CN106519251A - Cobalt polymer formed by terephthalic acid and 4-phenylpyridine and preparation method thereof - Google Patents
Cobalt polymer formed by terephthalic acid and 4-phenylpyridine and preparation method thereof Download PDFInfo
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- CN106519251A CN106519251A CN201610869697.5A CN201610869697A CN106519251A CN 106519251 A CN106519251 A CN 106519251A CN 201610869697 A CN201610869697 A CN 201610869697A CN 106519251 A CN106519251 A CN 106519251A
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- terephthalic acid
- tpa
- cobalt
- distilled water
- phenylpyridines
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
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- Pyridine Compounds (AREA)
Abstract
The invention discloses a cobalt polymer formed by terephthalic acid and 4-phenylpyridine and a preparation method thereof. the preparation method comprises the steps: (1) weighing 0.3-0.6 mmol of cobalt nitrate hexahydrate, and dissolving in 2-4 ml of distilled water; (2) weighing 0.3-0.6 mmol of terephthalic acid, and dissolving in 5-10 ml of distilled water; (3) weighing 0.3-0.6 mmol of 4-phenylpyridine, and dissolving in 2-4 ml of distilled water; (4) weighing 0.6-1.2 mmol of sodium hydroxide, and dissolving in 1-2 ml of distilled water; (5) adding the solutions prepared in the step (1), (2), (3) and (4) to a polytetrafluoroethylene reaction kettle liner, carrying out magnetic stirring for 0.5-1 h at room temperature, sleeving a stainless steel reaction kettle jacket, putting into a 145 DEG C drying oven, carrying out a reaction for 48-72 h, after the completion of the reaction, cooling to room temperature at a gradient of 10 DEG C per hour, allowing to stand for 12-24 h, opening the kettle, to obtain a red solution, and filtering to obtain a rose red transparent massive crystal on filter paper, namely the cobalt polymer. The method has the advantages of simple process, low cost and good repeatability.
Description
Technical field
It is the invention belongs to complex preparing technical field, particularly a kind of to be constructed with terephthalic acid (TPA) and 4- phenylpyridines
Cobalt polymer and preparation method.
Background technology
Carboxylic acids metal organic complex is to develop more rapid class I organic-inorganic hybridized material nearly ten years, its
In, organic carboxyl acid metal complexes are in occupation of larger ratio.Using carboxylic acid, this class has special construction and performance to people
Organic micromolecule ligand and metal ion it is unique in structure and performance by the complex for being coordinated bond formed.By many
The research of pyridine and aromatic carboxylic acids class part synthesizing new metallic organic framework is the molecule assembling emphasis in this field.Many pyridines
There is intramolecular to be conjugated big π keys for part and its derivative, be not only excellent chromophore, and with good intramolecular
Electron transmission and energy transmission property.Hydroxy-acid group it also there is rich and varied coordination mode and coordination mode, such as monodentate is matched somebody with somebody
Position, double coordination, bridging, chelating etc., can form the complex with large specific surface area and hole with transition metal ions.
The content of the invention
It is an object of the invention to provide a kind of cobalt polymer constructed with terephthalic acid (TPA) and 4- phenylpyridines and preparation side
Method.
The thinking of the present invention：Using terephthalic acid (TPA), 4- phenylpyridines and cabaltous nitrate hexahydrate, cobalt is obtained by hydro-thermal method
Polymer.
The cobalt polymer that should be constructed with terephthalic acid (TPA) and 4- phenylpyridines belongs to anorthic system, and space group isPī.This is matched somebody with somebody
One elementary cell of compound includes a cobalt ions, terephthaldehyde's acid anion and two 4- phenylpyridine molecules.At this
In complex, the carboxyl on terephthalic acid (TPA) is coordinated with metal ion Co (II) in the form of bidentate bridging, 4- phenylpyridines
Coordination is participated in the form of monodentate.Central metal Co (II) ion respectively from from four different phthalic acid parts
On four oxygen atoms（O1B、O2、O3、O4B）, each nitrogen-atoms of two 4- phenylpyridines（N1、N2）Coordination.Six coordinations
Atom is arranged around Co (II) ion in the form of distorted octahedron.O1B, O2, O3, O4B occupy four on equatorial plane
Position, average departure 0.0043, N1 and N2 then occupy axial location.Co (II) ion deflections equatorial plane 0.0209, Co-
Between 2.0745-2.1035, Co-N bond distance is 2.1654 to O bond distance.
The preparation method of the cobalt polymer constructed with terephthalic acid (TPA) and 4- phenylpyridines is concretely comprised the following steps：
(1) weigh 0.3 ~ 0.6 mM of cabaltous nitrate hexahydrate to be dissolved in 2 ~ 4 milliliters of distilled water, cobalt nitrate solution is obtained.
(2) weigh 0.3 ~ 0.6 mM of terephthalic acid (TPA) to be dissolved in 5 ~ 10 milliliters of distilled water, terephthalic acid (TPA) is obtained molten
Liquid.
(3) weigh 0.3 ~ 0.6 mM of 4- phenylpyridine to be dissolved in 2 ~ 4 milliliters of distilled water, 4- phenylpyridines are obtained molten
Liquid.
(4) weigh 0.6 ~ 1.2 mM of NaOH to be dissolved in 1 ~ 2 milliliter of distilled water, sodium hydroxide solution is obtained.
(5) step (1), (2), (3) and solution obtained in (4) are added in ptfe autoclave inner bag, in room
The lower magnetic agitation of temperature 0.5 ~ 1 hour, puts during stainless steel cauldron overcoat is put into 145 degrees Celsius of baking ovens and reacts 48 ~ 72 hours, instead
Room temperature is down to 10 degrees Celsius of gradients per hour after the completion of answering, kettle is driven after standing 12 ~ 24 hours and is obtained red solution, filter in filter paper
On obtain rose transparent cake crystal, the cobalt polymer as constructed with terephthalic acid (TPA) and 4- phenylpyridines.
The present invention has the advantages that process is simple, with low cost, reproducible, has successfully synthesized cobalt polymer, has been conjunction
Polymer into transition metal provides certain foundation.
Description of the drawings
Fig. 1 is the molecular structure of the cobalt polymer that the present invention is constructed with terephthalic acid (TPA) and 4- phenylpyridines.
Specific embodiment
Embodiment：
(1) weigh 0.3 mM（0.0871 gram）Cabaltous nitrate hexahydrate is dissolved in 2 milliliters of distilled water, and cobalt nitrate solution is obtained.
(2) weigh 0.3 mM（0.0498 gram）Terephthalic acid (TPA) is dissolved in 5 milliliters of distilled water, and terephthaldehyde is obtained
Acid solution.
(3) weigh 0.3 mM（0.0466 gram）4- phenylpyridines are dissolved in 2 milliliters of distilled water, and 4- phenyl pyrazolines are obtained
Pyridine solution.
(4) weigh 0.6 mM（0.0240 gram）NaOH is dissolved in 1 milliliter of distilled water, NaOH is obtained molten
Liquid.
(5) step (1), (2), (3) and solution obtained in (4) are added in ptfe autoclave inner bag, in room
The lower magnetic agitation of temperature 0.5 hour, puts during stainless steel cauldron overcoat is put into 145 degrees Celsius of baking ovens and reacts 72 hours, reacted
Room temperature is down to 10 degrees Celsius of gradients per hour into after, kettle is driven after standing 12 hours and is obtained red solution, filtration is obtained on filter paper
Rose transparent cake crystal, the cobalt polymer as constructed with terephthalic acid (TPA) and 4- phenylpyridines.
Fig. 1 is shown in the cobalt polymer architecture that terephthalic acid (TPA) and 4- phenylpyridines are constructed, crystallographic structural analysis show, should be with
The cobalt polymer that terephthalic acid (TPA) and 4- phenylpyridines are constructed belongs to anorthic system, and space group isPī.The complex one is basic
Unit includes a cobalt ions, terephthaldehyde's acid anion and two 4- phenylpyridine molecules.In the complex, to benzene
Carboxyl on dioctyl phthalate is coordinated with metal ion Co (II) in the form of bidentate bridging, and 4- phenylpyridines are in the form of monodentate
Participate in coordination.Central metal Co (II) ion respectively from four oxygen atoms on four different phthalic acid parts
（O1B、O2、O3、O4B）, each nitrogen-atoms of two 4- phenylpyridines（N1、N2）Coordination.Six coordination atoms Co (II) from
Arranged in the form of distorted octahedron around sub.O1B, O2, O3, O4B occupy four positions on equatorial plane, average departure
0.0043, N1 and N2 then occupies axial location.Co (II) ion deflections equatorial plane 0.0209, Co-O bond distance is 2.0745
Between -2.1035, Co-N bond distance is 2.1654.
Claims (2)
1. a kind of cobalt polymer constructed with terephthalic acid (TPA) and 4- phenylpyridines, it is characterised in that it is described with terephthalic acid (TPA) and
The structural formula of the cobalt polymer that 4- phenylpyridines are constructed is：
The cobalt polymer constructed with terephthalic acid (TPA) and 4- phenylpyridines belongs to anorthic system, and space group is；The cooperation
One elementary cell of thing includes a cobalt ions, terephthaldehyde's acid anion and two 4- phenylpyridine molecules；Match somebody with somebody at this
In compound, the carboxyl on terephthalic acid (TPA) is coordinated with metal ion Co (II) in the form of bidentate bridging, and 4- phenylpyridines are equal
Coordination is participated in the form of monodentate；Central metal Co (II) ion respectively from four different phthalic acid parts
Four oxygen atoms are O1B, O2, O3 and O4B, and each nitrogen-atoms of two 4- phenylpyridines is N1 and N2 coordinations；Six coordinations are former
Son is arranged around Co (II) ion in the form of distorted octahedron；O1B, O2, O3, O4B occupy four positions on equatorial plane
Put, average departureN1 and N2 then occupy axial location；Co (II) ion deflection equatorial planeCo-O
Bond distance existsBetween, Co-N bond distance is
2. the preparation method of cobalt polymer according to claim 1, it is characterised in that concretely comprise the following steps：
(1) weigh 0.3～0.6 mM of cabaltous nitrate hexahydrate to be dissolved in 2～4 milliliters of distilled water, cobalt nitrate solution is obtained；
(2) weigh 0.3～0.6 mM of terephthalic acid (TPA) to be dissolved in 5～10 milliliters of distilled water, terephthalic acid (TPA) is obtained molten
Liquid；
(3) weigh 0.3～0.6 mM of 4- phenylpyridine to be dissolved in 2～4 milliliters of distilled water, 4- phenylpyridine solution is obtained；
(4) weigh 0.6～1.2 mM of NaOH to be dissolved in 1～2 milliliter of distilled water, sodium hydroxide solution is obtained；
(5) step (1), (2), (3) and solution obtained in (4) are added in ptfe autoclave inner bag, at room temperature
Magnetic agitation 0.5～1 hour, puts during stainless steel cauldron overcoat is put into 145 degrees Celsius of baking ovens and reacts 48～72 hours, reaction
After the completion of be down to room temperature with 10 degrees Celsius of gradients per hour, drive kettle after standing 12～24 hours and obtain red solution, filter in filter paper
On obtain rose transparent cake crystal, the cobalt polymer as constructed with terephthalic acid (TPA) and 4- phenylpyridines.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417711A (en) * | 2017-04-24 | 2017-12-01 | 桂林理工大学 | Preparation, structure and its photoluminescent property of terephthalic acid (TPA) cadmium complex |
| CN109320560A (en) * | 2018-08-27 | 2019-02-12 | 天津理工大学 | Functional complexes humidity-sensitive material containing cobalt ions and its preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103951708A (en) * | 2014-04-18 | 2014-07-30 | 海南大学 | Multidentate carboxylic acid coordination polymer and preparation method thereof |
| CN104583172A (en) * | 2012-07-04 | 2015-04-29 | 株式会社可乐丽 | Metal complex, and absorbent, occlusion material and separation material produced therefrom |
| CN105237576A (en) * | 2015-10-19 | 2016-01-13 | 桂林理工大学 | Trinuclear manganese complex and preparation method thereof |
-
2016
- 2016-10-01 CN CN201610869697.5A patent/CN106519251A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104583172A (en) * | 2012-07-04 | 2015-04-29 | 株式会社可乐丽 | Metal complex, and absorbent, occlusion material and separation material produced therefrom |
| CN103951708A (en) * | 2014-04-18 | 2014-07-30 | 海南大学 | Multidentate carboxylic acid coordination polymer and preparation method thereof |
| CN105237576A (en) * | 2015-10-19 | 2016-01-13 | 桂林理工大学 | Trinuclear manganese complex and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107417711A (en) * | 2017-04-24 | 2017-12-01 | 桂林理工大学 | Preparation, structure and its photoluminescent property of terephthalic acid (TPA) cadmium complex |
| CN109320560A (en) * | 2018-08-27 | 2019-02-12 | 天津理工大学 | Functional complexes humidity-sensitive material containing cobalt ions and its preparation method and application |
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