CN110387048A - A kind of metal organic frame two-dimensional nano piece and preparation method thereof - Google Patents
A kind of metal organic frame two-dimensional nano piece and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of metal organic frame two-dimensional nano piece and preparation method thereof, which is metal salt (ZnAc2•2H2O) (lauryl sodium sulfate is assisted in surfactant with organic ligand (2-methylimidazole), that is SDS) the lower synthesis of effect, acetic acid dihydrate zinc, 2-methylimidazole, SDS solution is respectively configured under room temperature first, then first solution is uniformly mixed, it is placed in after insulating box stands 24 h again and uses methanol centrifuge washing, obtain 2D ZIF-8 nanometer sheet.This method is simple and easy, and carries out at normal temperature, and low energy consumption, and environmentally protective, product morphology is controllable, has a good application prospect.
Description
Technical field
The present invention relates to a kind of metal organic frame two-dimensional nano pieces and preparation method thereof, belong to the skill of nanostructure synthesis
Art field.
Background technique
Metal organic framework compound (MOFs) is a kind of crystalline state porous material with periodic network structure, by metal
(single metal ion or metal cluster) and organic ligand are self-assembly of by coordinate bond.MOFs is also referred to as coordination polymer
(coordination polymer) be a kind of hybrid inorganic-organic materials, has the rigidity and organic material of inorganic material concurrently
Flexible characteristic.MOFs can form different frame pore structures, this is because metal (single metal ion or metal cluster)
Arrangement with organic ligand has apparent directionality.Therefore, MOFs has that high porosity, high-specific surface area, duct be regular, hole
Diameter is adjustable and topological structure diversity and the advantages that Scalability, stores up in catalysis, nonlinear optics, ion exchange and gas
There is potential application in depositing and separating.(Kitaura R, Kitagawa S, Kubota Y, et al. Formation of
a one-dimensional array of oxygen in a microporous metal-organic solid.[J].
Science, 2002,298 (5602): 2358-2361.)
In recent years, traditional blocky MOF cannot fully meet many specific application demands, especially for biofacies
Application is closed, MOF needs smaller size to promote it to enter in cell, such as biomedical imaging, drug delivery and biology
Sensing etc., therefore the synthesis of the nanoscale MOF crystal with controlled dimensions and pattern has become an emerging topic.Nanoscale
The surface area of MOF is greater than the surface area of bulk MOF, its performance in terms of separation, catalysis and sensing is caused to improve.(Furukawa
S, Reboul J, Diring S, et al. Structuring of metal-organic frameworks at the
mesoscopic/macroscopic scale[J]. Chemical Society Reviews, 2014, 43(16):5700-
5734.) therefore, the synthesis of nanoscale MOF is most important.
There are mainly two types of methods for the synthesis of 2D MOF nanometer sheet, first is that synthetic method from top to bottom, this method is from blocky MOF
Upper removing;Second is that synthetic method, party's rule directly synthesize 2D MOF nanometer sheet using metal and organic ligand from bottom to top.
(Zhao M, Lu Q, Ma Q, et al. Two-Dimensional Metal-Organic Framework
Nanosheets [J] Small Methods, 2016,1 (1-2): 1600030.)
ZIFs is the one kind for reacting generation in organic solvent by the metal salts and imidazate or derivatives thereof such as divalent Zn, Co ligand
MOFs material with class skeleton structure of zeolite.Imidazate is a kind of five-membered ring with conjugated nature, by losing a matter
Son and metallic ion coordination, formed a connection type correspond exactly to Si-O-Si structure in zeolitic material, bond angle close to
145 ° of M-IM-M (M: transition metal ions;IM: imidazate), so ZIFs material combines metal-organic framework materials and boiling
The double dominant of stone, not only high porosity and bigger serface and adjustability of structure with MOFs material, but also there is inorganic boiling
The high stability of stone.(Park K S, Ni Z, C t é A P, et al. From the Cover:Exceptional
chemical and thermal stability of zeolitic imidazolate frameworks[J]. Proc
Natl Acad Sci U S A, 2006,103 (27): 10186-10191.) therefore, ZIFs material has latent at many aspects
Application value, such as gas absorption separation, ion exchange, chemical industry catalytic process and gas storage.
ZIF-8 is by metal Zn2+The ZnN to be formed is connect with the N atom in MIM4Tetrahedral structural unit.The aperture ZIF-8
0.34 nm, 11.6 nm of cage diameter, the feature with bigger serface and small-bore macropore cage.For electrical energy storage device,
Excellent electrode material has high surface area, high conductivity and good structural stability, and ZIF-8 during electric discharge-charging
The requirement can be reached as template and precursor.In addition to this, it can be synthesized by the ammonia treatment in situ in annealing process
The derivative carbide material of porous ZIF-8 with controllable pore size distribution.Therefore, ZIF-8 is successfully applied to lithium ion battery
(LIB) anode, the cathode of lithium-sulfur cell (LSB) and the component and supercapacitor of other battery systems.
Although the duct ZIF-8 is regular, large specific surface area, aperture is small, skeleton structure is open, structure is adjustable, various structures,
Be since its size is larger, so cannot be introduced into cell, and specific surface area, aperture cannot reach requirement in some applications,
And 2D ZIF-8 nanometer sheet has many advantages, such as easy film forming, large specific surface area, active site exposure, has development prospect.
Bottom-to-top method is used in the present invention.The critical issue of this method needs to limit MOF vertically
Growth, and growth transversely is unaffected., using easy anionic surfactant assisted synthesizing method, surface is living for we
Property agent not only limit the growth of MOF vertically, and help to disperse synthesis after size MOF nanometer sheet.
Summary of the invention
It is an object of the invention to: in view of the defects existing in the prior art, propose a kind of metal organic frame ZIF-8 two dimension
Nanometer sheet and preparation method thereof, this method is simple and easy, and carries out at normal temperature, and low energy consumption, and environmentally protective, product morphology can
Control, has a good application prospect.
To achieve the above object, the technical solution of the present invention is as follows: a kind of metal organic frame two-dimensional nano piece, feature exist
In: chemical formula is Zn [MeIM] 2(MeIM=2-methylimidazole), basic unit is constituted by 2-methylimidazole and metallic atom Zn.Institute
State metal organic frame two-dimensional nano piece be it is rectangular, length and width are in 200 ~ 500 nm, and thickness is in 2 ~ 5 nm.
A kind of preparation method of metal organic frame two-dimensional nano piece, comprising the following steps:
A. the acetic acid dihydrate zinc (ZnAC for being 2:1 ~ 2:20 by the ratio between amount of substance2•2H2O) solid medicine, dodecyl sulphate
Sodium (SDS) solid medicine, 2-methylimidazole solid medicine are dissolved in deionized water respectively, and ultrasound is uniformly, spare;
B. SDS aqueous solution is poured slowly into acetic acid dihydrate zinc aqueous solution, and ultrasound is uniformly, it is spare;
C. 2-MIM solution is added dropwise in the mixed solution of step 2,20 ~ 40 s is stirred after dripping, are then placed on 30 DEG C
Constant temperature stands 20 ~ 30 h in insulating box;
D. three times with methanol centrifuge washing, 10 h are freeze-dried, it is spare to obtain solid powdery sample.
Further, acetic acid dihydrate zinc, 2-methylimidazole and SDS the substance withdrawl syndrome ratio in respective aqueous solution are 2:
20:1~2。
Further, in the step 3, time of repose >=20 h, and time of repose≤48 h, it is advisable with 24 h or so.
The invention adopts the above technical scheme compared with prior art, has following technical effect that system provided by the invention
Preparation Method is simple and easy, and carries out at normal temperature, and low energy consumption, and environmentally protective, product morphology is controllable, before having good application
Scape.
Detailed description of the invention
The present invention will be further described below with reference to the drawings.
The SEM figure that Fig. 1 is metal organic frame two-dimensional nano crystalline substance ZIF-8 prepared by embodiment 1.
The TEM figure that Fig. 2 is metal organic frame two-dimensional nano crystalline substance ZIF-8 prepared by embodiment 1.
Fig. 3 is the altitude profile figure of metal organic frame two-dimensional nano crystalline substance ZIF-8 prepared by embodiment 1.
Fig. 4 is the XRD test result figure of metal organic frame two-dimensional nano crystalline substance ZIF-8 prepared by embodiment 1.
BET test result figure (a) freezing that Fig. 5 is metal organic frame two-dimensional nano crystalline substance ZIF-8 prepared by embodiment 1 is dry
Dry treated ZIF-8 nanometer sheet N2ZIF-8 nanometer sheet pore-size distribution after absorption-desorption thermoisopleth (b) freeze-drying process
Figure.
Specific embodiment
Hereinafter, the preferred embodiments of the present invention will be described in detail with reference to the drawings.However, these embodiments are only used for
Improving eyesight and be not intended to limit the present invention.
It is an object of that present invention to provide the synthetic methods of metal organic frame two-dimensional nano crystalline substance ZIF-NS a kind of, wherein not
The operation for indicating temperature is completed at room temperature.
The two-dimensional nano crystalline substance is metal salt (ZnAc2•2H2O it) is assisted with organic ligand (2-methylimidazole) in surfactant
(lauryl sodium sulfate, i.e. SDS) effect is lower to be synthesized, be respectively configured under room temperature first acetic acid dihydrate zinc, 2-methylimidazole,
Solution, is then first uniformly mixed by SDS solution, then is placed in after insulating box stands 24 h and uses methanol centrifuge washing, obtains 2D ZIF-
8。
Embodiment 1
1, the ZnAC of 0.6 g is added in 50 mL beakers2•2H2O adds 10 mL deionized waters and ultrasound uniformly;
2, the SDS of 0.394 g is added in 25 mL beakers, adds 10 mL deionized waters and ultrasound uniformly;
3,2 are added in 1 and ultrasonic mixing is uniformly spare;
4,2.24 g 2-MIM are added in 25 mL beakers, add 10 mL deionized waters and ultrasound uniformly;
5,4 are added dropwise in 1, after being added dropwise and stir 20 s constant temperature standing in 30 DEG C of insulating boxs;
6, methanol centrifuge washing is used three times after standing 24 h;Deionized water centrifuge washing three times, is freeze-dried 10 h, spare.
Wherein, nanometer sheet as shown in Figure 1 is rectangular, and for length and width between 200-500 nm, there is an aperture in centre.
Nanometer sheet as shown in Figure 2 has a small amount of hole, pattern is imperfect than relatively thin.
Nanometer sheet thickness as shown in Figure 3 is in 2-3 nm.
As shown in figure 4, it is more identical than standard card, illustrate that the product is ZIF-8, diffracted intensity there are some increasings on (200) face
Add, illustrates that ZIF-8 nanometer sheet is grown along (200) crystal face.
As shown in figure 5, measuring BET specific surface area after the freeze-drying of ZIF-8 nanometer sheet is 658.772477 m2/ g,
Langmuir specific surface area is 879.278175 m2/ g, aperture is in 2-3 nm.
Embodiment 2
1, the ZnAC of 0.6g is added in 50mL beaker2•2H2O adds 10 mL deionized waters and ultrasound uniformly;
2, the SDS of 0.788 g is added in 25 mL beakers, adds 10mL deionized water and ultrasound uniformly;
3,2 are added in 1 and ultrasonic mixing is uniformly spare;
4,2.24g 2-MIM is added in 25 mL beakers, adds 10mL deionized water and ultrasound uniformly;
5,4 are added dropwise in 1, after being added dropwise and stir 20 s constant temperature standing in 30 DEG C of insulating boxs;
6, methanol centrifuge washing is used three times after standing 24 h;Deionized water centrifuge washing three times, is freeze-dried 10 h, spare.
The foregoing is merely better embodiment of the invention, protection scope of the present invention is not with above embodiment
Limit, as long as those of ordinary skill in the art's equivalent modification or variation made by disclosure according to the present invention, should all be included in power
In the protection scope recorded in sharp claim.
Claims (6)
1. a kind of metal organic frame two-dimensional nano piece, it is characterised in that: chemical formula is Zn [MeIM]2(MeIM=2- methyl miaow
Azoles), basic unit is constituted by 2-methylimidazole and configuration metal ions Zn.
2. metal organic frame two-dimensional nano piece according to claim 1, it is characterised in that: the metal organic frame two
Tie up nanometer sheet be it is rectangular, long and wide in 200 ~ 500 nm, thickness is in 2 ~ 5 nm.
3. a kind of preparation method of metal organic frame two-dimensional nano piece as described in claim 1, it is characterised in that: including with
Lower step:
A. acetic acid dihydrate zinc (ZnAC2 2H2O) solid medicine, dodecyl sulphate for being 2:1 ~ 2:20 by the ratio between amount of substance
Sodium (SDS) solid medicine, 2-methylimidazole solid medicine are dissolved in deionized water respectively, and ultrasonic mixing is uniform, spare;
B. SDS aqueous solution is poured into dropwise in acetic acid dihydrate zinc aqueous solution, and ultrasonic mixing is uniform, it is spare;
C. 2-MIM solution is added dropwise in the mixed solution of step 2,20 ~ 40 s is stirred after dripping, are then placed on 30 DEG C
Constant temperature stands 20 ~ 30 h in insulating box;
D. solid product is centrifuged and is washed three times with methanol, is freeze-dried 10 h, it is spare to obtain solid powdery sample.
4. the preparation method of metal organic frame two-dimensional nano piece according to claim 3, it is characterised in that: two hydration second
Sour zinc, 2-methylimidazole and SDS the substance withdrawl syndrome ratio in respective aqueous solution are 2:20:1 ~ 2.
5. the preparation method of metal organic frame two-dimensional nano piece according to claim 3, it is characterised in that: the step
In 3, time of repose >=20 h, and time of repose≤48 h, it is advisable with 24 h or so.
6. the preparation method of metal organic frame two-dimensional nano piece according to claim 5, it is characterised in that: the standing
Time is 24 hours.
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CN111326745A (en) * | 2020-02-12 | 2020-06-23 | 北京化工大学 | Two-dimensional zinc monoatomic/carbon nitrogen composite material and preparation method and application thereof |
CN111533921A (en) * | 2020-05-28 | 2020-08-14 | 南京工业大学 | Preparation method of ZIF-8 nano platelet and ultrathin film thereof |
CN111592661A (en) * | 2020-06-16 | 2020-08-28 | 南京邮电大学 | Preparation method of high-dispersity organic metal framework nano material |
CN113387889A (en) * | 2021-06-17 | 2021-09-14 | 湖南文理学院 | Novel porous imidazole metal compound nano powder and preparation method thereof |
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CN111326745B (en) * | 2020-02-12 | 2021-07-27 | 北京化工大学 | Two-dimensional zinc monoatomic/carbon nitrogen composite material and preparation method and application thereof |
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CN113387889A (en) * | 2021-06-17 | 2021-09-14 | 湖南文理学院 | Novel porous imidazole metal compound nano powder and preparation method thereof |
CN113387889B (en) * | 2021-06-17 | 2023-05-09 | 湖南文理学院 | Preparation method of porous imidazole metal compound nano-powder |
CN113527707A (en) * | 2021-08-06 | 2021-10-22 | 南通大学 | Normal-temperature rapid preparation method of copper-based MOF |
CN113648977A (en) * | 2021-09-10 | 2021-11-16 | 大连理工大学 | Modified zeolite-like imidazole framework adsorption material and preparation method and application thereof |
CN114632943A (en) * | 2022-03-21 | 2022-06-17 | 中国科学院苏州纳米技术与纳米仿生研究所 | Two-dimensional metal nanosheet and preparation method and application thereof |
CN114632943B (en) * | 2022-03-21 | 2023-10-03 | 中国科学院苏州纳米技术与纳米仿生研究所 | Two-dimensional metal nano sheet and preparation method and application thereof |
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CN116926616B (en) * | 2023-09-16 | 2024-01-02 | 山东海化集团有限公司 | Preparation method and application of flaky Cu-ZIF-8 material |
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