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 PDFInfo
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- 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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- Prior art keywords
- sulfonic acid
- phthalic acid
- lead
- oxygen atom
- acid
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- 229920001795 coordination polymer Polymers 0.000 title claims abstract description 18
- 239000013256 coordination polymer Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title abstract description 6
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 title abstract 4
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 title abstract 3
- 238000000034 method Methods 0.000 claims abstract description 4
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 12
- JVZRCNQLWOELDU-UHFFFAOYSA-N 4-Phenylpyridine Chemical compound C1=CC=CC=C1C1=CC=NC=C1 JVZRCNQLWOELDU-UHFFFAOYSA-N 0.000 claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- -1 hydroxide radical anions Chemical class 0.000 claims description 6
- ZHUXMBYIONRQQX-UHFFFAOYSA-N hydroxidodioxidocarbon(.) Chemical group [O]C(O)=O ZHUXMBYIONRQQX-UHFFFAOYSA-N 0.000 claims description 6
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 150000004696 coordination complex Chemical class 0.000 abstract description 2
- 229910052708 sodium Inorganic materials 0.000 abstract description 2
- 239000011734 sodium Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 230000001052 transient effect Effects 0.000 abstract description 2
- XOGODJOZAUTXDH-UHFFFAOYSA-M (N-methylanilino)methanesulfonate Chemical compound CN(CS([O-])(=O)=O)c1ccccc1 XOGODJOZAUTXDH-UHFFFAOYSA-M 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 238000012718 coordination polymerization Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical group [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 description 1
- 229920002338 polyhydroxyethylmethacrylate Polymers 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/24—Lead compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
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
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.
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Cited By (2)
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 |
Citations (4)
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CN104311579A (en) * | 2014-09-15 | 2015-01-28 | 桂林理工大学 | 5-sulfoisophthalic acid copper salt complex and preparation method thereof |
CN104672277A (en) * | 2015-03-13 | 2015-06-03 | 辽宁大学 | Metal organic framework material based on bowl-shaped structure and application thereof |
CN105367589A (en) * | 2015-10-19 | 2016-03-02 | 桂林理工大学 | Isophthalic acid-5-silver sulfonate coordination polymer and preparation method |
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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2016
- 2016-06-16 CN CN201610422437.3A patent/CN106083914A/en active Pending
Patent Citations (4)
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CN104311579A (en) * | 2014-09-15 | 2015-01-28 | 桂林理工大学 | 5-sulfoisophthalic acid copper salt complex and preparation method thereof |
CN104672277A (en) * | 2015-03-13 | 2015-06-03 | 辽宁大学 | Metal organic framework material based on bowl-shaped structure and application thereof |
CN105367589A (en) * | 2015-10-19 | 2016-03-02 | 桂林理工大学 | Isophthalic acid-5-silver sulfonate coordination polymer and preparation method |
CN105367609A (en) * | 2015-10-19 | 2016-03-02 | 桂林理工大学 | Trinuclear cobalt complex and preparation method thereof |
Non-Patent Citations (3)
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GUO HONG-XU等: "Synthesis and crystal structure of an interpentateing 3-D framework constructed from mixed ligands", 《JIEGOU HUAXUE》 * |
JIAN LÜ等: "Assembly of two novel three-dimensional networks driven by alkali metals with an irreversible structural conversion", 《POLYHEDRON》 * |
范超逸等: "间苯二甲酸-5-磺酸铜配合物的合成及其晶体结构", 《中国化学会第九届全国无机化学学术会议论文集-B配位化学》 * |
Cited By (2)
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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