CN101898997A - Method for preparing novel zinc terpyridine blue fluorescent powder - Google Patents

Method for preparing novel zinc terpyridine blue fluorescent powder Download PDF

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Publication number
CN101898997A
CN101898997A CN2009101133300A CN200910113330A CN101898997A CN 101898997 A CN101898997 A CN 101898997A CN 2009101133300 A CN2009101133300 A CN 2009101133300A CN 200910113330 A CN200910113330 A CN 200910113330A CN 101898997 A CN101898997 A CN 101898997A
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zinc
fluorescent powder
blue fluorescent
terpyridine
preparing novel
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王吉德
赵本桉
岳凡
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Xinjiang University
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Xinjiang University
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Abstract

The invention relates to a method for preparing novel zinc terpyridine blue fluorescent powder, which is characterized in that: 4'-(4-methoxyphenyl)-2,2':6'2''-terpyridine and a zinc salt are used as a raw materials; and a solvothermal method is adopted. The method is suitable for different zinc salts and can obtain different kinds of blue fluorescent powder with similar structures.

Description

A kind of preparation method of novel zinc terpyridine blue fluorescent powder
Technical field
The present invention relates to a kind of preparation method of zinc terpyridine blue fluorescent powder, can obtain the similar fluorescent material of series structure, and remarkable advantage is arranged on fluorescence intensity by this method.Its chemical formula general formula is: [Zn (C 22H 17N 3O) 2] (Y) 2, general structure is:
Figure B2009101133300D0000011
Y is the negatively charged ion of different zinc salts, can be perchlorate, nitrate radical, acetate or chlorion.
Background technology
The optical information material more and more causes the concern of scientific and technological circle as the technical support of information society.Embedded photoluminescent material becomes one of important topic of current research field.Up to the present, great variety of organic oneself be used as luminescent material research.The fluorescence quantum efficiency height of small molecules organic compound, and be easy to purify, but thermostability is relatively poor relatively.The high molecular polymer Heat stability is good, but purity is difficult for improving.
The character of metal complexes promptly has the advantage of organic high fluorescence quantum efficiency between organic and inorganics, therefore the characteristics of the good stability of organic/inorganic substance again are considered to have most a class luminescent material of application prospect.In recent ten years, the discovery of complex electroluminescent material and the widespread use in organic electroluminescence device thereof make the research of complex luminescent material step into a brand-new stage.Blue light material for one of three primary colors in the luminescent material also has some problems to need to be resolved hurrily (brightness, efficient is low) at present, and many scientific workers drop into great enthusiasm aspect the synthetic and research of blue fluorescent material.For this reason this paper select for use conjugated degree better and the stronger terpyridyl of coordination ability as raw material, adopt the preparation method of solvent thermal to obtain serial novel zinc terpyridine blue fluorescent material.
Summary of the invention
The object of the present invention is to provide a kind of easy method for preparing blue colour fluorescent powder.Can obtain serial luminous intensity and the higher zinc terpyridine blue fluorescent material of luminous efficiency by this method.
Embodiment
Embodiment 1: take by weighing 4 respectively '-(4-p-methoxy-phenyl)-2,2 ': 6 ', 2 " and terpyridyl (0.068g, 0.2mmol) and Zn (ClO 4) 26H 2O (0.037g, 0.1mmol), the ratio of amount of substance is 2: 1, join in the mixed solvent that contains 8ml ethanol and 4ml water, after at room temperature stirring 30min, join in the 15ml hydrothermal reaction kettle, reacted 3 days down at 160 ℃, drop to room temperature with 5 ℃ speed per hour then, brown bulk crystals 0.065g.Yield: 70%[is with Zn (ClO 4) 26H 2O calculates].When solid-state, this title complex is through λ ExAfter the optical excitation of=371nm, at λ EmA strong characteristic fluorescence appears in=416nm place.
Embodiment 2: take by weighing 4 respectively '-(4-p-methoxy-phenyl)-2,2 ': 6 ', 2 " and terpyridyl (0.068g, 0.2mmol) and Zn (NO 3) 26H 2O (0.030g, 0.1mmol), the ratio of amount of substance is 2: 1, join in the mixed solvent that contains 8ml ethanol and 4ml water, after at room temperature stirring 30min, join in the 15ml hydrothermal reaction kettle, reacted 3 days down at 160 ℃, drop to room temperature with 5 ℃ speed per hour then, yellow bulk crystals 0.057g.Yield: 66%[is with Zn (NO 3) 26H 2O calculates].When solid-state, this title complex is through λ ExAfter the optical excitation of=380nm, at λ EmA strong characteristic fluorescence appears in=425nm place
Embodiment 3: take by weighing 4 respectively '-(4-p-methoxy-phenyl)-2,2 ': 6 ', 2 " and terpyridyl (0.068g, 0.2mmol) and Zn (OAc) 22H 2O (0.03g, 0.1mmol), the ratio of amount of substance is 2: 1, join in the mixed solvent that contains 8ml ethanol and 4ml water, after at room temperature stirring 30min, join in the 15ml hydrothermal reaction kettle, reacted 3 days down at 160 ℃, drop to room temperature with 5 ℃ speed per hour then, yellow bulk crystals 0.053g.Yield: 61%[is with Zn (OAc) 26H 2O calculates].When solid-state, this title complex is through λ ExAfter the optical excitation of=365nm, at λ EmA strong characteristic fluorescence appears in=410nm place
Embodiment 4: take by weighing 4 respectively '-(4-p-methoxy-phenyl)-2,2 ': 6 ', 2 " and terpyridyl (0.068g, 0.2mmol) and ZnCl 2(0.014g, 0.1mmol), the ratio of amount of substance is 2: 1, join in the mixed solvent that contains 8ml ethanol and 4ml water, after at room temperature stirring 30min, join in the 15ml hydrothermal reaction kettle, reacted 3 days down at 160 ℃, drop to room temperature with 5 ℃ speed per hour then, colourless tabular crystal 0.061g.Yield: 75%[is with ZnCl 2Calculate].When solid-state, this title complex is through λ ExAfter the optical excitation of=390nm, at λ EmA strong characteristic fluorescence appears in=442nm place.

Claims (2)

1. the preparation method of a novel zinc terpyridine blue fluorescent powder, adopt 4 '-(4-p-methoxy-phenyl)-2,2 ': 6 ', 2 " terpyridyl and zinc salt are raw material.It is characterized in that adopting ' solvent-thermal method ' to prepare this series blue colour fluorescent powder.
2. preparation method according to claim 1 is characterized in that:
(1), reaction raw materials 4 '-(4-p-methoxy-phenyl)-2,2 ': 6 ', 2 " ratio of the amount of substance of terpyridyl and zinc salt is: 2: 1, wherein zinc salt can be zinc acetate, zinc nitrate, zinc perchlorate or zinc chloride.
(2), the solvent that solvent thermal adopted is an ethanol.
CN2009101133300A 2009-05-25 2009-05-25 Method for preparing novel zinc terpyridine blue fluorescent powder Pending CN101898997A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109280175A (en) * 2018-08-31 2019-01-29 华中科技大学 A kind of organic two-dimensional material of novel covalent metal and preparation method thereof
CN109608651A (en) * 2018-12-17 2019-04-12 华中科技大学 A kind of rare earth two-dimensional material, preparation method and application
CN111875624A (en) * 2020-06-06 2020-11-03 桂林理工大学 Preparation, structure and fluorescence application of four-core zinc complex based on bteb
CN112358696A (en) * 2020-11-05 2021-02-12 杭州锦新高分子材料有限公司 Calcium-zinc stabilizer

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109280175A (en) * 2018-08-31 2019-01-29 华中科技大学 A kind of organic two-dimensional material of novel covalent metal and preparation method thereof
CN109608651A (en) * 2018-12-17 2019-04-12 华中科技大学 A kind of rare earth two-dimensional material, preparation method and application
CN111875624A (en) * 2020-06-06 2020-11-03 桂林理工大学 Preparation, structure and fluorescence application of four-core zinc complex based on bteb
CN111875624B (en) * 2020-06-06 2022-06-14 桂林理工大学 Preparation, structure and fluorescence application of four-core zinc complex based on bteb
CN112358696A (en) * 2020-11-05 2021-02-12 杭州锦新高分子材料有限公司 Calcium-zinc stabilizer

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Application publication date: 20101201