CN107876014A - A kind of synthetic method of hollow nucleocapsid magnetic metal organic framework composite material - Google Patents
A kind of synthetic method of hollow nucleocapsid magnetic metal organic framework composite material Download PDFInfo
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- CN107876014A CN107876014A CN201610878221.8A CN201610878221A CN107876014A CN 107876014 A CN107876014 A CN 107876014A CN 201610878221 A CN201610878221 A CN 201610878221A CN 107876014 A CN107876014 A CN 107876014A
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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
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
- B01J20/226—Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—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 form
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Abstract
A kind of synthetic method of hollow nucleocapsid magnetic metal organic framework composite material, the composite are Fe3O4The@ZIF 8 of/ZIF 67, zeolite imidazole fat skeleton (ZIFs) is one kind of MOFs materials, it is a kind of new nano-porous structure with zeolite topological for having transition metal atoms (Zn/Co) to link and generate with imidazoles or imdazole derivatives, wherein ZIFs is as follows by the built-up metal-organic framework materials of metal ion zinc cobalt and 2 methylimidazoles, step respectively：Iron chloride and anhydrous sodium acetate are dissolved in ethylene glycol diethylene glycol (DEG) in the mixed solvent and carry out pyroreaction Fe is made3O4Magnetic nano-particle；By Zn (NO3)2·6H2O、Co(NO3)2·6H2O, 2 methylimidazoles are dissolved in specific solvent respectively；By Fe3O4Magnetic nano-particle is dispersed in specific solvent again respectively by Zn (NO3)2·6H2O、Co(NO3)2·6H2O, 2 methyl imidazole solutions add and can be prepared by object.It is an advantage of the invention that：The composite is using easy package method and solvent structure, have the magnetic response characteristic of magnetic nano-particle and the excellent specific property of zeolite imidazole fat skeleton (ZIFs) concurrently, quick separation and concentration can be achieved using Magneto separate, can be as the adsorbent or solid extracting agent of a kind of excellent performance.
Description
Technical field
The present invention relates to magnetic metal organic framework composite material, particularly a kind of hollow nucleocapsid magnetic metal organic framework
Composite Fe3O4/ ZIF-67@ZIF-8 synthetic method.
Background technology
Metal-organic framework materials (MOFs), a kind of new porous material with pore passage structure, it is a metalloid
The mesh skeleton structure that ion or metal cluster are self-assembly of by coordination and organic ligand, has that specific surface area is big, hole
The characteristics such as road compound with regular structure, the shape and size in hole are controllable, have in absorption, catalysis, separation and wide apply future.
Zeolite imidazole fat framework material (ZIFs) is one kind of MOFs materials, and it is by bivalent metal ion and deprotonation
Imidazoles chain is connected and forms tetrahedral structure, due to there is stronger interaction between imidazoles chain and metal ion, so
ZIFs materials generally have higher heat endurance, resistance to hygroscopy and chemical stability than other MOFs materials.Research is also sent out
Existing ZIFs materials show good performance in catalysis, magnetic, bioactivity, gas storage and separation etc..
For the target contaminant in efficient, quick separation fluid matrix, magnetic separation technique is an optimal selection, magnetic
Property metal organic framework composite is due to without high speed centrifugation or membrane filtration, causing the great interest of people.It is with magnetic
The property magnetic response characteristic of nano-particle and the excellent specific property of ZIFs materials and enjoy favor.The synthesizing magnetic reported at present
MOFs methods have following several：1. embedding inlay technique：Magnetic-particle material is embedded in MOFs surfaces；2. lay-up method：MOFs layers are covered
Lid and superposition growth are in functional magnetic granular material surface；3. package method：MOFs materials around magnetic-particle around it into
Length is simultaneously wrapped up；4. mixing method：By physically or chemically acting on polymerization conjunction is occurred into for MOFs materials and Magnetism granule
Into.
The present invention is by Fe3O4Magnetic nano-particle is dispersed in certain solvent and adds its ZIFs precursor synthetic solvent
Enter wherein, 2-methylimidazole synthesizes nucleocapsid Fe as organic ligand by simple package method3O4/ ZIF-67@ZIF-8 composite woods
Material, then its synthetic product is transferred in the reactor with polytetrafluoro liner and obtains hollow core shell structure compound.Thus carry
Hollow nucleocapsid magnetic metal organic framework composite material Fe is easily synthesized for one kind3O4/ ZIF-67@ZIF-8 method.
The content of the invention
It is an object of the invention to provide a kind of hollow nucleocapsid magnetic metal organic framework composite material Fe3O4/ZIF-67@
ZIF-8 synthetic method, the synthetic method are to use package method and solvent-thermal method, simple, easy to implement, the environmentally friendly no dirt of technique
Dye；The hollow hud typed Fe of synthesis3O4/ ZIF-67@ZIF-8 composites with magnetic nano-particle magnetic response characteristic with
And the excellent specific property of ZIFs materials.
Technical scheme：
A kind of synthetic method of hollow nucleocapsid magnetic metal organic framework composite material, the hollow nucleocapsid magnetic metal have
Machine skeletal composite is Fe3O4/ ZIF-67 ZIF-8, wherein zeolite imidazole fat skeleton (ZIFs) be by metal ion zinc cobalt with
The built-up metal-organic framework materials of 2-methylimidazole (MOFs), synthesis step is as follows：
1) preparation of magnetic nano-particle
By FeCl3·6H2O and anhydrous sodium acetate are dissolved in ethylene glycol-diethylene glycol (DEG) (v/v 1: 1) in the mixed solvent, add table
Face covering simultaneously is allowed to dissolve, and then mixed solution is transferred in the reactor with polytetrafluoro liner, reacted at 200 DEG C
12h, Magneto separate reaction product after cooling, respectively with respectively cleaning 3 times of ultra-pure water and absolute ethyl alcohol, 12h, system are dried in vacuo at 60 DEG C
Obtain Fe3O4Magnetic nano-particle；
2) composite Fe3O4/ ZIF-67@ZIF-8 synthesis
By Fe obtained above3O4Magnetic nano-particle is dispersed in specific solvent and ultrasonic 60min, adds 2- methyl miaows
Azoles solution is stirred, and Co (NO are then slowly added at a temperature of 40 DEG C3)2·6H2O solution and ultrasonic 5min, then by Zn
(NO3)2·6H2O solution adds ultrasonic 10min, and composite Fe is thus made3O4/ZIF-67@ZIF-8；
3) hollow composite material Fe3O4/ ZIF-67@ZIF-8 preparation
120 DEG C continue 1- in the reactor that product after above-mentioned ultrasonic reaction is immediately transferred to have polytetrafluoro liner
8h, simultaneously Magneto separate reaction product is cooled down, with ultra-pure water and absolute ethyl alcohol respectively cleaning 3 times, is then dried in vacuo 12h at 60 DEG C,
It can be prepared by hollow nucleocapsid magnetic metal organic framework composite material Fe3O4/ZIF-67@ZIF-8。
Described surface capping agents can be sodium citrate, dopamine, hexamethylene diamine and polyvinylpyrrolidone.
Described specific solvent can be methanol, ethanol, DMF and ultra-pure water
Co (the NO3)2·6H2O、Zn(NO3)2·6H2O, 2-methylimidazole and specific solvent dosage amount ratio are 1mmol
∶1-4mmol∶3-10mmol∶10-50mL。
The Fe3O4Magnetic nano-particle and Co (NO in mixed liquor3)2·6H2O amount ratio is 5-80mg: 1mmol.
Advantages of the present invention and technique effect：The synthetic method is synthesized using the method for easy package method and solvent heat
Hollow nucleocapsid magnetic metal organic framework composite material Fe3O4/ ZIF-67 ZIF-8, the hollow core-shell composite material have magnetic concurrently
The magnetic response characteristic of nano-particle and the excellent specific property of zeolite imidazole fat skeleton (ZIFs).Without the means such as centrifugation, filtering, profit
Quickly separation can be achieved with Magneto separate, can be as the adsorbent or solid extracting agent of a kind of excellent performance.
Brief description of the drawings
Fig. 1 is the different Fe of magnetic nano-particle dosage3O4/ ZIF-67@ZIF-8TEM scheme (A, B, C Fe3O4Particle is used
Amount is respectively 50mg, 20mg and 10mg core-shell structure；D, E, F Fe3O4Particle dosage is respectively 50mg, 20mg and
10mg hollow composite structure).
Fig. 2 is ZIF-67@ZIF-8 and Fe3O4/ ZIF-67@ZIF-8 XRD.
Embodiment
Technical scheme is further described below by way of several specific embodiments.
Embodiment 1：
A kind of synthetic method of hollow nucleocapsid magnetic metal organic framework composite material, the hollow nucleocapsid magnetic metal have
Machine skeletal composite is Fe3O4/ ZIF-67 ZIF-8, wherein zeolite imidazole fat skeleton (ZIFs) be by metal ion zinc cobalt with
The built-up metal-organic framework materials of 2-methylimidazole (MOFs), synthesis step is as follows：
1) by 6mmol FeCl3·6H2O and 15mmol anhydrous sodium acetates are dissolved in 30mL ethylene glycol-diethylene glycol (DEG) mixed solvent
In, it is transferred into after adding polyvinylpyrrolidone stirring and dissolving in the reactor with polytetrafluoro liner, it is anti-at 200 DEG C
Answer 12h, Magneto separate reaction product and with ultra-pure water and each 3 times of washes of absolute alcohol is used respectively is dried in vacuo 12h at 60 DEG C,
Fe is made3O4Magnetic nano-particle；
2) by 2mmol Co (NO3)2·6H2O、4mmol Zn(NO3)2·6H2O and 15mmol 2-methylimidazoles difference is molten
In 5mL DMF and ultrasonic disperse, 50mg Fe obtained above will be taken3O4Magnetic nano-particle is dispersed in
Ultrasonic 60min in 15mL DMFs, is then added to above-mentioned solution by 2-methylimidazole solution, delays at 40 DEG C
It is slow to add Co (NO3)2·6H2O solution and ultrasonic 5min, then by Zn (NO3)2·6H2O solution adds ultrasonic 10min, thus makes
Obtain composite Fe3O4A schemes in/ZIF-67@ZIF-8 such as Fig. 1；
3) above-mentioned reaction product is transferred to 120 DEG C of lasting 2h in the reactor with polytetrafluoro liner, cooled down and by instead
Product Magneto separate is answered, with DMF and absolute ethyl alcohol respectively cleaning 3 times, 12h is then dried in vacuo at 60 DEG C, i.e.,
Hollow nucleocapsid magnetic metal organic framework composite material Fe can be made3O4D figures in/ZIF-67@ZIF-8 such as Fig. 1.
Fig. 2 is the hollow ZIF-67@ZIF-8 materials of synthesis and hollow Fe3O4/ ZIF-67@ZIF-8 XRD, figure
In show：Fe3O4The XRD of/ZIF-67@ZIF-8 composites and ZIF-67@ZIF-8 XRD coincide very much, thus prove
Fe3O4/ ZIF-67@ZIF-8 composites are by Fe3O4What magnetic nano-particle and ZIF-67@ZIF-8 were formed.Prove Fe3O4/
ZIF-67@ZIF-8 composites are by Fe3O4What magnetic nano-particle and ZIF-67@ZIF-8 were formed.
Embodiment 2：
A kind of synthetic method of hollow nucleocapsid magnetic metal organic framework composite material, synthesis step are as follows：
1) by 6mmol FeCl3·6H2O and 15mmol anhydrous sodium acetates are dissolved in 30mL ethylene glycol-diethylene glycol (DEG) mixed solvent
In, it is transferred into after adding hexamethylene diamine stirring and dissolving in the reactor with polytetrafluoro liner, 12h, magnetic is reacted at 200 DEG C
Separate reaction product and respectively with ultra-pure water and each 3 times of washes of absolute alcohol, be dried in vacuo 12h at 60 DEG C, Fe is made3O4Magnetic
Property nano-particle；
2) by 2mmol Co (NO3)2·6H2O、4mmol Zn(NO3)2·6H2O and 15mmol 2-methylimidazoles difference is molten
In 5mL ultra-pure water and ultrasonic disperse, 20mg Fe obtained above will be taken3O4Magnetic nano-particle is dispersed in 15mL ultra-pure waters
Middle ultrasonic 60min, is then added to above-mentioned solution by 2-methylimidazole solution, and Co (NO are slowly added at 40 DEG C3)2·6H2O is molten
Liquid and ultrasonic 5min, then by Zn (NO3)2·6H2O solution adds ultrasonic 10min, and composite Fe is thus made3O4/ZIF-
B schemes in 67@ZIF-8 such as Fig. 1；
3) above-mentioned reaction product is transferred to 120 DEG C of lasting 6h in the reactor with polytetrafluoro liner, cooled down and by instead
Magneto separate in product is answered, with ultra-pure water and absolute ethyl alcohol respectively cleaning 3 times, is then dried in vacuo 12h at 60 DEG C, you can in being made
Empty core-shell magnetic metal organic framework composite Fe3O4E schemes in/ZIF-67@ZIF-8 such as Fig. 1.
The electron microscope of detection, XRD and embodiment 1 are similar.
Embodiment 3：
A kind of synthetic method of hollow nucleocapsid magnetic metal organic framework composite material, synthesis step are as follows：
1) by 6mmol FeCl3·6H2O and 15mmol anhydrous sodium acetates are dissolved in 30mL ethylene glycol-diethylene glycol (DEG) mixed solvent
In, it is transferred into after adding dopamine stirring and dissolving in the reactor with polytetrafluoro liner, 12h, magnetic is reacted at 200 DEG C
Separate reaction product and respectively with ultra-pure water and washes of absolute alcohol each 3 times, the drying 12h under 60 DEG C of vacuum, obtained Fe3O4Magnetic
Property nano-particle；
2) by 2mmol Co (NO3)2·6H2O、4mmol Zn(NO3)2·6H2O and 15mmol 2-methylimidazoles difference is molten
In 5mL methanol and ultrasonic disperse, 10mg Fe obtained above will be taken3O4Magnetic nano-particle is dispersed in 15mL methanol solutions
Middle ultrasonic 60min, is then added to above-mentioned solution by 2-methylimidazole solution, and Co (NO are slowly added at 40 DEG C3)2·6H2O is molten
Liquid and ultrasonic 5min, then by Zn (NO3)2·6H2O solution adds ultrasonic 10min, and composite Fe is thus made3O4/ZIF-
C schemes in 67@ZIF-8 such as Fig. 1；
3) above-mentioned reaction product is transferred to 120 DEG C of lasting 4h in the reactor with polytetrafluoro liner, cooled down and by instead
Product Magneto separate is answered, with methanol and absolute ethyl alcohol respectively cleaning 3 times, is then dried in vacuo 12h at 60 DEG C, you can hollow core is made
Shell magnetic metal organic framework composite material Fe3O4F schemes in/ZIF-67@ZIF-8 such as Fig. 1.
The electron microscope of detection, XRD and embodiment 1 are similar.
Claims (5)
1. a kind of synthetic method of hollow nucleocapsid magnetic metal organic framework composite material, the hollow nucleocapsid magnetic metal are organic
Skeletal composite is Fe3O4/ ZIF-67@ZIF-8, wherein zeolite imidazole fat skeleton (ZIFs) be by metal ion zinc and cobalt with
The built-up metal-organic framework materials of 2-methylimidazole (MOFs), synthesis step is as follows：
1) by FeCl3·6H2O and anhydrous sodium acetate are dissolved in ethylene glycol-diethylene glycol (DEG) (v/v 1: 1) in the mixed solvent, add surface
Covering simultaneously is allowed to dissolve, and then mixed solution is transferred in the reactor with polytetrafluoro liner, reacted at 200 DEG C
12h, Magneto separate reaction product after cooling, respectively with respectively cleaning 3 times of ultra-pure water and absolute ethyl alcohol, 12h, system are dried in vacuo at 60 DEG C
Obtain Fe3O4Magnetic nano-particle；
2) by Fe obtained above3O4Magnetic nano-particle is dispersed in specific solvent and ultrasonic 60min, adds 2-methylimidazole
Solution is stirred, and Co (NO are then slowly added at a temperature of 40 DEG C3)2·6H2O and ultrasonic 5min, then by Zn (NO3)2·
6H2O solution adds ultrasonic 10min, and composite Fe is thus made3O4/ZIF-67@ZIF-8；
3) 120 DEG C continue 1-8h in the reactor for being immediately transferred to the product after above-mentioned ultrasonic reaction have polytetrafluoro liner,
Simultaneously Magneto separate reaction product is cooled down, with ultra-pure water and absolute ethyl alcohol respectively cleaning 3 times, is then dried in vacuo 12h at 60 DEG C, you can
Hollow nucleocapsid magnetic metal organic framework composite material Fe is made3O4/ZIF-67@ZIF-8。
2. the synthetic method of hollow nucleocapsid magnetic metal organic framework composite material according to claim 1, it is characterised in that：
Described surface capping agents can be sodium citrate, dopamine, hexamethylene diamine and polyvinylpyrrolidone.
3. the synthetic method of hollow nucleocapsid magnetic metal organic framework composite material according to claim 1, it is characterised in that：
Described specific solvent can be methanol, ethanol, DMF and ultra-pure water.
4. the synthetic method of hollow nucleocapsid magnetic metal organic framework composite material according to claim 1, it is characterised in that：
Co (the NO3)2·6H2O、Zn(NO3)2·6H2O, the amount ratio of 2-methylimidazole and specific solvent is 1mmol: 1-4mmol:
3-10mmol∶10-50mL。
5. the synthetic method of hollow nucleocapsid magnetic metal organic framework composite material according to claim 1, it is characterised in that：
The Fe3O4Magnetic nano-particle and Co (NO in mixed liquor3)2·6H2O amount ratio is 5-80mg: 1mmol.
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| CN109317067A (en) * | 2018-11-05 | 2019-02-12 | 国家纳米科学中心 | A kind of nucleocapsid heterojunction structure composite material and preparation method |
| CN109364899A (en) * | 2018-12-21 | 2019-02-22 | 上海纳米技术及应用国家工程研究中心有限公司 | The preparation method and products thereof of magnetic ZIF-8 Nano composite granules |
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