CN106496583A - 4 silver formate polymer of pyrazoles and preparation method thereof - Google Patents
4 silver formate polymer of pyrazoles and preparation method thereof Download PDFInfo
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- CN106496583A CN106496583A CN201610869709.4A CN201610869709A CN106496583A CN 106496583 A CN106496583 A CN 106496583A CN 201610869709 A CN201610869709 A CN 201610869709A CN 106496583 A CN106496583 A CN 106496583A
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- pyrazoles
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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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Abstract
The invention discloses 4 silver formate polymer of a kind of pyrazoles and preparation method thereof.The structural formula of the polymer is：；The present invention obtains silver-colored polymer using 4 formic acid of pyrazoles and silver nitrate by solvent-thermal method.The present invention has process is simple, with low cost, reproducible, has successfully synthesized monoclinic silver-colored polymer, provides certain foundation for synthesizing the silver-colored polymer of transition metal.
Description
Technical field
The invention belongs to technical field of polymer preparation, more particularly to a kind of pyrazoles -4- silver formates polymer and its preparation
Method.
Background technology
In recent years, the species of transition metal polymerization thing and number rapidly increase, and people are using with special construction and performance
Organic micromolecule ligand and metal ion coordination supramolecule, the polymerization of formation are synthesized by coordinate bond or other weak interactions
Thing is unique in structure and performance.By grinding for many pyridines and aromatic polycarboxylic acids class part synthesizing new metallic organic framework
It is the molecule assembling emphasis in this field to study carefully.In many pyridine ligands and its derivant, N Atomic coordinates pattern is single but coordination ability
By force, and with intramolecular big π keys are conjugated, are not only excellent chromophore, and with good intramolecular electron transmission
With energy transmission property.Hydroxy-acid group can be with monodentate, bidentate（Bridge-type, chelating）With multiple coordination modes and transition such as three flute profiles
Metal ion forms 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 pyrazoles -4- silver formate polymer and preparation method thereof.
The thinking of the present invention：Using pyrazoles -4- formic acid and silver nitrate, silver-colored polymer is obtained by solvent-thermal method.
Pyrazoles -4- silver formate polymer belongs to monoclinic system, and space group isC2/c, central metallic ions are Ag (I) ion.
The polymer each primitive includes Ag (I) ion, a pyrazoles -4- formic acid anion and a pyrazoles -4- formic acid molecule.
The N1 atoms of pyrazoles -4- formic acid are coordinated with cadmium ion.Central metallic ions Ag (I) respectively with from two pyrazoles -4- formic acid
Two nitrogen-atoms (N1, N1A) coordinations.It is connected by a hydrogen atom between each pyrazoles -4- formic acid carboxyl and carboxyl, by pyrrole
Azoles -4- formic acid is bridge, is connected to Ag (I) ions and hydrogen atom, makes the coordination compound form one-dimensional chain polymer.Ag-N bond distance is
2.1085, H-O bond distances are 1.234.
The preparation method of pyrazoles -4- silver formate polymer is concretely comprised the following steps：
(1) weigh 0.5 ~ 1 mM of anhydrous nitric acid silver to be dissolved in 4 ~ 8 milliliters of distilled water, silver nitrate solution is obtained；
(2) weigh 0.5 ~ 1 mM of pyrazoles -4- formic acid to be dissolved in 5 ~ 10 milliliters of dehydrated alcohol, pyrazoles -4- formic acid is obtained molten
Liquid；
(3) weigh 1 ~ 2 mM of sodium hydroxide to be dissolved in 1 ~ 2 milliliter of distilled water, sodium hydroxide solution is obtained；
(4) step (1), (2) and solution obtained in (3) are added in ptfe autoclave inner bag, put rustless steel anti-
Answer kettle overcoat to be put in 80 degrees Celsius of baking ovens to react 48 ~ 72 hours, after the completion of reaction, room is down to 10 degrees Celsius of gradients per hour
Temperature, drives kettle after standing 12 hours and obtains the colourless precipitation solution of floccule containing Lycoperdon polymorphum Vitt, and solution is stored at room temperature one week, obtains colourless block brilliant
Body, as pyrazoles -4- silver formates polymer.
The present invention has process is simple, with low cost, reproducible, has successfully synthesized silver-colored polymer, has been conjunction
Smaller ligand polymer into transition metal provides certain foundation.
Description of the drawings
Fig. 1 is the molecular structure of pyrazoles -4- silver formate polymer of the present invention.
Specific embodiment
Embodiment：
(1) 0.5 mM is weighed（0.0813 gram）Anhydrous nitric acid silver is dissolved in 4 milliliters of distilled water, and silver nitrate solution is obtained.
(2) 0.5 mM is weighed（0.0556 gram）Pyrazoles -4- formic acid is dissolved in 5 milliliters of dehydrated alcohol, and prepared pyrazoles -
4- formic acid solutions.
(3) 1 mM is weighed（0.0200 gram）Sodium hydroxide is dissolved in 2 milliliters of distilled water, and sodium hydroxide solution is obtained.
(4) step (1), (2) and solution obtained in (3) are added in ptfe autoclave inner bag, are put stainless
Steel reactor overcoat is put in 80 degrees Celsius of baking ovens and reacts 60 hours, is down to room with 10 degrees Celsius of gradients per hour after the completion of reaction
Temperature, drives kettle after standing 12 hours and obtains the colourless precipitation solution of floccule containing Lycoperdon polymorphum Vitt, and solution is stored at room temperature one week, obtains colourless block brilliant
Body, as pyrazoles -4- silver formates polymer.
Pyrazoles -4- silver formate polymer molecular structures are shown in that Fig. 1, crystallographic structural analysis show, the polymer belongs to monoclinic crystal
It is that space group isC2/c, central metallic ions are Ag (I) ion.The polymer each primitive includes Ag (I) ion, and one
Individual pyrazoles -4- formic acid anion and a pyrazoles -4- formic acid molecule.The N1 atoms of pyrazoles -4- formic acid are coordinated with cadmium ion.Center
Metal ion Ag (I) is coordinated with two nitrogen-atoms (N1, N1A) from two pyrazoles -4- formic acid respectively.Each pyrazoles -4- first
It is connected by a hydrogen atom between sour carboxyl and carboxyl, is bridge by pyrazoles -4- formic acid, is connected to Ag (I) ions and hydrogen atom,
The coordination compound is made to form one-dimensional chain polymer.It is 1.234 that Ag-N bond distance is 2.1085, H-O bond distances.
Claims (2)
1. a kind of pyrazoles -4- silver formate polymer, it is characterised in that the structural formula of pyrazoles -4- silver formate polymer is：
Pyrazoles -4- silver formate the polymer belongs to monoclinic system, and space group is C2/c, and central metallic ions are Ag (I) ion.
The polymer each primitive includes Ag (I) ion, a pyrazoles -4- formic acid anion and a pyrazoles -4- formic acid molecule.
The N1 atoms of pyrazoles -4- formic acid are coordinated with cadmium ion.Central metallic ions Ag (I) respectively with from two pyrazoles -4- formic acid
Two nitrogen-atoms (N1, N1A) coordinations.It is connected by a hydrogen atom between each pyrazoles -4- formic acid carboxyl and carboxyl, by pyrrole
Azoles -4- formic acid is bridge, is connected to Ag (I) ions and hydrogen atom, makes the coordination compound form one-dimensional chain polymer.Ag-N bond distance is H-O bond distance is
2. the preparation method of pyrazoles -4- silver formate polymer according to claim 1, it is characterised in that concretely comprise the following steps：
(1) weigh 0.5～1 mM of anhydrous nitric acid silver to be dissolved in 4～8 milliliters of distilled water, silver nitrate solution is obtained；
(2) weigh 0.5～1 mM of pyrazoles -4- formic acid to be dissolved in 5～10 milliliters of dehydrated alcohol, pyrazoles -4- formic acid is obtained molten
Liquid；
(3) weigh 1～2 mM of sodium hydroxide to be dissolved in 1～2 milliliter of distilled water, sodium hydroxide solution is obtained；
(4) step (1), (2) and solution obtained in (3) are added in ptfe autoclave inner bag, put rustless steel anti-
Answer kettle overcoat to be put in 80 degrees Celsius of baking ovens to react 48～72 hours, after the completion of reaction, room is down to 10 degrees Celsius of gradients per hour
Temperature, drives kettle after standing 12 hours and obtains the colourless precipitation solution of floccule containing Lycoperdon polymorphum Vitt, and solution is stored at room temperature one week, obtains colourless block brilliant
Body, as pyrazoles -4- silver formates polymer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610869709.4A CN106496583A (en) | 2016-10-01 | 2016-10-01 | 4 silver formate polymer of pyrazoles and preparation method thereof |
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| CN201610869709.4A CN106496583A (en) | 2016-10-01 | 2016-10-01 | 4 silver formate polymer of pyrazoles and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103203207A (en) * | 2012-01-12 | 2013-07-17 | 安徽大学 | Magnetic nano-pore metal-organic framework core-shell material preparation, functionalized design, and application. |
| CN104892684A (en) * | 2015-04-01 | 2015-09-09 | 广州科技贸易职业学院 | Heterometal-organic coordination polymer containing trinuclear copper cluster, and preparation method and application thereof |
| CN105646550A (en) * | 2016-01-26 | 2016-06-08 | 淮海工学院 | Silver coordination polymer and preparing method and application thereof |
-
2016
- 2016-10-01 CN CN201610869709.4A patent/CN106496583A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103203207A (en) * | 2012-01-12 | 2013-07-17 | 安徽大学 | Magnetic nano-pore metal-organic framework core-shell material preparation, functionalized design, and application. |
| CN104892684A (en) * | 2015-04-01 | 2015-09-09 | 广州科技贸易职业学院 | Heterometal-organic coordination polymer containing trinuclear copper cluster, and preparation method and application thereof |
| CN105646550A (en) * | 2016-01-26 | 2016-06-08 | 淮海工学院 | Silver coordination polymer and preparing method and application thereof |
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Application publication date: 20170315 |