CN106345525A - Iron-based metal-organic-framework material water oxidation catalyst and preparation method thereof - Google Patents
Iron-based metal-organic-framework material water oxidation catalyst and preparation method thereof Download PDFInfo
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- CN106345525A CN106345525A CN201610629278.4A CN201610629278A CN106345525A CN 106345525 A CN106345525 A CN 106345525A CN 201610629278 A CN201610629278 A CN 201610629278A CN 106345525 A CN106345525 A CN 106345525A
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- 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
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/1691—Coordination polymers, e.g. metal-organic frameworks [MOF]
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- 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
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2213—At least two complexing oxygen atoms present in an at least bidentate or bridging ligand
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/14—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
- C07C227/18—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions involving amino or carboxyl groups, e.g. hydrolysis of esters or amides, by formation of halides, salts or esters
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/418—Preparation of metal complexes containing carboxylic acid moieties
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- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/02—Compositional aspects of complexes used, e.g. polynuclearity
- B01J2531/0238—Complexes comprising multidentate ligands, i.e. more than 2 ionic or coordinative bonds from the central metal to the ligand, the latter having at least two donor atoms, e.g. N, O, S, P
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- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
- B01J2531/842—Iron
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Abstract
The invention provides an iron-based metal-organic-framework material water oxidation catalyst and a preparation method thereof. The preparation method includes the steps of firstly, dissolving an organic ligand [HO2C-C6H4-CO2H]R into N, N- dimethyl formamide, and stirring under room temperature to obtain a clear and transparent solution for standby; secondly, adding Fe III into the clear and transparent solution obtained in the first step, and evenly stirring under room temperature to obtain a mixed solution for standby; thirdly, transferring the mixed solution obtained in the second step into a reaction kettle, performing constant-temperature thermal reaction, cooling after the reaction, filtering obtained solid products, and washing with ethanol to obtain solid products, namely the iron-based metal-organic-framework material water oxidation catalyst FeIII(OH)[O2C-C6H4-CO2]R. The preparation method has the advantages that the structural unit with the water oxidation catalyzing function is implanted into a metal organic framework material, and the prepared iron-based metal-organic-framework material has excellent pore structures and is beneficial to the increasing of the water oxidation reaction catalyzing ability and efficiency.
Description
Technical field
The invention belongs to chemical catalyst technical field, refer in particular to a kind of ferrous metals organic framework material water oxidation reaction and urge
Agent and preparation method thereof.
Background technology
With becoming increasingly conspicuous of the energy and environmental problem, new forms of energy and new energy conversion are increasingly subject to storing technology
The attention of researcher, and water oxidation reaction is exactly one of key reaction in numerous clean energy resource systems.It is hydrogen energy source system
The core procedure of middle water-splitting, also with various regenerative resource devices, sewage disposal and biological medicine etc. are closely related.However,
The high overpotential of this course of reaction relatively causes water oxygen to be reacted to the bottleneck of water splitting processes.Catalytic water oxidation effectiveness is good at present
Catalyst many with noble metals such as ru or ir as catalytic active center, involve great expense；And with the normal transition metal such as mn, fe and co
Catalyst major part for active center needs for it immobilized just can there is catalytic on porous material or macromolecular material
Energy.On the other hand, the metal-organic framework materials that past 20 years developed rapidly are with its excellent porous, the easy function of skeleton
The advantages such as change, good heat stability and chemical stability have obtained the concern of people.If catalytic water oxidation can will be had
The construction unit of function is implanted in metal-organic framework materials, and the material obtaining, due to having excellent pore structure, is conducive to
Improve ability and the efficiency of catalytic water oxidation reaction.
Fe is content highest transition metal in the earth's crust, is also most widely used metal in daily life, if can apply
Undoubtedly there is great help in water oxidation catalyst to its large-scale application.
Content of the invention
It is an object of the invention to, for the relatively costly problem of above-mentioned existing water oxidation catalyst, a kind of ferrum is proposed
Base Metal organic framework material water oxidation catalyst and preparation method thereof, realizes the efficient combination of porous material and avtive spot,
The species of abundant water oxidation reaction catalyst, effectively facilitates the research of water oxidation reaction and its in the energy, environment and biological medicine
The application of aspect.
For achieving the above object, the technical solution used in the present invention is:
A kind of ferrous metals organic framework material water oxidation reaction catalyst, described water oxygen catalyst molecule structural formula is
feiii(oh)[o2c-c6h4-co2]r；
Wherein, r is h, nh2、oh、ch3、och3In any one, substituent group neither with feiiiCoordination.
The present invention is in feiii(oh)[o2c-c6h4-co2] on the basis of, from donor residuess, part is modified, regulation is urged
Agent photon absorbing intensity and scope, thus improve the activity of its photocatalysis water oxygen.
A kind of preparation method of ferrous metals organic framework material water oxidation reaction catalyst, comprises the following steps:
Step 1, take organic ligand [ho2c-c6h4-co2H] r, and it is dissolved in n, and in n- dimethylformamide (dmf), room
Under the conditions of temperature, stirring obtains the solution of clear, standby；
Fe is added in step 2, the solution of clear obtaining to step 1iii, stir under room temperature condition, mixed
Close solution, standby；
The mixed solution that step 2 obtains is transferred in reactor step 3, carries out constant temperature thermal response, after completion of the reaction, cold
But, filter gained solid product, with washing with alcohol, the solid product finally obtaining obtains ferrous metals organic framework material water
Oxidation reaction catalyst feiii(oh)[o2c-c6h4-co2]r.
In step 1, the structural formula of described organic ligand isWherein, described r is h, nh2、oh、ch3、och3
In any one.
In step 1, organic ligand [ho2c-c6h4-co2H] r and dmf the amount of material ratio be 1:200～300.
In step 2, the fe that usediiiWith organic ligand [ho2c-c6h4-co2H] r the amount of material ratio be 1:1～5.
In step 2, described feiiiFor fecl3·6h2o.
In step 3, the temperature of described constant temperature thermal response is 100～150 DEG C, and the response time is 48～72h.
Compared with prior art have the advantage that
1. the construction unit with catalytic water oxidative function is implanted in metal-organic framework materials, the material obtaining by
In having excellent pore structure, be conducive to improving ability and the efficiency of catalytic water oxidation reaction.
2. from different donor residuess, part is modified, scalable catalyst photon absorbing intensity and scope, thus adjusting
Become the activity of the photocatalysis water oxygen of material.
3. ferrous metals organic framework material preparation method of the present invention is simple, feasible, yield higher it is easy to industrialization.
4. this catalyst is respond well in catalytic water oxidation reaction；And in different solvents system, this catalyst also has
There is good catalytic effect.
Brief description
Fig. 1 is the pxrd diffraction spectrogram of ferrous metals organic framework material water oxidation reaction catalyst；
Fig. 2 is the ft-ir spectrogram of ferrous metals organic framework material water oxidation reaction catalyst；
Fig. 3 is the uv atlas of ferrous metals organic framework material water oxidation reaction catalyst；
Fig. 4 is the nitrogen adsorption curve of ferrous metals organic framework material water oxidation reaction catalyst；
Fig. 5 is the cyclic voltammetric spectrogram of ferrous metals organic framework material water oxidation reaction catalyst, and wherein, curve a is
Blank
Experiment, curve b is photosensitizing agent solution system；
Fig. 6 is ferrous metals organic framework material water oxidation reaction catalyst photocatalysis water oxygen in different solutions system
Situation；
Fig. 7 is the recycling situation of ferrous metals organic framework material water oxidation reaction catalyst.
Specific embodiment
Below in conjunction with example, the present invention is further described:
Embodiment 1:
The preparation of p-phthalic acid-ferrous metals organic framework material water oxidation catalyst
(1) take p-phthalic acid (166mg, 1.0mmol), and be dissolved in 16～24ml n, n- dimethylformamide
(dmf), in (or only adding 16ml), under room temperature condition, stirring 5～20min obtains the solution of clear, standby；
(2) add 270～1350mg fecl in the solution of the clear obtaining to step (1)3·6h2O, room temperature condition
Lower stirring 5～20min, obtains mixed solution, standby；
(3) mixed solution obtaining step (2) is transferred in reactor, under the conditions of 100～150 DEG C reaction 48～
72h, cooled and filtered, washing with alcohol, obtain solid product feiii(oh)[o2c-c6h4-co2] it is ferrous metals organic backbone
Material water oxidation catalyst.
Prepared ferrous metals organic framework material carries out characterizing that to demonstrate the framing structure of this material be mil-53 through xrd
(see accompanying drawing 1)；Carry out characterizing carboxyl coordination success (see accompanying drawing 2) demonstrating in fe and p-phthalic acid through ft-ir spectrum；Warp
Uv atlas (see accompanying drawing 3) demonstrate this material has absorption to visible ray；Nitrogen adsorption curve (see accompanying drawing 4) shows that this material is
Porous material；Cyclic voltammetric spectrogram (see accompanying drawing 5) shows that this material possesses the ability of catalytic water oxidation.
P-phthalic acid-ferrous metals organic framework material photocatalysis water oxygenization is evaluated by neutral fruit
(1) measure buffer solution and (wherein contain 80mm na2s2o8) 2ml, in 25ml round-bottomed flask, accurately measures 200 μ l
The bipyridyl ruthenium aqueous solution of 0.01m, adds 10mg catalyst, starts to react under illumination condition；
(2) connect gas chromatogram, open software and produce the volume of gas every 10 minutes records, to generation gas volume not
Till increasing again.
(3) catalytic effect evaluation
(a) when the phosphate buffer solution from ph=8.5, the ton=35.4 of catalyst, tof=0.27/min is (see attached
Fig. 6)；
(b) when the solution from ph=7, the ton=31.0 of catalyst, tof=0.22/min (see accompanying drawing 6)；
C (), in the phosphate buffer solution of ph=8.5, this material circulation reduces by 13.5% (see attached using oxygen-producing amount after 4 times
Fig. 7).
Embodiment 2:
The preparation of 2- amino p-phthalic acid-ferrous metals organic framework material water oxidation catalyst
(1) take 2- amino p-phthalic acid (181mg, 1.0mmol), and be dissolved in 16～24ml n, n- dimethyl methyl
In amide (dmf) (or only adding 24ml), under room temperature condition, stirring 5～20min obtains the solution of clear, standby；
(2) add 270～1350mg fecl in the solution of the clear obtaining to step (1)3·6h2O, room temperature condition
Lower stirring 5～20min, obtains mixed solution, standby；
(3) mixed solution obtaining step (2) is transferred in reactor, under the conditions of 100～150 DEG C reaction 48～
72h, cooled and filtered, washing with alcohol, obtain solid product feiii(oh)[o2c-c6h4-co2]nh2It is the organic bone of ferrous metals
Frame material water oxidation catalyst.
Embodiment 3:
The preparation of 2- hydroxyterephthalic acid-ferrous metals organic framework material water oxidation catalyst
(1) take 2- hydroxyterephthalic acid (182mg, 1.0mmol), and be dissolved in 16～24ml n, n- dimethyl methyl
In amide (dmf), under room temperature condition, stirring 5～20min obtains the solution of clear, standby；
(2) add 270～1350mg fecl in the solution of the clear obtaining to step (1)3·6h2O, room temperature condition
Lower stirring 5-20min, obtains mixed solution, standby；
(3) mixed solution obtaining step (2) is transferred in reactor, under the conditions of 100～150 DEG C reaction 48～
72h, cooled and filtered, washing with alcohol, obtain solid product feiii(oh)[o2c-c6h4-co2] oh is the organic bone of ferrous metals
Frame material water oxidation catalyst.
Embodiment 4:
The preparation of 2- methylterephthalic acid-ferrous metals organic framework material water oxidation catalyst
(1) take 2- methylterephthalic acid (180mg, 1.0mmol), and be dissolved in 16～24ml n, n- dimethyl methyl
In amide (dmf), under room temperature condition, stirring 5～20min obtains the solution of clear, standby；
(2) add 270～1350mg fecl in the solution of the clear obtaining to step (1)3·6h2O, room temperature condition
Lower stirring 5～20min, obtains mixed solution, standby；
(3) mixed solution obtaining step (2) is transferred in reactor, under the conditions of 100～150 DEG C reaction 48～
72h, cooled and filtered, washing with alcohol, obtain solid product feiii(oh)[o2c-c6h4-co2]ch3It is the organic bone of ferrous metals
Frame material water oxidation catalyst.
Embodiment 5:
The preparation of 2- methoxyl group p-phthalic acid-ferrous metals organic framework material water oxidation catalyst
(1) take 2- methoxyl group p-phthalic acid (196mg, 1.0mmol), and be dissolved in 16～24ml n, n- dimethyl
In Methanamide (dmf), under room temperature condition, stirring 5～20min obtains the solution of clear, standby；
(2) add 270～1350mg fecl in the solution of the clear obtaining to step (1)3·6h2O, room temperature condition
Lower stirring 5～20min, obtains mixed solution, standby；
(3) mixed solution obtaining step (2) is transferred in reactor, under the conditions of 100～150 DEG C reaction 48～
72h, cooled and filtered, washing with alcohol, obtain solid product feiii(oh)[o2c-c6h4-co2]och3It is that ferrous metals is organic
Framework material water oxidation catalyst.
The present invention be not limited to ferrous metals organic framework material water oxidation catalyst described in above-described embodiment and its
Preparation method, the change of r and the change of preparation method are all within protection scope of the present invention.
Purposes in photocatalytic water molecular device is one kind of ferrous metals organic framework material water oxidation catalyst of the present invention
Purposes is it is impossible to assert that ferrous metals organic framework material water oxidation catalyst of the present invention is only used for water oxidation catalyst, for this
For the those of ordinary skill of technical field that the present invention belongs to, based on ferrous metals organic framework material water oxidation catalysiss of the present invention
Agent is used under the consideration of same mechanism of water oxidation catalyst, can also make some simple inferences, draw the chemical combination of the present invention
The other application purposes of thing, all should be considered as belonging to protection scope of the present invention.
Finally it is noted that the foregoing is only the preferred embodiments of the present invention, it is not limited to the present invention,
Although being described in detail to the present invention with reference to the foregoing embodiments, for a person skilled in the art, it still may be used
To modify to the technical scheme described in foregoing embodiments, or equivalent is carried out to wherein some technical characteristics.
All any modification, equivalent substitution and improvement within the spirit and principles in the present invention, made etc., should be included in the present invention's
Within protection domain.
Claims (7)
1. a kind of ferrous metals organic framework material water oxidation reaction catalyst is it is characterised in that described water oxidation catalyst
Molecular structural formula is feiii(oh)[o2c-c6h4-co2]r；
Wherein, r is h, nh2、oh、ch3、och3In any one, substituent group neither with feiiiCoordination.
2. a kind of preparation method of ferrous metals organic framework material water oxidation reaction catalyst is it is characterised in that include following
Step:
Step 1, take organic ligand [ho2c-c6h4-co2H] r, and it is dissolved in n, in n- dimethylformamide, stir under room temperature condition
Mix the solution obtaining clear, standby；
Fe is added in step 2, the solution of clear obtaining to step 1iii, stir under room temperature condition, obtain mixing molten
Liquid, standby；
The mixed solution that step 2 obtains is transferred in reactor step 3, carries out constant temperature thermal response, after completion of the reaction, cooling,
Filter gained solid product, with washing with alcohol, the solid product finally obtaining obtains ferrous metals organic framework material water oxygen
Change catalysts feiii(oh)[o2c-c6h4-co2]r.
3. the preparation method of a kind of ferrous metals organic framework material water oxidation reaction catalyst according to claim 2,
It is characterized in that, in step 1, the structural formula of described organic ligand isWherein, described r is h, nh2、oh、ch3、
och3In any one.
4. the preparation method of a kind of ferrous metals organic framework material water oxidation reaction catalyst according to claim 2,
It is characterized in that, in step 1, organic ligand [ho2c-c6h4-co2H] r and dmf the amount of material ratio be 1:200～300.
5. the preparation method of a kind of ferrous metals organic framework material water oxidation reaction catalyst according to claim 2,
It is characterized in that, in step 2, the fe that usediiiWith organic ligand [ho2c-c6h4-co2H] r the amount of material ratio be 1:1
～5.
6. the preparation method of a kind of ferrous metals organic framework material water oxidation reaction catalyst according to claim 2,
It is characterized in that, in step 2, described feiiiFor fecl3·6h2o.
7. the preparation method of a kind of ferrous metals organic framework material water oxidation reaction catalyst according to claim 2,
It is characterized in that, in step 3, the temperature of described constant temperature thermal response is 100～150 DEG C, and the response time is 48～72h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107917910A (en) * | 2017-11-16 | 2018-04-17 | 武汉轻工大学 | It is a kind of to be used to detect class enzyme test peper of hydrogen peroxide and its preparation method and application |
| CN108554455A (en) * | 2018-03-28 | 2018-09-21 | 华南理工大学 | A kind of water oxidation catalyst and preparation method thereof immobilized with metal-organic framework material |
| CN113527700A (en) * | 2021-06-28 | 2021-10-22 | 长沙理工大学 | Method for regulating and controlling catalytic activity of MIL-88 material |
| CN115286806A (en) * | 2022-01-24 | 2022-11-04 | 昆明理工大学 | Application method and preparation method of metal organic framework (OER) nanomaterial regulated by phenolic hydroxyl group |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107917910A (en) * | 2017-11-16 | 2018-04-17 | 武汉轻工大学 | It is a kind of to be used to detect class enzyme test peper of hydrogen peroxide and its preparation method and application |
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| CN113527700A (en) * | 2021-06-28 | 2021-10-22 | 长沙理工大学 | Method for regulating and controlling catalytic activity of MIL-88 material |
| CN115286806A (en) * | 2022-01-24 | 2022-11-04 | 昆明理工大学 | Application method and preparation method of metal organic framework (OER) nanomaterial regulated by phenolic hydroxyl group |
| CN115286806B (en) * | 2022-01-24 | 2023-09-19 | 昆明理工大学 | Application method and preparation method of phenolic hydroxyl-regulated metal organic framework nanomaterial OER |
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