CN108610489A - The preparation method of the nano material of different dimensions based on metal-organic framework material - Google Patents
The preparation method of the nano material of different dimensions based on metal-organic framework material Download PDFInfo
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- CN108610489A CN108610489A CN201810641121.2A CN201810641121A CN108610489A CN 108610489 A CN108610489 A CN 108610489A CN 201810641121 A CN201810641121 A CN 201810641121A CN 108610489 A CN108610489 A CN 108610489A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a kind of preparation methods of the nano material of the different dimensions based on metal-organic framework material, belong to field of nano material preparation.The present invention first prepares metal organic frame Cu3(BTC)2Material, then the metal organic frame Cu that will obtain3(BTC)2Material is corroded with the ammonia spirit of different pH value, has obtained the nano material of nano wire, nanometer sheet, nano particle.The present invention realizes that the mode of self assembly in situ forms the nano material with different dimensions under the interaction of metal-organic framework material and ammonium hydroxide, it is by mechanically pulling off method to breach previous major part, the certain methods such as chemical deposition, and this method has the characteristics that easy to operate, product quality is high, mild condition, short preparation period, is suitble to large-scale production.
Description
Technical field
The invention belongs to field of nano material preparation, and in particular to a kind of different dimensions based on metal-organic framework material
Nano material preparation method.
Background technology
Cu3(BTC)2For a kind of MOF materials, due to their controllable pore structures and superelevation specific surface area and excellent urge
Change, the characteristics such as absorption, catalysis oxidation, gas absorption with detach, sensor, magnetic material and optical material etc. have
Larger purposes, thus Cu3(BTC)2Material has obtained relatively broad concern.Because MOFs materials possessed these are excellent
Performance and the appearance structure of itself have a close relationship, thus the hot issue that the pattern for changing MOFs materials is current.Mesh
It is preceding formed low-dimensional MOFs materials report it is still rarer, the low-dimension nano material now concerning MOFs be typically also
It is controlled during synthesis, but this method is too many to the regulation and control influence factor of pattern, so as to cause can seldom obtain
To the low-dimensional materials of anticipation.It can not more importantly be formed continuously the nano material of different dimensions by this method, and
Low yield.Therefore the rare report of nano material of low-dimensional is formed based on MOFs materials.Low-dimensional is formed currently based on MOFs materials
Nano material is still the difficult point and hot spot of this industry.
The application passes through ammonium hydroxide and metal organic frame Cu3(BTC)2Different dimensions nanometer is realized in the interaction of material
The preparation of material, it is often more important that metal organic frame Cu can be made by this method3(BTC)2Material realizes low-dimensional nanometer material
The consecutive variations of material.The low-dimension nano material formed in this way is not yet reported, and this method has operation
Simply, the features such as product quality height, mild condition, short preparation period, suitable large-scale production.
Invention content
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of based on metal organic frame Cu3(BTC)2Material
The preparation method of the different dimensions nano material of material.Pass through metal organic frame Cu3(BTC)2The interaction of material and ammonium hydroxide from
And realize the nano material of fabricated in situ different dimensions, and this method is with easy to operate, product quality is high, condition temperature
The features such as with short preparation period, suitable large-scale production.
For achieving the above object, the present invention adopts the following technical scheme that：
One kind being based on metal organic frame Cu3(BTC)2The nano material of the different dimensions of material, including nano wire, nanometer sheet and
Nano-particle material.
It is above-mentioned based on metal organic frame Cu3(BTC)2The preparation method of the nano material of the different dimensions of material, specifically
Include the following steps：
（1）By Cu (NO3)2·3H2O is dissolved in deionized water, and Cu (NO are formed after stirring3)2Solution；Simultaneously by trimesic acid
It is dissolved into ethyl alcohol, forms trimesic acid solution after stirring；The trimesic acid solution stirred evenly is poured slowly into and is stirred
Mix uniform Cu (NO3)2In solution, mixed solution is formed after stirring；Obtained mixed solution is fitted into water heating kettle, is carried out
Hydro-thermal reaction；Obtained blue precipitate is centrifuged after reaction, is washed, is dried to obtain metal organic frame Cu3(BTC)2Material；
（2）Weigh step（1）Obtained metal organic frame Cu3(BTC)2Material measures the different pH prepared in centrifuge tube
The ammonia spirit of value is poured into equipped with metal organic frame Cu3(BTC)2In the centrifuge tube of material, centrifuged after being shaken, gained
Precipitation is washed with deionized water and ethyl alcohol, and the nano material of different dimensions is obtained after dry.
Further, it is based on metal organic frame Cu3(BTC)2The preparation method of the nano material of the different dimensions of material,
Specifically include following steps：
（1）By 0.875 g Cu (NO3)2·3H2O is dissolved in 12 mL deionized waters, and Cu (NO are formed after stirring 30 min3)2It is molten
Liquid；0.42 g trimesic acids are dissolved into 12 mL ethyl alcohol simultaneously, trimesic acid solution is formed after stirring 30 min；
The trimesic acid solution stirred evenly is poured slowly into the Cu (NO stirred evenly3)2It is molten that mixing is formed in solution, after stirring
Liquid；Obtained mixed solution is fitted into 100 mL water heating kettles, 12 h are kept the temperature at 120 DEG C；The blue precipitate that will be obtained after reaction
It centrifuges, wash, being dried to obtain metal organic frame Cu3(BTC)2Material；
（2）Weigh 40 mg steps（1）Obtained metal organic frame Cu3(BTC)2Material is measured and is prepared not in centrifuge tube
The 7 mL ammonia spirits with pH value are poured into equipped with metal organic frame Cu3(BTC)2In the centrifuge tube of material, 3 are shaken
It is centrifuged after min, gained precipitation is washed with deionized water and ethyl alcohol, and the nano material of different dimensions is obtained after dry.
In above-mentioned steps（2）In, the pH value of the ammonia spirit is 10 ~ 11；It is obtained as the pH of ammonia spirit=10
To be based on metal organic frame Cu3(BTC)2Nano-material；It is obtained for based on metal as the pH of ammonia spirit=10.5
Organic frame Cu3(BTC)2Nanometer sheet material；It is obtained for based on metal organic frame Cu when the pH of ammonia spirit=113
(BTC)2Nano-particle material.
The beneficial effects of the present invention are：
（1）The present invention passes through metal organic frame Cu3(BTC)2The interaction of material and ammonium hydroxide is to realize in ammonium hydroxide one
The regulation and control of pH value in a smaller range can continuously prepare the low-dimension nano material of different dimensions, pass through in the past to breach
The problem of Mechanical Method or polishing, hydro-thermal method etc. prepares the unstability of nano material, and be not easy simultaneously in a smaller range
The preparation of different dimensions nano material is realized in the regulation and control of intrinsic factor；
（2）The preparation method of this method is easy to operate, product quality is high, mild condition, short preparation period, is suitble to extensive life
Production, passes through the metal organic frame Cu that will be prepared3(BTC)2Material and the ammonia spirit of different pH value are simply mixed,
Concussion can prepare the low-dimension nano materials of different dimensions, including nano wire, nanometer sheet and nano particle these nano materials,
A new field has been opened up to prepare different dimensions nano material, has been had a very important significance.
Description of the drawings
Fig. 1 is metal organic frame Cu3(BTC)2Material and be based on Cu3(BTC)2The nano material of the different dimensions of material
（Including nano wire, nanometer sheet and nano particle）XRD diffraction curves；
Fig. 2 is metal organic frame Cu3(BTC)2Material and be based on Cu3(BTC)2The nano material of the different dimensions of material（Including
Nano wire, nanometer sheet and nano particle）Infared spectrum；
Fig. 3 is the metal organic frame Cu prepared3(BTC)2The shape appearance figure of material and elemental analysis；
Fig. 4 is the preparation of embodiment 1 based on metal organic frame Cu3(BTC)2The pattern for the nano wire low-dimensional materials that material is formed
Figure and elemental analysis；
Fig. 5 is the preparation of embodiment 2 based on metal organic frame Cu3(BTC)2The pattern for the nanometer sheet low-dimensional materials that material is formed
Figure and elemental analysis；
Fig. 6 is the preparation of embodiment 3 based on metal organic frame Cu3(BTC)2The shape for the nano particle low-dimensional materials that material is formed
Looks figure and elemental analysis.
Specific implementation mode
Further to disclose rather than the present invention is limited, the present invention is described in further detail below in conjunction with example.
Embodiment 1
Based on metal organic frame Cu3(BTC)2Material preparation goes out the nano-material of low-dimensional, including step in detail below：
（1）With 0.875 g Cu (NO of electronics capacity of balance3)2·3H2O is dissolved into the deionized water of 12 mL, stirs 30min；
（2）It also weighs 0.42 g trimesic acids simultaneously to be dissolved into the ethyl alcohol of 12 mL, stirs 30 min；
（3）Uniformly mixed trimesic acid solution is slowly poured into uniformly mixed Cu (NO3)2In solution, stirring
30min；
（4）Mixed solution is packed into the water heating kettle of 100 mL, 12 h is kept the temperature at 120 DEG C, then centrifuges obtained precipitation,
Washing, is dried to obtain metal organic frame Cu3(BTC)2Material；
（5）The metal organic frame Cu weighed3(BTC)240 mg of material is placed in the test tube of 7 mL；
（6）The ammonia spirit of pH=10 is prepared, and by itself and step（5）The metal organic frame Cu of weighing3(BTC)2Material is mixed
It closes, vibrates 3 times, each 3min；
（7）The precipitation centrifugation that oscillation is obtained, washing, the dry nano-material that can be obtained by low-dimensional.
The powder being prepared by 1 method of embodiment is measured as object phase by Miniflex600M X-ray diffractometers
For metal organic frame Cu3(BTC)2Material, the 5700 Fourier's radar stealthy materials devices of Nicolet through power ＆ light company of the U.S. measure it still
So have through metal organic frame Cu3(BTC)2The ligand of material, through German karr Zeiss SUPAR55 field emission scanning electron microscopes into
Row scanning obtain SEM figure as shown in figure 4, obtain be low-dimensional nano-material.
Embodiment 2
Based on metal organic frame Cu3(BTC)2Material preparation goes out the nanometer sheet material of low-dimensional, including step in detail below：
（1）With 0.875 g Cu (NO of electronics capacity of balance3)2·3H2O is dissolved into the deionized water of 12 mL, stirs 30min；
（2）It also weighs 0.42 g trimesic acids simultaneously to be dissolved into the ethyl alcohol of 12 mL, stirs 30 min；
（3）Uniformly mixed trimesic acid solution is slowly poured into uniformly mixed Cu (NO3)2In solution, stirring
30min；
（4）Mixed solution is packed into the water heating kettle of 100 mL, 12 h is kept the temperature at 120 DEG C, then centrifuges obtained precipitation,
Washing, is dried to obtain metal organic frame Cu3(BTC)2Material；
（5）The metal organic frame Cu weighed3(BTC)240 mg of material is placed in the test tube of 7 mL；
（6）The ammonia spirit of pH=10.5 is prepared, and by itself and step（5）The metal organic frame Cu of weighing3(BTC)2Material is mixed
It closes, vibrates 3 times, each 3min；
（7）The precipitation centrifugation that oscillation is obtained, washing, the dry nanometer sheet material that can be obtained by low-dimensional.
The powder being prepared by 1 method of embodiment is measured as object phase by Miniflex600M X-ray diffractometers
For metal organic frame Cu3(BTC)2Material, the 5700 Fourier's radar stealthy materials devices of Nicolet through power ＆ light company of the U.S. measure it still
So have through metal organic frame Cu3(BTC)2The ligand of material, through German karr Zeiss SUPAR55 field emission scanning electron microscopes into
Row scanning obtain SEM figure as shown in figure 5, obtain be low-dimensional nanometer sheet material.
Embodiment 3
Based on metal organic frame Cu3(BTC)2Material preparation goes out the nano-particle material of low-dimensional, including step in detail below：
（1）With 0.875 g Cu (NO of electronics capacity of balance3)2·3H2O is dissolved into the deionized water of 12 mL, stirs 30min；
（2）It also weighs 0.42 g trimesic acids simultaneously to be dissolved into the ethyl alcohol of 12 mL, stirs 30 min；
（3）Uniformly mixed trimesic acid solution is slowly poured into uniformly mixed Cu (NO3)2In solution, stirring 30
min；
（4）Mixed solution is packed into the water heating kettle of 100 mL, 12 h is kept the temperature at 120 DEG C, then centrifuges obtained precipitation,
Washing, is dried to obtain metal organic frame Cu3(BTC)2Material；
（5）The metal organic frame Cu weighed3(BTC)240 mg of material is placed in the test tube of 7 mL；
（6）The ammonia spirit of pH=11 is prepared, and by itself and step（5）The metal organic frame Cu of weighing3(BTC)2Material is mixed
It closes, vibrates 3 times, each 3min；
（7）The precipitation centrifugation that oscillation is obtained, washing, the dry nano-particle material that can be obtained by low-dimensional.Pass through embodiment 3
It is Cu that the powder that method is prepared is measured as object mutually by Miniflex600M X-ray diffractometers2O, through U.S.'s thermoelectricity public affairs
The 5700 Fourier's radar stealthy materials devices of Nicolet of department, which measure it, still to be had through metal organic frame Cu3(BTC)2The ligand of material,
German karr Zeiss SUPAR55 field emission scanning electron microscopes are scanned to obtain SEM figures as shown in figure 5, obtaining being receiving for low-dimensional
Rice grain material.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification should all belong to the covering scope of the present invention.
Claims (4)
1. one kind being based on metal organic frame Cu3(BTC)2Different dimensions nano material preparation method, it is characterised in that：
Specifically include following steps：
（1）By Cu (NO3)2·3H2O is dissolved in deionized water, and Cu (NO are formed after stirring3)2Solution；Simultaneously by trimesic acid
It is dissolved into ethyl alcohol, forms trimesic acid solution after stirring；The trimesic acid solution stirred evenly is poured slowly into and is stirred
Mix uniform Cu (NO3)2In solution, mixed solution is formed after stirring；Obtained mixed solution is fitted into water heating kettle, is carried out
Hydro-thermal reaction；Obtained blue precipitate is centrifuged after reaction, is washed, is dried to obtain metal organic frame Cu3(BTC)2Material；
（2）Weigh step（1）Obtained metal organic frame Cu3(BTC)2Material measures the different pH value prepared in centrifuge tube
Ammonia spirit be poured into equipped with metal organic frame Cu3(BTC)2It in the centrifuge tube of material, is centrifuged after being shaken, gained is heavy
Shallow lake is washed with deionized water and ethyl alcohol, and the nano material of different dimensions is obtained after dry.
2. according to claim 1 a kind of based on metal organic frame Cu3(BTC)2Different dimensions nano material
Preparation method, it is characterised in that：Specifically include following steps：
（1）By 0.875 g Cu (NO3)2·3H2O is dissolved in 12 mL deionized waters, and Cu (NO are formed after stirring 30 min3)2It is molten
Liquid；0.42 g trimesic acids are dissolved into 12 mL ethyl alcohol simultaneously, trimesic acid solution is formed after stirring 30 min；
The trimesic acid solution stirred evenly is poured slowly into the Cu (NO stirred evenly3)2It is molten that mixing is formed in solution, after stirring
Liquid；Obtained mixed solution is fitted into 100 mL water heating kettles, 12 h are kept the temperature at 120 DEG C；The blue precipitate that will be obtained after reaction
It centrifuges, wash, being dried to obtain metal organic frame Cu3(BTC)2Material；
（2）Weigh 40 mg steps（1）Obtained metal organic frame Cu3(BTC)2Material is measured and is prepared not in centrifuge tube
The 7 mL ammonia spirits with pH value are poured into equipped with metal organic frame Cu3(BTC)2In the centrifuge tube of material, 3 are shaken
It is centrifuged after min, gained precipitation is washed with deionized water and ethyl alcohol, and the nano material of different dimensions is obtained after dry.
3. according to claim 1 or 2 a kind of based on metal organic frame Cu3(BTC)2Different dimensions nano material
Preparation method, it is characterised in that：In step（2）In, the pH value of the ammonia spirit is 10 ~ 11；When pH=10 of ammonia spirit
When, it is obtained for based on metal organic frame Cu3(BTC)2Nano-material；It is obtained as the pH of ammonia spirit=10.5
To be based on metal organic frame Cu3(BTC)2Nanometer sheet material；When the pH of ammonia spirit=11, obtained is organic based on metal
Frame Cu3(BTC)2Nano-particle material.
4. a kind of preparation method as claimed in claim 1 or 2 is obtained to be based on metal organic frame Cu3(BTC)2Different dimensional
The nano material of degree, it is characterised in that：The nano material of the different dimensions includes nano-material, nanometer sheet material and nanometer
Granular materials.
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Cited By (2)
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| CN109560277A (en) * | 2018-11-29 | 2019-04-02 | 重庆文理学院 | A kind of preparation method of nanometer of linear manganese selenide/carbon composite |
| CN113861483A (en) * | 2021-10-28 | 2021-12-31 | 深圳大学 | Preparation method of composite thermoelectric material based on metal organic framework |
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