CN106745317A - One-step method prepares method and its application of porous ferroferric oxide magnetic Nano microsphere - Google Patents

One-step method prepares method and its application of porous ferroferric oxide magnetic Nano microsphere Download PDF

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CN106745317A
CN106745317A CN201611034917.9A CN201611034917A CN106745317A CN 106745317 A CN106745317 A CN 106745317A CN 201611034917 A CN201611034917 A CN 201611034917A CN 106745317 A CN106745317 A CN 106745317A
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polyethyleneimine
porous
heavy metal
nano microsphere
magnetic nano
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吕挺
张川
赵红挺
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Hangzhou Dianzi University
Hangzhou Electronic Science and Technology University
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Hangzhou Electronic Science and Technology University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002Solid 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
    • B01J20/28004Sorbent size or size distribution, e.g. particle size
    • B01J20/28007Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002Solid 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
    • B01J20/28009Magnetic properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid 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 form
    • B01J20/28016Particle form
    • B01J20/28019Spherical, ellipsoidal or cylindrical
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/08Ferroso-ferric oxide (Fe3O4)
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions
    • C01P2004/32Spheres
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/42Magnetic properties

Abstract

The present invention relates to method and its application that one-step method prepares porous ferroferric oxide magnetic Nano microsphere.The method prepares porous Fe with polyethyleneimine as end-capping reagent by solvent thermal reaction one-step method3O4Nano microsphere, without extra template and template removal step.Polyethyleneimine end-capping reagent can control grain growth and packed structures so as to regulate and control the pore structure and specific surface area of magnetic microsphere, while the polyethyleneimine adhered on crystal grain possesses abundant amido, heavy metal has very strong sequestering power.The porous magnetic Nano microsphere that the present invention is obtained, preparation process is simple, adsorption capacity is big, and there is good application prospect in the heavy metal ion adsorbed field in water body.

Description

One-step method prepares method and its application of porous ferroferric oxide magnetic Nano microsphere
Technical field
The present invention relates to synthesize a kind of porous Fe suitable for removal of heavy metal ions3O4Magnetic Nano microsphere, and the magnetic The specifically used method of property Nano microsphere.Specifically related to polyethyleneimine as end-capping reagent, one-step method prepares porous Fe3O4Magnetic Nano microsphere and its application in heavy metal ion adsorbed field.
Background technology
With continuing to develop for industrial economy, increasing water body receives heavy metal ion (Pb2+、Cd2+、Cu2+Deng) Pollution, serious harm environment and health.At present, the minimizing technology both at home and abroad for Heavy Metals in Waters ion is mainly wrapped Include membrane separation process, absorption method, ion-exchange, chemical precipitation method and bio-flocculation process and restoration of the ecosystem method etc..Chemical precipitation Method is only limitted to high concentration effluent containing heavy metal ions, and is also easy to produce the substantial amounts of sludge containing heavy metal, so as to cause new environment to ask Topic.Ion-exchange is usually used in low concentration heavy metal water treatment, and adsorption capacity is relatively low.UF membrane although separative efficiency is higher, But equipment complexity, vulnerable to pollution, high energy consumption.Microbial technique generally existing cultivation cycle is long, and research is predominantly stayed at present Laboratory stage.By contrast, the absorption method advantage such as have selectivity high, easy to operate, low cost, efficiency high, but common suction There is the defects such as recovery difficulty in enclosure material.Because magnetic Nano microsphere prepares simple, surface modificability by force, in heavy metal containing sewage Process is simple, flexible, efficiency high in treatment, and easily recycle and reuse.These characteristics make it in effluent containing heavy metal ions treatment In application prospect very desirable.
Due to Fe3O4The absorption property of nano-particle heavy metal ion in itself is extremely limited, it usually needs using to a huge sum of money The stronger material of category ionic adsorption performance carries out surface modification, parcel or compound to it, and the magnetic that can just obtain excellent performance is inhaled Attached dose.For example with amino silane (Xu Z Y et al, Journal of Colloid and Interface Science, 2010,349,293-299;An Q D et al,Chemical Engineering Journal,2013,215-216,461- 471), shitosan (Liu X W et al, Langmuir, 2009,25,3-8;CN 104059167A;CN 102258980A;CN 103263895A), humic acid (Jiang G B et al, Environmental Science&Technology, 2008,42, 6949-6954), polyaniline (Wang H Y et al, Environmental Science&Technology, 2015,49, 5654-5662), polyvinyl alcohol (CN 104549083A;CN 105664884A), polyamide (CN 104525158A), black algae (Li G X et al, Desalination and Water Treatment, 2016,57,8480-8493), ethylenediamine tetrem Sour (CN 104724787A), mesoporous carbon (CN 104258827A), CNT (CN 104289200A), cellulose (CN 103183832A), plant cassava stalk (CN 104307488A) etc. is to Fe3O4Nano-particle carries out surface modification, parcel or multiple Close, show excellent heavy metal ion adsorbed performance.Current Fe3O4The preparation method of heavy metal ion magnetic adsorbent The overwhelming majority is limited to the above method, and obtained magnetic adsorbent adsorption effect is good, but preparation technology is still complex, consumption When.At present, prepared on one-step method and be applied to heavy metal ion adsorbed porous Fe3O4The method of Nano microsphere is rarely reported.
The content of the invention
In order to solve the above-mentioned technical problem the present invention, overcomes deficiency of the prior art, there is provided a kind of synthetic method is succinct , using technique easily, suitable for the porous Fe of Heavy Metals in Waters ion remaval3O4The preparation method of magnetic Nano microsphere.
To reach above-mentioned purpose, the present invention uses following technical scheme:
Method prepared by the magnetic nano-particle that the present invention is provided, comprises the following steps:
(1) iron chloride, sodium acetate, polyethyleneimine are dissolved in ethylene glycol respectively, then mix three kinds of solution, fully stirred Uniform mixed solution is formed after mixing.
(2) above-mentioned mixed solution is transferred in autoclave, the solvent thermal reaction under conditions of 180-220 DEG C;Treat anti- After answering temperature in the kettle to naturally cool to room temperature, black product is collected, repeatedly washing, obtains the polyethylene of the favorable dispersibility in water The porous Fe of imines modification3O4Magnetic Nano microsphere.
Further, in above-mentioned preparation method step (1), described polyethyleneimine amine content accounts for the quality point of mixed solution Number is 1.0~5.5%.
In above-mentioned preparation method step (1), described polyethyleneimine molecular weight is 300~10000.
In above-mentioned preparation method step (2), the described reaction time is 2~24h.
In above-mentioned preparation method step (2), the Fe of described favorable dispersibility position 0.3%3O4Aqueous microsphere dispersion liquid is quiet Put still uniform after 2h, do not occur substantially heavy poly-, its particle diameter distribution does not occur significant change.
Present invention also offers the amine-modified porous Fe of above-mentioned polyethyleneimine3O4Magnetic Nano microsphere is removed in water environment The application of heavy metal ion, these heavy metal ion include Pb2+、Cd2+、Cu2+In at least one.
The beneficial effects of the invention are as follows:
Inventor has found through further investigation, during solvent thermal reaction, Fe3O4Microballoon is piled up by crystal grain and formed, therefore brilliant The size of grain will produce large effect with accumulation mode to the size of Armco magnetic iron microballoon and porosity.Polyethyleneimine end-capping reagent On the one hand grain surface is can be adsorbed on, on the other hand can improves reaction medium viscosity, lift Growing Process of Crystal Particles resistance to mass tranfer, two Aspect factor can suppress Fe3O4The growth of microballoon component units (crystal grain).Therefore by adjusting polyethyleneimine consumption and molecule Amount controllable Fe3O4Crystal grain growth with aggregation, so as to further control Fe3O4The size and pattern of microballoon, finally give micro- The Fe that ball size reduces, porosity is lifted, specific surface area increases, polyethyleneimine adhesion amount increases3O4Magnetic porous microspheres.By Possess abundant amido in polyethyleneimine, with heavy metal ion and coordination chelant ability well, therefore above-mentioned microballoon can It is applied to heavy metal adsorption and separation field.
Preparation process of the present invention is simple, and specific surface area and the amido quantity of its magnetic microsphere can be carried out by polyethyleneimine Regulation and control.The amine-modified porous Fe of this kind of polyethyleneimine3O4Magnetic Nano microsphere favorable dispersibility in water, only need to use hand rolling 10s-60s can be well dispersed in effluent containing heavy metal ions, and the heavy metal ion in rapid adsorption water body.In extraneous magnetic In the presence of, heavy metal ion rapid within the 30s times can be separated from water body.The amido protonation when pH is less than 3 Height, the electrostatic repulsion of generation can promote heavy metal ion to be desorbed, therefore the magnetic particle for reclaiming can use the hydrochloric acid of pH=3.0 Solution regenerated from washing, is then reused for the absorption of heavy metal ion and separates.
In a word, the amine-modified porous Fe of polyethyleneimine prepared by the present invention3O4Magnetic Nano microsphere is inhaled in heavy metal ion It is attached to have much application value with separation field.
Brief description of the drawings
Fig. 1 is the amine-modified porous Fe of prepared polyethyleneimine in the embodiment of the present invention 23O4Magnetic Nano microsphere is transmitted Electron microscope picture.
Specific embodiment
The present invention is described in detail below by specific embodiment.
Embodiment 1:
Take 2.5g FeCl3·6H2O, 3.6g NaAc and 4.8g polyethyleneimines (molecular weight 10000) are dissolved in three parts respectively In ethylene glycol, three kinds of solution are then mixed into (ethylene glycol amounts to 72.5g), homogeneous solution is formed after being sufficiently stirred for.It is put into high pressure 24h is reacted in reactor at 180 DEG C, product is collected with magnet, and respectively cleaned three times with water, absolute ethyl alcohol, 50 DEG C of vacuum are done Dry 24h, obtains the amine-modified Fe of polyethyleneimine3O4Magnetic porous Nano microsphere.The magnetic microsphere saturation magnetization is 74.6emu/g, analyzes through hot weightless instrument, and polyethyleneimine amine content is 9.4%;Detected through nitrogen adsorption instrument, specific surface area is 78.5m2/g.Take 0.02g Fe3O4Microballoon adds (pH=5.5, Cu in 50mL copper ion waste water2+Concentration is 50mg/L), at 25 DEG C Magneto separate, Cu after lower concussion 2h2+Clearance is up to 98.6%.After recycling 5 times, its clearance is still up to 90.3%.
Embodiment 2:
Take 2.0g FeCl3·6H2O, 8.0g NaAc and 3.0g polyethyleneimines (molecular weight 10000) are dissolved in three parts respectively In ethylene glycol, three kinds of solution are then mixed into (ethylene glycol amounts to 72.5g), homogeneous solution is formed after being sufficiently stirred for.It is put into high pressure 6h is reacted in reactor at 200 DEG C, product is collected with magnet, and respectively cleaned three times with water, absolute ethyl alcohol, 50 DEG C of vacuum drying 24h, obtains the amine-modified Fe of polyethyleneimine3O4Magnetic porous Nano microsphere.The magnetic microsphere saturation magnetization is 75.2emu/ G, analyzes through hot weightless instrument, and polyethyleneimine amine content is 7.5%;Detect that specific surface area is 57.7m through nitrogen adsorption instrument2/g.Take 0.02g Fe3O4Microballoon adds (pH=5.5, Cu in 50mL copper ion waste water2+Concentration is 50mg/L), after shaking 2h at 25 DEG C Magneto separate, Cu2+Clearance is up to 95.6%.After recycling 5 times, its clearance is still up to 86.7%.
Embodiment 3:
Take 2.0g FeCl3·6H2O, 8.0g NaAc and 0.85g polyethyleneimines (molecular weight 1800) are dissolved in three parts respectively In ethylene glycol, three kinds of solution are then mixed into (ethylene glycol amounts to 72.5g), homogeneous solution is formed after being sufficiently stirred for.It is put into high pressure 2h is reacted in reactor at 220 DEG C, product is collected with magnet, and respectively cleaned three times with water, absolute ethyl alcohol, 50 DEG C of vacuum drying 24h, obtains the amine-modified Fe of polyethyleneimine3O4Magnetic porous Nano microsphere.The magnetic microsphere saturation magnetization is 67.9emu/ G, analyzes through hot weightless instrument, and polyethyleneimine amine content is 2.3%;Detect that specific surface area is 28.3m through nitrogen adsorption instrument2/g.Take 0.04g Fe3O4Microballoon adds (pH=5.5, Pb in 50mL lead ion waste water2+Concentration is 35mg/L), after shaking 2h at 25 DEG C Magneto separate, Pb2+Clearance is up to 96.3%.After recycling 5 times, its clearance is still up to 87.8%.
Embodiment 4:
Take 2.0g FeCl3·6H2O, 8.0g NaAc and 4.8g polyethyleneimines (molecular weight 300) are dissolved in three parts of second respectively In glycol, three kinds of solution are then mixed into (ethylene glycol amounts to 72.5g), homogeneous solution is formed after being sufficiently stirred for.It is put into high pressure anti- Answer and reacted at 200 DEG C in kettle 6h, product is collected with magnet, and respectively cleaned three times with water, absolute ethyl alcohol, 50 DEG C of vacuum drying 24h, obtains the amine-modified Fe of polyethyleneimine3O4Magnetic porous Nano microsphere.The magnetic microsphere saturation magnetization is 77.3emu/ G, analyzes through hot weightless instrument, and polyethyleneimine amine content is 8.7%;Detect that specific surface area is 46.8m through nitrogen adsorption instrument2/g.Take 0.02g Fe3O4Microballoon adds (pH=5.5, Cd in 50mL cadmium ion waste water2+Concentration is 20mg/L), after shaking 2h at 25 DEG C Magneto separate, Cd2+Clearance is up to 93.8%.After recycling 5 times, its clearance is still up to 83.4%.
Embodiment 5:
Take 2.0g FeCl3·6H2O, 8.0g NaAc and 3.0g polyethyleneimines (molecular weight 10000) are dissolved in three parts respectively In ethylene glycol, three kinds of solution are then mixed into (ethylene glycol amounts to 72.5g), homogeneous solution is formed after being sufficiently stirred for.It is put into high pressure 15h is reacted in reactor at 200 DEG C, product is collected with magnet, and respectively cleaned three times with water, absolute ethyl alcohol, 50 DEG C of vacuum are done Dry 24h, obtains the amine-modified Fe of polyethyleneimine3O4Magnetic porous Nano microsphere.The magnetic microsphere saturation magnetization is 77.5emu/g, analyzes through hot weightless instrument, and polyethyleneimine amine content is 7.3%;Detected through nitrogen adsorption instrument, specific surface area is 63.5m2/g.Take 0.02g Fe3O4Microballoon adds (pH=5.5, Cu in 50mL copper ion waste water2+Concentration is 50mg/L), at 25 DEG C Magneto separate, Cu after lower concussion 2h2+Clearance is up to 97.1%.After recycling 5 times, its clearance is still up to 89.3%.
The present invention can be summarized with others without prejudice to the concrete form of spirit or central characteristics of the invention.Therefore, nothing By from the point of view of which point, above-mentioned experimental program of the invention can only all be considered the description of the invention and can not limit this hair Bright, claim indicates the scope of the present invention, and the scope of the present invention is not pointed out in above-mentioned explanation, therefore, with this hair Any change in bright claims suitable implication and scope, is all considered as being included in the scope of claims It is interior.

Claims (7)

1. the method that one-step method prepares porous ferroferric oxide magnetic Nano microsphere, it is characterised in that methods described includes following Step:
(1) iron chloride, sodium acetate, polyethyleneimine are dissolved in ethylene glycol respectively, are then mixed three kinds of solution, after being sufficiently stirred for Form uniform mixed solution;
(2) mixed solution in step (1) is transferred in autoclave, the solvent thermal reaction under conditions of 180-220 DEG C;Treat After reactor temperature naturally cools to room temperature, black product is collected, repeatedly washing, obtains the polyethyleneimine of favorable dispersibility The porous Fe of modification3O4Magnetic Nano microsphere.
2. method according to claim 1, it is characterised in that polyethyleneimine accounts for the quality of mixed solution in step (1) Fraction is 1.0~5.5%.
3. method according to claim 1, it is characterised in that in step (1) polyethyleneimine molecular weight be 300~ 10000。
4. method according to claim 1, it is characterised in that the reaction time is 2~24h in step (2).
5. method according to claim 1, it is characterised in that the favorable dispersibility described in step (2) is 0.3% Fe3O4Aqueous microsphere dispersion liquid is still uniform after 2h is stood, and does not occur substantially to sink to gather, and its particle diameter distribution does not occur significant change.
6. using the porous Fe that polyethyleneimine obtained in the method described in claim 1-5 any one is amine-modified3O4Magnetic Nano The purposes of microballoon, it is characterised in that for the heavy metal ion in adsorbing separation water environment.
7. purposes according to claim 6, it is characterised in that the heavy metal ion is Cu2+、Pb2+、Cd2+In one kind Or it is various.
CN201611034917.9A 2016-11-16 2016-11-16 One-step method prepares method and its application of porous ferroferric oxide magnetic Nano microsphere Pending CN106745317A (en)

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CN108607514A (en) * 2018-05-22 2018-10-02 华东理工大学 A kind of preparation method of aminated magnetic porous microspheres
CN109400889A (en) * 2017-08-16 2019-03-01 中国科学院大连化学物理研究所 A kind of Metal Porous-Organic material of magnetic modification and its preparation and application
CN109437323A (en) * 2018-11-22 2019-03-08 江苏理工学院 A kind of preparation method of biology sympathy magnetic ferroferric oxide nano-particles
CN110724221A (en) * 2019-10-25 2020-01-24 西南石油大学 Magnetic super-hydrophobic polystyrene porous material and preparation method thereof
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109400889A (en) * 2017-08-16 2019-03-01 中国科学院大连化学物理研究所 A kind of Metal Porous-Organic material of magnetic modification and its preparation and application
CN109400889B (en) * 2017-08-16 2021-09-24 中国科学院大连化学物理研究所 Magnetic modified metal organic porous material and preparation and application thereof
CN108079978B (en) * 2017-12-15 2020-10-20 吉林化工学院 Fe3O4-NH2Preparation method and application of-PEI magnetic nano material
CN108607514A (en) * 2018-05-22 2018-10-02 华东理工大学 A kind of preparation method of aminated magnetic porous microspheres
CN109437323A (en) * 2018-11-22 2019-03-08 江苏理工学院 A kind of preparation method of biology sympathy magnetic ferroferric oxide nano-particles
CN110724221A (en) * 2019-10-25 2020-01-24 西南石油大学 Magnetic super-hydrophobic polystyrene porous material and preparation method thereof

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