CN104628789A - Microporous cobalt coordination polymer with broad-spectrum gas adsorption property and preparation method thereof - Google Patents
Microporous cobalt coordination polymer with broad-spectrum gas adsorption property and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a microporous cobalt coordination polymer with a broad-spectrum gas adsorption property and a preparation method thereof. The microporous cobalt coordination polymer is a compound with the following chemical formula: [Co3L2(H2O)2].(DMF)3.(H2O)4.(dioxane)2.5, wherein L is a 4,4',4''-(1,3,5-triphenoxy)tribenzoic acid anionic ligand; DMF is N,N'-dimethyl formamide; dioxane is 1,4-dioxane. The compound is prepared by adopting a solvothermal method. After free solvent molecules are removed, the microporous cobalt coordination polymer shows regular microporous ducts respectively approximate to a quadrangle and a circle in two crystallographic directions. Under normal pressure, the material has a wide stronger capacity in adsorbing nitrogen (77K), hydrogen (77K), oxygen (87K), argon (87K) and carbon dioxide (195K and 293K) and can be applied as a gas adsorption and storage material.
Description
Technical field
The present invention relates to coordination polymer material, particularly a kind of preparation of microporous cobalt ligand polymer and application thereof, described ligand polymer has the Co – 4 of pore size, 4', 4''-(1,3,5-triple phenoxyl) three phenylformic acid negatively charged ion two-dimensional network structure, to nitrogen, hydrogen, oxygen, argon gas and carbonic acid gas, all there is extensively stronger adsorptive power, can be used as absorbing and storing material by further Application and Development.
Background technology
Porous coordination polymer is a novel porous materials that class specific surface area is high, designability is strong, is subject to extensive concern (Bloch, the E. D. of each disciplinary study personnel in recent years; Hudson, M. R.; Mason, J. A.; Chavan, S.; Crocell à, V.; Howe, J. D.; Lee, K.; Dzubak, A. L.; Queen, W. L.; Zadrozny, J. M.; Geier, S. J.; Lin, L.-C.; Gagliardi, L.; Smit, B.; Neaton, J. B.; Bordiga, S.; Brown, C. M.; Long, J. R.
j. Am. Chem. Soc.2014,136,10752; Xuan, W.; Zhu, C.; Liu, Y.; Cui, Y.
chem. Soc. Rev.2012,41,1677; Zhao, X.; Bu, X.-H.; Wu, T.; Zheng, S.-T.; Wang, L.; Feng, P.-Y.
nat. Commun.2013,3,3344; He, Y.; Zhou, W.; Qian, G.; Chen, B.
chem. Soc. Rev.2014,43,5657; Dhakshinamoorthy, A.; Garcia, H.
chem. Soc. Rev.2014,43,5750 etc.).Compare with porous material with traditional inorganic zeolites, the synthesis condition of Porous coordination polymer is gentleer, good crystallinity, determines its accurate structural by X-ray single crystal diffraction technology, and the dependency further between its structure and fuction of research.In addition, the species of metal ion that can be used for constructing ligand polymer is enriched, and organic ligand various structures, therefore the designability of such material is very strong.These construction units of rational selection can assemble the various Porous coordination polymer of pore size size and shape.
Nearly ten years, scientist has prepared a large amount of ligand polymer based on carboxylic-acid part, and the Porous coordination polymer wherein formed by fixed tripod class Carboxylic acid ligand and metal ion shows good performance (Furukawa, H.; Go, Y.; Ko, N.; Park, Y. K.; Uribe-Romo, F. J.; Kim, J.; O ' Keeffe, M.; Yaghi, O. M.
inorg. Chem.2011,50,9147; Suh, M. P.; Choi, H. J.; So, S. M.; Kim, B. M.
inorg. Chem.2003,42,676; Chae, H. K.; Siberio-P é rez, D. Y.; Kim, J.; Go, Y.; Eddaoudi, M.; Matzger, A. J.; O ' Keeffe, M.; O. M. Yaghi,
nature2004,427,523; Lin, Q.; Wu, T.; Bu, X.; Feng, P.
dalton Trans.2012,41,3620; Lin, Z.; Zou, R.; Liang, J.; Xia, W.; Xia, D.; Wang, Y.; Lin, J.; Hu, T.; Chen, Q.; Wang, X.; Zhao, Y.; Burrell, A. K.
j. Mater. Chem.2012,22,7813 etc.).But, report then relatively less (Du, the M. of the Porous coordination polymer that flexible tripod type Carboxylic acid ligand is constructed; Chen, M.; Yang, X.-G.; Wen, J.; Wang, X.; Fang, S.-M.; Liu, C.-S.
j. Mater. Chem. A 2014,2,9828; Zhang, M.-D.; Di, C.-M.; Zheng, H.-G.Inorg. Chem. Commun.2013,27,88; Lin, X.-M.; Li, T.-T.; Wang, Y.-W.; Zhang, L.; Su, C.-Y.
chem. Asian J., and the hole size of this kind of material and shape are more easily by regulating and controlling, therefore in gas adsorption storage, have significant application value 2012,7,2796).
Summary of the invention
A kind of preparation method and application thereof of microporous cobalt ligand polymer are the object of the present invention is to provide.
For achieving the above object, the technical solution used in the present invention is as follows:
Microporous cobalt ligand polymer of the present invention, this compound has following chemical formula [Co
3l
2(H
2o)
2] (DMF)
3(H
2o)
4(dioxane)
2.5, wherein L=4,4', 4''-(1,3,5-triple phenoxyl) and three phenylformic acid anion ligands, DMF=N, N '-dimethyl methane amide, dioxane=Isosorbide-5-Nitrae-dioxane, the skeleton symbol of L is as follows:
The crystallization of described microporous cobalt ligand polymer is in trigonal system (Trigonal), and spacer is
r-3
c, unit cell parameters is
a=
b=17.4310 (11),
c=48.043 (5),
v=12641.7 (17)
3.
The basic structure of described compound is a two-dimensional network, one of them Co not with six oxygen atom ligands from six carboxyls, another Co and three carboxyl oxygen atom and a water molecule coordination; Ligand L and cobalt (II) ion are connected to form two-dimensional double-layer kgd type network by coordinate bond, on crystallography c direction between two-dimensional layer with (ABCDEF)
n after pattern is piled up, show approximate tetragon and circular regular micropore canals in the two directions respectively, in duct, be filled with solvent DMF, water and Isosorbide-5-Nitrae-dioxane molecule.
The preparation method with the microporous cobalt ligand polymer of wide spectrum gas adsorption performance of the present invention: under hydrothermal conditions, by 4,4', 4''-(1,3,5-triple phenoxyl) three phenylformic acid and cobalt salt be dissolved in DMF and Isosorbide-5-Nitrae-dioxane mixed solvent, this solution enclosed the hydrothermal reaction kettle of 25 mL, the temperature of 100 ~ 140 DEG C is warming up to the speed of 10 degrees Celsius per hour, maintain this temperature 3 days, be then naturally down to room temperature, namely obtain the purple column product of single crystal of this compound.
Described 4,4', 4''-(1,3,5-triple phenoxyl) three phenylformic acid parts are dissolved in DMF and Isosorbide-5-Nitrae-dioxane mixed solvent, and the volume ratio of DMF and Isosorbide-5-Nitrae-dioxane is 1:1, and making strength of solution is 0.02 ~ 0.20 mol L
– 1.
Described cobalt salt is cobalt chloride, and the volume ratio being dissolved in DMF and Isosorbide-5-Nitrae-dioxane in DMF and Isosorbide-5-Nitrae-dioxane mixed solvent is 1:1, and making strength of solution is 0.04 ~ 0.40 mol L
-1.
Ligand polymer provided by the invention gas adsorption experiment show, this compound can under normal pressure and differing temps absorption nitrogen, hydrogen, argon gas, oxygen and carbon dioxide.The energy and environment are two large hot issues of society.The day by day exhaustion of the with serious pollution natural energy source such as oil and coal, taps a new source of energy significant.And hydrogen energy source is because its pollution-free, reproducible advantage is considered to a kind of up-and-coming green novel energy source.But, hydrogen store safely and effectively be current hydrogen energy source universal in one of problem, and porous organo-metallic skeleton material has handiness functionally and good performance, is expected to become rare structured material that can meet above-mentioned all practical applications.Microporous coordination polymer provided by the present invention can be used as potential gas adsorption storage medium, has broad application prospects in Materials science and association area.
Accompanying drawing explanation
The coordination environment figure of cobalt (II) in Fig. 1 microporous cobalt ligand polymer;
The two-dimensional double-layer structural representation of Fig. 2 microporous cobalt ligand polymer;
The network topology schematic diagram of Fig. 3 microporous cobalt ligand polymer;
The one-dimensional channels schematic diagram of Fig. 4 microporous cobalt ligand polymer;
The Adsorption Isotherms of Fig. 5 microporous cobalt ligand polymer under 77 K;
The Adsorption Isotherms of Fig. 6 microporous cobalt ligand polymer under 87 K;
The Adsorption Isotherms of Fig. 7 microporous cobalt ligand polymer under 195 K;
The Adsorption Isotherms of Fig. 8 microporous cobalt ligand polymer under 293 K.
Embodiment
Microporous cobalt ligand polymer of the present invention, it is characterized in that described compound crystal is in trigonal system (Trigonal), spacer is
r-3
c, unit cell parameters is
a=
b=17.4310 (11),
c=48.043 (5),
v=12641.7 (17)
3.Basic structure is a two-dimensional network, comprises two crystallography independently cobalt (II) ion (occupation rate is respectively 1/3 and 1/6), 1/3 L part and 1/3 water molecules in its Asymmetry coordination unit.Wherein Co1 respectively with six oxygen atom ligands from six carboxyls, in octahedral coordination configuration, and Co2 and three carboxyl oxygen atom and a water molecule coordination, in tetrahedral coordination configuration.Ligand L and cobalt ion are connected to form two-dimensional double-layer kgd type network by coordinate bond, on crystallography c direction between two-dimensional layer with (ABCDEF)
n after pattern is piled up, show approximate tetragon and circular regular micropore canals in the two directions respectively, in duct, be filled with solvent DMF, water and Isosorbide-5-Nitrae-dioxane molecule.
In the preparation method of microporous cobalt ligand polymer of the present invention, 4,4', 4''-(1,3,5-triple phenoxyl) three phenylformic acid parts are dissolved in N, and in N '-dimethyl methane amide and Isosorbide-5-Nitrae-dioxane mixed solvent, making strength of solution is 0.02 ~ 0.20 mol L
– 1; Cobalt salts is dissolved in N, and in N '-dimethyl methane amide and Isosorbide-5-Nitrae-dioxane mixed solvent, the strength of solution made is 0.04 ~ 0.40 mol L
-1; Reaction conditions is that constant temperature drops to room temperature in 3 days afterwards naturally at 100 ~ 140 DEG C.
The preparation of embodiment 1 microporous cobalt ligand polymer
By 4,4', 4''-(1,3,5-triple phenoxyl) three phenylformic acid (0.1 mmol, 48.6 mg) and cobalt chloride (0.2 mmol, 47.6 mg) be dissolved in N, in N '-dimethyl methane amide (2 mL) and Isosorbide-5-Nitrae-dioxane (2 mL) mixed solvent, enclose the hydrothermal reaction kettle of 25 mL.Again reaction mixture is heated to 120 DEG C with 10 DEG C of intensifications per hour, maintain this temperature 3 days, be then down to room temperature, can obtain purple styloid, productive rate is about 40%.Main infrared absorption peak is: 3444m, 1594vs, 1557m, 1504m, 1463m, 1391vs, 1223w, 1157m, 1119m, 1006m, 872w, 780w, 707w, 647w, 408w.
The preparation of embodiment 2 microporous cobalt ligand polymer
By 4,4', 4''-(1,3,5-triple phenoxyl) three phenylformic acid (0.1 mmol, 48.6 mg) and cobalt chloride (0.2 mmol, 47.6 mg) be dissolved in N, in N '-dimethyl methane amide (2 mL) and Isosorbide-5-Nitrae-dioxane (3 mL) mixed solvent, enclose the hydrothermal reaction kettle of 25 mL.Again reaction mixture is heated to 100 DEG C with 10 DEG C of intensifications per hour, maintain this temperature 3 days, be then down to room temperature, can obtain purple styloid, productive rate is about 30%.Main infrared absorption peak is: 3444m, 1594vs, 1557m, 1504m, 1463m, 1391vs, 1223w, 1157m, 1119m, 1006m, 872w, 780w, 707w, 647w, 408w.
The preparation of embodiment 3 microporous cobalt ligand polymer
By 4,4', 4''-(1,3,5-triple phenoxyl) three phenylformic acid (0.8 mmol, 388.8 mg) and cobalt chloride (1.6mmol, 380.8 mg) be dissolved in N, in N '-dimethyl methane amide (2 mL) and Isosorbide-5-Nitrae-dioxane (2 mL) mixed solvent, enclose the hydrothermal reaction kettle of 25 mL.Again reaction mixture is heated to 140 DEG C with 10 DEG C of intensifications per hour, maintain this temperature 3 days, be then down to room temperature, can obtain purple styloid, productive rate is about 35%.Main infrared absorption peak is: 3444m, 1594vs, 1557m, 1504m, 1463m, 1391vs, 1223w, 1157m, 1119m, 1006m, 872w, 780w, 707w, 647w, 408w.
The preparation of embodiment 4 microporous cobalt ligand polymer
By 4,4', 4''-(1,3,5-triple phenoxyl) three phenylformic acid (1 mmol, 486 mg) and cobalt chloride (0.2 mmol, 47.6 mg) be dissolved in N, in N '-dimethyl methane amide (5 mL) and Isosorbide-5-Nitrae-dioxane (5 mL) mixed solvent, enclose the hydrothermal reaction kettle of 25 mL.Again reaction mixture is heated to 110 DEG C with 10 DEG C of intensifications per hour, maintain this temperature 3 days, be then down to room temperature, can obtain purple styloid, productive rate is about 40%.Main infrared absorption peak is: 3444m, 1594vs, 1557m, 1504m, 1463m, 1391vs, 1223w, 1157m, 1119m, 1006m, 872w, 780w, 707w, 647w, 408w.
The preparation of embodiment 5 microporous cobalt ligand polymer
By 4,4', 4''-(1,3,5-triple phenoxyl) three phenylformic acid (0.1 mmol, 48.6 mg) and cobalt chloride (2 mmol, 476 mg) be dissolved in N, in N '-dimethyl methane amide (5 mL) and Isosorbide-5-Nitrae-dioxane (5 mL) mixed solvent, enclose the hydrothermal reaction kettle of 25 mL.Again reaction mixture is heated to 130 DEG C with 10 DEG C of intensifications per hour, maintain this temperature 3 days, be then down to room temperature, can obtain purple styloid, productive rate is about 40%.Main infrared absorption peak is: 3444m, 1594vs, 1557m, 1504m, 1463m, 1391vs, 1223w, 1157m, 1119m, 1006m, 872w, 780w, 707w, 647w, 408w.
The preparation of embodiment 6 microporous cobalt ligand polymer
By 4,4', 4''-(1,3,5-triple phenoxyl) three phenylformic acid (2mmol, 972 mg) and cobalt chloride (2 mmol, 476 mg) be dissolved in N, in N '-dimethyl methane amide (5 mL) and Isosorbide-5-Nitrae-dioxane (5 mL) mixed solvent, enclose the hydrothermal reaction kettle of 25 mL.Again reaction mixture is heated to 115 DEG C with 10 DEG C of intensifications per hour, maintain this temperature 3 days, be then down to room temperature, can obtain purple styloid, productive rate is about 40%.Main infrared absorption peak is: 3444m, 1594vs, 1557m, 1504m, 1463m, 1391vs, 1223w, 1157m, 1119m, 1006m, 872w, 780w, 707w, 647w, 408w.
In Example 1, gained microporous cobalt ligand polymer characterizes further, and its process is as follows:
(1) crystal structure determination of microporous cobalt ligand polymer
Under polarizing microscope, choose the monocrystalline of suitable size, at room temperature carry out the experiment of X-ray single crystal diffraction.With the Mo – K through graphite monochromator monochromatization
aray (
l=0.71073), Yi φ – ω mode collects diffraction data.Reduction of data is carried out by CrysAlisPro program.Structure elucidation uses SHELXTL program to complete.First determine whole non-hydrogen atom coordinate by difference functions method and method of least squares, and obtain the hydrogen atom position of main body framework with theoretical hydrogenation method, then by method of least squares, refine is carried out to crystalline structure.Detailed axonometry data are in table 1, and important bond distance and bond angle data are in table 2.Crystalline structure is shown in Fig. 1 ~ 4.
table 1the predominant crystal data of microporous cobalt ligand polymer
a R 1= Σ||
F o| – |
F c||/Σ|
F o|.
b wR 2= |Σ
w(|
F o|
2 – |
F c|
2)|/Σ|
w(
F o)
2|
1/2, where
w = 1/[
s 2(
F o 2) + (
aP)
2+
bP].
P= (
F o 2+ 2
F c 2)/3.
table 2main bond distance's () of microporous cobalt ligand polymer and bond angle [°] *
* symmetrical code: #1=–
x+
y+ 1 ， –
x+ 1,
z; #2=–
y+ 1,
x–
y,
z; #3=–
x+ 4/3 ， –
x+
y+ 2/3 ， –
z+ 1/6
(2) the gas adsorption performance research of microporous cobalt ligand polymer
The full-automatic specific surface area of Micromeritics 3Flex that gas adsorption experiment at all temperature uses Micromeritics Instrument Corp. U.S.A to produce and lacunarity analysis instrument apparatus complete.Use high-purity gas, about 100 mg samples have been recycled all tests.The results are shown in Figure 5 ~ 8.
Above embodiment is only for illustration of content of the present invention, and in addition, the present invention also has other embodiment.But all employings are equal to replacement or the technical scheme that formed of equivalent deformation mode all drops in protection scope of the present invention.
Claims (5)
1. there is a microporous cobalt ligand polymer for wide spectrum gas adsorption performance, it is characterized in that described ligand polymer has following chemical formula: [Co
3l
2(H
2o)
2] (DMF)
3(H
2o)
4(dioxane)
2.5, wherein L=4,4', 4''-(1,3,5-triple phenoxyl) and three phenylformic acid anion ligands, DMF=N, N '-dimethyl methane amide, dioxane=Isosorbide-5-Nitrae-dioxane, the skeleton symbol of L is as follows:
Described ligand polymer crystallization is in trigonal system (Trigonal), and spacer is
r-3
c, unit cell parameters is
a=
b=17.4310 (11),
c=48.043 (5),
v=12641.7 (17)
3.
2. there is the microporous cobalt ligand polymer of wide spectrum gas adsorption performance as claimed in claim 1, it is characterized in that the basic structure of described compound is a two-dimensional network, one of them Co not with six oxygen atom ligands from six carboxyls, another Co and three carboxyl oxygen atom and a water molecule coordination; Ligand L and cobalt (II) ion are connected to form two-dimensional double-layer kgd type network by coordinate bond, on crystallography c direction between two-dimensional layer with (ABCDEF)
n after pattern is piled up, show approximate tetragon and circular regular micropore canals in the two directions respectively, in duct, be filled with solvent DMF, water and Isosorbide-5-Nitrae-dioxane molecule.
3. the preparation method with the microporous cobalt ligand polymer of wide spectrum gas adsorption performance according to claim 1, it is characterized in that: under hydrothermal conditions, by 4,4', 4''-(1,3,5-triple phenoxyl) three phenylformic acid and cobalt salt be dissolved in DMF and 1, in 4-dioxane mixed solvent, this solution is enclosed the hydrothermal reaction kettle of 25 mL, be warming up to the temperature of 100 ~ 140 DEG C with the speed of 10 degrees Celsius per hour, maintain this temperature 3 days, then be naturally down to room temperature, namely obtain the purple column product of single crystal of this compound.
4. there is the preparation method of the microporous cobalt ligand polymer of wide spectrum gas adsorption performance as claimed in claim 3, it is characterized in that: 4,4', 4''-(1,3,5-triple phenoxyl) three phenylformic acid parts are dissolved in DMF and 1, in 4-dioxane mixed solvent, the volume ratio of DMF and Isosorbide-5-Nitrae-dioxane is 1:1, and making strength of solution is 0.02 ~ 0.20 mol L
– 1.
5. there is the preparation method of the microporous cobalt ligand polymer of wide spectrum gas adsorption performance as claimed in claim 3, it is characterized in that: described cobalt salt is cobalt chloride, be dissolved in DMF and 1, DMF and 1 in 4-dioxane mixed solvent, the volume ratio of 4-dioxane is 1:1, and making strength of solution is 0.04 ~ 0.40 mol L
-1.
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Cited By (4)
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| CN106243159A (en) * | 2016-07-13 | 2016-12-21 | 郑州轻工业学院 | Porous cobalt-based organic-inorganic hybrid material and its preparation method and application |
| CN107226913A (en) * | 2017-06-28 | 2017-10-03 | 江汉大学 | A kind of framework complex material using four core cobalts as node and preparation method thereof |
| CN109433159A (en) * | 2018-10-25 | 2019-03-08 | 陕西科技大学 | A kind of cobalt coordination polymer iodine vapor support materials and its preparation method and application |
| CN112915982A (en) * | 2021-01-29 | 2021-06-08 | 兰州大学 | Synthetic method and application of cobalt-containing polymer uranyl ion adsorbent |
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| CN103864607A (en) * | 2014-03-21 | 2014-06-18 | 天津师范大学 | Preparation method and application of mesoporous metal-organic framework material with high stability |
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| CN103864607A (en) * | 2014-03-21 | 2014-06-18 | 天津师范大学 | Preparation method and application of mesoporous metal-organic framework material with high stability |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106243159A (en) * | 2016-07-13 | 2016-12-21 | 郑州轻工业学院 | Porous cobalt-based organic-inorganic hybrid material and its preparation method and application |
| CN106243159B (en) * | 2016-07-13 | 2019-02-26 | 郑州轻工业学院 | Porous cobalt-based organic-inorganic hybrid material and its preparation method and application |
| CN107226913A (en) * | 2017-06-28 | 2017-10-03 | 江汉大学 | A kind of framework complex material using four core cobalts as node and preparation method thereof |
| CN107226913B (en) * | 2017-06-28 | 2021-03-09 | 江汉大学 | Frame coordination material with tetranuclear cobalt as node and preparation method thereof |
| CN109433159A (en) * | 2018-10-25 | 2019-03-08 | 陕西科技大学 | A kind of cobalt coordination polymer iodine vapor support materials and its preparation method and application |
| CN109433159B (en) * | 2018-10-25 | 2021-05-18 | 陕西科技大学 | Cobalt coordination polymer iodine vapor load material and preparation method and application thereof |
| CN112915982A (en) * | 2021-01-29 | 2021-06-08 | 兰州大学 | Synthetic method and application of cobalt-containing polymer uranyl ion adsorbent |
| CN112915982B (en) * | 2021-01-29 | 2022-04-29 | 兰州大学 | Synthetic method and application of cobalt-containing polymer uranyl ion adsorbent |
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