CN103739562A - Trinuclear cadmium metal organic framework porous material and preparation method thereof - Google Patents
Trinuclear cadmium metal organic framework porous material and preparation method thereof Download PDFInfo
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- CN103739562A CN103739562A CN201310493717.XA CN201310493717A CN103739562A CN 103739562 A CN103739562 A CN 103739562A CN 201310493717 A CN201310493717 A CN 201310493717A CN 103739562 A CN103739562 A CN 103739562A
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/40—Nitrogen atoms
- C07D251/54—Three nitrogen atoms
- C07D251/70—Other substituted melamines
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Abstract
The invention discloses a trinuclear cadmium metal organic framework porous material which is an organic-inorganic hybrid compound formed by trinuclear cadmium and a tricarboxylic acid organic ligand. The molecular formula is C48H42N12O14Cd3, the crystal system is a cubic crystal system, the space group is P4[3]32, and the cell parameters comprise that: a=b=c=28.0397(9) angstroms, alpha=beta=gamma=90 degrees, and V=22046(1). Cadmium nitrate, the triazine tricarboxylic acid ligand and amino pyridine are mixed according to a certain ratio and are subjected to a reaction under conditions of a solvent and heating to obtain the compound. The compound has clear spatial structure, accurate molecular formula and simple synthetic method; and the compound has the characteristics of high porosity and ordered pore distribution, and can be used in the fields of catalytic reaction carriers, gas separation and storage, chromatographic analysis and the like.
Description
Technical field
The present invention relates to three-dimensional porous frame material field, be specifically related to a kind of cadmium metal and flexible tricarboxylic acid three-dimensional framework and preparation method thereof.
Background technology
Metal organic frame (MOF) is a kind of novel three-dimensional porous material being obtained by self-assembly mode by organic ligand and metal ion or metal cluster.Compared with traditional porous material (as zeolite, gac etc.), MOF has specific surface area that pore structure is orderly, large and structure and can regulate and control and the advantage such as can modify.Therefore, MOF has potential using value in fields such as gas adsorption separation, catalysis, chemical sensitisation and molecular recognition.As triazine and derivative thereof abundant containing N atom and that have electrophilic character, in chemosynthesis, play an important role, recently, the organic ligand containing triazine in MOF is synthetic receives great concern.
Summary of the invention
The object of the invention is to open a kind of three core cadmium metal organic frame porous materials and preparation method thereof, this framework has larger porosity, simple synthetic method, productive rate high.
The technical scheme that the present invention adopts is for achieving the above object: a kind of three core cadmium metal organic frame porous materials, is characterized in that: this porous material is that flexible triazine tricarboxylic acid connects the hybrid inorganic-organic compound that three core cadmiums form, and its molecular formula is: C
48h
42n
12o
14cd
3, crystallographic system is isometric system, spacer is P4
332, unit cell parameters a=b=c=28.0397 (9)
α=β=γ=90 °, V=22046(1).
Title complex basic structure described above is the three-dimensional frame structure with cys topological classification, and porosity theoretical value is 84.1%.In an asymmetry unit, contain two independently Cd
2+ion, Cd1 is hexa-coordinate, respectively with six carboxyls from six Different L parts on an O Atomic coordinate, in octahedral coordination environment; Cd2 is four-coordination, with three carboxyl O and the strict water molecules coordination of three Different L parts, in tetrahedral coordination environment.Like this, three core Cd bunches connect into by three linking ligand the three-dimensional frame structure that (6,3) connect.
Wherein part H used
3the structure of L is as follows:
A synthetic method for three core cadmium metal organic frame porous materials, comprises following steps:
1) the 3:1:1 mixing in molar ratio of cadmium nitrate, H3L part, structure directing agent is positioned in reaction unit, structure directing agent is the one in PA, 3-aminopyridine, 4-aminopyridine;
2) solvent DMF is joined in above-mentioned reaction unit, under room temperature, fully stir, reactant is fully mixed;
3) reaction unit is put into 90 degrees Celsius of heating units, reacted 10 days, then naturally cool to room temperature, open reaction unit and obtain cadmium complex;
4) with fresh DMF washing, obtain Cd title complex for several times.
Above-mentioned synthetic middle agents useful for same is analytical pure.
Compared with prior art, the invention has the advantages that: cadmium metal title complex three-dimensional framework material porosity of the present invention is large, and hole distribution is orderly, can be applicable to the fields such as catalyzed reaction carrier, gas delivery and storage and stratographic analysis; The synthetic method of cadmium metal title complex three-dimensional framework material of the present invention, the source take cadmium nitrate as metal ion, take triazine tricarboxylic acid as organic ligand, take aminopyridine as structure directing agent and acid-base modifier synthetic cadmium metal title complex frame material obtaining under solvent thermal condition, synthesis technique is simple, mild condition; Wherein, aminopyridine plays an important role in three-dimensional framework material of the present invention is synthetic, if do not add aminopyridine, can not obtain title complex of the present invention.Therefore the preparation method of cadmium metal title complex of the present invention is significant.
Accompanying drawing explanation
Fig. 1 is the space structure figure of three core cadmium metal organic frame porous materials
Embodiment
Embodiment mono-
Cadmium nitrate (0.3mmol), H3L part (0.1mmol), PA (0.1mmol) are mixed in 20mL vial; 6mL DMF is joined in above-mentioned vial, under room temperature, fully stir, reactant is fully mixed; Reaction unit is put into 90 degrees Celsius of heating units, react 10 days, then naturally cool to room temperature, open reaction unit and obtain cadmium complex; With fresh DMF washing, obtain Cd title complex for several times.
Embodiment bis-
Cadmium nitrate (0.3mmol), H3L part (0.1mmol), 3-aminopyridine (0.1mmol) are mixed in 20mL vial; 6mL DMF is joined in above-mentioned vial, under room temperature, fully stir, reactant is fully mixed; Reaction unit is put into 90 degrees Celsius of heating units, react 10 days, then naturally cool to room temperature, open reaction unit and obtain cadmium complex; With fresh DMF washing, obtain Cd title complex for several times.
Embodiment tri-
Cadmium nitrate (0.3mmol), H3L part (0.1mmol), 4-aminopyridine (0.1mmol) are mixed in 20mL vial; 6mL DMF is joined in above-mentioned vial, under room temperature, fully stir, reactant is fully mixed; Reaction unit is put into 90 degrees Celsius of heating units, react 10 days, then naturally cool to room temperature, open reaction unit and obtain cadmium complex; With fresh DMF washing, obtain Cd title complex for several times.
After measured, in above-described embodiment, the cadmium metal complex molecule formula of gained is C
48h
42n
12o
14cd
3, crystallographic system is isometric system, spacer is P4
332, unit cell parameters a=b=c=28.0397 (9)
, α=β=γ=90 °, V=22046(1), space structure figure is as shown in Figure 1.
Claims (2)
1. three core cadmium metal organic frame porous materials, is characterized in that: this porous material is that flexible triazine tricarboxylic acid connects the hybrid inorganic-organic compound that three core cadmiums form, and its molecular formula is: C
48h
42n
12o
14cd
3, crystallographic system is isometric system, spacer is P4
332, unit cell parameters a=b=c=28.0397 (9)
α=β=γ=90 °, V=22046(1).
2. a synthetic method for three core cadmium metal organic frame porous materials, comprises following steps:
1) by cadmium nitrate, H
3the 3:1:1 mixing in molar ratio of L part, structure directing agent is positioned in reaction unit, and structure directing agent is the one in PA, 3-aminopyridine, 4-aminopyridine;
2) solvent DMF is joined in above-mentioned reaction unit, under room temperature, fully stir, reactant is fully mixed;
3) reaction unit is put into 90 degrees Celsius of heating units, reacted 10 days, then naturally cool to room temperature, open reaction unit and obtain cadmium complex;
4) with fresh DMF washing, obtain Cd title complex for several times.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105617994A (en) * | 2015-12-29 | 2016-06-01 | 中国科学院福建物质结构研究所 | Metal organic framework material for effectively separating dyes similar in size |
| CN105936668A (en) * | 2016-01-26 | 2016-09-14 | 安庆师范大学 | Cd coordination compound based on flexible amido pyridine ligand and preparation method thereof |
| CN106046389A (en) * | 2016-06-16 | 2016-10-26 | 北京工商大学 | Flame retardant catalyst of metal organic frame complex and preparation method thereof |
| CN107793574A (en) * | 2017-10-20 | 2018-03-13 | 烟台智本知识产权运营管理有限公司 | The synthesis for the cadmium metal organic frame compound that cyanuric acid three (2 carboxyethyl) ester is constructed |
| CN112201786A (en) * | 2020-08-12 | 2021-01-08 | 中南大学 | Potassium phosphate metal salt organic compound cathode material taking vanadium as substrate and preparation method thereof |
| WO2021233065A1 (en) * | 2020-05-18 | 2021-11-25 | 上海科技大学 | Metal-organic framework material |
| CN114316291A (en) * | 2022-01-27 | 2022-04-12 | 德州学院 | Metal-organic framework based on trispyrazole ligand, preparation method and application of metal-organic framework in organic dye degradation |
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| CN103100373A (en) * | 2013-02-26 | 2013-05-15 | 河南师范大学 | Adsorbent, preparation method and application thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105617994A (en) * | 2015-12-29 | 2016-06-01 | 中国科学院福建物质结构研究所 | Metal organic framework material for effectively separating dyes similar in size |
| CN105617994B (en) * | 2015-12-29 | 2018-04-10 | 中国科学院福建物质结构研究所 | A kind of metal-organic framework materials are used for the dyestuff for efficiently separating adjoining dimensions |
| CN105936668A (en) * | 2016-01-26 | 2016-09-14 | 安庆师范大学 | Cd coordination compound based on flexible amido pyridine ligand and preparation method thereof |
| CN105936668B (en) * | 2016-01-26 | 2019-02-15 | 安庆师范大学 | A kind of Cd complex and preparation method thereof based on flexible amide pyridyl ligands |
| CN106046389A (en) * | 2016-06-16 | 2016-10-26 | 北京工商大学 | Flame retardant catalyst of metal organic frame complex and preparation method thereof |
| CN106046389B (en) * | 2016-06-16 | 2019-02-05 | 北京工商大学 | A kind of metallic organic frame complex flame retardation catalyst and preparation method thereof |
| CN107793574A (en) * | 2017-10-20 | 2018-03-13 | 烟台智本知识产权运营管理有限公司 | The synthesis for the cadmium metal organic frame compound that cyanuric acid three (2 carboxyethyl) ester is constructed |
| WO2021233065A1 (en) * | 2020-05-18 | 2021-11-25 | 上海科技大学 | Metal-organic framework material |
| CN112201786A (en) * | 2020-08-12 | 2021-01-08 | 中南大学 | Potassium phosphate metal salt organic compound cathode material taking vanadium as substrate and preparation method thereof |
| CN114316291A (en) * | 2022-01-27 | 2022-04-12 | 德州学院 | Metal-organic framework based on trispyrazole ligand, preparation method and application of metal-organic framework in organic dye degradation |
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Granted publication date: 20150909 Termination date: 20171020 |