CN109503669A - 5- 4,4 '-bipyridyl of amino isophthalic acid cobalt complex and preparation method - Google Patents
5- 4,4 '-bipyridyl of amino isophthalic acid cobalt complex and preparation method Download PDFInfo
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- CN109503669A CN109503669A CN201811303818.5A CN201811303818A CN109503669A CN 109503669 A CN109503669 A CN 109503669A CN 201811303818 A CN201811303818 A CN 201811303818A CN 109503669 A CN109503669 A CN 109503669A
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- Prior art keywords
- isophthalic acid
- amino isophthalic
- amino
- ion
- complex
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- -1 amino isophthalic acid cobalt Chemical compound 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 238000010668 complexation reaction Methods 0.000 title abstract description 4
- KBZFDRWPMZESDI-UHFFFAOYSA-N 5-aminobenzene-1,3-dicarboxylic acid Chemical compound NC1=CC(C(O)=O)=CC(C(O)=O)=C1 KBZFDRWPMZESDI-UHFFFAOYSA-N 0.000 claims abstract description 20
- 150000002500 ions Chemical class 0.000 claims abstract description 14
- MWVTWFVJZLCBMC-UHFFFAOYSA-N 4,4'-bipyridine Chemical compound C1=NC=CC(C=2C=CN=CC=2)=C1 MWVTWFVJZLCBMC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 7
- OQUOOEBLAKQCOP-UHFFFAOYSA-N nitric acid;hexahydrate Chemical compound O.O.O.O.O.O.O[N+]([O-])=O OQUOOEBLAKQCOP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 16
- 239000012153 distilled water Substances 0.000 claims description 12
- 150000001450 anions Chemical class 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- 229910020647 Co-O Inorganic materials 0.000 claims description 3
- 229910020676 Co—N Inorganic materials 0.000 claims description 3
- 229910020704 Co—O Inorganic materials 0.000 claims description 3
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 3
- 150000001455 metallic ions Chemical class 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- 150000003233 pyrroles Chemical class 0.000 claims description 2
- 150000005838 radical anions Chemical class 0.000 claims description 2
- 150000005837 radical ions Chemical class 0.000 claims description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims 1
- 239000003446 ligand Substances 0.000 abstract description 3
- 229910021645 metal ion Inorganic materials 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 3
- 229910052723 transition metal Inorganic materials 0.000 abstract description 3
- 150000003624 transition metals Chemical class 0.000 abstract description 3
- 150000004700 cobalt complex Chemical class 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 239000013256 coordination polymer Substances 0.000 description 3
- 229920001795 coordination polymer Polymers 0.000 description 3
- LDOMKUVUXZRECL-UHFFFAOYSA-N 2-aminobenzene-1,3-dicarboxylic acid Chemical compound NC1=C(C(O)=O)C=CC=C1C(O)=O LDOMKUVUXZRECL-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- WEOQCZRNQSXTCE-UHFFFAOYSA-N [Co].N1=CC=C(C=C1)C1=CC=NC=C1 Chemical compound [Co].N1=CC=C(C=C1)C1=CC=NC=C1 WEOQCZRNQSXTCE-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229930002839 ionone Natural products 0.000 description 1
- 150000002499 ionone derivatives Chemical class 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table
- C07F15/06—Cobalt compounds
- C07F15/065—Cobalt compounds without a metal-carbon linkage
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyridine Compounds (AREA)
Abstract
The invention discloses 5- 4,4 '-bipyridyl of amino isophthalic acid cobalt complex and preparation methods.The complex belongs to monoclinic system, and space group isP21/c.In the complex, amino and carboxyl on 5- amino isophthalic acid is with monodentate, the form and metal ion Co (II) ion coordination of bidentate chelating, 4,4 '-bipyridyls in the form of bidentate bridging with Metal Ions Cd (II) ion coordination, constituting the three-dimensional netted space structure of the complex by way of the multiple tooth bridging of 5- amino isophthalic acid and 4,4'-Bipyridine and center Co (II) ion.The present invention utilizes 5- amino isophthalic acid, 4,4 '-bipyridyls obtain cobalt complex by hydro-thermal method for ligand and cabaltous nitrate hexahydrate, have many advantages, such as simple process, low in cost, reproducible, provides certain foundation to synthesize the complex of transition metal.
Description
Technical field
The invention belongs to complex preparation technical field, in particular to a kind of 5- amino isophthalic acid 4,4'-Bipyridine
Cobalt complex and preparation method.
Background technique
The diversity of coordination polymer structure and in molecular sieve, catalysis, nonlinear optics, magnetic material and biosensor
Etc. potential application foreground, so that the synthesis of coordination polymer and research is become very active domain variability in supramolecular chemistry
Achieve progress at full speed.It is reasonable that organic ligand and metal ion is selected to be assembled for the design of Ideal Topology structure
Crystal to obtain having desired structure is still an arduous and challenging job, as 5- amino isophthalic acid is
There are many functional groups for a kind of band, are the good ligands for constructing novel coordination polymer.In addition, 4,4'-Bipyridine has intramolecular
It is conjugated big pi bond, product can be measured as highly effective chromophore, and there is good intramolecular electron transmission and energy
Measure hereditary property, it is possible to as good assistant ligand.Transition metal Co, 5- amino isophthalic acid and 4,4 '-connection pyrroles
There are rich and varied structures for the complex that pyridine is formed, and get a good eye meaning for the complex of design synthesis object construction.
Summary of the invention
Space group isP21/ c, central metallic ions are Co (II) ion.In the complex, minimum structural unit packet
Containing Co (II) ion, a 5- amino isophthalic acid root anion, half of 4,4'-Bipyridine neutral molecule, one is matched
Position hydrone and two dissociating water molecules.Center Co1 ion one with a 5- amino isophthalic acid root anion respectively
The oxygen atom (O2) of carboxyl is coordinated in the form of monodentate, a carboxyl with another 5- amino isophthalic acid radical ion
The form coordination that (O3A, O4A) is chelated with bidentate, also an amino (N1B) with a 5- amino isophthalic acid root anion
It is coordinated in the form of monodentate, and is coordinated with a hydrone (O5), form the octoploids structure of hexa-coordinate.O2,O3A,O4A,
N2 occupies equatorial plane, and O5, N1B occupy axial direction.Pass through 5- amino isophthalic acid and 4,4 '-bipyridyls and center Co
(II) mode of the multiple tooth bridging of ion constitutes the three-dimensional netted space structure of the complex.The average bond length of Co-O is
The average bond length of 2.165, Co-N is 2.129.
The 5- amino isophthalic acid 4,4 '-bipyridyl cobalt complex the preparation method comprises the following steps:
(1) it weighs 0.2 ~ 0.5 mM of cabaltous nitrate hexahydrate to be dissolved in 3 ~ 5 milliliters of distilled water, it is molten that cobalt nitrate is made
Liquid.
(2) it weighs 0.2 ~ 0.5 mM of 5- amino isophthalic acid to be dissolved in 3 ~ 5 milliliters of distilled water, 5- is made
Amino isophthalic acid solution.
(3) it weighs 0.2 ~ 0.5 mM of 4,4'-Bipyridine to be dissolved in 3 ~ 5 milliliters of distilled water, is made 4,4 '-
Bipyridyl solution.
(4) it weighs 0.4 ~ 1 mM of potassium hydroxide to be dissolved in 1 ~ 2 milliliter of distilled water, it is molten that potassium hydroxide is made
Liquid.
(5) solution made from step (1), (2), (3) and (4) is added in ptfe autoclave liner, is put on
Stainless steel cauldron housing is put into 170 degrees Celsius and reacts 48 ~ 72 hours, is down to after the reaction was completed with 10 degrees Celsius of gradients per hour
Room temperature opens kettle after standing 24 hours, filters to obtain red acicular crystal, as 5- amino isophthalic acid 4,4'-Bipyridine cobalt is matched
Close object.
The present invention has many advantages, such as simple process, low in cost, reproducible, has successfully synthesized 5- amino isophthalic diformazan
Sour 4,4'-Bipyridine cobalt complex provides certain foundation to synthesize the complex of transition metal.
Detailed description of the invention
Fig. 1 is 5- amino isophthalic acid 4,4 '-bipyridyl cobalt complex molecular structure of the invention.
Specific embodiment
Embodiment:
(1) it weighs 0.2 mM of (0.0582 gram) cabaltous nitrate hexahydrate to be dissolved in 3 milliliters of distilled water, it is molten that cobalt nitrate is made
Liquid.
(2) it weighs 0.2 mM of (0.0362 gram) 5- amino isophthalic acid to be dissolved in 5 milliliters of distilled water, 5- is made
Amino isophthalic acid solution.
(3) it weighs 0.2 mM of (0.0312 gram) 4,4'-Bipyridine to be dissolved in 5 milliliters of distilled water, is made 4,4 '-
Bipyridyl solution.
(4) it weighs 0.4 mM of (0.0224 gram) potassium hydroxide to be dissolved in 2 milliliters of distilled water, it is molten that potassium hydroxide is made
Liquid.
(5) solution made from step (1), (2), (3) and (4) is added in ptfe autoclave liner, is put on
Stainless steel cauldron housing is put into 170 degrees Celsius and reacts 48 hours, is down to room after the reaction was completed with 10 degrees Celsius of gradients per hour
Temperature opens kettle after standing 24 hours, filters to obtain red acicular crystal, and as 5- amino isophthalic acid 4,4'-Bipyridine cobalt cooperates
Object.
The complex belongs to monoclinic system, space group P21/c, and central metallic ions are Co (II) ion.In the cooperation
In object, minimum structural unit include Co (II) ion, a 5- amino isophthalic acid root anion, half 4,4 '-
Bipyridyl neutral molecule, a water of coordination molecule and two dissociating water molecules.Center Co1 ion respectively with a 5- amino isophthalic
The oxygen atom (O2) of one carboxyl of diformazan acid radical anion is coordinated in the form of monodentate, with another 5- amino isophthalic acid
The form coordination that one carboxyl (O3A, O4A) of radical ion is chelated with bidentate, also with a 5- amino isophthalic acid root yin from
One amino (N1B) of son is coordinated in the form of monodentate, and is coordinated with a hydrone (O5), and the octahedron of hexa-coordinate is formd
Configuration.O2, O3A, O4A, N2 occupy equatorial plane, and O5, N1B occupy axial direction.By 5- amino isophthalic acid and 4,
The mode of the multiple tooth bridging of 4 '-bipyridyls and center Co (II) ion constitutes the three-dimensional netted space structure of the complex.
The average bond length that the average bond length of Co-O is 2.165, Co-N is 2.129.
Claims (2)
1. a kind of 5- amino isophthalic acid 4,4 '-bipyridyl cobalt complex, it is characterised in that 5- amino isophthalic acid 4,
4 '-bipyridyl cobalt complexes belong to monoclinic system, and space group isP21/ c, central metallic ions are Co (II) ion;In the cooperation
In object, minimum structural unit include Co (II) ion, a 5- amino isophthalic acid root anion, half 4,4 '-
Bipyridyl neutral molecule, a water of coordination molecule and two dissociating water molecules;Center Co1 ion respectively with a 5- amino isophthalic
Oxygen atom, that is, O2 of one carboxyl of diformazan acid radical anion is coordinated in the form of monodentate, with another 5- amino isophthalic acid
The form coordination that carboxyl, that is, O3A, O4A for radical ion is chelated with bidentate, also with a 5- amino isophthalic acid root yin from
One amino, that is, N1B of son is coordinated in the form of monodentate, and is coordinated with a hydrone, that is, O5, and the octahedron of hexa-coordinate is formd
Configuration;O2, O3A, O4A, N2 occupy equatorial plane, and O5, N1B occupy axial direction;By 5- amino isophthalic acid and 4,
The mode of the multiple tooth bridging of 4 '-bipyridyls and center Co (II) ion constitutes the three-dimensional netted space structure of the complex;
The average bond length that the average bond length of Co-O is 2.165, Co-N is 2.129.
2. the preparation method of 5- amino isophthalic acid 4,4'-Bipyridine cobalt complex according to claim 1, special
Sign be the specific steps are that:
(1) it weighs 0.2 ~ 0.5 mM of cabaltous nitrate hexahydrate to be dissolved in 3 ~ 5 milliliters of distilled water, it is molten that cobalt nitrate is made
Liquid；
(2) it weighs 0.2 ~ 0.5 mM of 5- amino isophthalic acid to be dissolved in 3 ~ 5 milliliters of distilled water, 5- amino is made
M-phthalic acid solution；
(3) it weighs 0.2 ~ 0.5 mM of 4,4'-Bipyridine to be dissolved in 3 ~ 5 milliliters of distilled water, 4,4 '-connection pyrroles is made
Pyridine solution；
(4) it weighs 0.4 ~ 1 mM of potassium hydroxide to be dissolved in 1 ~ 2 milliliter of distilled water, potassium hydroxide solution is made；
(5) solution made from step (1), (2), (3) and (4) is added in ptfe autoclave liner, is put on stainless
Steel reaction kettle housing is put into 170 degrees Celsius and reacts 48 ~ 72 hours, is down to room after the reaction was completed with 10 degrees Celsius of gradients per hour
Temperature opens kettle after standing 24 hours, filters to obtain red acicular crystal, and as 5- amino isophthalic acid 4,4'-Bipyridine cobalt cooperates
Object.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112604517A (en) * | 2020-11-26 | 2021-04-06 | 连云港鹏辰特种新材料有限公司 | Preparation of inorganic-organic composite gel membrane and application thereof in separation of hydrocarbon mixture |
| CN113185439A (en) * | 2021-05-11 | 2021-07-30 | 合肥工业大学 | V-shaped chiral carboxylic acid ligand, preparation method and application thereof |
| CN116178737A (en) * | 2022-07-16 | 2023-05-30 | 延安大学 | Cadmium metal coordination polymer and preparation method and application thereof |
-
2018
- 2018-11-03 CN CN201811303818.5A patent/CN109503669A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112604517A (en) * | 2020-11-26 | 2021-04-06 | 连云港鹏辰特种新材料有限公司 | Preparation of inorganic-organic composite gel membrane and application thereof in separation of hydrocarbon mixture |
| CN113185439A (en) * | 2021-05-11 | 2021-07-30 | 合肥工业大学 | V-shaped chiral carboxylic acid ligand, preparation method and application thereof |
| CN113185439B (en) * | 2021-05-11 | 2024-03-12 | 合肥工业大学 | V-shaped chiral carboxylic acid ligand, preparation method and application thereof |
| CN116178737A (en) * | 2022-07-16 | 2023-05-30 | 延安大学 | Cadmium metal coordination polymer and preparation method and application thereof |
| CN116178737B (en) * | 2022-07-16 | 2024-05-07 | 延安大学 | Cadmium metal coordination polymer and preparation method and application thereof |
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Application publication date: 20190322 |