CN108929675A - A kind of preparation method of composition metal organic framework materials MIL-101 (Cr) - Google Patents
A kind of preparation method of composition metal organic framework materials MIL-101 (Cr) Download PDFInfo
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- CN108929675A CN108929675A CN201810708683.4A CN201810708683A CN108929675A CN 108929675 A CN108929675 A CN 108929675A CN 201810708683 A CN201810708683 A CN 201810708683A CN 108929675 A CN108929675 A CN 108929675A
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- 239000013178 MIL-101(Cr) Substances 0.000 title claims abstract description 47
- 239000000463 material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000012621 metal-organic framework Substances 0.000 title claims abstract description 15
- 239000000203 mixture Substances 0.000 title claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000002131 composite material Substances 0.000 claims abstract description 11
- 239000013049 sediment Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012452 mother liquor Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000005470 impregnation Methods 0.000 claims abstract description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 4
- 239000010935 stainless steel Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000007865 diluting Methods 0.000 claims 1
- 238000004220 aggregation Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 238000001291 vacuum drying Methods 0.000 abstract 2
- 239000000243 solution Substances 0.000 description 14
- 230000005284 excitation Effects 0.000 description 4
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000003446 ligand Substances 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000001044 red dye Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- IOOMXAQUNPWDLL-UHFFFAOYSA-N 2-[6-(diethylamino)-3-(diethyliminiumyl)-3h-xanthen-9-yl]-5-sulfobenzene-1-sulfonate Chemical compound C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=C(S(O)(=O)=O)C=C1S([O-])(=O)=O IOOMXAQUNPWDLL-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 229920001795 coordination polymer Polymers 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000013259 porous coordination polymer Substances 0.000 description 1
- 239000013265 porous functional material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 239000011540 sensing material Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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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
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
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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
- 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
- C09K2211/10—Non-macromolecular compounds
- C09K2211/1003—Carbocyclic compounds
- C09K2211/1007—Non-condensed systems
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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
- C09K2211/10—Non-macromolecular compounds
- C09K2211/1018—Heterocyclic compounds
- C09K2211/1025—Heterocyclic compounds characterised by ligands
- C09K2211/1088—Heterocyclic compounds characterised by ligands containing oxygen as the only heteroatom
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Abstract
The invention discloses a kind of preparation methods of composition metal organic framework materials MIL-101 (Cr), include the following steps: Cr (NO3)3.9H2O、H2BDC, hydrofluoric acid and ionized water are added to polytetrafluoroethyllining lining, are mixed evenly；Liner is put into the reaction kettle of stainless steel, reaction kettle is covered tightly and is put into baking oven, oven temperature rises to 200 DEG C by room temperature in 3h, and in 200 DEG C of holding 8h.It makes reaction kettle cooling, then filters, obtain the sediment of green；Sediment is subjected to washing 3 times with DMF and ETOH respectively, then filters and obtains solids；Solids is put and is dried in a vacuum drying oven, is made MIL-101 (Cr)；It is spare to configure SRB mother liquor, then dilutes mother liquor and obtains SRB solution；It takes MIL-101 (Cr) to be placed in SRB solution, stands impregnation for 24 hours in water-bath later.It is dried in a vacuum drying oven after filtering, MIL-101 (Cr)@SRB composite fluorescent material is made.The present invention has the advantages that realizing SRB and MIL-101 (Cr) composite fluorescence.The case where hole of octahedral MIL-101 (Cr) disperses SRB, and aggregation is avoided to be quenched, increase the diversity of luminescent properties.
Description
Technical field
The present invention relates to metal-organic framework material technical field, in particular to a kind of composition metal organic framework materials
The preparation method of MIL-101 (Cr).
Background technique
Since twentieth century nineties, science and technology makes constant progress, even closer and universal through exchanging between subject,
Promote science and technology more quickly progress.The field of chemistry and material is also not have limitary mutual discussion, it was found that Yi Zhongxin
Coordination polymer --- novel porous materials, i.e. metal-organic framework material (MOFs).Metal-organic framework material is by gold
Belong to the Porous coordination polymer that ion either metal cluster and organic bridging molecules are formed as ligand, it is in combination with inorganic
The function and feature of chunking and organic chunking have porosity, programmable frame structure, high specific surface area and good
Stability.A kind of porous functional material of the metal-organic framework material as designability plays excellent at many aspects
Effect: gas store with separate, medicament slow release, selective catalysis, host-guest interaction, photoelectric material, magnetic material, molecule
Identification and sensing material etc..
Currently, MIL-101 (Cr) metal-organic framework material that goes out of prior art preparation just for ligand and center from
The ratio of son, preparation process otherness is very big, so that the appearance structure that will appear the MIL-101 (Cr) of preparation differs greatly；It is unfavorable
In in conjunction with SRB.
That there are energy gaps is smaller by red dye SRB, non-radiative recombination easily occurs；Level-density parameter is carried out between difficult and doped body,
Energy transfer is not exclusively (low efficiency).There are stronger π-π to interact for red dye, in the case where high-dopant concentration and now
There is MIL-101 (Cr) combination, is easy to produce polymerization between molecule, leads to concentration quenching.
Summary of the invention
The present invention in view of the drawbacks of the prior art, provides a kind of composition metal organic framework materials MIL-101 (Cr)
Preparation method can effectively solve the above-mentioned problems of the prior art.
In order to realize the above goal of the invention, the technical solution adopted by the present invention is as follows:
A kind of preparation method of composition metal organic framework materials MIL-101 (Cr), includes the following steps:
S1: by the Cr (NO of 1 molar part3)3.9H2O, the H of 1 molar part2BDC, 2.8 molar parts hydrofluoric acid (wt.%,
35%) and the deionized water of 267 molar parts is added to polytetrafluoroethyllining lining, is mixed evenly.
S2: liner is put into the reaction kettle of stainless steel, reaction kettle is covered tightly and is put into baking oven, oven temperature is by room temperature in 3h
200 DEG C are risen to, and in 200 DEG C of holding 8h.
S3: baking oven power supply is closed, reaction kettle is allowed to be gradually cooling to room temperature in an oven.Then it is filtered, is obtained with sand core funnel
To the sediment of green.
S4: carrying out washing 3 times with DMF and ETOH respectively for sediment, then using filtering, obtain solids,
S5: solids is placed on in 150 DEG C of vacuum oven dry 12h.Thus being made in next experiment is made
MIL-101 (Cr).
S6: the solid SRB of 200mg is dissolved, and configuration SRB mother liquor is spare.Then dilution mother liquor obtains SRB solution；
S7: by the first 12h dry in 80 DEG C of vacuum oven of MIL-101 (Cr), it is real then to start next load
It tests.
S8: taking MIL-101 (Cr) to be placed in SRB solution, comes into full contact with to MIL-101 (Cr) with solution, later just 37
DEG C water-bath in stand impregnation for 24 hours.It filters later, then the dry 12h in 80 DEG C of vacuum ovens, is made MIL-101
(Cr)@SRB composite fluorescent material.
Further, in S4, the separation of washing process is to be centrifuged 5 minutes to obtain sediment, centrifugal rotational speed using centrifuge
For 8000rpm；
Further, in S6 dilute SRB mother liquid concentration obtain concentration are as follows: 2.5ppm, 5ppm, 10ppm, 15ppm, 20ppm,
The SRB solution of 25ppm；
Further, 6 parts of MIL-101 (Cr) is taken to be placed in the SRB solution of 6 kinds of various concentrations in S8.
Compared with prior art the present invention has the advantages that
Realize SRB and MIL-101 (Cr) composite fluorescence.The hole of octahedral MIL-101 (Cr) disperses SRB, avoids
The case where aggregation is quenched.The unique light-emitting mode for having multiple excitation state and depositing；Increase the diversity of luminescent properties.
Detailed description of the invention
Fig. 1 is MIL-101 (Cr) aspect graph of preparation of the embodiment of the present invention；
The PXRD figure that Fig. 2 is the MIL-101 (Cr) of preparation of the embodiment of the present invention；
Fig. 3 is the ultra-violet absorption spectrum and fluorescence emission spectrogram of compound of the MIL-101 (Cr) of preparation of the embodiment of the present invention；
Fig. 4 is the fluorescence emission spectrum of MIL-101 (Cr)@SRB series composite fluorescent material of preparation of the embodiment of the present invention
Figure.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention more comprehensible, below in conjunction with attached drawing and embodiment is enumerated,
The present invention is described in further details.
A kind of preparation method of composition metal organic framework materials MIL-101 (Cr), includes the following steps:
S1: by 0.8054gCr (NO3)3.9H2O (2mmol), 0.3326g H2BDC (2mmol), the hydrofluoric acid of 0.1mL
The polytetrafluoroethyllining lining of 50mL is added in the deionized water of (wt.%, 35%) and 9.6mL, is mixed evenly.
S2: liner is put into the reaction kettle of stainless steel, reaction kettle is covered tightly and is put into baking oven, oven temperature is by room temperature in 3h
200 DEG C are risen to, and in 200 DEG C of holding 8h.
S3: baking oven power supply is closed, reaction kettle is allowed to be gradually cooling to room temperature in an oven.Then it is filtered, is obtained with sand core funnel
To the sediment of green.
S4: sediment is subjected to washing 3 times with DMF and ETOH respectively, the separation of intermediate washings process is using centrifuge
It obtains sediment (revolving speed 8000rpm) within centrifugation 5 minutes, for the last time using filtering, obtains solids,
S5: solids is placed on in 150 DEG C of vacuum oven dry 12h.Thus being made in next experiment is made
MIL-101 (Cr).
S6: a series of SRB solution of various concentrations is configured using the method for gradient dilution.It is first that the solid SRB of 200mg is molten
Constant volume is solved into the volumetric flask of 100mL, the SRB mother liquor for configuring 200ppm is spare.Then female using pipette and volumetric flask dilution
Liquid obtains: the Sulforhodamine B solution (SRB solution) of 2.5ppm, 5ppm, 10ppm, 15ppm, 20ppm, 25ppm of 200mL；
S7: then the first 12h dry in 80 DEG C of vacuum oven of metal-organic framework material starts next negative
Experiment is carried, load test is carried out in 37 DEG C of thermostat water bath.
S8: in the bottle for the label that the MIL-101 (Cr) for respectively weighing 6 parts of 10mg is placed in 6 50mL, then toward bottle
It is middle move into 30mL various concentration SRB solution, 6 concentration are respectively: 2.5ppm, 5ppm, 10ppm, 15ppm, 20ppm,
25ppm。
S9: when solution has just poured bottle into, shaking the bottle, and MIL-101 (Cr) comes into full contact with solution, later just 37
DEG C water-bath in stand impregnation for 24 hours.It filters later, then the dry 12h in 80 DEG C of vacuum ovens, is made MIL-101
(Cr)@SRB composite fluorescent material.
As shown in Fig. 2, the x-ray diffractogram of powder with the MIL-101 (Cr) of simulation of the MIL-101 (Cr) for synthesis
Spectrum, the position of MIL-101 (Cr) diffraction maximum of synthesis and relative intensity are consistent with what is simulated, show MIL-101 (Cr) at
Function preparation.
As shown in figure 3, MIL-101 (Cr) uv absorption spectra and the fluorescent emission under the light excitation of 395nm wavelength
Spectrogram.MIL-101 (Cr) is also that a variety of excitation state are simultaneous.MIL-101 (Cr) is inhaled in 200-700nm with full spectral coverage
It receives, fluorescence emission spectrum three peaks of 485nm, 525nm, 580nm occurs simultaneously, and maximum opposite peak intensity is at 485nm
Emission peak.MIL-101 (Cr) is in addition to the charge transtion of ligand, and there is also other two emission peaks, it may be possible to which LMCT and MLCT is produced
Raw multiple excitation is simultaneously deposited caused.
As shown in figure 4, can be seen that from fluorescence emission spectrogram of compound above as to load to MIL-101 (Cr) inner by SRB
Face, composition metal organic framework materials still maintain the fluorescence peak near frame material 485nm, the fluorescence near script 530nm
The interference of SRB solution that emission peak is supported, and with the increase of load capacity and slowly smooth.Meanwhile composite material occurs
SRB fluorescence peak at 580nm, and then as the increase of concentration has also appeared the emission peak near long wave direction 610nm.
We it may be speculated that with carried dye increase, the interaction of SRB and MIL-101 (Cr) increases, and new transmitting occurs
Peak, and with the increase of load capacity, the fluorescence of composite fluorescent material sent out extends to feux rouges direction.By MIL-101 (Cr)@
SRB line fluorescent launching light spectrogram is imported into GoCIE software, obtains the composite fluorescent material chromaticity coordinates in chromatic diagram point
Cloth, and calculate the information that opposite colour temperature obtains table 1 using chromaticity coordinates and colour temperature switching software and summarize.
Table 1MIL-101 (Cr)@SRB series composite fluorescent material relevant information table
Those of ordinary skill in the art will understand that the embodiments described herein, which is to help reader, understands this hair
Bright implementation method, it should be understood that protection scope of the present invention is not limited to such specific embodiments and embodiments.Ability
The those of ordinary skill in domain disclosed the technical disclosures can make its various for not departing from essence of the invention according to the present invention
Its various specific variations and combinations, these variations and combinations are still within the scope of the present invention.
Claims (4)
1. a kind of preparation method of composition metal organic framework materials MIL-101 (Cr), which comprises the steps of:
S1: by the Cr (NO of 1 molar part3)3.9H2O, the H of 1 molar part2BDC, the hydrofluoric acid wt.% of 2.8 molar parts are 35% He
The deionized water of 267 molar parts is added to polytetrafluoroethyllining lining, is mixed evenly；
S2: liner is put into the reaction kettle of stainless steel, reaction kettle is covered tightly and is put into baking oven, oven temperature is risen by room temperature in 3h
To 200 DEG C, and in 200 DEG C of holding 8h；
S3: baking oven power supply is closed, allows reaction kettle to be gradually cooling to room temperature in an oven, is then filtered with sand core funnel, obtained green
The sediment of color；
S4: sediment is subjected to washing 3 times with DMF and ETOH respectively, then using filtering, obtains solids；
S5: solids is placed on in 150 DEG C of vacuum oven dry 12h, is made MIL-101 (Cr)；
S6: the solid SRB of 200mg is dissolved, and configuration SRB mother liquor is spare, is then diluted mother liquor and is obtained SRB solution；
S7: by the first 12h dry in 80 DEG C of vacuum oven of MIL-101 (Cr), then start next load test；
S8: taking MIL-101 (Cr) to be placed in SRB solution, comes into full contact with to MIL-101 (Cr) with solution, later just at 37 DEG C
Impregnation is stood for 24 hours in water-bath；It filters later, then the dry 12h in 80 DEG C of vacuum ovens, is made MIL-101 (Cr)@
SRB composite fluorescent material.
2. according to the method described in claim 1, it is characterized by: the separation of washing process is using centrifuge centrifugation 5 in S4
Minute obtains sediment, centrifugal rotational speed 8000rpm.
3. according to the method described in claim 1, it is characterized by: diluting SRB mother liquid concentration in S6 obtains concentration are as follows:
The SRB solution of 2.5ppm, 5ppm, 10ppm, 15ppm, 20ppm, 25ppm.
4. according to the method described in claim 3, it is characterized by: 6 parts of MIL-101 (Cr) is taken to be placed in 6 kinds of various concentrations in S8
SRB solution in.
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| CN112980425A (en) * | 2021-02-25 | 2021-06-18 | 电子科技大学 | Solid powder color-changing material for non-contact induction quick response and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112980425A (en) * | 2021-02-25 | 2021-06-18 | 电子科技大学 | Solid powder color-changing material for non-contact induction quick response and preparation method thereof |
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Application publication date: 20181204 |