0.3g PVP-K30 are poured in there-necked flask, moves in oil bath pan and be heated to 70 DEG C.Ultrasonic good mixed monomer solution is joined in there-necked flask, adds 0.5 g crosslinking agent pentaerythritol triacrylate and 0.1 g AIBN, stirring reaction 10h in the environment of nitrogen is protected.After completing with ethanol with deionization hydromagnetic analysis separation cleaning several times, it is vacuum dried 12 h in 50 DEG C, obtains organic-capping magnetic nanometer adsorbent.
Embodiment 2
The preparation of organic-capping magnetic nanometer adsorbent
(1) preparation of magnetic core: quick and precisely weigh 2.5 g
FeCl3·6H2O is dissolved in 70 mL ethylene glycol, adds 6.0 g anhydrous sodium acetates to mix in beaker.Mixed liquor magnetic stirring apparatus is stirred, and move in 60 DEG C of water bath, continue strong stirring 30 min, until solute is completely dissolved the homogeneous orange solution of formation, this solution is sealed in 100 mL polytetrafluoroethylene (PTFE) reactors, it with stainless steel outer sleeve locking, is placed in 210 DEG C of reacting furnaces heating reaction 10 h.It is cooled to room temperature after taking-up in atmosphere, remove product, and wash for several times respectively by absolute ethyl alcohol and deionized water, to remove residuals.It is dried 24 h in 50 DEG C of vacuum drying chambers, obtain magnetic nano-particle.
(2) organic-capping magnetic particle: by 0.3 g Fe3O4It is scattered in 20 mL ethanol, add 2 mL 4-VP and 2 mL PEGMA, sonic oscillation 30 min.The 20 mL ethanol solutions dissolved with 0.5g PVP-K30 are poured in there-necked flask, moves in oil bath pan and be heated to 80 DEG C.Ultrasonic good mixed monomer solution is joined in there-necked flask, adds the crosslinking agent pentaerythritol triacrylate of 1.0 g and the AIBN of 0.2 g, stirring reaction 12 h in the environment of nitrogen is protected.After completing with ethanol with deionization hydromagnetic analysis separation cleaning several times, it is vacuum dried 12 h in 50 DEG C, obtains organic-capping magnetic nanometer adsorbent.
Embodiment 3
The preparation of organic-capping magnetic nanometer adsorbent
(1) preparation of magnetic core: quick and precisely weigh 2.2g
FeCl3·6H2O is dissolved in 65 mL ethylene glycol, adds 5.5g anhydrous sodium acetate to mix in beaker.Mixed liquor magnetic stirring apparatus is stirred, and move in 55 DEG C of water bath, continue strong stirring 25min, until solute is completely dissolved the homogeneous orange solution of formation, this solution is sealed in 100 mL polytetrafluoroethylene (PTFE) reactors, it with stainless steel outer sleeve locking, is placed in 200 DEG C of reacting furnaces heating reaction 8h.It is cooled to room temperature after taking-up in atmosphere, remove product, and wash for several times respectively by absolute ethyl alcohol and deionized water, to remove residuals.It is dried 24 h in 50 DEG C of vacuum drying chambers, obtain magnetic nano-particle.
(2) organic-capping magnetic particle: by 0.25 g Fe3O4It is scattered in 18 mL ethanol, add 1.5mL 4-VP and 1.5 mL PEGMA, sonic oscillation 25min.Will be dissolved with 0.4g
The 15 mL ethanol solutions of PVP-K30 are poured in there-necked flask, move in oil bath pan and are heated to 75 DEG C.Ultrasonic good mixed monomer solution is joined in there-necked flask, adds the crosslinking agent pentaerythritol triacrylate and 0.15 of 0.8 g
The AIBN of g, stirring reaction 11 h in the environment of nitrogen is protected.After completing with ethanol with deionization hydromagnetic analysis separation cleaning several times, it is vacuum dried 12 h in 50 DEG C, obtains organic-capping magnetic nanometer adsorbent.
Organic-capping magnetic nanometer adsorbent morphology characterization
Sem observation is used to obtain the particle diameter of organic-capping magnetic nanometer adsorbent and overall pattern.Fig. 1 is that the ESEM of magnetic nano-particle amplifies 20 000 times of figures.Electronic Speculum figure shows, the magnetic nano-particle good dispersion of synthesis, and particle diameter distribution is homogeneous, and pattern is solid sphere.
Organic-capping magnetic nanometer adsorbent XRD characterizes
X-ray powder diffraction is used to measure crystal structure and the phase structure of organic-capping magnetic nanometer adsorbent.Result such as Fig. 2, it occurs in that the crystal diffraction peak of multiple varying strength in the range of 10-90 °, and it has good crystallinity.Comparing different diffraction maximums with the standard diagram of JCPDS, can obtaining, adsorbent is spinel structure.And after organic coating, magnetic particle crystal structure does not change.
The impact on organic-capping magnetic nanometer adsorbent absorption property for the pH
Investigate pH adsorbent impact on Cu (II) absorption property under the conditions of 3.0-7.5, use flame atomic absorption method (FAAS) to record its absorptivity.Fig. 3 is the impact on organic-capping magnetic nanometer adsorbent Adsorption of Cu (II) performance for the pH.The ion concentration of its initial Cu (II): 2 mg/L；PH:3.0 ~ 7.5；Adsorbent amount: 5 mg；Ultrasonic time: 30 min；Volume of sample: 20 mL；Temperature: 25 DEG C.
Application examples
The extracting and enriching of Cu (II) and mensuration in actual water sample
With clean container in administrative north, University of Fuzhou new district front pond, building water sampling 1 L, filtered immediately and saved backup.Take the water sample that 50 mL filter, utilize buffer solution to regulate its pH value to 7.0, extracting and enriching under best sample adsorption conditions, then the ion being adsorbed with the hydrochloric acid solution wash-out of 2 mL 0.6 mol/L, measure the Cu (II) in eluent with FAAS.Meanwhile, being tested water sample also by adding calibration method herein, experimental technique is identical with non-mark-on experiment, and mark-on amount is respectively 100 μ g/L, 200 μ g/L, all parallel gathering and measuring of each method three times.Result is as shown in table 1.Test result indicate that, the concentration of the Cu (II) recording lake water by the method is 10.4
μg/L.In country's water environment quality standard, Cu (II) the upper limit of concentration value of regulation one-level surface water is 10 μ g/L, therefore lake water Cu (II) concentration of institute's collecting test is slightly above a national class surface water standard, meets two grades of surface water standards.The mensuration and mark-on of actual water sample is tested and recorded Cu (II) the ion rate of recovery between 97.0-101.0 %.Using same method to carry out extracting and enriching and mensuration to University of Fuzhou's running water, result is as shown in table 2, shows that the method is reliably feasible to the analysis of water sample, and result is satisfactory.
The measurement result of Cu (II) content in table 1 lake water
The measurement result of Cu (II) content in table 2 running water
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent with modify, all should belong to the covering scope of the present invention.
Claims (3)
1. the preparation method of the magnetic nanometer adsorbent of an organic-capping, it is characterised in that: comprise the following steps:
(1) preparation of magnetic nano-particle；
(2) preparation of the magnetic nano-particle of organic-capping；
Specifically comprise the following steps that
(1) 2.0 ~ 2.5 g FeCl are quick and precisely weighed3·6H2O, and be dissolved in 60 ~ 70 mL ethylene glycol, adding 5.0 ~ 6.0 g anhydrous sodium acetates, magnetic agitation is uniform, in 50 ~ 60 DEG C of water bath, continue strong stirring 20 ~ 30 min, until solute is completely dissolved, 190 ~ 210 DEG C of reaction 6 ~ 10 h, it is cooled to room temperature, wash for several times respectively by absolute ethyl alcohol and deionized water, 50 DEG C of drying 24 h, prepare magnetic nano-particle；
(2) 0.2 ~ 0.3 g magnetic nano-particle is scattered in 15 ~ 20 mL ethanol, adds 1 ~ 2 mL 4-vinylpridine and 1 ~ 2 mL polyethylene glycol methacrylate-styrene polymer, sonic oscillation 20 ~ 30 min；
0.3 ~ 0.5g polyvinylpyrrolidone-K30 is dissolved in 10 ~ 20 mL ethanol; it is heated to 70 ~ 80 DEG C; add ultrasonic good mixed monomer solution, 0.5 ~ 1.0 g pentaerythritol triacrylate and 0.1 ~ 0.2 g AIBN; stir reaction 10 ~ 12 h under nitrogen protection; analyse separation cleaning with ethanol with deionization hydromagnetic; 50 DEG C of vacuum drying 12 h, obtain the magnetic nano-particle of organic-capping, the magnetic nanometer adsorbent of i.e. described organic-capping.
2. the magnetic nanometer adsorbent of the organic-capping that the method for claim 1 prepares, it is characterised in that: the particle diameter of adsorbent is 270 ~ 290
nm。
3. the application of the magnetic nanometer adsorbent of the organic-capping that the method for claim 1 prepares, it is characterised in that: described adsorbent is for the enrichment pretreatment of trace Cu (II) in environmental water sample.
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