Novel polyoxometallate polymer and preparation method thereof

A polyoxometalate and polymer technology, which is applied in the fields of organic, polymer chemistry, inorganic and material chemistry, can solve the problems that polyoxometallate polymers have not been reported, and facilitate industrial production and popularization and application. Simple synthesis process and high product purity

Inactive Publication Date: 2013-08-21
NANKAI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation of polyoxometalate polymers by ring-o

Method used

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  • Novel polyoxometallate polymer and preparation method thereof
  • Novel polyoxometallate polymer and preparation method thereof
  • Novel polyoxometallate polymer and preparation method thereof

Examples

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Embodiment 1

[0033] Embodiment 1: N-dodecanoic acid-cis-5-norbornene-external-2,3-dicarboximide (norb-C 11 -COOH) synthesis

[0034] In a 25ml single-necked round bottom flask equipped with a water trap, add 164mg (1mmol) of cis-5-norbornene-exo-2,3-dicarboxylic anhydride, 237mg (1.1mmol) of 12-amino-dodecanoic acid Acid, 10ml toluene, reflux for 20h, stop the reaction. It was dissolved in 20 ml of ethyl acetate, washed three times with distilled water and saturated brine, dried over anhydrous sodium sulfate, filtered, spin-dried, and recrystallized from ethyl acetate to obtain 343 mg (0.95 mmol) of a white solid, with a yield of 95%.

Embodiment 2

[0035] Example 2: N-12-[tris(hydroxymethyl)methylamino]-dodecamide-cis-5-norbornene-external-2,3-dicarboximide (norb-C12-tris )Synthesis

[0036] In a 100ml single-necked round bottom flask, 1.09g (3.02mmol) of N-dodecanoic acid-cis-5-norbornene-exo-2,3-dicarboximide, 0.44g (3.63mmol) of trihydroxy Methylaminomethane, 1.12g (4.53mmol) was dissolved in 50ml of absolute ethanol, and refluxed for 12h. Spin dry, dissolve dichloromethane, filter to remove excess trishydroxymethylaminomethane, use 20:1 (v / v) dichloromethane:methanol as eluent, and pass through silica gel (100-200 mesh) column chromatography 998 mg (2.15 mmol) of the target compound were isolated with a yield of 71%.

Embodiment 3

[0037] Example 3: norbornenylated polyoxometalate hybrids (norb-C 12 -POM) synthesis

[0038] In a 50ml single-necked round bottom flask, add 46mg (0.098mmol) N-12-[tris(hydroxymethyl)methylamino]-dodecamide-cis-5-norbornene-exo-2,3-dimethyl imide, 484 mg (0.089 mmol) [(n-Bu) 4 N] 6 h 3 P 2 W 15 V 3 o 62 , 20ml of N,N-dimethylformamide, reacted at 85°C for 7 days. Concentrate, precipitate with ether, and centrifuge to obtain 510 mg of a yellow solid with a yield of 98%.

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Abstract

The invention innovatively relates to a novel polyoxometallate polymer obtained by directly polymerizing norbornylene functional polyoxometallate monomers by adopting an ROMP (Ring Opening Metathesis Polymerization) method, and measures the molecular weight distribution of the novel polyoxometallate polymer. The method disclosed by the invention is simple, convenient, fast, efficient and controllable, can obtain the target polymers at high yield within several hours through polymerization reaction in an open system, is simple in post processing, can be used for accurately controlling the molecular weight and easy to realize the industrialization; and the novel polyoxometallate polymer retains the excellent property of inorganic polyoxometallate and has potential application value on the aspects of catalysis, materials, medicines, and the like.

Description

technical field [0001] The present invention relates to polymer chemistry, organic, inorganic and material chemistry, especially a kind of polymerization technique that adopts ring-opening metathesis polymerization method to prepare polyoxometalate polymer, utilizes this polymerization method to make norbornene derivative functional Polyoxometalate polymerized directly to obtain a new type of polyoxometallate polymer. Background technique [0002] Polyoxometallate (POM) is a class of pre-transition metal atoms such as molybdenum (Mo), tungsten (W), vanadium (V) and central atoms such as phosphorus (P) and silicon (Si). A class of unimolecular clusters with a defined structure. Because of its rich chemical composition, diverse topological structures, special redox potential, and its excellent properties in catalysis, medicine, and optical, electrical, and magnetic functional materials, it has attracted widespread attention. , and has been deeply researched and applied. How...

Claims

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Application Information

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IPC IPC(8): C08F132/08
Inventor 王维苗文科王晓乐颜雨坤杨海宽吴涵任丽君
Owner NANKAI UNIV
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