CN110170337A - Metal-organic framework materials MIL-53(Fe) hole-closing structure preparation method - Google Patents
Metal-organic framework materials MIL-53(Fe) hole-closing structure preparation method Download PDFInfo
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- CN110170337A CN110170337A CN201910416588.1A CN201910416588A CN110170337A CN 110170337 A CN110170337 A CN 110170337A CN 201910416588 A CN201910416588 A CN 201910416588A CN 110170337 A CN110170337 A CN 110170337A
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- organic framework
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- 239000000463 material Substances 0.000 title claims abstract description 32
- 239000013206 MIL-53 Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000012621 metal-organic framework Substances 0.000 title claims abstract description 14
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims abstract description 29
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims abstract description 29
- 239000004094 surface-active agent Substances 0.000 claims abstract description 13
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 38
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 26
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 24
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 3
- 210000003850 cellular structure Anatomy 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000011148 porous material Substances 0.000 description 11
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 9
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 6
- 238000002336 sorption--desorption measurement Methods 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
-
- B01J35/39—
-
- B01J35/612—
-
- B01J35/613—
-
- B01J35/643—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
Abstract
The present invention provides a kind of metal-organic framework materials MIL-53(Fe) preparation method of hole-closing structure, belong to photochemical catalyst preparation technical field.Its preparation process use solvent-thermal process method, addition surfactant tetraethyl ammonium hydroxide (TEAOH) auxiliary preparation metal-organic framework materials MIL-53(Fe) cellular structure be hole-closing structure；Raw material sources of the present invention are extensive, low in cost, and synthesis technology is easy, easily operated, have Development volue and application prospect.
Description
Technical field
The invention belongs to photochemical catalyst preparation technical field, in particular to a kind of metal-organic framework materials MIL-53 (Fe)
The preparation method of hole-closing structure.
Background technique
Metal-organic framework materials MIL-53 (Fe) has light-catalysed performance (Journal of Hazardous
Materials,2011,190(1-3):945-951).The many because being known as of properties of catalyst are influenced, specifically include that crystal phase knot
Structure, particle size, surface nature, specific surface area etc..The pore structure of metal-organic framework materials MIL-53 (Fe) is necessarily to its light
Catalytic performance has a major impact.It is known that the skeleton structure of MIL-53 (Fe) is flexible skeletal structure, with extraneous variation
(temperature, guest molecules) adjust self-framework structure, and the duct of material occurs expansion or shrinks, in open bore and narrower bore two
Become between kind form, referred to as " cell breath " (Chem.Mater.2010,20:4237-4245).Currently, control metal is organic
There are two ways to framework material MIL-53 (Fe) cellular structure: (1) temperature.Adjustment temperature can control the hole of MIL-53 (Fe)
Road degrees of expansion.However, the temperature of the duct degrees of expansion of control MIL-53 (Fe) may be with MIL-53 (Fe) practical application
Temperature is not consistent.(2) guest molecule.Guest molecule can control the duct degrees of expansion of MIL-53 (Fe).However, MIL-53
(Fe) duct is occupied by guest molecule, and application value is little.
Currently, so far, about the preparation method of metal-organic framework materials MIL-53 (Fe) hole-closing structure, being easy to grasp
Make, there is the method for practical application meaning to still belong to blank, there is not been reported.
Summary of the invention
The present invention controls a kind of metal organic framework material in view of the above-mentioned problems of the prior art, developing a kind of simplicity
Expect the preparation method of MIL-53 (Fe) hole-closing structure.Solves the problems, such as prior art blank.The present invention is for the first time by surface-active
Controlling agent of the agent tetraethyl ammonium hydroxide (TEAOH) as material duct closed pore mode, is applied to metal-organic framework materials
In the preparation process of MIL-53 (Fe), realizes and artificially the duct of metal-organic framework materials MIL-53 (Fe) is controlled.
Technical scheme is as follows:
A kind of preparation method of metal-organic framework materials MIL-53 (Fe) hole-closing structure, comprising the following steps:
A. iron chloride (FeCl is successively weighed3·6H2O), terephthalic acid (TPA) (H2BDC), n,N-Dimethylformamide (DMF),
It is n (FeCl according to the mass ratio of the material3·6H2O):n(H2BDC): n (DMF)=1:1:280 ratio is mixed；
B. step a mixing after be added dropwise Different adding amount surfactant tetraethyl ammonium hydroxide (TEAOH), make its with
The mass ratio of the material of iron chloride is n (FeCl3·6H2O): n (TEAOH)=1:0.1~1:0.4.
C. two hours of product ultrasonic vibration after synthesizing in step b are poured into polytetrafluoroethylene (PTFE) after stirring two hours
In reaction kettle；
D. the reaction kettle in step c is put into 150 DEG C of constant temperature oven, reacts 15h；
E. after reaction, reaction kettle is cooled to room temperature for the reaction kettle of step d；
F. the resulting sample of step e cleaned with deionized water, filtered, after EtOH Sonicate vibrates 2h, in 150 DEG C of vacuum
(vacuum degree: 50mbar) for 24 hours is activated in drying box, obtains final sample.
The advantages of the present invention
The advantages of the present invention are: the prices of raw materials are cheap, and preparation process is simple, the duct of obtained material
Structure is easily controllable.
Detailed description of the invention
Fig. 1 is the XRD diagram of embodiment 1-4 closed pore MIL-53 (Fe) sample；
Fig. 2 is the N of embodiment 1 closed pore MIL-53 (Fe) sample2Adsorption-desorption isothermal；
Fig. 3 is the N of embodiment 2 closed pore MIL-53 (Fe) sample2Adsorption-desorption isothermal；
Fig. 4 is the N of embodiment 3 closed pore MIL-53 (Fe) sample2Adsorption-desorption isothermal；
Fig. 5 is the N of embodiment 4 closed pore MIL-53 (Fe) sample2Adsorption-desorption isothermal.
Specific embodiment:
In order to further illustrate the present invention, the present invention is described in detail with reference to the accompanying drawings and embodiments, but not
They can be interpreted as limiting the scope of the present invention.
Embodiment 1
Successively weigh iron chloride (FeCl3·6H2O), terephthalic acid (TPA) (H2BDC), n,N-Dimethylformamide (DMF), is pressed
It is n (FeCl according to the mass ratio of the material3·6H2O):n(H2BDC): n (DMF)=1:1:280 ratio is mixed.Then, it is added dropwise
Surfactant tetraethyl ammonium hydroxide (TEAOH), making the mass ratio of the material of itself and iron chloride is respectively n (FeCl3·6H2O):n
(TEAOH)=1:0.1.After two hours of ultrasonic vibration, after stirring two hours, pour into ptfe autoclave.It will be anti-
It answers kettle to be put into 150 DEG C of constant temperature oven, reacts 15h.After reaction, reaction kettle is cooled to room temperature.Gained sample is spent
Ionized water cleaning filters, and after EtOH Sonicate vibrates 2h, (vacuum degree: 50mbar) for 24 hours is activated in 150 DEG C of vacuum oven,
Obtain sample.
Embodiment 2
Successively weigh iron chloride (FeCl3·6H2O), terephthalic acid (TPA) (H2BDC), n,N-Dimethylformamide (DMF), is pressed
It is n (FeCl according to the mass ratio of the material3·6H2O):n(H2BDC): n (DMF)=1:1:280 ratio is mixed.Then, it is added dropwise
Surfactant tetraethyl ammonium hydroxide (TEAOH), making the mass ratio of the material of itself and iron chloride is respectively n (FeCl3·6H2O):n
(TEAOH)=1:0.2.After two hours of ultrasonic vibration, after stirring two hours, pour into ptfe autoclave.It will be anti-
It answers kettle to be put into 150 DEG C of constant temperature oven, reacts 15h.After reaction, reaction kettle is cooled to room temperature.Gained sample is spent
Ionized water cleaning filters, and after EtOH Sonicate vibrates 2h, (vacuum degree: 50mbar) for 24 hours is activated in 150 DEG C of vacuum oven,
Obtain sample.
Embodiment 3
Successively weigh iron chloride (FeCl3·6H2O), terephthalic acid (TPA) (H2BDC), n,N-Dimethylformamide (DMF), is pressed
It is n (FeCl according to the mass ratio of the material3·6H2O):n(H2BDC): n (DMF)=1:1:280 ratio is mixed.Then, it is added dropwise
Surfactant tetraethyl ammonium hydroxide (TEAOH), making the mass ratio of the material of itself and iron chloride is respectively n (FeCl3·6H2O):n
(TEAOH)=1:0.3.After two hours of ultrasonic vibration, after stirring two hours, pour into ptfe autoclave.It will be anti-
It answers kettle to be put into 150 DEG C of constant temperature oven, reacts 15h.After reaction, reaction kettle is cooled to room temperature.Gained sample is spent
Ionized water cleaning filters, and after EtOH Sonicate vibrates 2h, (vacuum degree: 50mbar) for 24 hours is activated in 150 DEG C of vacuum oven,
Obtain sample.
Embodiment 4
Successively weigh iron chloride (FeCl3·6H2O), terephthalic acid (TPA) (H2BDC), n,N-Dimethylformamide (DMF), is pressed
It is n (FeCl according to the mass ratio of the material3·6H2O):n(H2BDC): n (DMF)=1:1:280 ratio is mixed.Then, it is added dropwise
Surfactant tetraethyl ammonium hydroxide (TEAOH), making the mass ratio of the material of itself and iron chloride is respectively n (FeCl3·6H2O):n
(TEAOH)=1:0.4.After two hours of ultrasonic vibration, after stirring two hours, pour into ptfe autoclave.It will be anti-
It answers kettle to be put into 150 DEG C of constant temperature oven, reacts 15h.After reaction, reaction kettle is cooled to room temperature.Gained sample is spent
Ionized water cleaning filters, and after EtOH Sonicate vibrates 2h, (vacuum degree: 50mbar) for 24 hours is activated in 150 DEG C of vacuum oven,
Obtain sample.
The pore structure property of 1 sample of table
Table 1Pore characteristics of samples
| sample | BET surface area(m2·g-1) | pore volume(cm3·g-1) |
| Embodiment 1 | 10.71 | 0.048 |
| Embodiment 2 | 7.98 | 0.018 |
| Embodiment 3 | 5.02 | 0.016 |
| Embodiment 4 | 4.35 | 0.015 |
Metal-organic framework materials MIL-53 (Fe) sample of surfactant tetraethyl ammonium hydroxide (TEAOH) auxiliary preparation
The characterization of the crystal phase structure of product, is shown in Fig. 1.It will be seen from figure 1 that surfactant tetraethyl ammonium hydroxide (TEAOH) auxiliary system
The XRD spectra of standby product go out peak position it is consistent with document report result (Chemistry of Materials, 2010,22
(14): 4237-4245), it was demonstrated that testing the sample synthesized is MIL-53 (Fe) crystal phase structure.It is provided from the XRD diagram of material
Information may determine that MIL-53 (Fe) sample by surfactant TEAOH auxiliary preparation is duct MIL-53 (Fe) of narrower bore
Structure (Journal of the American Chemical Society, 2010,132:1127-1136).
The N of sample2Adsorption-desorption isothermal curve at 77K is as shown in Figure 2-5.The curve form of four kinds of samples is identical,
Belong to typical IVth class adsorption isotherm, i.e. the pore structure of material is to contain mesoporous hierarchical porous structure.Table 1 gives sample
Specific surface area and Kong Rong, as can be seen from Table 1 with the increase of surfactant (TEAOH) additive amount, the specific surface of sample
Long-pending and Kong Rong is greatly lowered.The specific surface area of 1 sample of embodiment is only 10.71m2·g-1, the ratio table of other embodiments sample
Area is smaller.The specific surface area and Kong Rong of sample are greatly lowered with the addition of surfactant TEAOH.Illustrate synthesizing
It is added after surfactant (TEAOH) in the process, the pore structure for preparing sample is hole-closing structure.
The above is only a preferred embodiment of the present 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 (1)
1. a kind of metal-organic framework materials MIL-53(Fe) preparation method of hole-closing structure, it is characterised in that: including following step
It is rapid:
A. iron chloride, terephthalic acid (TPA), n,N-Dimethylformamide are successively weighed, the ratio for being 1:1:280 according to the mass ratio of the material
Example is mixed；
B. the surfactant tetraethyl ammonium hydroxide of Different adding amount is added dropwise after step a mixing, makes its object with iron chloride
The amount ratio of matter is iron chloride: tetraethyl ammonium hydroxide=1:0.1 ~ 1:0.4；
C. two hours of product ultrasonic vibration after synthesizing in step b are poured into polytetrafluoroethyl-ne alkene reaction after stirring two hours
In kettle;
D. the reaction kettle in step c is put into 150 DEG C of constant temperature oven, reacts 15 h；
E. after reaction, reaction kettle is cooled to room temperature for the reaction kettle of step d；
F. the resulting sample of step e cleaned with deionized water, filtered, it is dry in 150 DEG C of vacuum after EtOH Sonicate vibrates 2 h
24 h are activated in dry case, vacuum degree: 50 mbar obtain final sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910416588.1A CN110170337A (en) | 2019-05-20 | 2019-05-20 | Metal-organic framework materials MIL-53(Fe) hole-closing structure preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910416588.1A CN110170337A (en) | 2019-05-20 | 2019-05-20 | Metal-organic framework materials MIL-53(Fe) hole-closing structure preparation method |
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| CN110170337A true CN110170337A (en) | 2019-08-27 |
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| CN201910416588.1A Withdrawn CN110170337A (en) | 2019-05-20 | 2019-05-20 | Metal-organic framework materials MIL-53(Fe) hole-closing structure preparation method |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170173565A1 (en) * | 2014-05-16 | 2017-06-22 | Dow Global Technologies Llc | Process for synthesizing iron carbide fischer-tropsch catalysts |
| CN106957438A (en) * | 2017-03-21 | 2017-07-18 | 华南理工大学 | A kind of preparation of modified MIL 53 (Fe) metal organic framework and its method for organic wastewater treatment through persulfate activation |
| CN107446137A (en) * | 2017-08-04 | 2017-12-08 | 中南大学 | The method that one kind prepares ferrous metals organic framework material MIL 100 (Fe) |
| CN108129672A (en) * | 2017-12-18 | 2018-06-08 | 中南大学 | A kind of polymer changes the microwave synthesis method of MIL-53-Fe patterns |
| CN108329486A (en) * | 2018-05-09 | 2018-07-27 | 北京化工大学 | A kind of preparation method and application of the metal-organic framework materials of hybrid mesoporous structure |
-
2019
- 2019-05-20 CN CN201910416588.1A patent/CN110170337A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170173565A1 (en) * | 2014-05-16 | 2017-06-22 | Dow Global Technologies Llc | Process for synthesizing iron carbide fischer-tropsch catalysts |
| CN106957438A (en) * | 2017-03-21 | 2017-07-18 | 华南理工大学 | A kind of preparation of modified MIL 53 (Fe) metal organic framework and its method for organic wastewater treatment through persulfate activation |
| CN107446137A (en) * | 2017-08-04 | 2017-12-08 | 中南大学 | The method that one kind prepares ferrous metals organic framework material MIL 100 (Fe) |
| CN108129672A (en) * | 2017-12-18 | 2018-06-08 | 中南大学 | A kind of polymer changes the microwave synthesis method of MIL-53-Fe patterns |
| CN108329486A (en) * | 2018-05-09 | 2018-07-27 | 北京化工大学 | A kind of preparation method and application of the metal-organic framework materials of hybrid mesoporous structure |
Non-Patent Citations (3)
| Title |
|---|
| THOMAS DEVIC ET AL.: "Functionalization in Flexible Porous Solids: Effects on the Pore Opening and the Host-Guest Interactions", 《J. AM. CHEM. SOC.》 * |
| 刘澳琦等: "MIL-53材料的制备及其光催化性能的研究", 《化工科技》 * |
| 卢圆圆等: "MIL-53(Fe)的合成及光催化降解罗丹明Ｂ的研究", 《辽宁石油化工大学学报》 * |
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Application publication date: 20190827 |