CN104624175B - Nano-magnetic adsorbent and preparation method thereof - Google Patents
Nano-magnetic adsorbent and preparation method thereof Download PDFInfo
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- CN104624175B CN104624175B CN201510079357.8A CN201510079357A CN104624175B CN 104624175 B CN104624175 B CN 104624175B CN 201510079357 A CN201510079357 A CN 201510079357A CN 104624175 B CN104624175 B CN 104624175B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3028—Granulating, agglomerating or aggregating
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
Abstract
The invention discloses a nano-magnetic adsorbent and a preparation method thereof, relating to an organic-inorganic composite material. The nano-magnetic adsorbent comprises hollow polymer microspheres and magnetic Fe3O4 nanoparticles, which are hybridized; the hollow polymer microspheres contain complexible pyridine nitrogen atoms, coordinate bonds exist between the hollow polymer microspheres and the magnetic Fe3O4 nanoparticles, and the magnetic Fe3O4 nanoparticles stably grow on the surfaces of the hollow polymer microspheres; the hollow polymer microspheres are formed by copolymerizing styrene and vinylpyridine monomers through a seed emulsion polymerization method according to the mass ratio of (2-5):1. The preparation method comprises the following steps: firstly preparing the hollow polymer microspheres formed by copolymerizing styrene and vinylpyridine monomers through a seed emulsion polymerization method, and then growing the magnetic Fe3O4 nanoparticles on the hollow polymer microspheres by adopting in-situ precipitation method, to prepare high-efficiency nano-magnetic adsorbent. The nano-magnetic adsorbent is high in loading rate, large in specific area, fast in adsorption speed, and good in adsorption performance.
Description
Technical field
The present invention relates to organic/inorganic composite material, it is specifically related to a kind of nano-magnetic adsorbent and preparation method thereof.
Background technology
At home, water pollution problems be increasingly subject to people concern, and the high speed development of modern industry so that water pollution increasingly
Seriously.Especially dyeing waste water and heavy metal wastewater thereby are very big to environmental destruction, need effectively to be administered.Industrial wastewater
Treating method has oxidation-reduction method, coagulant sedimentation, sonication, electrochemical process and absorption method etc..Wherein, absorption method master
Pretreatment and advanced treatment to be applied to.Absorption method has two key points: one is that can adsorbent quickly and efficiently adsorb pollution
Thing molecule, two is that can adsorbent be easy to reclaim separation from water body, it is to avoid secondary pollution.
At present, adsorbent species are various, it usually needs select different absorption according to concrete production technology and process object
Agent.Due to fe304Magnetic-particle has absorption property and separating property simultaneously, thus is considered as a kind of good adsorbent.Receive
The particle size of rice magnetic adsorbent is little, and specific surface area is big, and high adsorption capacity is it is most important that nano-magnetic adsorbent is in outer magnetic
In the presence of, can separate from water body rapidly, reduce secondary pollution, ultra-fine adsorbing material can be overcome simultaneously easily to flow
The disadvantage lost.For example, Zhang Panyue et al. (a kind of method that magnetic nano adsorption material removes waste water cationic organic dyestuff,
Chinese patent, publication number: cn 101670266b) combine humic acid and magnetic fe304The advantage of nano-particle, by humic acid
In fe304Nano grain surface, prepares the magnetic adsorbent that adsorption capacity is big, the rate of adsorption is high, utilizes externally-applied magnetic field after absorption
Can realize rapidly separating.But, nanometer fe304There is very strong Van der Waals force between nano grain surface, tend to reunite, lead
Their stability in the solution of cause are poor, and adsorption molecule needs longer time to aggregate diffusion inside, leads to application to be subject to
Arrive certain restriction.For this reason, how to reduce reunion, improving adsorption rate becomes one of research direction.For example: Cheng Zhipeng etc. (receives
Rice fe304The preparation method of cladding attapulgite magnetic composite adsorbent, Chinese patent, publication number: cn 102258978a) by nanometer
fe304Granule is firmly attached to the surface of attapulgite, makes a nanometer fe304Cladding attapulgite magnetic composite adsorbent, effectively keeps away
Exempt from a meter fe304Agglomeration, substantially reduce fe304The adsorption cycle of nano adsorber, improves adsorption efficiency, but concavo-convex
Rod soil size is larger, monodispersity very poor so that nanometer fe304Cladding attapulgite magnetic composite adsorbent is easy to settle, and impact should
The adsorption efficiency of adsorbent.Therefore, seek a kind of preparation process is simple, specific surface area is big, monodispersity is good, fe304Nano-particle
The high nano-magnetic adsorbent of load factor seems extremely important in field of Environment Protection.
Content of the invention
It is an object of the invention to provide a kind of nano-magnetic adsorbent and preparation method thereof.
Described nano-magnetic adsorbent is by hollow polymer microsphere and magnetic fe304Nano-particle hydridization forms；Described hollow
Polymer microballoon contains complexible pyridine nitrogen atom, hollow polymer microsphere and fe304There is coordinate bond between nano-particle,
fe304Nanoparticles stable is grown in hollow polymer microsphere surface；Described hollow polymer microsphere is by styrene and vinylpyridine
Pyridine class monomer is formed by seeded emulsion polymerization method copolymerization, and the mass ratio of described styrene and vinylpyridine class monomer is (2
～5): 1.
Hollow polymer microsphere surface has certain roughness, makes hollow polymer microsphere and magnetic fe304Nano-particle is miscellaneous
Change body to be difficult to reunite, good dispersion, specific surface area is big, and the rate of adsorption is fast, and absorption property is good.The particle diameter of hollow polymer microsphere is
200nm about；The hollow-core construction of described hollow polymer microsphere be by normal octane in monomer polymerization process with produce be polymerized
Formed separated between thing chain and produce, the hollow lumen diameter of hollow polymer microsphere can be 100～150nm.
Described fe304Nano-particle is prepared using in situ deposition method and is supported on hollow polymer microsphere surface.
The preparation method of described nano-magnetic adsorbent, comprises the following steps:
1) preparation of hollow polymer microsphere emulsion
Sodium lauryl sulphate sds, deionized water water bath sonicator are mixed to form aqueous phase, by styrene and normal octane mixing
Form oil phase, oil phase is put into after water bath sonicator in aqueous phase, then gained system is transferred in water-bath, anti-under nitrogen atmosphere
Should, add water soluble starter and continue reaction, be subsequently adding the dehydrated alcohol mixed liquor reaction of vinylpyridine class monomer, cold
But, after, obtain final product hollow polymer microsphere emulsion；
2) preparation of nano-magnetic adsorbent
By fecl3And fecl2·4h2O adds in deionized water, adds step 1) gained hollow polymer microsphere emulsion
In, water bath sonicator, then gained system is transferred in water-bath, add ammonia, after reacting under nitrogen atmosphere, cooling, centrifugation,
Washing, after being dried, obtains final product nano-magnetic adsorbent, and gained nano-magnetic adsorbent is in powder.
In step 1) in, the described temperature by sodium lauryl sulphate sds, deionized water water bath sonicator can be 35～40
℃；Described by oil phase put into aqueous phase in water bath sonicator condition can at 35～40 DEG C water bath sonicator 15～30min；Described water-bath
The temperature of pot can be 75～80 DEG C；Under described nitrogen atmosphere, the condition of reaction mechanical agitation can make it start instead under nitrogen atmosphere
Should；The described time adding water soluble starter to continue reaction can be 6～8h；Described water soluble starter is selected from persulfuric acid
Ammonium, potassium peroxydisulfate, 2, one of 2 '-azo (2- methyl-propyl amidine) dihydrochloride etc., the consumption of water soluble starter presses matter
Amount percentage ratio can be the 0.1%～1% of styrene monomer；The dehydrated alcohol mixed liquor of described addition vinylpyridine class monomer is anti-
The time answered can be 8～12h；Described vinylpyridine class monomer is selected from 2- vinylpyridine, 4-vinylpridine, 2- ethylene
One of the derivant of yl pyridines, derivant of 4-vinylpridine etc.；The consumption of described normal octane can be complete in mass ratio
1～4 times of portion's monomer.
In step 2) in, the time of described water bath sonicator can be 10～30min；The temperature of described water-bath can be 60～80
℃；Described reaction under nitrogen atmosphere can press the speed mechanical stirring reaction 1～3h of 300～500r/min under nitrogen atmosphere；
Described washing can be using absolute ethanol washing 2～3 times；Described drying can be vacuum dried at 65～70 DEG C；Described fecl3、
fecl2·4h2O, ammonia, the mass ratio of vinylpyridine class monomer can be (3～2): 1: (20～10): (8～2).Obtained
The Xylene Red 73 aqueous solution stimulated dye wastewater that the Characterization of Adsorption of nano-magnetic adsorbent can be 98% using purity, utilizes
Ultraviolet-visible extinction photometer measures uv absorption change.
Nano-magnetic adsorbent prepared by the present invention is by hollow polymer microsphere and magnetic fe304Nano-particle hydridization and
Become, can apply in field of waste water treatment.The present invention first passes through seeded emulsion polymerization method and styrene and vinylpyridine is obtained
The hollow polymer microsphere of pyridine class monomer copolymerization, then generates magnetic fe using in situ deposition method on hollow polymer microsphere304
Nano-particle, prepares efficient nano magnetic adsorbent.Wherein its component of hollow polymer microsphere contains complexible pyridine nitrogen
Atom, with fe304There is coordinate bond between nano-particle, so that fe304It is micro- that nano-particle can stably be grown in hollow polymer
Ball surface, load factor is high.Additionally, hollow polymer microsphere surface has certain roughness, make hollow polymer microsphere and magnetic
fe304Nano-particle hybrid is difficult to reunite, good dispersion.The nano-magnetic adsorbent specific surface area of the present invention is big, the rate of adsorption
Hurry up, absorption property is good.
Brief description
Fig. 1 is the tem figure (scale is 200nm) of the nano-magnetic adsorbent of embodiment 1 preparation.
Fig. 2 is the tem figure (scale is 100nm) of the nano-magnetic adsorbent of embodiment 1 preparation.
Fig. 3 is the adsorption effect figure of the efficient nano magnetic adsorbent that embodiment 1～4 is obtained.
Specific embodiment
Following examples combine accompanying drawing, and the invention will be further described.
Embodiment 1
(1) preparation of hollow polymer microsphere emulsion
Weigh 0.06g sodium lauryl sulphate sds, add in the there-necked flask equipped with 60ml deionized water, water-bath at 40 DEG C
Ultrasonic 10min is so that sodium lauryl sulphate is thoroughly mixed to form homogeneous aqueous phase.In addition weigh 1g styrene, 2g normal octane mixes
Close, form homogeneous oil phase.Oil phase is put in above-mentioned aqueous phase, 40 DEG C of water bath sonicator 30min.Again gained system is transferred to 80 DEG C
In water-bath, under nitrogen atmosphere, mechanical agitation (300r/min) makes it start to react, and after temperature stabilization, adds 0.01g over cure
Sour kalium ps, after reaction 8h, takes 0.4g 4-vinylpridine, is dissolved in formation mixed liquor in 9ml dehydrated alcohol, is added dropwise over supreme
State in reaction system, be cooled to room temperature after reaction 12h and can get hollow polymer microsphere emulsion.
(2) preparation of dispersed nano magnetic adsorbent
Weigh 324mg fecl3、126mg fecl2·4h2O and 10ml deionized water, after fully dissolving, adds step (1)
In gained hollow polymer microsphere emulsion, water bath sonicator 30min at lower 25 DEG C of nitrogen atmosphere, then gained system is transferred to 70 DEG C
In water-bath, and add 4ml nh3·h2O (25%), after mechanical agitation (300r/min) reaction 3h under nitrogen atmosphere, is cooled to
Room temperature.After products therefrom is centrifuged, washed 3 times with dehydrated alcohol, then through being vacuum dried at 70 DEG C, you can obtain a kind of efficient nano
Magnetic adsorbent powder sample.
The structure of obtained efficient nano magnetic adsorbent is characterized by jem-2100 high-resolution-ration transmission electric-lens, from Fig. 1 and 2
In visible, efficient nano magnetic adsorbent is by hollow polymer microsphere and magnetic fe304Nano-particle is constituted, efficient nano magnetic
Adsorbent particle diameter is about 150～200nm, and monodispersity is good, fe3o4Nano-particle is wrapped in hollow polymer microsphere surface, polymerization
Thing microsphere is hollow structure, as shown in Fig. 1 and 2.
Embodiment 2～4
With embodiment 1 technique, change step (1) medium vinyl pyridine consumption and be followed successively by 0.2g, 0.5g, 0.7g.
(3) adsorption experiment to Xylene Red 73 stimulated dye wastewater for the efficient nano magnetic adsorbent
1. compound concentration is the Xylene Red 73 stimulated dye wastewater 540ml of 100mg/l, with the hc1 solution of 0.lmol/l and
It is 5.00 that the naoh solution of 0.lmol/l adjusts its ph.
2. 1. weigh described efficient nano magnetic adsorbent 60mg adds 100ml in solution, sonic oscillation.
3. purple is used respectively when adsorbing 1min, 3min, 5min, 7min, l0min, 20min, 40min, 60min, 90min
Outward-spectrophotometric measures the supernatant, and maximum absorption wavelength is set as 509nm.
Adsorption experimental results are as shown in Figure 3.It can be seen that, described efficient nano magnetic adsorbent is high to the adsorbance of Xylene Red 73
Reach 155mg/g, the rate of adsorption is fast, and absorption property is excellent.
The nano-magnetic adsorbent of the present invention is by hollow polymer microsphere and magnetic fe304Nano-particle hydridization forms.This
Not only particle diameter is little for bright efficient nano magnetic adsorbent, and surface area is big, good dispersion, high adsorption capacity, and due to hollow poly-
Compound microsphere component contains complexible pyridine nitrogen atom, makes fe304Nano-particle load factor on hollow polymer microsphere is high, holds
Easily separated from absorption system and be enriched with, therefore led in environmental protection such as treatment of dyeing wastewater, the improvement of heavy metal wastewater thereby and recovery
Domain has good using value.
Claims (10)
1. a kind of nano-magnetic adsorbent is it is characterised in that by hollow polymer microsphere and magnetic fe3o4Nano-particle hydridization group
Become；Described hollow polymer microsphere contains complexible pyridine nitrogen atom, hollow polymer microsphere and fe3o4Between nano-particle
There is coordinate bond, fe3o4Nanoparticles stable is grown in hollow polymer microsphere surface；Described hollow polymer microsphere is by benzene second
Alkene and vinylpyridine class monomer are formed by seeded emulsion polymerization method copolymerization, described styrene and vinylpyridine class monomer
Mass ratio be (2～5): 1.
2. as claimed in claim 1 a kind of preparation method of nano-magnetic adsorbent it is characterised in that comprising the following steps:
1) preparation of hollow polymer microsphere emulsion
Sodium lauryl sulphate sds, deionized water water bath sonicator are mixed to form aqueous phase, styrene and normal octane are mixed to form
Oil phase, oil phase is put into after water bath sonicator in aqueous phase, then gained system is transferred in water-bath, reacts under nitrogen atmosphere, then
Add water soluble starter to continue reaction, be subsequently adding the dehydrated alcohol mixed liquor reaction of vinylpyridine class monomer, after cooling,
Obtain final product hollow polymer microsphere emulsion；
2) preparation of nano-magnetic adsorbent
By fecl3And fecl2·4h2O adds in deionized water, adds step 1) in gained hollow polymer microsphere emulsion, water
Bath is ultrasonic, then gained system is transferred in water-bath, adds ammonia, after reacting under nitrogen atmosphere, cooling, and centrifugation, washing,
After drying, obtain final product nano-magnetic adsorbent, gained nano-magnetic adsorbent is in powder.
3. as claimed in claim 2 a kind of preparation method of nano-magnetic adsorbent it is characterised in that in step 1) in, described will
Sodium lauryl sulphate sds, the temperature of deionized water water bath sonicator are 35～40 DEG C；Water-bath in the described input aqueous phase by oil phase surpasses
The condition of sound is water bath sonicator 15～30min at 35～40 DEG C；The temperature of described water-bath is 75～80 DEG C.
4. as claimed in claim 2 a kind of preparation method of nano-magnetic adsorbent it is characterised in that in step 1) in, described nitrogen
The condition that atmosphere encloses lower reaction is that mechanical agitation makes it start to react under nitrogen atmosphere.
5. as claimed in claim 2 a kind of preparation method of nano-magnetic adsorbent it is characterised in that in step 1) in, described plus
The time entering water soluble starter continuation reaction is 6～8h；Described water soluble starter be selected from Ammonium persulfate., potassium peroxydisulfate, 2,
One of 2 '-azo (2- methyl-propyl amidine) dihydrochloride, the consumption of water soluble starter is styrene by mass percentage
The 0.1%～1% of monomer.
6. as claimed in claim 2 a kind of preparation method of nano-magnetic adsorbent it is characterised in that in step 1) in, described plus
The time entering the dehydrated alcohol mixed liquor reaction of vinylpyridine class monomer is 8～12h.
7. as claimed in claim 2 a kind of preparation method of nano-magnetic adsorbent it is characterised in that in step 1) in, described second
Thiazolinyl pyridines monomer is selected from 2- vinylpyridine, 4-vinylpridine, the derivant of 2- vinylpyridine, 4-vinylpridine
One of derivant；The consumption of described normal octane is 1～4 times of whole monomers in mass ratio.
8. as claimed in claim 2 a kind of preparation method of nano-magnetic adsorbent it is characterised in that in step 2) in, described water
Bathe the ultrasonic time for 10～30min；The temperature of described water-bath is 60～80 DEG C；Described reaction under nitrogen atmosphere is in nitrogen
Atmosphere enclose under by 300～500r/min speed mechanical stirring reaction 1～3h.
9. as claimed in claim 2 a kind of preparation method of nano-magnetic adsorbent it is characterised in that in step 2) in, described wash
Wash using absolute ethanol washing 2～3 times；Described drying is vacuum drying at 65～70 DEG C.
10. as claimed in claim 2 a kind of preparation method of nano-magnetic adsorbent it is characterised in that in step 2) in, described
fecl3、fecl2·4h2O, ammonia and step 1) in vinylpyridine class monomer mass ratio be (3～2): 1: (20～10)
: (8～2).
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| CN105820707B (en) * | 2016-04-01 | 2019-01-15 | 厦门大学 | A kind of radiation shielding coating and preparation method thereof of graphene doping |
| CN106543450B (en) * | 2016-10-21 | 2019-01-22 | 西安建筑科技大学 | A kind of preparation method and application of functional magnetic bipyridyliums coordination polymer |
| CN112958051B (en) * | 2021-03-08 | 2022-09-27 | 河西学院 | Modified magnetic particle/attapulgite composite oil-absorbing resin and preparation method and application thereof |
| CN115814763A (en) * | 2021-12-01 | 2023-03-21 | 肇庆领誉环保实业有限公司 | Chelating adsorbent for electroplating wastewater treatment and preparation method thereof |
| TR2022007799A2 (en) * | 2022-05-13 | 2022-06-21 | Bursa Uludag Ueniversitesi | Use of Magnetic-Photocatalytic m-[poly(ethyleneglycoldimethacrylate-2-vinylpyridine)]-TiO2 Polymer Martis Composite Particles in the Treatment of Textile Waste Water |
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| CN101259403A (en) * | 2004-11-11 | 2008-09-10 | 中国科学院化学研究所 | Method for preparing hollow ball with polymer complex structure by swelling polymerization |
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