CN107033173A - The structure and its photoluminescent property for the cadmium complex constructed with terephthalic acid (TPA) and pyrazine - Google Patents

The structure and its photoluminescent property for the cadmium complex constructed with terephthalic acid (TPA) and pyrazine Download PDF

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Publication number
CN107033173A
CN107033173A CN201710272886.9A CN201710272886A CN107033173A CN 107033173 A CN107033173 A CN 107033173A CN 201710272886 A CN201710272886 A CN 201710272886A CN 107033173 A CN107033173 A CN 107033173A
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China
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tpa
terephthalic acid
complex
pyrazine
cadmium
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张秀清
李家星
杨洪利
倪萌
劳思思
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Guilin University of Technology
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Guilin University of Technology
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    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F3/00Compounds containing elements of Groups 2 or 12 of the Periodic Table
    • C07F3/003Compounds containing elements of Groups 2 or 12 of the Periodic Table without C-Metal linkages
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    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/06Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07BGENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B2200/00Indexing scheme relating to specific properties of organic compounds
    • C07B2200/13Crystalline forms, e.g. polymorphs
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K2211/00Chemical nature of organic luminescent or tenebrescent compounds
    • C09K2211/18Metal complexes
    • C09K2211/188Metal complexes of other metals not provided for in one of the previous groups

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses the preparation of terephthalic acid (TPA) pyrazine cadmium complex, structure and its photoluminescent property.The complex belongs to anorthic system, and space group is

Description

The structure and its photoluminescent property for the cadmium complex constructed with terephthalic acid (TPA) and pyrazine
Technical field
The invention belongs to complex preparing technical field, more particularly to a kind of system of terephthalic acid (TPA) pyrazine cadmium complex Standby, structure and its photoluminescent property.
Background technology
Carboxylic acids organic coordination compound is developed rapidly in recent years, and as carboxylic acids part, because it is special A large amount of presence of the weak interaction such as coordination ability and hydrogen bond, receive the extensive concern of domestic and international chemist.To benzene two Formic acid had been widely used in the construction unit of conformation function type coordination polymer in recent years, and not only its carboxyl has monodentate ligand, Double coordination, bridging, a variety of coordination modes such as chelating, and its phenyl ring can also form π complexs.In addition, for pyrazine, it Big pi bond is conjugated with intramolecular, product can be determined as highly effective chromophore, and with good intramolecular electricity Son transmission and energy transmission property, are a kind of good assistant ligands.
The content of the invention
It is an object of the invention to provide a kind of preparation, structure and its photoluminescent property of terephthalic acid (TPA) pyrazine cadmium complex.
The thinking of the present invention:It is that part and cadmium nitrate obtain terephthaldehyde by hydro-thermal method using terephthalic acid (TPA), pyrazine Sour pyrazine cadmium complex.
The structure of terephthalic acid (TPA) pyrazine cadmium complex is shown in accompanying drawing 1.The complex belongs to anorthic system, and space group is P ī, In the complex, the carboxyl on terephthalic acid (TPA) is coordinated in the form of chelating with Metal Ions Cd (II), and pyrazine is with bridge The oxygen that the form of connection is participated in coordination, water provides lone pair electrons and is coordinated with Metal Ions Cd (II) formation coordinate bond, and Hydrone and another hydrone formation hydrogen bond, more strengthen the stability of complex.Central metallic ions Cd (II) is respectively with coming From four oxygen atoms (O3, O4, O6, O5) on two different terephthalic acid (TPA) parts, each nitrogen-atoms of two pyrazines Oxygen atom (O9) coordination in (N1, N2A), hydrone.Cd-O bond distance existsBetween, Cd-N bond distance is
The preparation method of the terephthalic acid (TPA) pyrazine cadmium complex is:
(1) weigh 0.3~0.6 mM of six nitric hydrate cadmium to be dissolved in 2~4 milliliters of distilled water, cadmium nitrate is made molten Liquid;
(2) weigh 0.3~0.6 mM of terephthalic acid (TPA) to be dissolved in 5~10 milliliters of distilled water, terephthalic acid (TPA) is made Solution;
(3) weigh 0.3~0.6 mM of pyrazine to be dissolved in 2~4 milliliters of distilled water, pyrazine solution is made;
(4) above-mentioned solution is mixed and added into 0.6~1.2 mM of triethylamine;
(5) solution obtained above is added in ptfe autoclave inner bag, at room temperature magnetic agitation 0.5~ 1 hour, put stainless steel cauldron overcoat be put into 130 degrees Celsius react 48~72 hours, taken the photograph after the completion of reaction with per hour 10 Family name's degree gradient is down to room temperature, and driving kettle after standing 12~24 hours obtains colourless solution, filters to obtain water white transparency bulk crystals, is pair Phthalic acid pyrazine cadmium complex.
The present invention has the advantages that technique is simple, with low cost, reproducible, has successfully synthesized terephthalic acid (TPA) pyrazine Cadmium complex, the complex for synthesis transition metal provides certain foundation.
The test of fluorescence property is carried out to part terephthalic acid (TPA) and complex at room temperature, as shown in Figure 2.To benzene Dioctyl phthalate is in the case where 280nm wavelength is excited, and maximum emission wavelength is at 385nm.Complex under 290nm excitation wavelengths, Fluorescent quenching.
Brief description of the drawings
Fig. 1 is the molecular structure of the terephthalic acid (TPA) pyrazine cadmium complex of the present invention.
Fig. 2 is the terephthalic acid (TPA) of the present invention and the room temperature solid fluorescence emission spectrum of complex.
Embodiment
Embodiment:
(1) weigh 0.3 mM of (0.0709 gram) cadmium nitrate to be dissolved in 3 milliliters of distilled water, nitric acid cadmium solution is made;
(2) weigh 0.3 mM of (0.0498 gram) terephthalic acid (TPA) to be dissolved in 5 milliliters of distilled water, terephthaldehyde is made Acid solution;
(3) weigh 0.3 mM of (0.0240 gram) pyrazine to be dissolved in 2 milliliters of distilled water, pyrazine solution is made;
(4) above-mentioned solution is mixed and added into 0.6 mM of (0.0607 gram) triethylamine;
(5) solution made from step (1), (2), (3) and (4) is added in ptfe autoclave inner bag, in room The lower magnetic agitation of temperature 0.5 hour, puts stainless steel cauldron overcoat and is put into 130 degrees Celsius and react 72 hours, after the completion of reaction with 10 degrees Celsius of gradients are down to room temperature per hour, and driving kettle after standing 12 hours obtains colourless solution, filters to obtain water white transparency bulk crystals, As terephthalic acid (TPA) pyrazine cadmium complex.
The complex belongs to anorthic system, and space group is P ī, and in the complex, the carboxyl on terephthalic acid (TPA) is with chela The form of conjunction is coordinated with Metal Ions Cd (II), and the oxygen that pyrazine is participated in the form of bridging in coordination, water provides lone pair electrons It is coordinated with Metal Ions Cd (II) formation coordinate bond, and hydrone and another hydrone formation hydrogen bond, more strengthen and match somebody with somebody The stability of compound.Central metallic ions Cd (II) respectively from four oxygen originals on two different terephthalic acid (TPA) parts Oxygen atom (O9) coordination in sub (O3, O4, O6, O5), each nitrogen-atoms (N1, N2A) of two pyrazines, hydrone.Cd-O keys Length exists Between, Cd-N bond distance is

Claims (3)

1. a kind of structure of terephthalic acid (TPA) pyrazine cadmium complex.The complex belongs to anorthic system, and space group is P ī, is matched somebody with somebody at this In compound, the carboxyl on terephthalic acid (TPA) is coordinated in the form of chelating with Metal Ions Cd (II), and pyrazine is with the shape of bridging The oxygen that formula is participated in coordination, water provides lone pair electrons and is coordinated with Metal Ions Cd (II) formation coordinate bond, and hydrone With another hydrone formation hydrogen bond, the stability of complex is more strengthened.Central metallic ions Cd (II) respectively with from two Four oxygen atoms (O3, O4, O6, O5) on different terephthalic acid (TPA) parts, each nitrogen-atoms (N1, N2A) of two pyrazines, Oxygen atom (O9) coordination in hydrone.Cd-O bond distance existsBetween, Cd-N bond distance is
2. the preparation method of terephthalic acid (TPA) pyrazine cadmium complex according to claim 1, it is characterised in that specific steps For:
(1) weigh 0.3~0.6 mM of six nitric hydrate cadmium to be dissolved in 2~4 milliliters of distilled water, nitric acid cadmium solution is made;
(2) weigh 0.3~0.6 mM of terephthalic acid (TPA) to be dissolved in 5~10 milliliters of distilled water, terephthalic acid (TPA) is made molten Liquid;
(3) weigh 0.3~0.6 mM of pyrazine to be dissolved in 2~4 milliliters of distilled water, pyrazine solution is made;
(4) above-mentioned solution is mixed and added into 0.6~1.2 mM of triethylamine;
(5) solution obtained above is added in ptfe autoclave inner bag, magnetic agitation 0.5~1 is small at room temperature When, put stainless steel cauldron overcoat be put into 130 degrees Celsius react 48~72 hours, with 10 degrees Celsius per hour after the completion of reaction Gradient is down to room temperature, and driving kettle after standing 12~24 hours obtains colourless solution, filters to obtain water white transparency bulk crystals, is to benzene two Formic acid pyrazine cadmium complex.
3. the photoluminescent property of complex
The test of fluorescence property has been carried out to part terephthalic acid (TPA) and complex at room temperature.Terephthalic acid (TPA) is 280nm's Wavelength is excited down, and maximum emission wavelength is at 385nm.Complex is under 290nm excitation wavelengths, fluorescent quenching.
CN201710272886.9A 2017-04-24 2017-04-24 The structure and its photoluminescent property for the cadmium complex constructed with terephthalic acid (TPA) and pyrazine Pending CN107033173A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106366101A (en) * 2016-09-12 2017-02-01 桂林理工大学 Phthalic acid cadmium complex and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106366101A (en) * 2016-09-12 2017-02-01 桂林理工大学 Phthalic acid cadmium complex and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
LEE, CHIN-FEN ET AL.: "Self-adaptation of a conformationally flexible yet restricted "piperazine-pyrazine" building block toward the design of coordination polymers", 《CRYSTENGCOMM》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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