CN107353413A - A kind of preparation method of the nanometer organic metal framework material based on conjugated polymer - Google Patents
A kind of preparation method of the nanometer organic metal framework material based on conjugated polymer Download PDFInfo
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- CN107353413A CN107353413A CN201710609236.9A CN201710609236A CN107353413A CN 107353413 A CN107353413 A CN 107353413A CN 201710609236 A CN201710609236 A CN 201710609236A CN 107353413 A CN107353413 A CN 107353413A
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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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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/18—Metal complexes
- C09K2211/183—Metal complexes of the refractory metals, i.e. Ti, V, Cr, Zr, Nb, Mo, Hf, Ta or W
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Abstract
The present invention designs a kind of preparation method of the nanometer organic metal framework material based on conjugated polymer, belongs to a kind of porous material synthesized by structure design, is named as P MOFs.Synthesis only needs part and complex ion being dispersed in a certain amount of surfactant, reaches the condition of self assembly in autoclave by being rested under 80 DEG C of environment to obtain required product.The present invention is simple to operate, and cost is low, only needs reactant and surfactant, reproducible reaction safety and stability in part and complex ion self assembling process.Because it has a porous of nanoscale and height, the ligand fluorescence in material should be able to be unaffected for the machine metal framework material of preparation.Simultaneously as using Zr, as ligand ion, the material for obtaining synthesis has the advantages that good stability, biocompatibility.
Description
Technical field
Invention design herein is related to a kind of preparation method of the nanometer organic metal framework material based on conjugated polymer.
Background technology
Metal-organic framework material (metal-organic frameworks, MOFs) is with containing by metal ion (cluster)
The crystalline material with periodicity network structure that the organic ligand of oxygen or nitrogen is formed by connecting by self assembly, there is super large
The advantages that specific surface area and pore volume, adjustable aperture and topological structure, good heat endurance and chemical stability.It is easy to
The characteristics of control, can be designed that stablize regular pore structure is used for all kinds of purposes by metal-organic framework material.
Compared with traditional inorganic porous material, MOFs materials have a bigger specific surface area, higher porosity, structure and
Function is more various, thus has been widely used in gas absorption and has separated, the neck such as sensor, medicament slow release, catalytic reaction
In domain.Simultaneously as they also have nanoscale, it is easy to functionalization, the advantages that good biocompatibility, organic metal framework material
Material starts to be applied to the association area such as sensor.
The content of the invention
Present invention aims at providing a kind of preparation method of the nanometer organic metal framework material based on conjugated polymer,
The present invention is realized by following experimental program：
A is by 4,4 '-(2,5-dimethoxy-1,4-phenylene) bis (ethyne-2,1-diyl) dibenzoic acid
（P-acid）With ZrCL4Solid is dissolved in DMF solution, and solution is arrived completely by the solid in solution is fully dispersed using ultrasonic wave
In；
B is transferred the solution into the reactor of polytetrafluoroethylliner liner, and it is 80 DEG C that preheating is put into after reactor is closed completely
Vacuum drying chamber in, stand reaction；
After completion of the reaction, obtained mixture obtains yellow crystals by centrifugation and precipitated c, and obtained yellow crystals are precipitated and used
Absolute ethyl alcohol washs, and obtains desired yellow crystals after removing surfactant, product is P-MOFs here.
The ratio of reactant is P-acid and ZrCL in step a of the present invention4The amount ratio of material is 1:1, P-acid
With ZrCl4It is every to there is 0.01mol to need to use 18mL DMF solvents.
The reaction time stood in step b of the present invention is 72h.
The washing times of absolute ethyl alcohol are 5 times in step c of the present invention.
The present invention is simple to operate, and cost is low, only needs reactant to be lived with surface in part and complex ion self assembling process
Property agent, reproducible reaction safety and stability.The machine metal framework material of preparation is because it has the porous of nanoscale and height
Property, the ligand fluorescence in material should be able to be unaffected.Simultaneously as Zr is used to obtain synthesis as ligand ion
Material there is the advantages that good stability, biocompatibility.
Brief description of the drawings
Fig. 1：The scanning electron microscope diagram of P-MOFs materials.
Fig. 2：The X ray diffracting spectrum of P-MOFs materials.
Embodiment
In order to further illustrate the fluorescent functional nanoscale organic metal framework material based on conjugated polymer part
Preparation method, the present embodiment implemented according to technical solution of the present invention, provides specific embodiment：All it is with reactant
Exemplified by 0.64mol, by 0.27g P-ACID powder and 1.5g ZrCL4Solid is dissolved in DMF solution, using ultrasonic wave by solution
In solid it is fully dispersed completely into solution；Transfer the solution into the reactor of polytetrafluoroethylliner liner, reactor is sealed
Preheating is put into after closing completely in 80 DEG C of vacuum drying chamber, to stand reaction；After completion of the reaction, the mixture obtained by from
Gains in depth of comprehension are precipitated to yellow crystals, and obtained precipitation is washed 5 times using absolute ethyl alcohol, obtained after removing surfactant desired
Organic metal framework material P-MOF based on fluorescent ligand.
Obtained sample is scanned electron microscope（SEM）And X-ray diffracting spectrum（XRD）Analysis, as a result referring to
Accompanying drawing 1,2.
Sem analysis：With the pattern of the thermal field emission SEM of QUANTA FEG 250 observation zinc oxide；From Fig. 1
In it can be seen that prepare organic metal framework material pattern；From figure one it can be seen that prepared organic metal framework material
For sheet, edge is irregular, and diameter is in 80-100 nm or so.
XRD analysis：Promoted in D8 with XRD analysis and carried out on diffractometer；From Fig. 2 X diffracting spectrums it is recognised that product
Two diffraction maximums of XRD spectrum are obvious, without obvious miscellaneous peak, it was demonstrated that are a kind of crystal of pure phase made from this method, simultaneously
Two diffraction maximums also demonstrate two kinds of lattice shapes in the MOF materials of design and are obtained for realization.
Claims (4)
- A kind of 1. preparation method of the nanometer organic metal framework material based on conjugated polymer, it is characterised in that the preparation method Comprise the following steps：A is by 4,4 '-(2,5-dimethoxy-1,4-phenylene) bis (ethyne-2,1-diyl) dibenzoic acid （P-acid）With ZrCL4Solid is dissolved in DMF, referred to as DMF, in solution, using ultrasonic wave by solution Solid is fully dispersed completely into solution；B is transferred the solution into the reactor of polytetrafluoroethylliner liner, and it is 80 DEG C that preheating is put into after reactor is closed completely Vacuum drying chamber in, stand reaction；After completion of the reaction, obtained mixture obtains yellow crystals by centrifugation and precipitated c, and obtained precipitation is used into absolute ethyl alcohol Washing, desired fluorescent functional nanometer organic metal framework material is obtained after removing surfactant, P- can be referred to as MOFs。
- 2. the preparation method of the nanometer organic metal framework material according to claim 1 based on conjugated polymer, it is special Sign is P-acid and ZrCL in the ratio of the reactant in step a4The amount ratio of material is 1:1, P-acid and ZrCl4It is every to have 0.01mol needs to use 18mL DMF as surfactant..
- 3. the preparation method of the nanometer organic metal framework material according to claim 1 based on conjugated polymer, it is special It is 72h that step, which is levied, in the reaction time stood in b.
- 4. the preparation method of the nanometer organic metal framework material according to claim 1 based on conjugated polymer, it is special It is 5 times that step, which is levied, in the washing times of the absolute ethyl alcohol in c.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111909386A (en) * | 2020-07-16 | 2020-11-10 | 南京邮电大学 | Conjugated polymer-organic metal framework composite nano material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105080495A (en) * | 2015-09-16 | 2015-11-25 | 北京工业大学 | Metal-organic framework material of Zr and preparation method and application thereof |
| CN105218832A (en) * | 2015-09-16 | 2016-01-06 | 北京工业大学 | A kind of metal-organic framework materials based on low symmetrical four tooth Carboxylic acid ligand Cu and preparation method thereof |
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2017
- 2017-07-25 CN CN201710609236.9A patent/CN107353413A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105080495A (en) * | 2015-09-16 | 2015-11-25 | 北京工业大学 | Metal-organic framework material of Zr and preparation method and application thereof |
| CN105218832A (en) * | 2015-09-16 | 2016-01-06 | 北京工业大学 | A kind of metal-organic framework materials based on low symmetrical four tooth Carboxylic acid ligand Cu and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| ANDREAS SCHAATE，等: "Porous Interpenetrated Zirconium-Organic Frameworks (PIZOFs): A Chemically Versatile Family of Metal-Organic Frameworks", 《CHEMISTRY-A EUROPEAN JOURNAL》 * |
| HIROYASU FURUKAWA，等: "Water Adsorption in Porous Metal−Organic Frameworks and Related Materials", 《JOURNAL OF THE AMERICAN CHEMICAL SOCIETY》 * |
| 高升: "Zr基金属有机框架的设计、合成与性能研究", 《广东药科大学硕士论文》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111909386A (en) * | 2020-07-16 | 2020-11-10 | 南京邮电大学 | Conjugated polymer-organic metal framework composite nano material and preparation method thereof |
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Application publication date: 20171117 |