CN104164227A - Preparation method and properties of series of organometallic host-guest composite materials - Google Patents
Preparation method and properties of series of organometallic host-guest composite materials Download PDFInfo
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- CN104164227A CN104164227A CN201310206912.XA CN201310206912A CN104164227A CN 104164227 A CN104164227 A CN 104164227A CN 201310206912 A CN201310206912 A CN 201310206912A CN 104164227 A CN104164227 A CN 104164227A
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Abstract
The invention discloses a preparation method and properties of series of organometallic host-guest composite materials, and belongs to the technical field of material chemistry. A reported material is taken as the raw material, and then the material is subjected to a methanol pretreatment. After the pretreatment, the material is made to carry out reactions with guest materials namely tetrathiafulvalene (TTF), 7,7,8,8-tetracyanoquinodimethane (TCNQ), 1,1'-dimethyl-4,4'-dichlorodipyridyl onium (MV2+), N,N,N,N-tetramethyl-p-phenylenediamine (TMPD) and azobenzene. The colorless processed material turns into a red color, a green color, a grey color, a purple color, and an orange-yellow color when being dipped into TTF, TCNQ, MV2+, TMPD, and ABZ respectively. Through carrying out element and thermo-gravimetric analysis, it is found that 2 TTF, 6 TCNQ, 3.5 MV2+, 1 TMPD, and 2.5 ABZ enter the hollow material. The preparation is simple and easy to operate, and the cost is low.
Description
Technical field
The invention belongs to material chemistry technical field, the preparation and the thermogravimetric that are specifically related to a series of host-guest composite materials characterize.
Background technology
In recent years, host-guest composite material was the focus of Organometallic scholar and material supply section scholar research.Macroscopic void material, because it is in absorption, separates the potential application of the aspects such as catalysis and useful for drug delivery and receiving much concern.The guest molecule that has specific function is obtained to the dream that multi-functional material is scientist together with macroscopic void Material cladding.2004, hexanaphthene was processed the metallo organic material of macroscopic void for Fujita seminar, after by oil of mirbane, naphthalene, anthracene successfully parcel enters this material, and obtains structure.2007, Jaheon Kim seminar prepares the terbium metal organic compound of hole diameter 3.9nm and 4.7nm, when holding structure is complete, at 100 DEG C, the ferrocene of easily distillation is successfully wrapped up and enters this material, overcome macroscopic void, high-specific surface area material is unsettled shortcoming in air.2011, Shengqian Ma seminar successfully enters terbium material by the enzyme Microperoxidase-11 parcel that is of a size of 3.3*1.7*1.1nm by biological culture, and Microperoxidase-11 enzyme demonstrates higher catalytic activity than in silica supports.2007, Koshiro Toriumi processed by chloroform and the method for soaking enters DMA parcel in organometallics.2010, it was 100lm that Tetsuro Majima seminar prepares BET specific surface
2/ g, the europium organometallics that hole diameter is 2nm, by cyanid successfully by N, N, N ', N '-tetramethyl-para-phenylene diamine (TMPD), Vermitin, 2,4,6-triphenylamine, thioanisole, triethylamine parcel enters this material, obtains having the anti-oxidant photocatalyst of size selectivity.2010, Roland A.Fischer seminar at 300 DEG C by the object N compared with macromole volume, N-bis-(2,6-3,5-dimethylphenyl)-3,4:9,10-perylene tetracarboxylic imide (DXP) parcel enters in the organometallics of macroscopic void, obtains the luminescent material of object control.2012, Jingcao Dai seminar entered methyl viologen in metallo organic material by heat packs at 85 DEG C, successfully obtains structure, and had studied the mechanism of its illumination or thermo-color.
Research shows, the method for above processing macroscopic void material or use the organic solvent that health is had to very big injury effect, or need to be heated to very high temperature, condition is harsher comparatively speaking.
Summary of the invention
For the above state of the art, technical problem to be solved by this invention is to provide a kind of reaction conditions gentleness, and preparation process is simple, with low cost, can characterize well again the method that Subjective and Objective combines simultaneously.
The technical solution used in the present invention comprises the following steps:
(1) the macroscopic void material 1 that the metal of being prepared by Jaheon Kim seminar is made a mistake is immersed in appropriate methyl alcohol three days, and in these three days, all will change methyl alcohol every day one time, to ensure that the solvent in methyl alcohol and material exchanges fully.After three days, material is put into vacuum drying oven and be heated to 70 DEG C and reduce pressure in dry, until methyl alcohol is removed completely;
(2) macroscopic void material 3.9mg tetrathiafulvalene (TTF) and 9.5mg being fully dried is put in the beaker that 6ml methylene dichloride is housed in the lump, silently places 10 days;
(3) by 4.5mg7, the macroscopic void material that 7,8,8-Tetracyanoquinodimethane (TCNQ) and 9.5mg are fully dried is put in the beaker that 6ml methylene dichloride is housed in the lump, silently places 10 days;
(4) by 6.5mg1,1 '-dimethyl-4,4 '-dichloride dipyridyl (MV
2+) and the macroscopic void material that is fully dried of 9.5mg put in the lump in the beaker that 6ml methylene dichloride is housed, silently place 10 days;
(5) by 4.9mgN, N, N ', the macroscopic void material that N '-tetramethyl-para-phenylene diamine (TMPD) and 9.5mg are fully dried is put in the beaker that 6ml methylene dichloride is housed in the lump, silently places 10 days;
(6) macroscopic void material 4.2mg nitrogen benzide (ABZ) and 9.5mg being fully dried is put in the beaker that 6ml methylene dichloride is housed in the lump, silently places 10 days;
After (7) 10 days, above-mentioned beaker being put into vacuum drying oven drying under reduced pressure a whole night finds to remove after being attached to the guest molecule showing: immerse TTF, TCNQ, MV
2+, TMPD, the colourless material of ABZ becomes respectively redness (3@MOF-1) green (2@MOF-1) grey (6@MOF-1) purple (4@MOF-1) and safran (5@MOF-1) material;
(8) above-mentioned materials is carried out to ultimate analysis and the discovery of thermogravimetric performance characterization: have respectively 2 TTF, 6 TCNQ, 3.5 MV
2+, 1 TMPD and 2.5 nitrogen benzides enter in macroscopic void material.
Compared with prior art, the invention has the advantages that: the pre-treatment solvent methanol methylene dichloride of selecting to HUMAN HEALTH without injury, treatment condition gentleness, characterizing method is simple, easy to operate, testing apparatus is simple.
Brief description of the drawings
Fig. 1 is the colour-change of gained functional materials after colourless material is processed.
Fig. 2 is the thermogravimetric performance characterization of resulting materials.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
The macroscopic void material of making a mistake taking the metal of having reported in document is raw material, the amount of being divided into is that 9mg-15mg is some part, it is carried out to pre-treatment 3-5 days with 5-10ml methyl alcohol, and drying under reduced pressure is removed methanol molecules, after by a certain amount of guest molecule tetrathiafulvalene (TTF), 7,7,8,8-four cyano quinoline methane (TCNQ), 1,1 '-dimethyl-4,4 '-dichloride dipyridyl (MV
2+), N, N, N, N-tetramethyl-para-phenylene diamine (TMPD) and nitrogen benzide (ABZ) are put into 5～10ml methylene dichloride 10-20 days with the raw material of processing, and the material obtaining is carried out to drying under reduced pressure and process 1-2 days to remove the residual guest molecule of material surface, observe and find to immerse TTF in electron microscope, TCNQ, MV
2+, TMPD, the colourless material of ABZ becomes respectively redness, green, grey, purple and safran.To material carry out ultimate analysis and around the thermogravimetric in environment characterize and find there are respectively 2 TTF, 6 TCNQ, 3.5 MV
2+, 1 TMPD and 2.5 nitrogen benzides enter in macroscopic void material.
Claims (1)
1. preparation method and the performance of the organic host-guest composite material of a series of metals, is characterized in that comprising the following steps and method:
(1) the macroscopic void material of preparation is immersed in appropriate methyl alcohol to three days, in these three days, all will change methyl alcohol every day one time, to ensure that the solvent in methyl alcohol and material exchanges fully.After three days, material put into vacuum drying oven and be heated to 70 DEG C of drying under reduced pressure, until methyl alcohol is removed completely;
(2) macroscopic void material 10-18mg tetrathiafulvalene (TTF) and 9.5mg being fully dried is put in the beaker that 6ml methylene dichloride is housed in the lump, silently places 10 days;
(3) by 10-18mg7, the macroscopic void material that 7,8,8-Tetracyanoquinodimethane (TCNQ) and 9.5mg are fully dried is put in the beaker that 6ml methylene dichloride is housed in the lump, silently places 10 days;
(4) by 10-18mg1,1 '-dimethyl-4,4 '-dichloride dipyridyl (MV
2+) and the macroscopic void material that is fully dried of 9.5mg put in the lump in the beaker that 6ml methylene dichloride is housed, silently place 10 days;
(5) by 10-18mg N, N, N, the macroscopic void material that N-tetramethyl-para-phenylene diamine (TMPD) and 9.5mg are fully dried is put in the beaker that 6ml methylene dichloride is housed in the lump, silently places 10 days;
(6) macroscopic void material 10-18mg nitrogen benzide (ABZ) and 9.5mg being fully dried is put in the beaker that 6ml methylene dichloride is housed in the lump, silently places 10 days;
After (7) 10 days, above-mentioned beaker being put into vacuum drying oven drying under reduced pressure a whole night finds to remove after being attached to the guest molecule showing: immerse TTF, TCNQ, MV
2+, TMPD, the colourless material of ABZ becomes respectively redness, green, grey, purple and safran;
(8) above-mentioned materials is carried out to ultimate analysis and the discovery of thermogravimetric performance characterization:
Raw-material ultimate analysis: C.48.2, H.2, N.7, O.16;
There are respectively 2 TTF C.47.71, H.2.01, N.6.75, O.15.42
6 TCNQ C.50.77, H.2.00, N.9.35, O.14.25
3.5 MV
2+c.48.91, H.2.31, N.7.37, O.14.70
1 TMPD C.48.66, H.2.14, N.7.20, O.15.81
2.5 ABZ C.49.64, H.2.17, N.7.41, O.15.35
Enter in macroscopic void material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109201009A (en) * | 2018-11-22 | 2019-01-15 | 天津工业大学 | Load the preparation and application of the photosensitive chromium metal organic framework porous material of azo |
| CN112390960A (en) * | 2020-10-10 | 2021-02-23 | 南京大学 | Dinitrogen coordination polymer applicable to nitrogen fixation and reduction and application thereof |
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| US20030004364A1 (en) * | 2001-04-30 | 2003-01-02 | Yaghi Omar M. | Isoreticular metal-organic frameworks, process for forming the same, and systematic design of pore size and functionality therein, with application for gas storage |
| WO2009011545A2 (en) * | 2007-07-16 | 2009-01-22 | Insilicotech Co., Ltd. | Compound or solvate thereof with mesoporous metal-organic framework |
| US20100209354A1 (en) * | 2007-10-01 | 2010-08-19 | Centre National De La Recherche Scientifique - Cnrs | Organic/inorganic hybrid nanoparticulates made from iron carboxylates |
| WO2012049451A1 (en) * | 2010-10-11 | 2012-04-19 | University Court Of The Univesrity Of St Andrews | Novel large pore metal organic frameworks |
| CN102936239A (en) * | 2012-11-16 | 2013-02-20 | 山东师范大学 | Organic ligand, metal organic frames based on Cu (I) ions, synthetic method for organic ligand and metal organic frames based on Cu (I) ions and application |
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- 2013-05-15 CN CN201310206912.XA patent/CN104164227A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030004364A1 (en) * | 2001-04-30 | 2003-01-02 | Yaghi Omar M. | Isoreticular metal-organic frameworks, process for forming the same, and systematic design of pore size and functionality therein, with application for gas storage |
| WO2009011545A2 (en) * | 2007-07-16 | 2009-01-22 | Insilicotech Co., Ltd. | Compound or solvate thereof with mesoporous metal-organic framework |
| US20100209354A1 (en) * | 2007-10-01 | 2010-08-19 | Centre National De La Recherche Scientifique - Cnrs | Organic/inorganic hybrid nanoparticulates made from iron carboxylates |
| WO2012049451A1 (en) * | 2010-10-11 | 2012-04-19 | University Court Of The Univesrity Of St Andrews | Novel large pore metal organic frameworks |
| CN102936239A (en) * | 2012-11-16 | 2013-02-20 | 山东师范大学 | Organic ligand, metal organic frames based on Cu (I) ions, synthetic method for organic ligand and metal organic frames based on Cu (I) ions and application |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109201009A (en) * | 2018-11-22 | 2019-01-15 | 天津工业大学 | Load the preparation and application of the photosensitive chromium metal organic framework porous material of azo |
| CN109201009B (en) * | 2018-11-22 | 2021-10-29 | 天津工业大学 | Preparation and application of azo-loaded photosensitive chromium metal organic framework porous material |
| CN112390960A (en) * | 2020-10-10 | 2021-02-23 | 南京大学 | Dinitrogen coordination polymer applicable to nitrogen fixation and reduction and application thereof |
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Application publication date: 20141126 |