CN107715843A - A kind of method of the materials of micro-diplopore ZIF 8 in Fast back-projection algorithm at normal temperatures - Google Patents
A kind of method of the materials of micro-diplopore ZIF 8 in Fast back-projection algorithm at normal temperatures Download PDFInfo
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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
- 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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- B01J20/28054—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 surface properties or porosity
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Abstract
The invention discloses a kind of method of the materials of micro-diplopore ZIF 8 in Fast back-projection algorithm at normal temperatures, generated time successfully can be reduced into 20min using this method.This method comprises the following steps：First, it is zinc oxide is soluble in water；2nd, it is Zinc diacetate dihydrate is soluble in water；3rd, 2 methylimidazoles are dissolved in N, in N dimethylformamides；4th, burnett's solution is mixed with zinc acetate solution, be sufficiently stirred；5th, 2 methyl imidazole solutions and bromohexadecane are added into the mixed solution of zinc oxide and zinc acetate, is sufficiently stirred；6th, products therefrom is filtered, dries, obtain the materials of multi-stage porous ZIF 8.The present invention greatly shortens generated time by adding zinc oxide and template bromohexadecane, not only easy to operate, mild condition.Product has abundant pore passage structure, not only possesses high specific surface area, and Stability Analysis of Structures, has preferable application prospect in terms of the absorption and catalysis of macromolecular.
Description
Technical field
The invention belongs to the quick preparation field of multi-stage porous metal organic framework, and in particular to a kind of conjunction quick at normal temperatures
Into the method for middle micro-diplopore ZIF-8 materials.
Background technology
In recent two decades, metal-organic framework materials (MOFs) have caused researcher as emerging porous material
Great interest.[Zhou H C,Long J R,Yaghi O M.Introduction to metal–organic
Frameworks [J] .2012.] its structure diversity, it is very big that adjustability and porous make MOFs have in multifunctional application
Potentiality.[Liu J,Chen L,Cui H,et al.Applications of metal–organic frameworks in
heterogeneous supramolecular catalysis[J].Chemical Society Reviews,2014,43
(16):6011-6061.] wherein, the hole of MOFs materials plays vital role.Although some mesoporous MOFs are
Be reported [Li P Z, Wang X J, Tan S Y, et al.Clicked isoreticular metal-organic
frameworks and their high performance in the selective capture and separation
of large organic molecules[J].Angewandte Chemie International Edition,2015,54
(43):12748-12752.], but experimental study shows, MOFs aperture is mainly adjustable under micropore state, this in practice for
The application of material is unfavorable.Because small aperture has slowed down the diffusion rate of molecule and has limited the motion of macromolecular.Institute
It is our research emphasis with multi-stage porous MOFs.Multi-stage porous MOFs not only inherits the characteristics of traditional MOFs micropores, and is being situated between
Innovated in terms of hole, macropore.Micropore is the sizable specific surface area of material manufacture and mesoporous and macropore is advantageous to molecule
Transmission and diffusion.Multi-stage porous MOFs synthesis is our focus.
Fang et al. [Fang Q R, Makal T A, Young M D, et al.Recent advances in the
study of mesoporous metal-organic frameworks[J].Comments on Inorganic
Chemistry,2010,31(5-6):165-195.] and Xuan et al. [Xuan W, Zhu C, Liu Y, et
al.Mesoporous metal–organic framework materials[J].Chemical Society Reviews,
2012,41(5):1677-1695.] more detailed summary has been done to mesoporous MOFs.It is and mesoporous in most of reports
In MOFs, most it is worth we go research be aperture control and the stability of material.Typically multistage is produced using solvent method
Hole MOFs materials, made MOFs duct are generally occupied by solvent molecule, and solvent molecule must be removed permanent to obtain
Porosity is without causing its structural collapse.The hole of usual material is bigger, then the easier avalanche of its framework.Although MOFs can
To be built by well-designed organic ligand (framework connector) to produce macropore, but framework generally interpenetrates, and causes material
Appearance runs through structure, and such material is also unstable.Therefore, realize permanent void ratio in its micropore class in mesoporous MOFs
Like more difficult in thing.Through employing some strategies, by using elongated organic ligand and other extendable connectors
Mesoporous MOFs is built together, and this makes it easy to the secondary structure unit (SBU) to form stable large volume.In addition, modified after synthesis
It is still to produce the process useful with adjustable mesopore MOFs materials.In principle, can be using the part that can be extended linearly
Larger passage or hole are introduced during mesoporous MOF synthesis.However, tend to be fast after part removal by the MOFs of longer part structure
Fast avalanche, cause interpenetrating between multiple ducts, this considerably reduce aperture, so as to limit the entrance of macromolecular.Find and close
Suitable part, it is one of our work to prepare mesoporous MOFs.2002, [Eddaoudi M, the Kim J, Rosi such as Eddaoudi
N,et al.Systematic design of pore size and functionality in isoreticular MOFs
and their application in methane storage[J].Science,2002,295(5554):469-472.]
First mesoporous MOF (Zn has been synthesized using organic ligand trityl dicarboxylic ester (TPDC)4O(TPDC)3(DMF)12(H 2O
)2).The material has the expection topological structure of six line borates (CaB 6), the mesoporous MOF being made up of the SBU of octahedral shape.
2010, Yaghi ' s seminars [Furukawa H, Ko N, Go Y B, et al.Ultrahigh porosity in
metal-organic frameworks[J].Science,2010,329(5990):424-428.] closed using tribenzoate
Into MOF-180, the MOF-177 structure cells that its volume ratio is traditional are big 2 times, and the porosity of crystal is more up to 89%.Wang
Et al. [Wang X S, Ma S, Sun D, et al.A Mesoporous Metal-Organic Framework with
Permanent Porosity[J].Journal of the American Chemical Society,2006,128(51):
16474-16475.] the mesoporous MOF-1 for not having mutually to run through in structure is reported, and material presents good heat and learned surely
It is qualitative.
Now, we chemically the good MOF of stability can start with, and by adding longer part, draw to MOFs materials
Enter mesoporous.Zeolite imidazole ester frame structure material (ZIFs) is a kind of new MOFs.ZIFs materials are not only all with MOFs
Advantage, it also possesses outstanding heat endurance and chemical resistance, but its aperture generally only hasTherefore synthesis multi-stage porous
ZIFs improves the concern that its performance receives researchers.We can contemplate certain by being added in building-up process
The part of length, material meso-hole structure unit is occurred, prepare multilevel hole material.
The present invention, as template, rapidly synthesizes a kind of middle micro-diplopore metal-organic framework material using bromohexadecane
Material.
The content of the invention
It is an object of the invention to provide a kind of method of micro-diplopore ZIF-8 materials in Fast back-projection algorithm at normal temperatures, it is intended to
Easy rapidly synthesis has micropore, the ZIF-8 materials in mesoporous two kinds of ducts simultaneously.
Raw material of the present invention is zinc oxide, Zn (CH3COO)2·2H2O (Zinc diacetate dihydrate), 2-methylimidazole, template bromine
For hexadecane (being purchased from lark prestige), DMF, bimetal salt, bromo 16 are formed using zinc oxide and zinc acetate
Alkane is as structure directing agent, you can Fast back-projection algorithm goes out a kind of ZIF-8 materials rich in a variety of pore passage structures.
The purpose of the present invention is achieved through the following technical solutions.
A kind of method of Fast back-projection algorithm multi-stage porous ZIF-8 materials, comprises the following steps：
(1) it is zinc oxide is soluble in water, stirring, obtain zinc oxide aqueous solution；
(2) it is Zinc diacetate dihydrate is soluble in water, stirring, obtain zinc acetate aqueous solution；
(3) 2-methylimidazole is dissolved in DMF, stirs, obtain 2-methylimidazole solution；
(4) zinc oxide aqueous solution of step (1) is mixed with the zinc acetate aqueous solution of step (2), stir, obtain zinc oxide and
The mixed solution of zinc acetate；
(5) in the mixed solution of the zinc oxide to step (4) and zinc acetate add step (3) 2-methylimidazole solution and
Bromohexadecane, it is sufficiently stirred；
(6) step (5) products therefrom is filtered, places into vacuum drying chamber and dry, multi-stage porous ZIF-8 materials are made.
Preferably, the mixing time in step (1) is 20-30 minutes.
Preferably, the mixing time in step (2), (3) is 10-20 minutes.
Preferably, the mixing time in step (4) is 20-30 minutes.
Preferably, the time of step (5) described stirring is 20-30 minutes, more preferably 20 minutes.
Preferably, the temperature of step (6) described drying is 110-120 DEG C, and the dry time is 10-12h.
Preferably, step (1), step (2), step (3), step (4), step (5) are carried out at normal temperatures.
Preferably, the Zn (CH3COO)2·2H2O, zinc oxide, 2-methylimidazole, the mol ratio of bromohexadecane are (1-
1.1)：(0.7-0.8)：(1.2-1.3)：(0.7-0.8).
Relative to prior art, the invention has the advantages that and effect：
(1) method of the invention only can synthesize ZIF-8 materials by 20min, and the material possesses abundant hole
Road structure (micropore and mesoporous), not only Stability Analysis of Structures, and have high specific surface area, has in terms of the absorption and catalysis of macromolecular
Preferable application prospect.
(2) method cost of material of the invention is cheap, and environmental pollution is few, it is possible to achieve industrialization.
(3) present invention is by adding zinc oxide and template, you can Fast back-projection algorithm multi-stage porous ZIF-8 materials at normal temperatures,
It is simple to operate, mild condition, the steps such as heating, ultrasound are avoided, save the energy.
Brief description of the drawings
The X-ray diffraction for the middle micro-diplopore ZIF-8 materials that Fig. 1 is prepared for the ZIF-8 materials and embodiment 1 of computer simulation
Figure.
Fig. 2 is the N of middle micro-diplopore ZIF-8 materials prepared by embodiment 12Adsorption-desorption isothermal figure.
Fig. 3 is the complete opening pore size distribution curve that middle micro-diplopore ZIF-8 materials prepared by embodiment 1 calculate according to DFT models
Figure.
Fig. 4 is the stereoscan photograph of middle micro-diplopore ZIF-8 materials prepared by the embodiment of the present invention 1.
Fig. 5 is the transmission electron microscope photo of middle micro-diplopore ZIF-8 materials prepared by the embodiment of the present invention 1.
Embodiment
The invention will be further described with reference to the accompanying drawings and examples, but the scope of protection of present invention is not
It is confined to the scope of embodiment statement.
Embodiment 1
0.285g zinc oxide is dissolved in 5mL deionized waters, stirs 20 minutes, obtains burnett's solution；By the water of 1.097g bis-
Close zinc acetate to be dissolved in 5mL deionized waters, stir 10 minutes, obtain zinc acetate solution；0.492g 2-methylimidazoles are dissolved in
5mLN, in dinethylformamide, stir 10 minutes, obtain 2-methylimidazole solution；Burnett's solution and zinc acetate solution are mixed
Close, stir 20 minutes, obtain the mixed solution of zinc oxide and zinc acetate；2- first is added into the mixed solution of zinc oxide and zinc acetate
Base imidazole solution and 1.07g bromohexadecanes, stir 20 minutes；Products therefrom is filtered, is put into 110 DEG C of vacuum drying chambers
Middle drying 10 hours, middle micro-diplopore ZIF-8 materials are obtained, labeled as sample A.
Embodiment 2
0.296g zinc oxide is dissolved in 5mL deionized waters, stirs 30 minutes, obtains burnett's solution；By the water of 1.097g bis-
Close zinc acetate to be dissolved in 5mL deionized waters, stir 20 minutes, obtain zinc acetate solution；0.485g2- methylimidazoles are dissolved in 5mLN,
In dinethylformamide, stir 20 minutes, obtain 2-methylimidazole solution；Burnett's solution is mixed with zinc acetate solution, stirred
Mix 30 minutes, obtain the mixed solution of zinc oxide and zinc acetate；2- methyl miaows are added into the mixed solution of zinc oxide and zinc acetate
Azoles solution and 1.11g bromohexadecanes, stir 30 minutes；Products therefrom is filtered, is put into 120 DEG C of vacuum drying chambers and does
Dry 12 hours, middle micro-diplopore ZIF-8 materials are obtained, labeled as sample B.
Analyzed using middle micro-diplopore ZIF-8 materials prepared by embodiment 1 as representative, other embodiments are micro- double in preparing
The analysis result of hole ZIF-8 materials does not provide one by one substantially with embodiment 1.
(1) at normal temperatures in Fast back-projection algorithm micro-diplopore ZIF-8 materials crystal structure properties
Crystalline substance using the D8-ADVANCE models X-ray diffractometer that German Bruker companies produce to the embodiment of the present invention 1
Body structure is characterized.
The wide-angle X for the multi-stage porous ZIF-8 materials that Fig. 1 is prepared for the ZIF-8 materials and the embodiment of the present invention 1 of computer simulation is penetrated
Ray diffraction diagram.The ZIF-8 of computer simulation is the perfect cystal that zinc ion is formed with 2-methylimidazole, can fully demonstrate its crystal formation knot
Structure, it can be compareed with experimental result.From figure 1 it appears that compared with the ZIF-8 materials of computer simulation, what embodiment 1 was prepared
There is the characteristic diffraction peak of stronger ZIF-8 metal organic frameworks in sample A, illustrates the ZIF-8 of high-crystallinity in product be present
Component.
(2) at normal temperatures in Fast back-projection algorithm micro-diplopore ZIF-8 materials pore properties
Using holes of the ASAP2460 of Micro companies of U.S. production than surface apertures distribution instrument to sample prepared by the present invention
Structure is characterized, as a result as shown in table 1.As can be seen from Table 1, the ZIF-8 materials prepared by the present invention have higher micro-
Hole and mesoporous pore volume.
Table 1
Fig. 2 is the N of middle micro-diplopore ZIF-8 materials prepared by the embodiment of the present invention 12Adsorption-desorption isothermal figure, in P/P0<
I type adsorption isotherms are shown as under 0.01 pressure, adsorbance steeply rises, and shows that sample has microcellular structure.In relative pressure
0.85 or so there are IV type adsorption hysteresis rings, and this is mesoporous material in N2Characteristic feature in adsorption desorption curve, show that material contains
Have mesoporous.
Fig. 3 DFT full aperture distribution maps show that multi-stage porous ZIF-8 materials prepared by embodiment 1 are except possessing a large amount of 1nm
The micropore canals of left and right, while possess a large amount of 40nm or so mesoporous and bigger macropore duct.Macropore be not material in itself
Have, but accumulation hole is formd by the accumulation of material granule.Show by this method can with Fast back-projection algorithm middle micro-diplopore
ZIF-8 materials.
(3) SEM of micro-diplopore ZIF-8 materials schemes in Fast back-projection algorithm at normal temperatures
Product is characterized using JSM-6330F types ESEM (electronics corporation JEOL, Japan).As a result such as Fig. 4 institutes
Show, it can be seen that the sample A of preparation is in coccoid, and material surface has abundant micropore and mesoporous, and little particle is packed together, shape
Into accumulation hole.
(4) TEM of micro-diplopore ZIF-8 materials schemes in Fast back-projection algorithm at normal temperatures
Product is characterized using JEM-2100HR types transmission electron microscope (electronics corporation JEOL, Japan).As a result
As shown in Figure 5, it can be seen that abundant micropore and mesoporous in the sample of preparation be present.
Above-described embodiment is the comparatively ideal embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, letter
Change, should be equivalent substitute mode, be included within protection scope of the present invention.
Claims (9)
1. a kind of method of micro-diplopore ZIF-8 materials in Fast back-projection algorithm at normal temperatures, it is characterised in that comprise the following steps：
（1）Zinc oxide is soluble in water, stirring, obtain zinc oxide aqueous solution；
（2）Zinc diacetate dihydrate is soluble in water, stirring, obtain zinc acetate aqueous solution；
（3）2-methylimidazole is dissolved in DMF, stirs, obtains 2-methylimidazole solution；
（4）By step（1）Zinc oxide aqueous solution and step（2）Zinc acetate aqueous solution mixing, stirring, obtain zinc oxide and acetic acid
The mixed solution of zinc；
（5）To step（4）Zinc oxide and zinc acetate mixed solution in add step（3）2-methylimidazole solution and bromo
Hexadecane, it is sufficiently stirred；
（6）By step（5）Products therefrom filters, and places into vacuum drying chamber and dries, micro-diplopore ZIF-8 materials in being made.
2. according to the method for claim 1, it is characterised in that：Step（1）The time of the stirring is 20-30 minutes.
3. according to the method for claim 1, it is characterised in that：Step（2）, step（3）The time of the stirring is 10-
20 minutes.
4. according to the method for claim 1, it is characterised in that：Step（4）The time of the stirring is 20-30 minutes.
5. according to the method for claim 1, it is characterised in that：Step（5）The time of the stirring is 20-30 minutes.
6. according to the method for claim 5, it is characterised in that：The time of the stirring is 20 minutes.
7. according to the method for claim 1, it is characterised in that：Step（6）The temperature of the drying is 110-120 DEG C, is done
The dry time is 10-12h.
8. according to the method for claim 1, it is characterised in that：Step（1）, step（2）, step（3）, step（4）, step
（5）Carry out at normal temperatures.
9. according to the method for claim 1, it is characterised in that：The Zinc diacetate dihydrate, zinc oxide, 2-methylimidazole,
The mol ratio of bromohexadecane is (1-1.1)：（0.7-0.8）：（1.2-1.3）：（0.7-0.8）.
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| CN112280052A (en) * | 2020-09-30 | 2021-01-29 | 华南理工大学 | Hierarchical pore ZIF-8 material and preparation method and application thereof |
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| CN112295264A (en) * | 2020-11-30 | 2021-02-02 | 清华大学深圳国际研究生院 | Method for manufacturing solid phase micro-extraction probe |
| CN112295264B (en) * | 2020-11-30 | 2022-04-12 | 清华大学深圳国际研究生院 | Method for manufacturing solid phase micro-extraction probe |
| CN113171754A (en) * | 2021-04-27 | 2021-07-27 | 郑州大学 | Hierarchical porous metal organic framework material ZIF-8 and preparation method and application thereof |
| CN113171754B (en) * | 2021-04-27 | 2022-09-27 | 郑州大学 | Hierarchical porous metal organic framework material ZIF-8 and preparation method and application thereof |
| CN114349182A (en) * | 2022-01-07 | 2022-04-15 | 南京工业大学 | Method for degrading bisphenol A in solutions with different pH values by using metal organic framework ZIF-8 immobilized laccase |
| CN114349182B (en) * | 2022-01-07 | 2023-11-14 | 南京工业大学 | Method for degrading bisphenol A in solutions with different pH values by adopting metal-organic framework ZIF-8 immobilized laccase |
| CN114958167A (en) * | 2022-03-23 | 2022-08-30 | 苏州谱融传感科技有限公司 | Preparation method and application of wide-spectrum low-heat-capacity infrared absorption coating |
| WO2023191609A1 (en) * | 2022-03-29 | 2023-10-05 | Universite Mohammed VI Polytechnique | Process for producing zif-8, the chitosan@zif-8 composite thereof, and the use of zif-8 and of the chitosan@zif-8 composite thereof |
| CN116173286A (en) * | 2023-04-19 | 2023-05-30 | 清泽医疗科技(广东)有限公司 | Medical adhesive, preparation method and application thereof |
| CN116173286B (en) * | 2023-04-19 | 2024-01-16 | 清泽医疗科技(广东)有限公司 | Medical adhesive, preparation method and application thereof |
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