CN110527105A - A kind of ultra-thin two-dimension porous metals organic frame nanometer sheet and preparation method thereof - Google Patents
A kind of ultra-thin two-dimension porous metals organic frame nanometer sheet and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of ultra-thin two-dimension porous metals organic frame nanometer sheets and preparation method thereof, belong to field of new materials, the method replaced using coordination, pass through first wife's body benzimidazole in methylimidazole substituted metal organic frame nanometer sheet, reduce interlayer conjugation, realize that delamination effect, the method have the advantages that yield is high, at low cost.Ligand and metal coordination centers of the present invention using benzimidazole, zinc nitrate hexahydrate as MOF, substitution ligand of the 2-methylimidazole as MOF；Using solvent thermal technology and filter the two-dimensional MOF nanometer sheet of technology synthesis；Porous structure is formed in obtained two-dimentional MOF nanometer sheet using Freeze Drying Technique；The ratio for controlling 2-methylimidazole and benzimidazole, obtains the porous MOF nanometer sheet of ultra-thin two-dimension.
Description
Technical field
The invention belongs to new material technology field more particularly to a kind of ultra-thin two-dimension porous metals organic frame nanometer sheet and
Preparation method.
Background technique
Metal organic frame (English: Metal-Organic Framework, abbreviation MOF) is by organic ligand and metal
The hybrid inorganic-organic materials with molecule inner pore that ion or cluster are self-assembly of by coordinate bond.Two dimension (English:
Two Dimension, abbreviation 2D) material refer to electronics only can on the non-nanosize of two dimensions free movement (plane fortune
It is dynamic) material.The features such as 2D MOFs has porosity high, large specific surface area, stable structure, hydrogen storage, gas absorption with
The fields such as separation, sensor, catalysis reaction have broad application prospects.
In recent years, two-dimension nano materials are with the specific surface area of its superelevation, excellent optical clarity and outstanding conduction
Heating conduction is got the attention.With zero-dimension nano particle, one-dimensional nano line/nanometer rods/nanotube, three-dimensional classifying nano knot
Structure is compared with massive material, and two-dimension nano materials have many unique characteristics.For example, atomic-level thickness is two-dimensional nano thin slice
Higher mechanical flexibility and optical transparence are provided, the preferred material of flexible and transparent electronic device is become；Ultra-thin
Thickness and biggish lateral dimension make two-dimension nano materials can be applied to low transmission resistance, high-throughput ultra-thin gas separation
Film；It is efficiently effective that the specific surface area of super large and high volume atomic ratio make it that can provide more horn of plenty in catalysis reaction
Catalytic site.
The preparation method of ultra-thin two-dimension metal organic frame nanometer sheet can be divided into two kinds, including top-down preparation side
Method and preparation method from bottom to top.Top-down preparation method is two to hierarchical structure by means physically or chemically
Dimension metal organic frame nanometer sheet is removed, including ultrasonic delamination, mechanical delamination, chemical delamination and lithium ion intercalation
Deng.Preparation method from bottom to top refers to directly from biometallic joint and organic ligand materials synthesis ultra-thin two-dimension metal organic frame
Nanometer sheet, including interface synthesis, three laminated at the synthesis of, surfactant auxiliary, modulation synthesis and ultrasound synthesis etc., this
A little methods have the shortcomings that synthetic strategy route is complicated, separation is difficult.
Summary of the invention
The present invention provides a kind of ultra-thin two-dimension porous metals organic frame nanometer sheets and preparation method thereof, use coordination
It is total to reduce interlayer by first wife's body benzimidazole in methylimidazole substituted metal organic frame nanometer sheet for substituted method
Yoke effect realizes that delamination effect, the method have the advantages that yield is high, at low cost.
In order to achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of ultra-thin two-dimension porous metals organic frame nanometer sheet, comprising the following steps:
Step 1: benzimidazole, zinc nitrate hexahydrate are dissolved in DMF, then 2-methylimidazole is dissolved in solution, six water
The amount for closing zinc nitrate is 0.03-0.04g/mL, and the amount of the benzimidazole is 0.006-0.008g/mL, the 2-methylimidazole
Molar ratio with the benzimidazole is (0-3): (1-3)；
Step 2: being reacted solution obtained in step 1 72 hours at 100 DEG C using solvent thermal technology；
Step 3: using synthesis two dimension MOF nanometer sheet in suction filtration technology purification step 2；
Step 4: porous structure being formed in the two-dimentional MOF nanometer sheet that step 3 obtains using Freeze Drying Technique, obtains ultra-thin two
Tie up porous MOF nanometer sheet.
In step described above, the molar ratio of 2-methylimidazole and benzimidazole is 1:1 in step 1；Described in step 3
The cleaning solvent used in suction filtration technology is deionized water, filter sizes 220nm, and suction filtration temperature is room temperature, relative degree of vacuum
<-0.1Mpa；Condenser temperature is less than -75 DEG C when freezing in Freeze Drying Technique described in step 4, and temperature of charge is less than -50 DEG C,
Vacuum degree is less than 10Pa when dry, and sublimation drying is 48 hours.
A kind of ultra-thin two-dimension porous metals organic frame nanometer sheet prepared using approach described above.
The utility model has the advantages that the present invention provides a kind of ultra-thin two-dimension porous metals organic frame nanometer sheet and preparation method thereof,
Using a kind of novel synthetic schemes from bottom to top: coordination replaces, and benzimidazole, zinc nitrate hexahydrate are matched as MOF's
Body and metal coordination centers, substitution ligand of the 2-methylimidazole as MOF, are received by 2-methylimidazole substituted metal organic frame
First wife's body benzimidazole in rice piece, reduces interlayer conjugation, realizes delamination effect, passes through control 2-methylimidazole and benzo
The usage ratio of imidazoles obtains the porous MOF nanometer sheet of ultra-thin two-dimension.Method of the invention solves other ultra-thin two-dimension metals
The disadvantages of organic framework synthetic strategy route is complicated, separation is difficult, easily rupturable, it is organic to realize ultra-thin two-dimension porous metals
Frame nanometer sheet is efficient, prepared by a large amount stablize.
Detailed description of the invention
Fig. 1 is the flow chart of preparation method of the present invention；
Fig. 2 is the X-ray of the two-dimentional MOF of the 2-methylimidazole of different mol ratio example and benzimidazole ligand in the embodiment of the present invention
Diffraction pattern；
Fig. 3 is the high power that molar ratio is the 2-methylimidazole of 0:1 and the two-dimentional MOF of benzimidazole ligand in implementation column of the present invention
Transmission electron microscope photo；
Fig. 4 is the high power that molar ratio is the 2-methylimidazole of 1:3 and the two-dimentional MOF of benzimidazole ligand in implementation column of the present invention
Transmission electron microscope photo；
Fig. 5 is the high power that molar ratio is the 2-methylimidazole of 1:1 and the two-dimentional MOF of benzimidazole ligand in implementation column of the present invention
Transmission electron microscope photo.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings:
Embodiment 1
As shown in Figure 1, a kind of preparation method of ultra-thin two-dimension porous metals organic frame nanometer sheet, comprising the following steps:
Step 1: benzimidazole, zinc nitrate hexahydrate are dissolved in DMF, then 2-methylimidazole is dissolved in solution, six water
The amount for closing zinc nitrate is 0.03g/mL, DMF 60mL, and the amount of the benzimidazole is 0.006g/mL, the 2-methylimidazole with
The molar ratio of the benzimidazole is 0:1；
Step 2: being reacted solution obtained in step 1 72 hours at 100 DEG C using solvent thermal technology；
Step 3: using synthesis two dimension MOF nanometer sheet in suction filtration technology purification step 2；
Step 4: porous structure being formed in the two-dimentional MOF nanometer sheet that step 3 obtains using Freeze Drying Technique, obtains ultra-thin two
Tie up porous MOF nanometer sheet.
In step described above, the cleaning solvent used in suction filtration technology described in step 3 is deionized water, filter sizes
For 220nm, suction filtration temperature is room temperature, relative degree of vacuum < -0.1Mpa；Cold-trap when being freezed in Freeze Drying Technique described in step 4
Temperature is less than -75 DEG C, and temperature of charge is less than -50 DEG C, and vacuum degree is less than 10Pa when dry, and sublimation drying is 48 hours.
As shown in Fig. 2, the X-ray diffractogram explanation of Zn (BIM) x is 10 ° and 21 ° or so in 2 θ and has stronger diffraction maximum,
As shown in figure 3, gained two dimension porous metals organic frame nanometer sheet has thicker stacking, belong to block structure.
Embodiment 2
As shown in Figure 1, a kind of preparation method of ultra-thin two-dimension porous metals organic frame nanometer sheet, comprising the following steps:
Step 1: benzimidazole, zinc nitrate hexahydrate are dissolved in DMF, then 2-methylimidazole is dissolved in solution, six water
The amount for closing zinc nitrate is 0.03g/mL, DMF 60mL, and the amount of the benzimidazole is 0.006g/mL, the 2-methylimidazole with
The molar ratio of the benzimidazole is 1:3；
Step 2: being reacted solution obtained in step 1 72 hours at 100 DEG C using solvent thermal technology；
Step 3: using synthesis two dimension MOF nanometer sheet in suction filtration technology purification step 2；
Step 4: porous structure being formed in the two-dimentional MOF nanometer sheet that step 3 obtains using Freeze Drying Technique, obtains ultra-thin two
Tie up porous MOF nanometer sheet.
In step described above, the cleaning solvent used in suction filtration technology described in step 3 is deionized water, filter sizes
For 220nm, suction filtration temperature is room temperature, relative degree of vacuum < -0.1Mpa；Cold-trap when being freezed in Freeze Drying Technique described in step 4
Temperature is less than -75 DEG C, and temperature of charge is less than -50 DEG C, and vacuum degree is less than 10Pa when dry, and sublimation drying is 48 hours.
As shown in Fig. 2, the X-ray diffractogram of 25% Zn (BIM) x shows that 2 θ are that 21 ° of peak is substantially reduced, show with benzo
Imidazoles is that the MOF of ligand is partially replaced, as shown in figure 4, gained two dimension porous metals organic frame nanometer sheet is relative to implementation
The stacking of example 1 significantly reduces, and belongs to flake structure.
Embodiment 3
As shown in Figure 1, a kind of preparation method of ultra-thin two-dimension porous metals organic frame nanometer sheet, comprising the following steps:
Step 1: benzimidazole, zinc nitrate hexahydrate are dissolved in DMF, then 2-methylimidazole is dissolved in solution, six water
The amount for closing zinc nitrate is 0.03g/mL, DMF 60mL, and the amount of the benzimidazole is 0.006g/mL, the 2-methylimidazole with
The molar ratio of the benzimidazole is 1:1；
Step 2: being reacted solution obtained in step 1 72 hours at 100 DEG C using solvent thermal technology；
Step 3: using synthesis two dimension MOF nanometer sheet in suction filtration technology purification step 2；
Step 4: porous structure being formed in the two-dimentional MOF nanometer sheet that step 3 obtains using Freeze Drying Technique, obtains ultra-thin two
Tie up porous MOF nanometer sheet.
In step described above, the cleaning solvent used in suction filtration technology described in step 3 is deionized water, filter sizes
For 220nm, suction filtration temperature is room temperature, relative degree of vacuum < -0.1Mpa；Cold-trap when being freezed in Freeze Drying Technique described in step 4
Temperature is less than -75 DEG C, and temperature of charge is less than -50 DEG C, and vacuum degree is less than 10Pa when dry, and sublimation drying is 48 hours.
As shown in Fig. 2, the X-ray diffractogram of 50% Zn (BIM) x shows that 2 θ are 33 ° and 60 ° and new diffraction nearby occur
Peak shows that a large amount of benzimidazoles are substituted caused MOF number of plies reduction and change the crystal form of material, as shown in figure 5, institute
Obtaining two-dimentional porous metals organic frame nanometer sheet has apparent lamella, belongs to ultra-thin two-dimension structure special property.
Embodiment 4
As shown in Figure 1, a kind of preparation method of ultra-thin two-dimension porous metals organic frame nanometer sheet, comprising the following steps:
Step 1: benzimidazole, zinc nitrate hexahydrate are dissolved in DMF, then 2-methylimidazole is dissolved in solution, six water
The amount for closing zinc nitrate is 0.03g/mL, DMF 60mL, and the amount of the benzimidazole is 0.006g/mL, the 2-methylimidazole with
The molar ratio of the benzimidazole is 3:1；
Step 2: being reacted solution obtained in step 1 72 hours at 100 DEG C using solvent thermal technology；
Step 3: using synthesis two dimension MOF nanometer sheet in suction filtration technology purification step 2；
Step 4: porous structure being formed in the two-dimentional MOF nanometer sheet that step 3 obtains using Freeze Drying Technique, obtains ultra-thin two
Tie up porous MOF nanometer sheet.
In step described above, the cleaning solvent used in suction filtration technology described in step 3 is deionized water, filter sizes
For 220nm, suction filtration temperature is room temperature, relative degree of vacuum < -0.1Mpa；Cold-trap when being freezed in Freeze Drying Technique described in step 4
Temperature is less than -75 DEG C, and temperature of charge is less than -50 DEG C, and vacuum degree is less than 10Pa when dry, and sublimation drying is 48 hours.
As shown in Fig. 2, the X-ray diffractogram of 75% Zn (BIM) x shows that 2 θ disappear for the diffraction maximum near 10 ° and 20 °
It loses, shows to disappear by the MOF crystal of ligand of benzimidazole, lamellar structure is destroyed.
Embodiment 5
As shown in Figure 1, a kind of preparation method of ultra-thin two-dimension porous metals organic frame nanometer sheet, comprising the following steps:
Step 1: benzimidazole, zinc nitrate hexahydrate are dissolved in DMF, then 2-methylimidazole is dissolved in solution, six water
The amount for closing zinc nitrate is 0.04g/mL, DMF 60mL, and the amount of the benzimidazole is 0.008g/mL, the 2-methylimidazole with
The molar ratio of the benzimidazole is 0:1；
Step 2: being reacted solution obtained in step 1 72 hours at 100 DEG C using solvent thermal technology；
Step 3: using synthesis two dimension MOF nanometer sheet in suction filtration technology purification step 2；
Step 4: porous structure being formed in the two-dimentional MOF nanometer sheet that step 3 obtains using Freeze Drying Technique, obtains ultra-thin two
Tie up porous MOF nanometer sheet.
In step described above, the cleaning solvent used in suction filtration technology described in step 3 is deionized water, filter sizes
For 220nm, suction filtration temperature is room temperature, relative degree of vacuum < -0.1Mpa；Cold-trap when being freezed in Freeze Drying Technique described in step 4
Temperature is less than -75 DEG C, and temperature of charge is less than -50 DEG C, and vacuum degree is less than 10Pa when dry, and sublimation drying is 48 hours.
Embodiment 6
As shown in Figure 1, a kind of preparation method of ultra-thin two-dimension porous metals organic frame nanometer sheet, comprising the following steps:
Step 1: benzimidazole, zinc nitrate hexahydrate are dissolved in DMF, then 2-methylimidazole is dissolved in solution, six water
The amount for closing zinc nitrate is 0.03g/mL, DMF 60mL, and the amount of the benzimidazole is 0.007g/mL, the 2-methylimidazole with
The molar ratio of the benzimidazole is 1:1；
Step 2: being reacted solution obtained in step 1 72 hours at 100 DEG C using solvent thermal technology；
Step 3: using synthesis two dimension MOF nanometer sheet in suction filtration technology purification step 2；
Step 4: porous structure being formed in the two-dimentional MOF nanometer sheet that step 3 obtains using Freeze Drying Technique, obtains ultra-thin two
Tie up porous MOF nanometer sheet.
In step described above, the cleaning solvent used in suction filtration technology described in step 3 is deionized water, filter sizes
For 220nm, suction filtration temperature is room temperature, relative degree of vacuum < -0.1Mpa；Cold-trap when being freezed in Freeze Drying Technique described in step 4
Temperature is less than -75 DEG C, and temperature of charge is less than -50 DEG C, and vacuum degree is less than 10Pa when dry, and sublimation drying is 48 hours.
The above is only some embodiments of the invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (5)
1. a kind of preparation method of ultra-thin two-dimension porous metals organic frame nanometer sheet, which comprises the following steps:
Step 1: first benzimidazole, zinc nitrate hexahydrate are dissolved in DMF, then 2-methylimidazole is dissolved in solution, described six
The amount of nitric hydrate zinc is 0.03-0.04g/mL, and the amount of the benzimidazole is 0.006-0.008g/mL, the 2- methyl miaow
The molar ratio of azoles and the benzimidazole is (0-3): (1-3)；
Step 2: being reacted solution obtained in step 1 72 hours at 100 DEG C using solvent thermal technology；
Step 3: using synthesis two dimension MOF nanometer sheet in suction filtration technology purification step 2；
Step 4: porous structure being formed in the two-dimentional MOF nanometer sheet that step 3 obtains using Freeze Drying Technique, obtains ultra-thin two
Tie up porous MOF nanometer sheet.
2. the preparation method of ultra-thin two-dimension porous metals organic frame nanometer sheet according to claim 1, which is characterized in that
The molar ratio of 2-methylimidazole and benzimidazole is 1:1 in step 1.
3. the preparation method of ultra-thin two-dimension porous metals organic frame nanometer sheet according to claim 1, which is characterized in that
The cleaning solvent used in suction filtration technology described in step 3 is deionized water, filter sizes 220nm, and suction filtration temperature is room temperature,
Relative degree of vacuum < -0.1Mpa.
4. the preparation method of ultra-thin two-dimension porous metals organic frame nanometer sheet according to claim 1, which is characterized in that
Condenser temperature is less than -75 DEG C when freezing in Freeze Drying Technique described in step 4, and temperature of charge is less than -50 DEG C, vacuum when dry
Degree is less than 10Pa, and sublimation drying is 48 hours.
5. a kind of ultra-thin two-dimension porous metals organic frame nanometer sheet prepared using claim 1-4 the method.
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| CN113698617A (en) * | 2021-08-25 | 2021-11-26 | 福州大学 | Synthesis method of ultrathin two-dimensional hierarchical porous ZIF-67 |
| CN115181283A (en) * | 2022-06-23 | 2022-10-14 | 湖北大学 | Micron-sized ultrathin two-dimensional light-responsive metal organic framework nanosheet and macro preparation method thereof |
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| CN113698617A (en) * | 2021-08-25 | 2021-11-26 | 福州大学 | Synthesis method of ultrathin two-dimensional hierarchical porous ZIF-67 |
| CN115181283A (en) * | 2022-06-23 | 2022-10-14 | 湖北大学 | Micron-sized ultrathin two-dimensional light-responsive metal organic framework nanosheet and macro preparation method thereof |
| CN115181283B (en) * | 2022-06-23 | 2023-10-20 | 湖北大学 | Micrometer-sized ultrathin two-dimensional light-responsive metal-organic framework nano sheet and macro preparation method thereof |
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