CN106366329A - Terephthalic acid binuclear cadmium polymer and preparation method thereof - Google Patents
Terephthalic acid binuclear cadmium polymer and preparation method thereof Download PDFInfo
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- CN106366329A CN106366329A CN201610813592.8A CN201610813592A CN106366329A CN 106366329 A CN106366329 A CN 106366329A CN 201610813592 A CN201610813592 A CN 201610813592A CN 106366329 A CN106366329 A CN 106366329A
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Abstract
The invention discloses a terephthalic acid binuclear cadmium polymer and a preparation method thereof. By means of terephthalic acid, bis(4-pyridine)amine and cadmium nitrate, the cadmium polymer, namely the terephthalic acid binuclear cadmium polymer is obtained through a hydrothermal method. The structural formula of the terephthalic acid binuclear cadmium polymer is shown in the specification. The terephthalic acid binuclear cadmium polymer and the preparation method thereof have the advantages of being simple in process, low in cost, good in repeatability and the like, the terephthalic acid binuclear cadmium polymer is successfully synthesized, and a certain basis is provided for synthesis of a multi-element complex of transition metal.
Description
Technical field
The invention belongs to technical field of polymer preparation, particularly to a kind of p-phthalic acid double-core cadmium polymer and its system
Preparation Method.
Background technology
In recent years, the species of transition multicomponent complex and number rapidly increase, and people are using having special construction and performance
Organic micromolecule ligand and metal ion pass through coordinate bond or other weak interaction synthesizes coordination supramolecule, the cooperation of formation
Thing is unique in structure and performance.But, the report for multinuclear multicomponent complex is still few.Many by many pyridines and fragrance
The research of carboxylic acidss part synthesizing new metallic organic framework is the molecule assembling emphasis in this field.Many pyridine ligands and its spread out
Biology have intramolecular be conjugated big π key, be not only excellent chromophore, and have good intramolecular electron transmission and
Energy transmission property.Hydroxy-acid group can be with multiple coordination modes such as monodentate, bidentate (bridge-type, chelating) and three flute profiles and transition gold
Belong to ion and form the coordination compound with large specific surface area and hole.
Content of the invention
It is an object of the invention to provide a kind of p-phthalic acid double-core cadmium polymer and preparation method thereof.
The thinking of the present invention: using p-phthalic acid, double (4- pyridine radicals) amine and cadmium nitrate, cadmium is obtained by hydro-thermal method and gathers
Compound, as p-phthalic acid double-core cadmium polymer.
The structural formula of the p-phthalic acid double-core cadmium polymer of the present invention is:
.
This p-phthalic acid double-core cadmium polymer belongs to monoclinic system, and space group isp21/n, this p-phthalic acid double-core cadmium
The elementary cell of polymer is made up of two cadmium ions, two terephthaldehyde's acid anions, two double (4- pyridine radicals) amine, one
Two carboxyls of p-phthalic acid participate in being coordinated all in the form of bidentate bridging, and two carboxyls of another p-phthalic acid are respectively
Participate in coordination in the form of monodentate and chelating；Two double (4- pyridine radicals) amine participate in being coordinated all in the form of bridging；Central metal
Ion cd1 respectively with four oxygen atoms o2, o4a, o7a and o8a on three p-phthalic acid parts, and two double
Two nitrogen-atoms n3a and n6a coordinations of (4- pyridine radicals) amine；Six coordination atoms are around cd (ii) ion with distorted octahedron
Form arrangement；O2, o4a, o7a and o8a occupy four positions on equatorial plane, average departure 0.2073, n3a and n6a
Then occupy axial location；Central metallic ions cd2 respectively with three oxygen atom o1 on two p-phthalic acid parts,
O3a and o5, and two nitrogen-atoms n1 and n4 coordinations of two double (4- pyridine radicals) amine；Five coordination atoms are in cd (ii) ion
Surrounding is arranged in the form of double trigonal biyramids；O1, o3a and o5 occupy three positions on equatorial plane, average departure 0.0685
, n1 and n4 then occupy axial location；Cd-o bond distance between 2.2164-2.4539, co-n bond distance 2.2677-
2.3363 between.
The preparation method of above-mentioned p-phthalic acid double-core cadmium polymer is:
(1) weigh 0.5 ~ 1 mM of four nitric hydrate cadmium to be dissolved in 2 ~ 4 milliliters of distilled water, prepared nitric acid cadmium solution.
(2) weigh 0.5 ~ 1 mM of p-phthalic acid to be dissolved in 5 ~ 10 milliliters of distilled water, prepared p-phthalic acid is molten
Liquid.
(3) weigh 0.5 ~ 1 mM of double (4- pyridine radicals) amine solvent in 2 ~ 4 milliliters of distilled water, double (4- pyridines are obtained
Base) amine aqueous solution.
(4) weigh 1 ~ 2 mM of sodium hydroxide to be dissolved in 1 ~ 2 milliliter of distilled water, prepared sodium hydroxide solution.
(5) solution that step (1), (2), (3) and (4) is obtained is added in ptfe autoclave inner bag, in room
The lower magnetic agitation of temperature 0.5 hour, puts stainless steel cauldron overcoat and puts in 130 degrees Celsius of baking ovens and react 48 ~ 72 hours, reaction
After the completion of room temperature is cooled to per hour 10 degrees Celsius of velocity gradient, standing is driven kettle after 12 ~ 24 hours and is obtained yellow solution, mistake
Filter obtains pale yellow transparent bulk crystals, as p-phthalic acid double-core cadmium polymer on filter paper.
The present invention has the advantages that process is simple, with low cost, reproducible, has successfully synthesized p-phthalic acid double-core
Cadmium polymer, the multicomponent complex for synthesizing transition metal provides certain foundation.
Brief description
Fig. 1 is the molecular structure of the p-phthalic acid double-core cadmium polymer of the present invention.
Specific embodiment
Embodiment:
(1) weigh 0.5 mM of (0.1042 gram) four nitric hydrate cadmium to be dissolved in 2 milliliters of distilled water, prepared nitric acid cadmium solution.
(2) weigh 0.5 mM of (0.0831 gram) p-phthalic acid to be dissolved in 5 milliliters of distilled water, prepared terephthaldehyde
Acid solution.
(3) weigh 0.5 mM of (0.0855 gram) double (4- pyridine radicals) amine solvent in 2 milliliters of distilled water, double (4-s are obtained
Pyridine radicals) amine aqueous solution.
(4) weigh 1 mM of (0.0400 gram) sodium hydroxide to be dissolved in 1 milliliter of distilled water, prepared sodium hydroxide solution.
(5) solution that step (1), (2), (3) and (4) is obtained is added in ptfe autoclave inner bag, in room
The lower magnetic agitation of temperature 0.5 hour, puts stainless steel cauldron overcoat and puts in 130 degrees Celsius of baking ovens and react 72 hours, reacted
After one-tenth, room temperature is cooled to per hour 10 degrees Celsius of velocity gradient, standing is driven kettle and obtained yellow solution after 12 hours, filter
Pale yellow transparent bulk crystals, as p-phthalic acid double-core cadmium polymer are obtained on filter paper.Its structure is:
.
Crystallographic structural analysis show, this p-phthalic acid double-core cadmium polymer belongs to monoclinic system, and space group isp21/n.
This polymer elementary cell is made up of two cadmium ions, two terephthaldehyde's acid anions, two double (4- pyridine radicals) amine.At this
In coordination compound, two carboxyls of a p-phthalic acid participate in being coordinated all in the form of bidentate bridging, another p-phthalic acid
Two carboxyls respectively with monodentate and chelating in the form of participate in coordination.Two double (4- pyridine radicals) amine are participated in all in the form of bridging
Coordination.Central metallic ions cd1 respectively with three p-phthalic acid parts four oxygen atoms (o2, o4a, o7a,
O8a), two nitrogen-atoms (n3a, n6a) coordinations of two double (4- pyridine radicals) amine.Six coordination atoms are around cd (ii) ion
Arranged in the form of distorted octahedron.O2, o4a, o7a, o8a occupy four positions on equatorial plane, average departure 0.2073
, n3a and n6a then occupy axial location.Central metallic ions cd2 respectively with three on two p-phthalic acid parts
Oxygen atom (o1, o3a, o5), two nitrogen-atoms (n1, n4) coordinations of two double (4- pyridine radicals) amine.Five coordination atoms are in cd
(ii) arranged in the form of double trigonal biyramids around ion.O1, o3a, o5 occupy three positions on equatorial plane, average departure
0.0685, n1 and n4 then occupies axial location.Between 2.2164-2.4539, co-n bond distance's cd-o bond distance exists
2.2677 between -2.3363.
Claims (2)
1. a kind of p-phthalic acid double-core cadmium polymer is it is characterised in that the structural formula of this p-phthalic acid double-core cadmium polymer
For:
；
Described p-phthalic acid double-core cadmium polymer belongs to monoclinic system, and space group isp21/n, this p-phthalic acid double-core cadmium gather
The elementary cell of compound is made up of two cadmium ions, two terephthaldehyde's acid anions, two double (4- pyridine radicals) amine, and one right
Two carboxyls of phthalic acid participate in being coordinated all in the form of bidentate bridging, two carboxyls of another p-phthalic acid respectively with
The form of monodentate and chelating participates in coordination；Two double (4- pyridine radicals) amine participate in being coordinated all in the form of bridging；Central metal from
Sub- cd1 respectively with four oxygen atoms o2, o4a, o7a and o8a on three p-phthalic acid parts, and two double (4-
Pyridine radicals) amine two nitrogen-atoms n3a and n6a coordination；Six coordination atoms are around cd (ii) ion with distorted octahedron
Form is arranged；O2, o4a, o7a and o8a occupy four positions on equatorial plane, average departure 0.2073, n3a and n6a is then
Occupy axial location；Central metallic ions cd2 respectively with three oxygen atoms o1, o3a on two p-phthalic acid parts
And o5, and two nitrogen-atoms n1 and n4 coordinations of two double (4- pyridine radicals) amine；Five coordination atoms are in cd (ii) ion week
Enclose arrangement in the form of double trigonal biyramids；O1, o3a and o5 occupy three positions on equatorial plane, average departure 0.0685,
N1 and n4 then occupies axial location；Cd-o bond distance between 2.2164-2.4539, co-n bond distance 2.2677-
2.3363 between.
2. a kind of method preparing p-phthalic acid double-core cadmium polymer as claimed in claim 1 is it is characterised in that concrete walk
Suddenly it is:
(1) weigh 0.5 ~ 1 mM of four nitric hydrate cadmium to be dissolved in 2 ~ 4 milliliters of distilled water, prepared nitric acid cadmium solution；
(2) weigh 0.5 ~ 1 mM of p-phthalic acid to be dissolved in 5 ~ 10 milliliters of distilled water, prepared terephthalic acid solution；
(3) weigh 0.5 ~ 1 mM of double (4- pyridine radicals) amine solvent in 2 ~ 4 milliliters of distilled water, double (4- pyridine radicals) amine are obtained
Solution；
(4) weigh 1 ~ 2 mM of sodium hydroxide to be dissolved in 1 ~ 2 milliliter of distilled water, prepared sodium hydroxide solution；
(5) solution that step (1), (2), (3) and (4) is obtained is added in ptfe autoclave inner bag, at room temperature
Magnetic agitation 0.5 hour, puts stainless steel cauldron overcoat and puts in 130 degrees Celsius of baking ovens and react 48 ~ 72 hours, reaction completes
Afterwards room temperature is cooled to per hour 10 degrees Celsius of velocity gradient, standing is driven kettle and obtained yellow solution after 12 ~ 24 hours, filter
Pale yellow transparent bulk crystals, as p-phthalic acid double-core cadmium polymer are obtained on filter paper.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957440A (en) * | 2017-04-25 | 2017-07-18 | 桂林理工大学 | Preparation, structure and its photoluminescent property of phthalic acid zinc complex |
| CN110256688A (en) * | 2019-06-27 | 2019-09-20 | 商丘师范学院 | A kind of different metal [CdMn] fluorescence magnetic refrigerating material and preparation method thereof |
| CN112142765A (en) * | 2020-09-29 | 2020-12-29 | 桂林理工大学 | Crystal structure of isophthalic acid cadmium complex and fluorescence property thereof |
| CN113845535A (en) * | 2021-10-26 | 2021-12-28 | 四川省产品质量监督检验检测院 | Binuclear cadmium complex and preparation method and application thereof |
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| CN104230968A (en) * | 2014-09-09 | 2014-12-24 | 段晶晶 | Cadmium-containing dual-core polymer with mixed-ligand and preparation method of cadmium-containing dual-core polymer |
| CN105669999A (en) * | 2016-04-14 | 2016-06-15 | 淮南师范学院 | Pamoic acid cadmium light-emitting material containing dipyridyl type ligand and preparation method of pamoic acid cadmium light-emitting material |
| CN105820346A (en) * | 2016-04-27 | 2016-08-03 | 齐鲁工业大学 | Synthetic method of cadmium coordination polymer containing pyridyl benzimidazole and isophthalic acid |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104230968A (en) * | 2014-09-09 | 2014-12-24 | 段晶晶 | Cadmium-containing dual-core polymer with mixed-ligand and preparation method of cadmium-containing dual-core polymer |
| CN105669999A (en) * | 2016-04-14 | 2016-06-15 | 淮南师范学院 | Pamoic acid cadmium light-emitting material containing dipyridyl type ligand and preparation method of pamoic acid cadmium light-emitting material |
| CN105820346A (en) * | 2016-04-27 | 2016-08-03 | 齐鲁工业大学 | Synthetic method of cadmium coordination polymer containing pyridyl benzimidazole and isophthalic acid |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957440A (en) * | 2017-04-25 | 2017-07-18 | 桂林理工大学 | Preparation, structure and its photoluminescent property of phthalic acid zinc complex |
| CN110256688A (en) * | 2019-06-27 | 2019-09-20 | 商丘师范学院 | A kind of different metal [CdMn] fluorescence magnetic refrigerating material and preparation method thereof |
| CN110256688B (en) * | 2019-06-27 | 2021-03-23 | 商丘师范学院 | Dissimilar metal [ CdMn ] fluorescent magnetic refrigeration material and preparation method thereof |
| CN112142765A (en) * | 2020-09-29 | 2020-12-29 | 桂林理工大学 | Crystal structure of isophthalic acid cadmium complex and fluorescence property thereof |
| CN113845535A (en) * | 2021-10-26 | 2021-12-28 | 四川省产品质量监督检验检测院 | Binuclear cadmium complex and preparation method and application thereof |
| CN113845535B (en) * | 2021-10-26 | 2022-03-08 | 四川省产品质量监督检验检测院 | Binuclear cadmium complex and preparation method and application thereof |
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