CN106083914A - M-phthalic acid 5 sulfonic acid lead coordination polymer and preparation method thereof - Google Patents

M-phthalic acid 5 sulfonic acid lead coordination polymer and preparation method thereof Download PDF

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Publication number
CN106083914A
CN106083914A CN201610422437.3A CN201610422437A CN106083914A CN 106083914 A CN106083914 A CN 106083914A CN 201610422437 A CN201610422437 A CN 201610422437A CN 106083914 A CN106083914 A CN 106083914A
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China
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sulfonic acid
phthalic acid
lead
oxygen atom
acid
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CN201610422437.3A
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Inventor
张秀清
范超逸
倪萌
李家星
韦华传
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Guilin University of Technology
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Guilin University of Technology
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Priority to CN201610422437.3A priority Critical patent/CN106083914A/en
Publication of CN106083914A publication Critical patent/CN106083914A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00Compounds containing elements of Groups 4 or 14 of the Periodic System
    • C07F7/24Lead compounds

Abstract

The invention discloses a kind of M-phthalic acid 5 sulfonic acid lead coordination polymer and preparation method thereof.Utilizing M-phthalic acid 5 sodium sulfonate, 4 phenylpyridines to prepare this M-phthalic acid 5 sulfonic acid lead coordination polymer for part and plumbi nitras by hydro-thermal method, its structural formula is:;The present invention has the advantages such as technique is simple, with low cost, reproducible, has successfully synthesized lead coordination polymer, provides certain foundation for synthesis transient metal complex.

Description

M-phthalic acid-5-sulfonic acid lead coordination polymer and preparation method thereof
Technical field
The invention belongs to complex preparing technical field, particularly to a kind of M-phthalic acid-5-sulfonic acid lead coordination polymerization Thing and preparation method thereof.
Background technology
Lead atom radius is relatively big, and ligancy is a lot, is coordinated to ten coordinations from two and all has been reported.The electron outside nucleus distribution of lead For 4f145d106s2, there are lone pair electrons, ligancy can be made to reduce, owing to the repulsive interaction of lone pair electrons reduces coordinate bond Distributed areas.Carboxyl coordination mode has a variety of, for example, and monodentate, bidentate, chelating, bridging, chelating bridging etc..With containing carboxylic The part of base and lead react, and can form the various complex of coordination mode, and application prospect is extensive.
Content of the invention
It is an object of the invention to provide a kind of M-phthalic acid-5-sulfonic acid lead coordination polymer and preparation method thereof.
The thinking of the present invention: utilize 5-sodium sulfo isophthalate, 4-phenylpyridine to pass through hydro-thermal for part and plumbi nitras Method obtains lead coordination polymer.
The structural formula of the M-phthalic acid-5-sulfonic acid lead coordination polymer of the present invention is:
This M-phthalic acid-5-sulfonic acid lead coordination polymer belongs to anorthic system, and space group is P-1;This polymer is basic Construction unit includes four lead ions, two M-phthalic acid-5-sulfonic acid anions, two hydroxide radical anions and two moisture Son, two carboxyls of M-phthalic acid-5-sulfonic acid anion are all the coordination modes and two kinds of lead ions using and chelating bridging Pb1, Pb2 are coordinated, and sulfonate radical is coordinated with Pb1 by an oxygen atom;Wherein Pb1 is hexa-coordinate, different from from two Sulfonic oxygen atom O5B in M-phthalic acid-5-sulfonic acid anion, carboxyl oxygen atom O6, O7 are coordinated, also different from two Oxygen atom O9, O9A hydroxy, and a hydrone oxygen atom O8 coordination;The Pb2 isophthalic diformazan different from from three Carboxyl oxygen atom O1F, O1C, O2C, O6 in acid-5-sulfonic acid anion and a hydroxyl O9 coordination, ligancy is 5;Pb-O Bond distance is between 2.3427 (2) ~ 2.3995 (2).
The preparation method of above-mentioned M-phthalic acid-5-sulfonic acid lead coordination polymer is:
(1) weigh 0.2 ~ 1 mM of plumbi nitras to be dissolved in the distilled water of 5 ~ 10 milliliters, prepare lead nitrate solution.
(2) weigh 0.1 ~ 0.5 mM of 5-sodium sulfo isophthalate to be dissolved in 10 ~ 12 milliliters of distilled water, by gained It is in the reactor of 25 milliliters that solution moves into volume, then add in reactor 0.2 ~ 1 mM of NaOH, 0.1 ~ 0.5 MM 4-phenylpyridine and step (1) prepare lead nitrate solution, by reactor seal, isothermal reaction 3 at 160 DEG C My god, it is then slowly cooled to room temperature, filter, obtain white chunks crystal, be M-phthalic acid-5-sulfonic acid lead coordination polymerization Thing.
The present invention has the advantages such as technique is simple, with low cost, reproducible, has successfully synthesized M-phthalic acid-5- Sulfonic acid lead coordination polymer, provides certain foundation for synthesis transient metal complex.
Brief description
Fig. 1 is the molecular structure of the M-phthalic acid-5-sulfonic acid lead coordination polymer of the present invention.
Detailed description of the invention
Embodiment:
(1) weigh 0.1 mM of (0.0331 g) plumbi nitras to be dissolved in the distilled water of 5 milliliters, prepare lead nitrate solution.
(2) weigh 0.1 mM of (0.0268 g) 5-sodium sulfo isophthalate to be dissolved in 10 milliliters of distilled water, will Gained solution moves in the reactor that volume is 25 milliliters, then adds 0.2 mM of (0.008 g) hydroxide in reactor Reactor is sealed by the lead nitrate solution that sodium, the 4-phenylpyridine of 0.1 mM (0.0155 g) and step (1) prepare, At 160 DEG C, isothermal reaction 3 days, are then slowly cooled to room temperature, and filter, obtain white chunks crystal, be M-phthalic acid-5- Sulfonic acid lead coordination polymer.Its structural formula is:
Crystallographic structural analysis shows, it is tiltedly brilliant that the present embodiment gained M-phthalic acid-5-sulfonic acid lead coordination polymer belongs to three System, space group is P-1.This polymer basic structural unit includes four lead ions, two M-phthalic acid-5-sulfonic acid cloudy from Son, two hydroxide radical anions and two hydrones, two carboxyls of M-phthalic acid-5-sulfonic acid anion are all to use chelating The coordination mode of bridging and two kinds of lead ion Pb1, Pb2 coordinations, sulfonate radical is coordinated with Pb1 by an oxygen atom.Wherein Pb1 is Hexa-coordinate, the sulfonic oxygen atom O5B in M-phthalic acid-5-sulfonic acid anion different from from two, carboxyl oxygen Atom O6, O7 are coordinated, also different from two oxygen atom O9, O9A hydroxy, and the oxygen atom O8 coordination of a hydrone. Carboxyl oxygen atom O1F, O1C, O2C, O6 in the Pb2 M-phthalic acid-5-sulfonic acid anion different from from three and one Hydroxyl O9 is coordinated, and ligancy is 5.Pb-O bond distance is between 2.3427 (2) ~ 2.3995 (2).

Claims (2)

1. a M-phthalic acid-5-sulfonic acid lead coordination polymer, it is characterised in that this M-phthalic acid-5-sulfonic acid lead polycomplexation The structural formula of compound is:
Described M-phthalic acid-5-sulfonic acid lead coordination polymer belongs to anorthic system, and space group is P-1;This polymer is tied substantially Structure unit includes four lead ions, two M-phthalic acid-5-sulfonic acid anions, two hydroxide radical anions and two moisture Son, two carboxyls of M-phthalic acid-5-sulfonic acid anion are all the coordination modes and two kinds of lead ions using and chelating bridging Pb1, Pb2 are coordinated, and sulfonate radical is coordinated with Pb1 by an oxygen atom;Wherein Pb1 is hexa-coordinate, different from from two Sulfonic oxygen atom O5B in M-phthalic acid-5-sulfonic acid anion, carboxyl oxygen atom O6, O7 are coordinated, also different from two Oxygen atom O9, O9A hydroxy, and a hydrone oxygen atom O8 coordination;The Pb2 isophthalic diformazan different from from three Carboxyl oxygen atom O1F, O1C, O2C, O6 in acid-5-sulfonic acid anion and a hydroxyl O9 coordination, ligancy is 5;Pb-O Bond distance is between 2.3427 (2) ~ 2.3995 (2).
2. the method preparing M-phthalic acid-5-sulfonic acid lead coordination polymer as claimed in claim 1, it is characterised in that Concretely comprise the following steps:
(1) weigh 0.2 ~ 1 mM of plumbi nitras to be dissolved in the distilled water of 5 ~ 10 milliliters, prepare lead nitrate solution;
(2) weigh 0.1 ~ 0.5 mM of 5-sodium sulfo isophthalate to be dissolved in 10 ~ 12 milliliters of distilled water, by gained solution Move in the reactor that volume is 25 milliliters, in reactor, then add 0.2 ~ 1 mM of NaOH, 0.1 ~ 0.5 mmoles Reactor is sealed, isothermal reaction 3 days at 160 DEG C, so by the lead nitrate solution that your 4-phenylpyridine and step (1) prepare After be slowly cooled to room temperature, filter, obtain white chunks crystal, be M-phthalic acid-5-sulfonic acid lead coordination polymer.
CN201610422437.3A 2016-06-16 2016-06-16 M-phthalic acid 5 sulfonic acid lead coordination polymer and preparation method thereof Pending CN106083914A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106800659A (en) * 2017-01-19 2017-06-06 洛阳理工学院 A kind of three-dimensional lead coordination polymer with fluorescence property and preparation method thereof
CN107057081A (en) * 2017-04-24 2017-08-18 桂林理工大学 Preparation, structure and its photoluminescent property of M-phthalic acid lead polymer

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CN105367609A (en) * 2015-10-19 2016-03-02 桂林理工大学 Trinuclear cobalt complex and preparation method thereof
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CN104672277A (en) * 2015-03-13 2015-06-03 辽宁大学 Metal organic framework material based on bowl-shaped structure and application thereof
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106800659A (en) * 2017-01-19 2017-06-06 洛阳理工学院 A kind of three-dimensional lead coordination polymer with fluorescence property and preparation method thereof
CN107057081A (en) * 2017-04-24 2017-08-18 桂林理工大学 Preparation, structure and its photoluminescent property of M-phthalic acid lead polymer

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