CN109336914A - Trimellitic acid cadmium complex and preparation method - Google Patents
Trimellitic acid cadmium complex and preparation method Download PDFInfo
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- CN109336914A CN109336914A CN201811303809.6A CN201811303809A CN109336914A CN 109336914 A CN109336914 A CN 109336914A CN 201811303809 A CN201811303809 A CN 201811303809A CN 109336914 A CN109336914 A CN 109336914A
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- CN
- China
- Prior art keywords
- trimellitic acid
- complex
- bipyridyl
- cadmium
- milliliters
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- ARCGXLSVLAOJQL-UHFFFAOYSA-N trimellitic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 17
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000010668 complexation reaction Methods 0.000 title abstract description 5
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical group N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 claims abstract description 9
- 150000002500 ions Chemical class 0.000 claims abstract description 9
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 6
- 239000001257 hydrogen Substances 0.000 claims abstract description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 5
- 230000000694 effects Effects 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 150000001450 anions Chemical class 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- QCUOBSQYDGUHHT-UHFFFAOYSA-L cadmium sulfate Chemical compound [Cd+2].[O-]S([O-])(=O)=O QCUOBSQYDGUHHT-UHFFFAOYSA-L 0.000 claims description 3
- 229910000331 cadmium sulfate Inorganic materials 0.000 claims description 3
- AGHQMAQBLOTWPQ-UHFFFAOYSA-H cadmium sulfate hydrate Chemical compound O.O.O.O.O.O.O.O.[Cd+2].[Cd+2].[Cd+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O AGHQMAQBLOTWPQ-UHFFFAOYSA-H 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 150000001455 metallic ions Chemical class 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 125000004433 nitrogen atom Chemical group N* 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
- 239000000126 substance Substances 0.000 claims description 2
- 239000003446 ligand Substances 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 4
- 241000023813 Isia Species 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
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- VRFRVKRTIMIRNG-UHFFFAOYSA-L cadmium(2+);hydrogen sulfate;hydroxide Chemical class O.[Cd+2].[O-]S([O-])(=O)=O VRFRVKRTIMIRNG-UHFFFAOYSA-L 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 229910021645 metal ion Inorganic materials 0.000 abstract 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- UJMDYLWCYJJYMO-UHFFFAOYSA-N benzene-1,2,3-tricarboxylic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1C(O)=O UJMDYLWCYJJYMO-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229920002338 polyhydroxyethylmethacrylate Polymers 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- -1 Benzenetricarboxylic acid cadmium Chemical compound 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 229920001795 coordination polymer Polymers 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 125000005590 trimellitic acid group Chemical group 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
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/003—Compounds containing elements of Groups 2 or 12 of the Periodic Table without C-Metal linkages
-
- 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)
Abstract
The invention discloses a kind of trimellitic acid cadmium complex and preparation methods.Trimellitic acid cadmium complex belongs to monoclinic system, and space group isIa.In the complex, carboxyl on trimellitic acid in the form of monodentate with Metal Ions Cd (II) ion coordination, 2, the form and Metal Ions Cd (II) ion coordination that 2- bipyridyl is chelated with bidentate constitute the three-dimensional netted space structure of the complex by the effects of bidentate bridging and hydrogen bond of trimellitic acid.The present invention is ligand and eight Cadmium sulfate hydrates by hydro-thermal method acquisition cadmium complex using trimellitic acid, 2,2- bipyridyl, has many advantages, such as simple process, low in cost, reproducible, the complex for synthesis transition metal provides certain foundation.
Description
Technical field
The invention belongs to complex preparation technical field, in particular to a kind of trimellitic acid cadmium complex and preparation side
Method.
Background technique
Carboxylic acids organic coordination compound is rapidly developed in recent years, and as carboxylic acids ligand, due to its coordination
A large amount of presence of the weak interactions such as the special and hydrogen bond of ability, receive the extensive concern of domestic and international chemist.Inclined benzene
Tricarboxylic acid can be used as organic carboxyl acid metalloid in the structural unit for being widely used in conformation function type coordination polymer in recent years
The popular ligand of organic coordination compound, not only its carboxyl have monodentate ligand, double coordination, bridging, chelating etc. a variety of coordination modes,
And its phenyl ring is also capable of forming π complex, coordination mode it is varied, receive the favor of numerous scholars.In addition, 2,
There is 2- bipyridyl intramolecular to be conjugated big pi bond, and product can be measured as highly effective chromophore, and have good
Intramolecular electron transmission and energy transmission property, it is possible to as good assistant ligand.Transition metal Cd, trimellitic acid
There are rich and varied structures for the complex formed with 2,2- bipyridyl, have very much for the complex of design synthesis object construction
Research significance.
Summary of the invention
The object of the present invention is to provide a kind of trimellitic acid cadmium complex and preparation methods.
Thinking of the invention: being that ligand and eight Cadmium sulfate hydrates pass through hydro-thermal method using trimellitic acid, 2,2- bipyridyl
Obtain cadmium complex.
The molecular structure of trimellitic acid cadmium complex of the present invention is shown in attached drawing 1.The complex belongs to monoclinic system,
Space group isIa, central metallic ions are Cd (II) ion.In the complex, minimum structural unit by a Cd (II) from
Son, a trimellitic acid root anion, 2, a 2- bipyridyl neutral molecule and two water of coordination molecule compositions.Center Cd1
Ion is coordinated in the form of monodentate with the oxygen atom (O3, O2A) of two carboxyls of two trimellitic acid root anion respectively, with
Two nitrogen-atoms (N1, N2) of 2,2- bipyridyl neutral molecule be coordinated in the form of chelating and with two hydrones (O7, O8)
Coordination, forms the distorted octahedron structure of hexa-coordinate.Tetra- atoms of O7, O8, N1, N2 form equatorial plane, and O3, O2A are in axis
To distribution.The three-dimensional netted space knot of the complex is constituted by the effects of bidentate bridging and hydrogen bond of trimellitic acid
Structure.The average bond length of Cd-O is that 2.298, Cd-N bond distance is respectively 2.376 and 2.311.
The terephthalic acid (TPA) cadmium complex the preparation method comprises the following steps:
(1) it weighs 0.2 ~ 0.5 mM of eight Cadmium sulfate hydrate to be dissolved in 3 ~ 5 milliliters of distilled water, it is molten that cadmium sulfate is made
Liquid.
(2) it weighs 0.2 ~ 0.5 mM of trimellitic acid to be dissolved in 3 ~ 5 milliliters of distilled water, inclined benzene front three is made
Acid solution.
(3) it weighs 0.2 ~ 0.5 mM of 2,2- bipyridyl to be dissolved in 3 ~ 5 milliliters of distilled water, 2,2- connection is made
Pyridine solution.
(4) solution made from step (1), (2) and (3) is added in ptfe autoclave liner, dropwise addition 2 ~
4 drops analyze pure triethylamine, put on stainless steel cauldron housing and are put into 120 degrees Celsius of reactions 48 ~ 72 hours, after the reaction was completed with every
Hour, 10 degrees Celsius of gradients were down to room temperature, and kettle is opened after standing 12 ~ 24 hours, and filtering and standing obtains colourless needles crystalline substance after one week
Body, as trimellitic acid cadmium complex.
The present invention has many advantages, such as simple process, low in cost, reproducible, has successfully synthesized trimellitic acid cadmium and has matched
Object is closed, provides certain foundation to synthesize the complex of transition metal.
Detailed description of the invention
Fig. 1 is trimellitic acid cadmium complex molecular structure of the invention.
Specific embodiment
Embodiment:
(1) it weighs 0.2 mM of (0.1538 gram) eight Cadmium sulfate hydrate to be dissolved in 5 milliliters of distilled water, it is molten that cadmium sulfate is made
Liquid.
(2) it weighs 0.2 mM of (0.0420 gram) trimellitic acid to be dissolved in 5 milliliters of distilled water, inclined benzene front three is made
Acid solution.
(3) it weighs 0.2 mM of (0.0312 gram) 2,2- bipyridyl to be dissolved in 5 milliliters of distilled water, 2,2- connection is made
Pyridine solution.
(4) solution made from step (1), (2) and (3) is added in ptfe autoclave liner, 3 drops is added dropwise
Pure triethylamine is analyzed, stainless steel cauldron housing is put on and is put into 120 degrees Celsius of reactions 72 hours, after the reaction was completed with per hour 10
Degree Celsius gradient is down to room temperature, opens kettle after standing 24 hours, filtering and standing obtains colourless acicular crystal after one week, as partially
Benzenetricarboxylic acid cadmium complex.
The complex belongs to monoclinic system, and space group isIa, central metallic ions are Cd (II) ion.In the complex
In, minimum structural unit is by Cd (II) ion, a trimellitic acid root anion, 2, a 2- bipyridyl neutrality
Molecule and two water of coordination molecule compositions.Center Cd1 ion respectively with two carboxyls of two trimellitic acid root anion
Oxygen atom (O3, O2A) is coordinated in the form of monodentate, and two nitrogen-atoms (N1, N2) with 2,2- bipyridyl neutral molecule are to chelate
Form coordination and be coordinated with two hydrones (O7, O8), form the distorted octahedron structure of hexa-coordinate.O7,O8,N1,
Tetra- atoms of N2 form equatorial plane, and O3, O2A are in axial distribution.Made by the bidentate bridging of trimellitic acid and hydrogen bond etc.
With constituting the three-dimensional netted space structure of the complex.The average bond length of Cd-O is that 2.298, Cd-N bond distance is respectively
2.376 with 2.311.
Claims (2)
1. a kind of trimellitic acid cadmium complex, it is characterised in that trimellitic acid cadmium complex belongs to monoclinic system, space group
ForIa, central metallic ions are Cd (II) ion;In the complex, minimum structural unit is by Cd (II) ion, and one
A trimellitic acid root anion, 2, a 2- bipyridyl neutral molecule and two water of coordination molecule compositions;Center Cd1 ion
Oxygen atom, that is, O3, O2A with two carboxyls of two trimellitic acid root anion is coordinated in the form of monodentate respectively, and 2,
Two nitrogen-atoms, that is, N1, N2 of 2- bipyridyl neutral molecule are coordinated in the form chelated and match with two i.e. O7, O8 of hydrone
Position, forms the distorted octahedron structure of hexa-coordinate;Tetra- atoms of O7, O8, N1, N2 form equatorial plane, and O3, O2A are in axial
Distribution;The three-dimensional netted space structure of the complex is constituted by the effects of bidentate bridging and hydrogen bond of trimellitic acid;
The average bond length of Cd-O is that 2.298, Cd-N bond distance is respectively 2.376 and 2.311.
2. the preparation method of trimellitic acid cadmium complex according to claim 1, it is characterised in that specific steps are as follows:
(1) it weighs 0.2 ~ 0.5 mM of eight Cadmium sulfate hydrate to be dissolved in 3 ~ 5 milliliters of distilled water, it is molten that cadmium sulfate is made
Liquid；
(2) it weighs 0.2 ~ 0.5 mM of trimellitic acid to be dissolved in 3 ~ 5 milliliters of distilled water, it is molten that trimellitic acid is made
Liquid；
(3) it weighs 0.2 ~ 0.5 mM of 2,2- bipyridyl to be dissolved in 3 ~ 5 milliliters of distilled water, 2,2- bipyridyl is made
Solution；
(4) solution made from step (1), (2) and (3) is added in ptfe autoclave liner, 2 ~ 4 drops is added dropwise
Pure triethylamine is analyzed, stainless steel cauldron housing is put on and is put into 120 degrees Celsius of reactions 48 ~ 72 hours, after the reaction was completed with every small
When 10 degrees Celsius of gradients be down to room temperature, kettle is opened after standing 12 ~ 24 hours, filtering and standing obtains colourless needles crystalline substance after one week
Body, as trimellitic acid cadmium complex.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811303809.6A CN109336914A (en) | 2018-11-03 | 2018-11-03 | Trimellitic acid cadmium complex and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811303809.6A CN109336914A (en) | 2018-11-03 | 2018-11-03 | Trimellitic acid cadmium complex and preparation method |
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| CN109336914A true CN109336914A (en) | 2019-02-15 |
Family
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|---|---|---|---|
| CN201811303809.6A Withdrawn CN109336914A (en) | 2018-11-03 | 2018-11-03 | Trimellitic acid cadmium complex and preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110483558A (en) * | 2019-08-26 | 2019-11-22 | 皖西学院 | A kind of synthetic method and its application of the micropore cadmium compound with anion frame |
| CN111704627A (en) * | 2020-05-26 | 2020-09-25 | 信阳师范学院 | Cadmium complex of 2,3, 3', 4' -biphenyltetracarboxylic acid and 4,4' -bipyridine, preparation method and application thereof |
-
2018
- 2018-11-03 CN CN201811303809.6A patent/CN109336914A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110483558A (en) * | 2019-08-26 | 2019-11-22 | 皖西学院 | A kind of synthetic method and its application of the micropore cadmium compound with anion frame |
| CN111704627A (en) * | 2020-05-26 | 2020-09-25 | 信阳师范学院 | Cadmium complex of 2,3, 3', 4' -biphenyltetracarboxylic acid and 4,4' -bipyridine, preparation method and application thereof |
| CN111704627B (en) * | 2020-05-26 | 2022-06-28 | 信阳师范学院 | Cadmium complex of 2,3,3 ', 4' -biphenyltetracarboxylic acid and 4,4' -bipyridine, preparation method and application thereof |
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| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20190215 |
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