CN109336933A - 5- amino isophthalic acid nickel complex and preparation method - Google Patents
5- amino isophthalic acid nickel complex and preparation method Download PDFInfo
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- CN109336933A CN109336933A CN201811303808.1A CN201811303808A CN109336933A CN 109336933 A CN109336933 A CN 109336933A CN 201811303808 A CN201811303808 A CN 201811303808A CN 109336933 A CN109336933 A CN 109336933A
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- CN
- China
- Prior art keywords
- isophthalic acid
- amino isophthalic
- amino
- complex
- ion
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- -1 5- amino isophthalic acid nickel Chemical compound 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 238000010668 complexation reaction Methods 0.000 title abstract description 3
- 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 22
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 17
- 150000002500 ions Chemical class 0.000 claims abstract description 15
- 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
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 8
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 7
- 230000036571 hydration Effects 0.000 claims abstract description 5
- 238000006703 hydration reaction Methods 0.000 claims abstract description 5
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000012153 distilled water Substances 0.000 claims description 12
- 150000001450 anions Chemical class 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 229910018553 Ni—O 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
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims 1
- 150000003233 pyrroles Chemical class 0.000 claims 1
- 239000003643 water by type Substances 0.000 claims 1
- 229910052759 nickel Inorganic materials 0.000 abstract description 4
- 229910052723 transition metal Inorganic materials 0.000 abstract description 4
- 150000003624 transition metals Chemical class 0.000 abstract description 4
- 239000003446 ligand Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 229910021645 metal ion Inorganic materials 0.000 abstract 2
- 229920001795 coordination polymer Polymers 0.000 description 3
- 239000013256 coordination polymer Substances 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
- 230000005540 biological transmission Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000005838 radical anions Chemical class 0.000 description 1
- 150000005837 radical ions Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 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
- C07F15/04—Nickel compounds
- C07F15/045—Nickel compounds without a metal-carbon linkage
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyridine Compounds (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of 5- amino isophthalic acid nickel complex and preparation methods.5- amino isophthalic acid nickel 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 nickel complex by hydro-thermal method for ligand and six hydration nickel sulfate, 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 nickel complex and system
Preparation Method.
Background technique
Coordination polymer is a kind of important hybrid inorganic-organic system, is developed towards the direction of functionalization.We
Modified using structure of the group appropriate to transition metal, with obtain it is new form, new structure, new performance, and 5-
Amino isophthalic acid contains multiple carboxyls, has a variety of coordination modes, can form one-dimensional, two-dimentional, three-dimensional coordination polymer,
And by various intermolecular weak effects, i.e. hydrogen bond, pi-pi accumulation, Van der Waals force etc., the module assembled of low-dimensional is had at higher-dimension
The coordination polymer of special construction.In addition, there is 4,4'-Bipyridine intramolecular to be conjugated big pi bond, can be used as highly effective
Chromophore measures product, and has good intramolecular electron transmission and energy transmission property, it is possible to as good
Assistant ligand.There are rich and varied for the complex that transition metal Ni, 5- amino isophthalic acid are formed with 4,4 '-bipyridyls
Structure, for design synthesis object construction complex get a good eye meaning.
Summary of the invention
Thinking of the invention: being that ligand and six hydration nickel sulfate are logical using 5- amino isophthalic acid, 4,4 '-bipyridyls
It crosses hydro-thermal method and obtains nickel complex.
The molecular structure of 5- amino isophthalic acid nickel complex of the present invention is shown in attached drawing 1.The complex belongs to list
Oblique system, space group areP21/ c, central metallic ions are Ni (II) ion.In the complex, minimum structural unit includes
One Ni (II) ion, a 5- amino isophthalic acid root anion, half of 4,4'-Bipyridine neutral molecule, a coordination
Hydrone and two dissociating water molecules.A center Ni1 ion carboxylic with a 5- amino isophthalic acid root anion respectively
The oxygen atom (O3) of base is coordinated in the form of monodentate, with a carboxyl of another 5- amino isophthalic acid radical ion (O1A,
O2A) with the form coordination of bidentate chelating, also an amino (N1B) with a 5- amino isophthalic acid root anion is with list
The form of tooth is coordinated, and is coordinated with a hydrone (O5), and the octoploids structure of hexa-coordinate is formd.O1A, O2A, O3, N2 are accounted for
According to equatorial plane, O5, N1B occupy axial direction.Pass through 5- amino isophthalic acid and 4,4 '-bipyridyls and center Ni (II)
The mode of the multiple tooth bridging of ion constitutes the three-dimensional netted space structure of the complex.The average bond length of Ni-O is 2.112
, the average bond length of Ni-N is 2.086.
The 5- amino isophthalic acid nickel complex the preparation method comprises the following steps:
(1) it weighs 0.2 ~ 0.5 mM of six hydration nickel sulfate to be dissolved in 3 ~ 5 milliliters of distilled water, it is molten that nickel sulfate 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 150 degrees Celsius and reacts 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 green rhabdolith, as 5- amino isophthalic acid nickel complex.
The present invention has many advantages, such as simple process, low in cost, reproducible, has successfully synthesized 5- amino isophthalic diformazan
Sour nickel complex provides certain foundation to synthesize the complex of transition metal.
Detailed description of the invention
Fig. 1 is 5- amino isophthalic acid nickel complex molecular structure of the invention.
Specific embodiment
Embodiment:
(1) it weighs 0.2 mM of (0.0526 gram) six hydration nickel sulfate to be dissolved in 3 milliliters of distilled water, it is molten that nickel sulfate 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 150 degrees Celsius and reacts 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 green rhabdolith, as 5- amino isophthalic acid nickel complex.
The complex belongs to monoclinic system, and space group isP21/ c, central metallic ions are Ni (II) ion.In the cooperation
In object, minimum structural unit include Ni (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 Ni1 ion respectively with a 5- amino isophthalic
The oxygen atom (O3) 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 (O1A, O2A) 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.O1A, O2A, O3, 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 Ni (II) ion constitutes the three-dimensional netted space structure of the complex.
The average bond length that the average bond length of Ni-O is 2.112, Ni-N is 2.086.
Claims (2)
1. a kind of 5- amino isophthalic acid nickel complex, it is characterised in that the complex belongs to monoclinic system, and space group isP21/
C, central metallic ions are Ni (II) ion;In the complex, minimum structural unit include Ni (II) ion, one
5- amino isophthalic acid root anion, half of 4,4'-Bipyridine neutral molecule, a water of coordination molecule and two free waters
Molecule;Center Ni1 ion respectively oxygen atom, that is, O3 with a carboxyl of a 5- amino isophthalic acid root anion with list
The form of tooth is coordinated, the shape chelated with carboxyl, that is, O1A, O2A for another 5- amino isophthalic acid radical ion with bidentate
Formula coordination, also an amino, that is, N1B with a 5- amino isophthalic acid root anion is coordinated in the form of monodentate, and with one
A hydrone, that is, O5 coordination, forms the octoploids structure of hexa-coordinate;O1A, O2A, O3, N2 occupy equatorial plane, and O5, N1B are accounted for
According to axial direction;By way of the multiple tooth bridging of 5- amino isophthalic acid and 4,4 '-bipyridyls and center Ni (II) ion
Constitute the three-dimensional netted space structure of the complex;The average bond length of Ni-O is that the average bond length of 2.112, Ni-N is
2.086 Å。
2. the preparation method of 5- amino isophthalic acid nickel complex according to claim 1, it is characterised in that it is specific
Step are as follows:
(1) it weighs 0.2 mM of (0.0526 gram) six hydration nickel sulfate to be dissolved in 3 milliliters of distilled water, it is molten that nickel sulfate 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- amino is made
M-phthalic acid solution；
(3) it weighs 0.2 mM of (0.0312 gram) 4,4'-Bipyridine to be dissolved in 5 milliliters of distilled water, 4,4 '-connection pyrroles is made
Pyridine solution；
(4) it weighs 0.4 mM of (0.0224 gram) potassium hydroxide to be dissolved in 2 milliliters 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 150 degrees Celsius and reacts 72 hours, is down to room temperature after the reaction was completed with 10 degrees Celsius of gradients per hour, quiet
Kettle is opened after setting 24 hours, filters to obtain green rhabdolith, as 5- amino isophthalic acid nickel complex.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811303808.1A CN109336933A (en) | 2018-11-03 | 2018-11-03 | 5- amino isophthalic acid nickel complex and preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811303808.1A CN109336933A (en) | 2018-11-03 | 2018-11-03 | 5- amino isophthalic acid nickel complex and preparation method |
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| Publication Number | Publication Date |
|---|---|
| CN109336933A true CN109336933A (en) | 2019-02-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201811303808.1A Withdrawn CN109336933A (en) | 2018-11-03 | 2018-11-03 | 5- amino isophthalic acid nickel complex and preparation method |
Country Status (1)
| Country | Link |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112745510A (en) * | 2020-12-29 | 2021-05-04 | 温州大学 | Multilayer columnar functional complex containing nickel cluster structural unit and sodium ions and application thereof |
-
2018
- 2018-11-03 CN CN201811303808.1A patent/CN109336933A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112745510A (en) * | 2020-12-29 | 2021-05-04 | 温州大学 | Multilayer columnar functional complex containing nickel cluster structural unit and sodium ions and application thereof |
| CN112745510B (en) * | 2020-12-29 | 2022-08-05 | 温州大学 | Multilayer columnar functional complex containing nickel cluster structural unit and sodium ions and application thereof |
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| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20190215 |
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