CN109679111A - A kind of preparation method of HKUST-1 complex nanoparticle - Google Patents
A kind of preparation method of HKUST-1 complex nanoparticle Download PDFInfo
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- CN109679111A CN109679111A CN201910032185.7A CN201910032185A CN109679111A CN 109679111 A CN109679111 A CN 109679111A CN 201910032185 A CN201910032185 A CN 201910032185A CN 109679111 A CN109679111 A CN 109679111A
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- 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
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Abstract
The present invention relates to a kind of metal organic complex HKUST-1 nanoparticles and preparation method thereof, belong to novel nano catalysis material preparation field.Material therefor synthetic method of the present invention is solwution method.Specific step is as follows: trimesic acid and sodium hydroxide being dissolved into deionized water first, deionized water and N are added in beaker, dinethylformamide, the solution of trimesic acid and sodium hydroxide is added in beaker, then copper nitrate aqueous solution is added, magnetic agitation is the nano material by sky blue pulverulent solids are obtained after products therefrom centrifugation, washing, drying.Preparation method of the present invention is simple and easy to do, and the catalytic nanometer material property of synthesis is stablized, and experiment condition is environmentally protective, the not harsh suitable large-scale production of experiment condition.
Description
Technical field
The present invention relates to a kind of metal organic complex HKUST-1 nanoparticles and preparation method thereof, belong to functional material
Technical field.
Background technique
Metal organic framework (Metal-Organic Frameworks, MOFs) material be by ion cluster or metal from
A kind of novel inorganic-organic Hybrid Materials that son is formed under the connection of various organic ligands have large specific surface area, porosity
The high, good characteristics such as performance is stable, density is small, in recent years gas store with separate, be catalyzed, in terms of show
Excellent properties and be concerned.It is well known that physical and chemical performance is often as the size reduction of material is to nanometer range
Significant change occurs.After the size reduction to nanoscale of metal organic framework complex, its structure is adjustable, property retaining
While the characteristics such as energy multiplicity, it can be further improved its specific surface area, enhance it in the property in the fields such as gas absorption, catalysis
Energy.Thus, the preparation method research of Nanosized metal organic backbone complex has great importance.
The HKUST-1 complex constructed by copper ion and trimesic acid ligand since by Chui et al. report i.e. by
Extensive concern.HKUST-1 has more than 1000m2The specific surface area of/g is still able to maintain good skeleton under high-temperature calcination
Structure has important application in gas absorption separation and catalytic field.However the synthetic method of HKUST-1 generally has at present
Have the shortcomings that the reaction time is long, energy consumption is high and preparation condition is complicated.Such as: the HKUST-1 of solvent-thermal method preparation is easy to get to larger
Crystal grain, and the Cu easily generated for being unfavorable for subsequent applications at high temperature under high pressure2O, the reaction time generally 12 hours with
Upper (Chiericatti C, Micropor. Mesopor. Mater., 2012,162:60-63)；Prepared by microwave method
HKUST-1 scantling it is larger and require the condition of microwave radiation (Tari N E, J. Porous Mater., 2015,22:
1161-1169).Therefore, develop a kind of simple and easy, the reaction time is short, the low HKUST-1 complex preparation method of energy consumption of reaction
Have great importance.
Summary of the invention
For the above-mentioned shortcoming of the prior art, the present invention provides a kind of metal organic complex HKUST-1 nanometers
Particle and its supper-fast preparation method can prepare size uniformity at room temperature by diffusion method in 10 seconds, regular appearance
HKUST-1 nanoparticle.Its preparation process is simple, rapidly and efficiently, it is low in cost, be suitble to large-scale industrial production.
The purpose of the present invention is what is be achieved through the following technical solutions:
1) trimesic acid and NaOH solid are weighed in conical flask by certain mol proportion and deionized water is added, ultrasound is to promote
It is dissolved；
2) a certain amount of copper nitrate is weighed in beaker, and deionized water is added, prepares certain density copper nitrate aqueous solution；
3) a certain proportion of deionized water and n,N-Dimethylformamide are added in beaker, it is molten adds gained in step 1)
Liquid, magnetic agitation are uniformly mixed it；
4) copper nitrate solution obtained by step 2 is added in step 3) acquired solution and magnetic agitation is reacted；
5) reaction mixture obtained by step 4) is centrifugated, and uses deionized water and ethanol washing, dried with blast drier
Final product is obtained afterwards.
Beneficial effects of the present invention:
(1) the present invention provides a kind of preparation method of novel metal organic complex HKUST-1 nanoparticle, preparation methods
It is simple to operation, do not need special equipment, it is low in cost and be suitable for large scale preparation, it can satisfy the demand of practical application；
(2) metal organic complex HKUST-1 nanoparticle preparation speed prepared by the present invention is fast, greatly improves synthesis effect
Rate；
(3) metal organic complex HKUST-1 particle prepared by the present invention is nano-scale, compares bulk metal organic coordination compound
HKUST-1 has higher specific surface area and is easier to disperse, and application is stronger；
(4) of the invention preparation method is simple, is not required to special equipment；
The raw materials used in the present invention is cheap, and materials synthesis is at low cost, is suitble to mass production.
Detailed description of the invention
Fig. 1 is metal organic complex HKUST-1 nanoparticle Japan Electronics JEOL- prepared by the method for the present invention
One of in multiple transmission electron microscope (TEM) photos shot after 1400 transmission electron microscope observations；Wherein, Fig. 1 a has for metal
Machine complex HKUST-1 nanoparticle low power TEM image, Fig. 1 b are metal organic complex HKUST-1 nanoparticle high power TEM
Image；
Fig. 2 is the X-ray diffraction (XRD) figure of metal organic complex HKUST-1 nanoparticle prepared by the method for the present invention.
Specific embodiment
The contents of the present invention are described in further detail below by specific implementation example with reference, but these realities
It applies example and is not intended to limit protection scope of the present invention.
Embodiment 1
2 mmol trimesic acids are weighed first and 4 mmol sodium hydroxides are dissolved into 2 mL deionized waters, are added in beaker
Beaker is added in the solution of trimesic acid and sodium hydroxide by 9.5 mL deionized waters and 8 mL n,N-Dimethylformamide
In, it is rear to be added 0.025 mmol copper nitrate solution, after 10 s of magnetic agitation, gained reaction mixture is centrifugated, and spends
Ionized water and ethanol washing, then 60oC blast drier is dry, and metal organic complex HKUST-1 nanoparticle is made.
Embodiment 2
4 mmol trimesic acids are weighed first and 8 mmol sodium hydroxides are dissolved into 2 mL deionized waters, are added in beaker
Beaker is added in the solution of trimesic acid and sodium hydroxide by 20 mL deionized waters and 15 mL n,N-Dimethylformamide
In, it is rear to be added 0.050 mmol copper nitrate solution, after 10 s of magnetic agitation, gained reaction mixture is centrifugated, and spends
Ionized water and ethanol washing, then 60oC blast drier is dry, and metal organic complex HKUST-1 nanoparticle is made.
Embodiment 3
2 mmol trimesic acids are weighed first and 4 mmol sodium hydroxides are dissolved into 2 mL deionized waters, are added in beaker
Beaker is added in the solution of trimesic acid and sodium hydroxide by 9.5 mL deionized waters and 8 mL n,N-Dimethylformamide
In, it is rear to be added 0.025 mmol copper nitrate solution, after 5 s of magnetic agitation, gained reaction mixture is centrifugated, and spend from
Sub- water and ethanol washing, then 60oC blast drier is dry, and metal organic complex HKUST-1 nanoparticle is made.
Embodiment 4
3 mmol trimesic acids are weighed first and 6 mmol sodium hydroxides are dissolved into 2 mL deionized waters, are added in beaker
Beaker is added in the solution of trimesic acid and sodium hydroxide by 12 mL deionized waters and 10 mL n,N-Dimethylformamide
In, it is rear to be added 0.033 mmol copper nitrate solution, after 10 s of magnetic agitation, gained reaction mixture is centrifugated, and spends
Ionized water and ethanol washing, then 60oC blast drier is dry, and metal organic complex HKUST-1 nanoparticle is made.
Claims (5)
1. a kind of metal organic complex HKUST-1 nanoparticle, the nanoparticle is octahedron, and size is about 100 nm.
2. a kind of preparation method of metal organic complex HKUST-1 nanoparticle, it is characterised in that the step of preparation method such as
Under:
1) trimesic acid of certain mol proportion is weighed, sodium hydroxide dissolves in deionized water；
2) deionized water and N,N-dimethylformamide in the mixed solvent is added in step 1) acquired solution；
3) copper nitrate aqueous solution being added into step 2) acquired solution, magnetic agitation reaction；
4) it is centrifuged and washs to obtain sky blue powdery product.
3. the preparation method of metal organic complex HKUST-1 nanoparticle according to claim 2, which is characterized in that
Preparation method used be solwution method, solvent be deionized water and n,N-Dimethylformamide, the two volume ratio 1:1 to 2:1 it
Between.
4. the preparation method of metal organic complex HKUST-1 nanoparticle according to claim 2, which is characterized in that
Copper nitrate used, trimesic acid molar ratio in 1:50 between 1:200.
5. the preparation method of metal organic complex HKUST-1 nanoparticle according to claim 2, which is characterized in that
Reaction temperature section described in step 3) is 10-35oC, reaction time are 5 to 30 seconds.
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| CN201910032185.7A CN109679111A (en) | 2019-01-14 | 2019-01-14 | A kind of preparation method of HKUST-1 complex nanoparticle |
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| CN201910032185.7A CN109679111A (en) | 2019-01-14 | 2019-01-14 | A kind of preparation method of HKUST-1 complex nanoparticle |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102336774A (en) * | 2011-07-20 | 2012-02-01 | 中国科学院化学研究所 | Method for synthesizing BTC (1,3,5-benzenetricarboxylic acid)-based nanoscale organometallic framework material |
| CN103785363A (en) * | 2014-02-13 | 2014-05-14 | 天津大学 | Preparation method for preparing polymer skeleton with surface coated with HKUST-1 through 3D printing, and application of polymer skeleton |
| CN106947977A (en) * | 2017-04-28 | 2017-07-14 | 合肥工业大学 | A kind of copper-based low-temp reversible thermochromic material and preparation method thereof |
| CN108373164A (en) * | 2018-03-12 | 2018-08-07 | 江苏师范大学 | A kind of C claddings Cu2The synthetic method of O cuboctahedron nucleocapsids |
-
2019
- 2019-01-14 CN CN201910032185.7A patent/CN109679111A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102336774A (en) * | 2011-07-20 | 2012-02-01 | 中国科学院化学研究所 | Method for synthesizing BTC (1,3,5-benzenetricarboxylic acid)-based nanoscale organometallic framework material |
| CN103785363A (en) * | 2014-02-13 | 2014-05-14 | 天津大学 | Preparation method for preparing polymer skeleton with surface coated with HKUST-1 through 3D printing, and application of polymer skeleton |
| CN106947977A (en) * | 2017-04-28 | 2017-07-14 | 合肥工业大学 | A kind of copper-based low-temp reversible thermochromic material and preparation method thereof |
| CN108373164A (en) * | 2018-03-12 | 2018-08-07 | 江苏师范大学 | A kind of C claddings Cu2The synthetic method of O cuboctahedron nucleocapsids |
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Application publication date: 20190426 |