CN106496578A - Phthalic acid manganese polymer and preparation method thereof - Google Patents
Phthalic acid manganese polymer and preparation method thereof Download PDFInfo
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- CN106496578A CN106496578A CN201610869690.3A CN201610869690A CN106496578A CN 106496578 A CN106496578 A CN 106496578A CN 201610869690 A CN201610869690 A CN 201610869690A CN 106496578 A CN106496578 A CN 106496578A
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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
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- C08G83/008—Supramolecular polymers
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Abstract
The invention discloses a kind of phthalic acid manganese polymer and preparation method thereof.(1) weigh 0.5 ~ 1 mM of four anhydrous manganese to be dissolved in 2 ~ 4 milliliters of distilled water.(2) weigh 0.5 ~ 1 mM of phthalic acid to be dissolved in 5 ~ 10 milliliters of distilled water.(3) weigh 1 ~ 2 mM of sodium hydroxide to be dissolved in 1 ~ 2 milliliter of distilled water.(4) step (1), (2) and solution obtained in (3) are added in ptfe autoclave inner bag, put stainless steel cauldron overcoat and be put in 140 degrees Celsius of baking ovens and react 48 ~ 72 hours, room temperature is down to 10 degrees Celsius of gradients per hour after the completion of reaction, drive kettle to obtain without colour band white powder precipitation solution after standing 12 hours, after filtration, filtrate is put in beaker and stands 20 30 days, cup bottom separates out colourless acicular crystal, as phthalic acid manganese polymer.Present invention process is simple, with low cost, reproducible, provides certain foundation for synthesizing the manganese polymer of the rhombic system of transition metal.
Description
Technical field
The invention belongs to technical field of polymer preparation, more particularly to a kind of phthalic acid manganese polymer and its preparation side
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.Research by aromatic polycarboxylic acids class part synthesizing new metallic organic framework is this
The molecule assembling emphasis in field.Hydroxy-acid group can be with monodentate, bidentate（Bridge-type, chelating）With multiple coordination modes such as three flute profiles with
Transition metal ionss 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 phthalic acid manganese polymer and preparation method thereof.
The thinking of the present invention：Using phthalic acid and manganese sulfate, manganese complex is obtained by hydro-thermal method.
Phthalic acid manganese polymer belongs to rhombic system, and space group isPbca, central metallic ions are Mn (II) ion.
The polymer each primitive includes Mn (II) ion, an O-phthalic acid anion and a water of coordination molecule.Adjacent benzene
One carboxyl of dioctyl phthalate is coordinated with manganese ion in the form of three tooth of bridge-type, another carboxyl chelating-three tooth of bridge-type in the form of
It is coordinated with manganese ion.Central metallic ions Mn (II) respectively with from four phthalic acids six oxygen atoms (O1, O2B,
O2C, O3A, O3B, O4A), and oxygen atom (O5) coordination of a hydrone.Seven coordination atoms are around Mn (II) ion
With irregularly decahedral form arrangement.Mn-O bond distance is between 2.246-2.462.
The preparation method of phthalic acid manganese polymer is concretely comprised the following steps：
(1) weigh 0.5 ~ 1 mM of four anhydrous manganese to be dissolved in 2 ~ 4 milliliters of distilled water, manganese sulfate solution is obtained.
(2) weigh 0.5 ~ 1 mM of phthalic acid to be dissolved in 5 ~ 10 milliliters of distilled water, phthalic 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, are put stainless
Steel reactor overcoat is put in 140 degrees Celsius of baking ovens and reacts 48 ~ 72 hours, with 10 degrees Celsius of gradient drops per hour after the completion of reaction
To room temperature, kettle being driven after standing 12 hours and being obtained without colour band white powder precipitation solution, after filtration, filtrate is put in beaker and stands 20-30
My god, cup bottom separates out colourless acicular crystal, as manganese polymer.
The present invention has process is simple, with low cost, reproducible, has successfully synthesized manganese complex, has been conjunction
Manganese polymer into the rhombic system of transition metal provides certain foundation.
Description of the drawings
Fig. 1 is the molecular structure of phthalic acid manganese polymer of the present invention.
Specific embodiment
Embodiment：
(1) 0.5 mM is weighed（0.1115 gram）Four anhydrous manganeses are dissolved in 2 milliliters of distilled water, and manganese sulfate solution is obtained.
(2) 0.5 mM is weighed（0.0885 gram）Phthalic acid is dissolved in 5 milliliters of distilled water, and O-phthalic is obtained
Acid solution.
(3) 1 mM is weighed（0.0400 gram）Sodium hydroxide is dissolved in 1 milliliter 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 140 degrees Celsius of baking ovens and reacts 48 ~ 72 hours, with 10 degrees Celsius of gradient drops per hour after the completion of reaction
To room temperature, kettle being driven after standing 12 hours and being obtained without colour band white powder precipitation solution, after filtration, filtrate is put in beaker and stands 20-30
My god, cup bottom separates out colourless acicular crystal, as phthalic acid manganese polymer.
Phthalic acid manganese polymer molecular structure is shown in that Fig. 1, crystallographic structural analysis show, the polymer belongs to orthorhombic
It is that space group isPbca, central metallic ions are Mn (II) ion.The polymer each primitive comprising Mn (II) ion,
One O-phthalic acid anion and a water of coordination molecule.One carboxyl of phthalic acid is in the form of three tooth of bridge-type and manganese
Ion coordination, another carboxyl chelating-three tooth of bridge-type in the form of be coordinated with manganese ion.Central metallic ions Mn (II) respectively with
From six oxygen atoms (O1, O2B, O2C, O3A, O3B, O4A) of four phthalic acids, and the oxygen atom of a hydrone
(O5) it is coordinated.Seven coordination atoms are around Mn (II) ion with irregularly decahedral form arrangement.Mn-O bond distance is 2.246
Between -2.462.
Claims (2)
1. a kind of phthalic acid manganese polymer, it is characterised in that the structural formula of phthalic acid manganese polymer is：
The phthalic acid manganese polymer belongs to rhombic system, and space group is Pbca, and central metallic ions are Mn (II) ion；
The polymer each primitive includes Mn (II) ion, an O-phthalic acid anion and a water of coordination molecule；Adjacent benzene
One carboxyl of dioctyl phthalate is coordinated with manganese ion in the form of three tooth of bridge-type, another carboxyl chelating-three tooth of bridge-type in the form of
It is coordinated with manganese ion；Central metallic ions Mn (II) with six oxygen atoms from four phthalic acids be respectively O1, O2B,
O2C, O3A, O3B, O4A, and the oxygen atom of a hydrone be O5 coordination；Seven coordination atoms around Mn (II) ion with
Irregularly decahedral form arrangement；Mn-O bond distance existsBetween.
2. the preparation method of phthalic acid manganese polymer according to claim 1, it is characterised in that concretely comprise the following steps：
(1) weigh 0.5～1 mM of four anhydrous manganese to be dissolved in 2～4 milliliters of distilled water, manganese sulfate solution is obtained；
(2) weigh 0.5～1 mM of phthalic acid to be dissolved in 5～10 milliliters of distilled water, phthalic acid solution is obtained；
(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 140 degrees Celsius of baking ovens to react 48～72 hours, be down to 10 degrees Celsius of gradients per hour after the completion of reaction
Room temperature, drives kettle and obtains without colour band white powder precipitation solution after standing 12 hours, after filtration, filtrate is put in beaker and stands 20-30
My god, cup bottom separates out colourless acicular crystal, as phthalic acid manganese polymer.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610869690.3A CN106496578A (en) | 2016-10-01 | 2016-10-01 | Phthalic acid manganese polymer and preparation method thereof |
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| CN201610869690.3A CN106496578A (en) | 2016-10-01 | 2016-10-01 | Phthalic acid manganese polymer and preparation method thereof |
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Cited By (1)
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232492A (en) * | 2013-02-04 | 2013-08-07 | 昆明学院 | Mn binuclear magnetic single crystal complex and its preparation method and use |
| CN105237576A (en) * | 2015-10-19 | 2016-01-13 | 桂林理工大学 | Trinuclear manganese complex and preparation method thereof |
| CN105399774A (en) * | 2015-11-20 | 2016-03-16 | 天津工业大学 | Manganese complex containing bi(triazol) butane and pyrazine diacid and preparation method of manganese complex |
-
2016
- 2016-10-01 CN CN201610869690.3A patent/CN106496578A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232492A (en) * | 2013-02-04 | 2013-08-07 | 昆明学院 | Mn binuclear magnetic single crystal complex and its preparation method and use |
| CN105237576A (en) * | 2015-10-19 | 2016-01-13 | 桂林理工大学 | Trinuclear manganese complex and preparation method thereof |
| CN105399774A (en) * | 2015-11-20 | 2016-03-16 | 天津工业大学 | Manganese complex containing bi(triazol) butane and pyrazine diacid and preparation method of manganese complex |
Cited By (1)
| 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 |
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Application publication date: 20170315 |
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