CN106378111B - A kind of magnetic Fe with nucleocapsid3O4/ PMMA nano-compound adsorbents and preparation method thereof - Google Patents
A kind of magnetic Fe with nucleocapsid3O4/ PMMA nano-compound adsorbents and preparation method thereof Download PDFInfo
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- CN106378111B CN106378111B CN201610977891.5A CN201610977891A CN106378111B CN 106378111 B CN106378111 B CN 106378111B CN 201610977891 A CN201610977891 A CN 201610977891A CN 106378111 B CN106378111 B CN 106378111B
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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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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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Abstract
The invention belongs to water-treatment technology field, specially a kind of magnetic Fe with nucleocapsid3O4/ PMMA nano-compound adsorbents and preparation method thereof.The present invention controls chemical oxidative polymerization method to prepare the Fe of hollow structure using iron salt solutions3O4Magnaglo, by PMMA（Polymethyl methacrylate）It is coated on Fe3O4On Magnaglo, to obtain the magnetic Fe of nucleocapsid3O4/ PMMA nano-compound adsorbents.The present invention is prepared for the magnetic Fe of nucleocapsid using ultrasound assisted chemical oxidative polymerization method green under conditions of no surfactant, crosslinking agent or organic stabilizer3O4/ PMMA nano-compound adsorbents.This kind of novel adsorbent can quickly remove the heavy metal in waste water, and absorbent can be with regenerative adsorption, and the absorption of this kind of adsorbent is still with very high adsorption efficiency after continuous several times desorption, with larger industrial utility value.
Description
Technical field
The invention belongs to water-treatment technology fields, specifically, are related to a kind of magnetic Fe with nucleocapsid3O4/PMMA
Nano-compound adsorbent and preparation method thereof.
Background technology
Heavy metal pollution in sewage has caused more and more concerns.Wherein, heavy metal due to its high toxicity and
Mobility has very detrimental effect to environment and human health.In waste water, following several places usually may be used in heavy metal
Reason method：Electrochemical reducing, the precipitation method, hyperfiltration, ion-exchange and absorption method.Titanium dioxide nanoparticle, green
The Fe of synthesis3O4The adsorbents such as nano-particle have been used to the processing and disposition of heavy metal in waste water cadmium.However, separation and recycling
These materials are a challenges, especially when grain size drops to nanoscale.It is at low cost due to adsorbing, it is useless that low concentration can be effectively removed
Heavy metal in water so, be a kind of advantageous and feasible method using absorption method.Compared with common adsorbents, magnetic absorption
The characteristic that agent has physics and chemical stability is good, high mechanical strength and wearability are good.Iron and ferriferous oxide nano material by
As the material for restoring or adsorbing heavy metal.However, on the one hand in an acidic solution, pure nano-particle is easy to aoxidize.It is another
In a continuous-flow system, these nano-particles are difficult to recycle aspect.Therefore, in order to protect magnetic nano-particle from oxygen
Change, has selected the structure of core-shell type.
Due to Fe3O4Double low attributes with toxicity and cost, it has been widely used in the preparation process of magnetic material
In and have been realized in commercialized production.From 2010, China had become the second largest electron wastes in the world
The producer, and PMMA is an important component part in electron wastes, annual discarded amount is also very big.
Invention content
For overcome the deficiencies in the prior art, the purpose of the present invention is to provide a kind of magnetism with nucleocapsid
Fe3O4/ PMMA nano-compound adsorbents and preparation method thereof.The preparation method is simple, and obtained adsorbent can be removed quickly
Heavy metal in waste water, and can be with regenerative adsorption, the absorption of this kind of adsorbent is still with very high absorption after continuous several times desorption
Efficiency has larger industrial utility value.
Magnetic Fe proposed by the present invention with nucleocapsid3O4/ PMMA nano-compound adsorbents are one kind with magnetic nothing
The Fe of machine3O4For core, using the method for ultrasound assisted chemical oxidation polymerization, in one layer of PMMA of magnetic nano particle daughter nucleus outer wrapping and
The magnetic Nano compound adsorbent of composition.Work as Fe3O4When Magnaglo is under weakly acidic condition, due to a large amount of hydroxyls of surface of inorganic particles
The weak electrostatic effect of base, Fe3O4Surface can adsorb a large amount of H+, the Fe of protonation3O4It is placed in ethanol solution, and adds PMMA
Afterwards, since nitrogen-atoms easily combines proton, PMMA is made to be adsorbed on the magnetic core on surface.After adding ammonium persulfate, it is super to carry out interval
Sound can be assisted to improve the dispersibility of sample.Finally, polymer is gradually deposited at magnetic core Fe3O4Surface forms nucleocapsid.One
Denier monomer polymerize on the surface of the samples, and polymerization will continue to react, and polymer chain is made to increase.Present invention synthesis is obtained
Magnetic Nano compound adsorbent has better monodispersity, and the thickness of cladding is uniform.The thickness of shell can pass through control
Reaction time controls.
Technical scheme of the present invention is specifically described as follows.
The present invention provides a kind of magnetic Fe with nucleocapsid3O4/ PMMA nano-compound adsorbents are in nucleocapsid,
The Fe of hollow structure3O4For core, PMMA layers are cladding shell.Preferably, the Fe of hollow structure3O4Grain size be 50-300 nanometers,
PMMA layers of thickness is 15 ~ 25nm.
The present invention also provides a kind of above-mentioned magnetic Fes with nucleocapsid3O4The preparation side of/PMMA nano-compound adsorbents
Method is as follows：The Fe of hollow structure is prepared first3O4Magnaglo；Then by Fe3O4Magnaglo is dispersed in diluted acid
In, it is used in combination EtOH Sonicate to disperse；Be eventually adding PMMA and ammonium persulfate hybrid reaction, after reaction again magnet separation, washing,
It is dry, obtain magnetic Fe3O4/ PMMA nano-compound adsorbents；Wherein：Fe3O4The mass ratio of Magnaglo and PMMA are 1:1-
10:1.Preferably, the Fe of hollow structure3O4Magnaglo is by ferric chloride hexahydrate and sodium acetate, polyethylene glycol at 190 ~ 210 DEG C
At a temperature of, it reacts and is prepared in ethyl alcohol.
In the present invention, magnetic Fe3O4/ PMMA nano-compound adsorbents can be used for handling heavy metal cadmium；Magnetism after use
Fe3O4/ PMMA nano-compound adsorbents, can first pass through that magnet is isolated, then be placed in the sodium hydroxide solution of 0.5 ~ 1mol/L
Stirring, then wash drying, you can recycling.
Compared to the prior art, the beneficial effects of the present invention are：
（1）In the present invention, used PMMA samples can be such that from electron wastes recycling obtains, and can be controlled with useless
It is useless, resource is comprehensively utilized, the recycling and processing to electronic waste also have certain meaning.
（2）In the present invention, the magnetic Fe of tool that provides3O4/ PMMA nano-compound adsorbents, it is different from the past to be reported
Material, its preparation method is simple, environmentally friendly non-secondary pollution.And there is good dispersibility, magnetic response is high, microballoon shape
It is uniform.The present invention takes full advantage of the characteristic of magnetic material, is detached using magnet, there is raw material to be easy to get, synthetic adsorbent purity
High, it is easy to regenerative adsorption feature.
（3）Prepared adsorbent is perspective good for handling heavy metal cadmium in the present invention, and adsorption efficiency is high.It is suitable for
Waste water and sanitary sewage in extensive processing industry.
Description of the drawings
Fig. 1 is magnetic Fe prepared by embodiment 13O4The SEM of/PMMA nano-compound adsorbents（Scanning electron microscope）Shape
Looks figure.
Fig. 2 is magnetic Fe3O4The TEM of/PMMA nano-compound adsorbents（Transmission electron microscope）Pattern illustrates.（a）It is real
The magnetic Fe prepared when the PMMA that example 1 is applied to be recycled in electron wastes is monomer3O4/ PMMA nano-compound adsorbents；（b）It is real
The magnetic Fe prepared when applying example 4 using pure PMMA as monomer3O4/ PMMA nano-compound adsorbents.
Fig. 3 is various concentration cadmium solution concentration magnetic Fe in embodiment 73O4The removal of the nano combined absorption cadmiums of/PMMA
Efficiency.
Fig. 4 is magnetic Fe in embodiment 83O4The regenerative adsorption figure of/PMMA nano-compound adsorbents.
Specific implementation mode
The present invention will be described in detail with reference to the accompanying drawings and examples.
Embodiment 1
（1）Fe3O4The experimental program of the preparation of Magnaglo is as follows：1.622 grams of ferric chloride hexahydrates are taken to be dissolved in 100 millis
Uniformly mixed solution is obtained in the ethyl alcohol risen, and is stirred evenly, 3.6 grams of sodium acetates and 1.0 grams of polyethylene glycol are then added
6000.Obtained yellow liquid is completely transferred in crucible, closed preservation.At 200 DEG C, mixture is heated 48 hours.
Magnet detaches, and is washed by distilled water and ethyl alcohol, repeats this operation and is repeated 3 times.Finally, 40 DEG C of vacuum of the substance obtained are dry
It is dry 6 hours, repeatedly dry multiple, until the sample being fully cured.
（2）Magnetic Fe3O4Preparing for/PMMA nano-compound adsorbents is as follows：By the Fe of the 0.1g of above-mentioned preparation3O4It is magnetic
Powder adds in 0.1 mole of every liter of hydrochloric acid.With nitrogen protection, mixture ultrasonic disperse 10 minutes is distributed until magnetic powder at room temperature
Uniformly.After standing 12 hours, 10 milliliters of ethyl alcohol simultaneously ultrasonic disperse 10 minutes are added.Under nitrogen protection, 0.1 gram is added from electronics
The PMMA recycled in waste（Purity is 96 %, in addition to containing C, H, also contains N and S）It mixes, is stirred continuously with ammonium persulfate
It goes forward side by side ultrasonic disperse of in the ranks having a rest（It is 5 minutes ultrasonic every 10 minutes）.Magnet detaches again, and distilled water and ethyl alcohol wash 3 times.Finally,
Obtained substance vacuum drying chamber is dry 6 hours under the conditions of 40 DEG C, can be with until the sample being fully cured
It is repeatedly dry multiple.The Fe of gained hollow structure3O4The grain size of magnetic-particle is 300nm, and the thickness of PMMA shells is 20nm.
Fig. 1 is magnetic Fe prepared by embodiment 13O4The SEM of/PMMA nano-compound adsorbents（Scanning electron microscope）Shape
Looks figure.
Embodiment 2
（1）Fe3O4The experimental program of the preparation of Magnaglo is as follows：3.244 grams of ferric chloride hexahydrates are taken to be dissolved in 100 millis
Uniformly mixed solution is obtained in the ethyl alcohol risen, and is stirred evenly, 7.2 grams of sodium acetates and 2.0 grams of polyethylene glycol are then added
6000.Obtained yellow liquid is completely transferred in crucible, closed preservation.At 200 DEG C, mixture is heated 48 hours.
Magnet detaches, and is washed by distilled water and ethyl alcohol, repeats this operation and is repeated 3 times.Finally, 40 DEG C of vacuum of the substance obtained are dry
It is dry 6 hours, repeatedly dry multiple, until the sample being fully cured.
（2）Magnetic Fe3O4Preparing for/PMMA nano-compound adsorbents is as follows：By the Fe of the 0.1g of above-mentioned preparation3O4It is magnetic
Powder adds in 0.1 mole of every liter of hydrochloric acid.With nitrogen protection, mixture ultrasonic disperse 10 minutes is distributed until magnetic powder at room temperature
Uniformly.After standing 12 hours, 20 milliliters of ethyl alcohol simultaneously ultrasonic disperse 20 minutes are added.Under nitrogen protection, 0.1 gram is added from electronics
The PMMA recycled in waste is mixed with ammonium persulfate, is stirred continuously ultrasonic disperse of in the ranks having a rest of going forward side by side（Every 10 minutes 5 points of ultrasounds
Clock）.Magnet detaches again, and distilled water and ethyl alcohol wash 3 times.Finally, the substance vacuum drying chamber obtained is done under the conditions of 40 DEG C
It dry 6 hours, until the sample being fully cured, can dry repeatedly repeatedly.
Wherein, the Fe of gained hollow structure3O4The grain size of magnetic-particle is 320nm, and the thickness of PMMA shells is 27nm.
Embodiment 3
（1）Fe3O4The experimental program of the preparation of Magnaglo is as follows：4.866 grams of ferric chloride hexahydrates are taken to be dissolved in 100 millis
Uniformly mixed solution is obtained in the ethyl alcohol risen, and is stirred evenly, 10.8 grams of sodium acetates and 3.0 grams of polyethylene glycol are then added
6000.Obtained yellow liquid is completely transferred in crucible, closed preservation.At 200 DEG C, mixture is heated 48 hours.
Magnet detaches, and is washed by distilled water and ethyl alcohol, repeats this operation and is repeated 3 times.Finally, 40 DEG C of vacuum of the substance obtained are dry
It is dry 6 hours, repeatedly dry multiple, until the sample being fully cured.
（2）Magnetic Fe3O4Preparing for/PMMA nano-compound adsorbents is as follows：By the Fe of the 0.1g of above-mentioned preparation3O4It is magnetic
Powder adds in 0.1 mole of every liter of hydrochloric acid.With nitrogen protection, mixture ultrasonic disperse 10 minutes is distributed until magnetic powder at room temperature
Uniformly.After standing 12 hours, 30 milliliters of ethyl alcohol simultaneously ultrasonic disperse 30 minutes are added.Under nitrogen protection, 0.1 gram is added from electronics
The PMMA recycled in waste is mixed with ammonium persulfate, is stirred continuously ultrasonic disperse of in the ranks having a rest of going forward side by side（Every 10 minutes 5 points of ultrasounds
Clock）.Magnet detaches again, and distilled water and ethyl alcohol wash 3 times.Finally, the substance vacuum drying chamber obtained is done under the conditions of 40 DEG C
It dry 6 hours, until the sample being fully cured, can dry repeatedly repeatedly.
Wherein, the Fe of gained hollow structure3O4The grain size of magnetic-particle is 330nm, and the thickness of PMMA shells is 34nm.
Embodiment 4
（1）Fe3O4The experimental program of the preparation of Magnaglo is as follows：1.622 grams of ferric chloride hexahydrates are taken to be dissolved in 100 millis
Uniformly mixed solution is obtained in the ethyl alcohol risen, and is stirred evenly, 7.2 grams of sodium acetates and 2.0 grams of polyethylene glycol are then added
6000.Obtained yellow liquid is completely transferred in crucible, closed preservation.At 200 DEG C, mixture is heated 48 hours.
Magnet detaches, and is washed by distilled water and ethyl alcohol, repeats this operation and is repeated 3 times.Finally, 40 DEG C of vacuum of the substance obtained are dry
It is dry 6 hours, repeatedly dry multiple, until the sample being fully cured.
（2）Magnetic Fe3O4Preparing for/PMMA nano-compound adsorbents is as follows：By the Fe of the 0.1g of above-mentioned preparation3O4It is magnetic
Powder adds in 0.1 mole of every liter of hydrochloric acid.With nitrogen protection, mixture ultrasonic disperse 10 minutes is distributed until magnetic powder at room temperature
Uniformly.After standing 12 hours, 10 milliliters of ethyl alcohol simultaneously ultrasonic disperse 10 minutes are added.Under nitrogen protection, be added 0.1 gram it is pure
PMMA is mixed with ammonium persulfate, is stirred continuously ultrasonic disperse of in the ranks having a rest of going forward side by side（It is 5 minutes ultrasonic every 10 minutes）.Magnet point again
From distilled water and ethyl alcohol wash 3 times.Finally, the substance vacuum drying chamber obtained is 6 hours dry under the conditions of 40 DEG C, until
Until the sample being fully cured, it can dry repeatedly repeatedly.
Wherein, the Fe of gained hollow structure3O4The grain size of magnetic-particle is 350nm, and the thickness of PMMA shells is 28nm.
Embodiment 5
（1）Fe3O4The experimental program of the preparation of Magnaglo is as follows：3.244 grams of ferric chloride hexahydrates are taken to be dissolved in 100 millis
Uniformly mixed solution is obtained in the ethyl alcohol risen, and is stirred evenly, 7.2 grams of sodium acetates and 2.0 grams of polyethylene glycol are then added
6000.Obtained yellow liquid is completely transferred in crucible, closed preservation.At 200 DEG C, mixture is heated 48 hours.
Magnet detaches, and is washed by distilled water and ethyl alcohol, repeats this operation and is repeated 3 times.Finally, 40 DEG C of vacuum of the substance obtained are dry
It is dry 6 hours, repeatedly dry multiple, until the sample being fully cured.
（2）Magnetic Fe3O4Preparing for/PMMA nano-compound adsorbents is as follows：By the Fe of the 1g of above-mentioned preparation3O4Magnetic powder
End adds in 0.1 mole of every liter of hydrochloric acid.With nitrogen protection, at room temperature mixture ultrasonic disperse 10 minutes until magnetic powder distribution it is equal
It is even.After standing 12 hours, 20 milliliters of ethyl alcohol simultaneously ultrasonic disperse 20 minutes are added.Under nitrogen protection, 0.1 gram of pure PMMA is added
It is mixed with ammonium persulfate, is stirred continuously ultrasonic disperse of in the ranks having a rest of going forward side by side（It is 5 minutes ultrasonic every 10 minutes）.Magnet detaches again, steams
Distilled water and ethyl alcohol wash 3 times.Finally, the substance vacuum drying chamber obtained is 6 hours dry under the conditions of 40 DEG C, until obtaining
Until the sample being fully cured, it can dry repeatedly repeatedly.
Wherein, the Fe of gained hollow structure3O4The grain size of magnetic-particle is 360nm, and the thickness of PMMA shells is 35nm.
Embodiment 6
（1）Fe3O4The experimental program of the preparation of Magnaglo is as follows：4.844 grams of ferric chloride hexahydrates are taken to be dissolved in 100 millis
Uniformly mixed solution is obtained in the ethyl alcohol risen, and is stirred evenly, 7.2 grams of sodium acetates and 2.0 grams of polyethylene glycol are then added
6000.Obtained yellow liquid is completely transferred in crucible, closed preservation.At 200 DEG C, mixture is heated 48 hours.
Magnet detaches, and is washed by distilled water and ethyl alcohol, repeats this operation and is repeated 3 times.Finally, 40 DEG C of vacuum of the substance obtained are dry
It is dry 6 hours, repeatedly dry multiple, until the sample being fully cured.
（2）Magnetic Fe3O4Preparing for/PMMA nano-compound adsorbents is as follows：By the Fe of the 0.5g of above-mentioned preparation3O4It is magnetic
Powder adds in 0.1 mole of every liter of hydrochloric acid.With nitrogen protection, mixture ultrasonic disperse 10 minutes is distributed until magnetic powder at room temperature
Uniformly.After standing 12 hours, 30 milliliters of ethyl alcohol simultaneously ultrasonic disperse 30 minutes are added.Under nitrogen protection, be added 0.1 gram it is pure
PMMA is mixed with ammonium persulfate, is stirred continuously ultrasonic disperse of in the ranks having a rest of going forward side by side（It is 5 minutes ultrasonic every 10 minutes）.Magnet point again
From distilled water and ethyl alcohol wash 3 times.Finally, the substance vacuum drying chamber obtained is 6 hours dry under the conditions of 40 DEG C, until
Until the sample being fully cured, it can dry repeatedly repeatedly.
Wherein, the Fe of gained hollow structure3O4The grain size of magnetic-particle is 375nm, and the thickness of PMMA shells is 40nm.
Embodiment 7
Compound concentration is the cadmium chloride solution of 0.2 ~ 1.2 grams per liter respectively, is added in embodiment 1 into every part of solution
Magnetic Fe3O40.1 gram of/PMMA nano-compound adsorbents.It is 1.5 with 12 moles every liter of hydrochloric acid tune pH value, after ultrasonic disperse, often
Make its separation of solid and liquid under extraneous magnetic fields every a period of time, pipettes wherein 10 milliliters of solution and taken in 100 milliliters of volumetric flasks
10 milliliters absorption after solution, repeatedly after, be averaged, calculate the content that cadmium is adsorbed, make adsorption curve figure, such as
Shown in Fig. 3.The results show that under the conditions of the present embodiment, magnetic Fe3O4The chlorination of 0.2 ~ 0.8g/L of/PMMA nano-compound adsorbents pair
Cadmium solution adsorption efficiency is all 95% or more.
Embodiment 8
Embodiment 7 has been adsorbed to the magnetic Fe of cadmium3O4/ PMMA nano-compound adsorbents, are placed in 50 milliliter 0.5 at room temperature
Stirred 0.5 hour in mole every liter of sodium hydroxide solution, distillation water washing for several times after, be re-used for the absorption of metal ion,
Determine maximum adsorbance.It after repeatedly, is averaged, calculates the adsorption efficiency of cadmium, make adsorption curve figure, such as Fig. 4
It is shown.Wherein, the 4th absorption property is slightly lower, to adsorption efficiency after the 5th desorption all 90% or more after desorbing for the first time,
Adsorption efficiency after desorbing for the first time is 95.5%, and the adsorption efficiency after the 5th parsing is 91.2%.
Claims (2)
1. a kind of magnetic Fe with nucleocapsid3O4The preparation method of/PMMA nano-compound adsorbents, which is characterized in that specific
Steps are as follows：The Fe of hollow structure is prepared first3O4Magnaglo；Then by Fe3O4Magnaglo is dispersed in diluted acid, is used in combination
EtOH Sonicate disperses；It is eventually adding the PMMA recycled from electron wastes and ammonium persulfate hybrid reaction, after reaction again
Magnet separation, washing, drying, obtain magnetic Fe3O4/ PMMA nano-compound adsorbents；Wherein： Fe3O4Magnaglo and PMMA
Mass ratio be 1:1-10:1；Magnetic Fe3O4/ PMMA nano-compound adsorbents are in nucleocapsid, the Fe of hollow structure3O4For core,
PMMA layers are cladding shell, the Fe of hollow structure3O4Grain size be 50-300 nanometer, PMMA layers of thickness is 15 ~ 25nm；It is described
The purity of the PMMA recycled in electron wastes is 96%, except C is contained, outside H, also contains N and S.
2. preparation method as described in claim 1, which is characterized in that the Fe of hollow structure3O4Magnaglo is by six chloride hydrates
Iron and sodium acetate, polyethylene glycol are reacted in ethyl alcohol and are prepared at a temperature of 190 ~ 210 DEG C.
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| CN110746743B (en) * | 2019-10-16 | 2020-10-30 | 武汉理工大学 | Lipophilic photon nanometer magnetic chain and preparation method thereof |
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