CN109503856A - Polymer 4- (bis- (4- carboxyl phenyl) amino of N, N ' -) benzene sulfonic acid lead and synthetic method - Google Patents
Polymer 4- (bis- (4- carboxyl phenyl) amino of N, N ' -) benzene sulfonic acid lead and synthetic method Download PDFInfo
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- CN109503856A CN109503856A CN201811649867.4A CN201811649867A CN109503856A CN 109503856 A CN109503856 A CN 109503856A CN 201811649867 A CN201811649867 A CN 201811649867A CN 109503856 A CN109503856 A CN 109503856A
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- 238000010189 synthetic method Methods 0.000 title claims abstract description 8
- 229920000642 polymer Polymers 0.000 title claims abstract description 7
- -1 bis- (4- carboxyl phenyl) amino Chemical group 0.000 title abstract description 14
- HJKRMLJVGDBFRF-UHFFFAOYSA-N benzenesulfonic acid;lead Chemical compound [Pb].OS(=O)(=O)C1=CC=CC=C1 HJKRMLJVGDBFRF-UHFFFAOYSA-N 0.000 title abstract description 4
- YNPNZTXNASCQKK-UHFFFAOYSA-N Phenanthrene Natural products C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 claims abstract description 72
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims abstract description 67
- 239000013078 crystal Substances 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 5
- 239000012153 distilled water Substances 0.000 claims abstract description 5
- 229940046892 lead acetate Drugs 0.000 claims abstract description 5
- DNHVXYDGZKWYNU-UHFFFAOYSA-N lead;hydrate Chemical compound O.[Pb] DNHVXYDGZKWYNU-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 239000000178 monomer Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- HEWXLVDOSJBJME-UHFFFAOYSA-N 4-[[N-[(4-carboxyphenyl)methyl]-4-sulfoanilino]methyl]benzoic acid Chemical compound C(=O)(O)C1=CC=C(CN(CC2=CC=C(C=C2)C(=O)O)C2=CC=C(C=C2)S(=O)(=O)O)C=C1 HEWXLVDOSJBJME-UHFFFAOYSA-N 0.000 claims 1
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 claims 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract description 8
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 abstract description 6
- 229940092714 benzenesulfonic acid Drugs 0.000 abstract description 6
- 238000004458 analytical method Methods 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 3
- 239000000470 constituent Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000003446 ligand Substances 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000013256 coordination polymer Substances 0.000 description 2
- 229920001795 coordination polymer Polymers 0.000 description 2
- LENBSQBVUYZKPX-UHFFFAOYSA-N 4-[[(4-carboxyphenyl)methylamino]methyl]benzoic acid Chemical compound C1=CC(C(=O)O)=CC=C1CNCC1=CC=C(C(O)=O)C=C1 LENBSQBVUYZKPX-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000004467 single crystal X-ray diffraction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
Classifications
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- 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
- C07F7/003—Compounds containing elements of Groups 4 or 14 of the Periodic Table without C-Metal linkages
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a kind of polymer 4- (bis- (4- carboxyl phenyl) amino of N, N ' -) benzene sulfonic acid lead and synthetic methods.The monomer molecule formula of polymer are as follows: C92H68N10O16Pb3S2, molecular weight are as follows: 2255.25, H3L is 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid, and phen is point 1, a 10- Phen.Pure H will be analyzed3L and the pure phen of analysis are dissolved in the mixed solution of secondary distilled water and dehydrated alcohol, after adjusting pH is 8, is added the pure three water lead acetate of analysis, are placed in polytetrafluoroethylene (PTFE) autoclave, are placed in 170oC baking oven takes out after three days, is cooled to room temperature, and opens autoclave, colourless transparent sheet-like crystal i.e. { [Pb (phen) is arranged at bottom2]·[Pb2(L)2(phen)2]}n.Present invention process is simple, low in cost, chemical constituent is easily controllable, reproducible and yield is high.
Description
Technical field
It is { [Pb the present invention relates to a kind of polymer 4- (bis- (4- carboxyl phenyl) amino of N, N ' -) benzene sulfonic acid lead
(phen)2]·[Pb2(L)2(phen)2]}n(H3L is to analyze pure 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid, phen
To analyze pure 1,10- phenanthroline) and synthetic method.
Background technique
Coordination polymer (coordination polymer) is a nearly more than ten years Coordinative Chemistry direction with fastest developing speed,
It is one and is related to the multi-disciplinary brand-new research topic such as inorganic chemistry, organic chemistry and Coordinative Chemistry.Have inorganic material concurrently
The flexible characteristic of rigidity and organic material, makes it show huge development potentiality and tempting hair in terms of modern material research
Exhibition prospect.
Summary of the invention
The object of the invention is to be design synthetic polymer 4- (bis- (4- carboxyl phenyl) amino of N, N ' -) benzene sulfonic acid lead,
Utilize solvent structure { [Pb (phen)2]·[Pb2(L)2(phen)2]}n。
{ [Pb (phen) of the present invention2]·[Pb2(L)2(phen)2]}nMonomer molecule formula are as follows:
C92H68N10O16Pb3S2, molecular weight are as follows: 2255.25, H3L is 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid, and phen is
1,10- Phen.Crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
One, of table { [Pb (phen)2]·[Pb2(L)2(phen)2]}nCrystallographic parameter
Two, of table { [Pb (phen)2]·[Pb2(L)2(phen)2]}nPart bond distanceWith bond angle (°)
{ [the Pb (phen)2]·[Pb2(L)2(phen)2]}nSynthetic method specific steps are as follows:
0.110-0.220g is analyzed into pure H3L and 0.050-0.100g analyze pure phen be dissolved in 8-16mL secondary distilled water and
In the mixed solution of 1-2mL dehydrated alcohol, after adjusting pH is 8, adds 0.094-0.188g and analyze pure three water lead acetate, be placed in
It in polytetrafluoroethylene (PTFE) autoclave, is placed in 170 DEG C of baking ovens and is taken out after three days, is cooled to room temperature, open autoclave, bottom
There is colourless transparent sheet-like crystal i.e. { [Pb (phen) in portion2]·[Pb2(L)2(phen)2]}n.{ [Pb is measured by single crystal diffractometer
(phen)2]·[Pb2(L)2(phen)2]}nStructure, crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
The present invention has many advantages, such as that simple process, low in cost, chemical constituent is easily controllable, reproducible and yield is high.
Detailed description of the invention
Fig. 1 is the present invention { [Pb (phen)2]·[Pb2(L)2(phen)2]}n4- (bis- (4- carboxybenzyl) ammonia of N, N '-used
Base) toluene structural schematic diagram.
Fig. 2 is the present invention { [Pb (phen)2]·[Pb2(L)2(phen)2]}nMonomer structure schematic diagram.
Fig. 3 is the present invention { [Pb (phen)2]·[Pb2(L)2(phen)2]}nThree-dimensional accumulation schematic diagram.
Single-crystal X-ray diffraction analysis shows { [Pb (phen)2]·[Pb2(L)2(phen)2]}nIt is anorthic system, space group
For P1.As can be seen from Figure 2, basic building unit includes three Pb (II) atoms, two L ligands and four phen ligands.Pb1 and come
From N1, N2, N3, N4 coordination of two phen ligands, four-coordination is formed.Pb2 with come from two H3Four oxygen atoms of L ligand
(O1, O2, O3A, O4A), N5, N6 coordination on a phen ligand, forms hexa-coordinate dodecahedron configuration.Pb3 coordination configuration
Identical as Pb2, wherein O3A, O8, O10B, O11B come from three H3L ligand, N8, N9 come from a phen ligand.
Specific embodiment
Embodiment 1:
{ [Pb (phen) of the present invention2]·[Pb2(L)2(phen)2]}nMonomer molecule formula are as follows:
C92H68N10O16Pb3S2, molecular weight are as follows: 2255.25, H3L is 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid, and phen is
1,10- Phen.Crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
{ [the Pb (phen)2]·[Pb2(L)2(phen)2]}nSynthetic method specific steps are as follows:
0.110g is analyzed into pure H3L and 0.050g analyze pure phen and are dissolved in, 8mL secondary distilled water and 1mL dehydrated alcohol
In mixed solution, after adjusting pH is 8, adds 0.094g and analyze pure three water lead acetate, be placed in polytetrafluoroethylene (PTFE) autoclave
In, it is placed in 170 DEG C of baking ovens and is taken out after three days, is cooled to room temperature, open autoclave, colourless transparent sheet-like crystal is arranged at bottom
That is { [Pb (phen)2]·[Pb2(L)2(phen)2]}n.{ [Pb (phen) is measured by single crystal diffractometer2]·[Pb2(L)2
(phen)2]}nStructure, crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
Embodiment 2:
{ [Pb (phen) of the present invention2]·[Pb2(L)2(phen)2]}nMonomer molecule formula are as follows:
C92H68N10O16Pb3S2, molecular weight are as follows: 2255.25, H3L is 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid, and phen is
1,10- Phen.Crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
{ [the Pb (phen)2]·[Pb2(L)2(phen)2]}nSynthetic method specific steps are as follows:
0.220g is analyzed into pure H3L and 0.100g analyze pure phen and are dissolved in, 16mL secondary distilled water and 2mL dehydrated alcohol
In mixed solution, after adjusting pH is 8, adds 0.188g and analyze pure three water lead acetate, be placed in polytetrafluoroethylene (PTFE) autoclave
In, it is placed in 170 DEG C of baking ovens and is taken out after three days, is cooled to room temperature, open autoclave, colourless transparent sheet-like crystal is arranged at bottom
That is { [Pb (phen)2]·[Pb2(L)2(phen)2]}n.{ [Pb (phen) is measured by single crystal diffractometer2]·[Pb2(L)2
(phen)2]}nStructure, crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
Claims (1)
1. a kind of polymer { [Pb (phen)2]·[Pb2(L)2(phen)2]}n, it is characterised in that polymer { [Pb (phen)2]·
[Pb2(L)2(phen)2]}nMonomer molecule formula are as follows: C92H68N10O16Pb3S2, molecular weight are as follows: 2255.25, H3L is 4- (N, N '-
Bis- (4- carboxybenzyl) amino) benzene sulfonic acid, phen 1,10- Phen；Crystal structural data is shown in Table one, bond distance's bond angle data
It is shown in Table two；
One, of table { [Pb (phen)2]·[Pb2(L)2(phen)2]}nCrystallographic parameter
Two, of table { [Pb (phen)2]·[Pb2(L)2(phen)2]}nPart bond distanceWith bond angle (°)
{ [the Pb (phen)2]·[Pb2(L)2(phen)2]}nSynthetic method specific steps are as follows:
0.110-0.220g is analyzed into pure H3L and 0.050-0.100g analyzes pure phen and is dissolved in 8-16mL secondary distilled water and 1-2mL
In the mixed solution of dehydrated alcohol, after adjusting pH is 8, adds 0.094-0.188g and analyze pure three water lead acetate, be placed in poly- four
It in vinyl fluoride autoclave, is placed in 170 DEG C of baking ovens and is taken out after three days, is cooled to room temperature, open autoclave, bottom has
Colorless and transparent flat crystal is { [Pb (phen)2]·[Pb2(L)2(phen)2]}n。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811649867.4A CN109503856A (en) | 2018-12-31 | 2018-12-31 | Polymer 4- (bis- (4- carboxyl phenyl) amino of N, N ' -) benzene sulfonic acid lead and synthetic method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811649867.4A CN109503856A (en) | 2018-12-31 | 2018-12-31 | Polymer 4- (bis- (4- carboxyl phenyl) amino of N, N ' -) benzene sulfonic acid lead and synthetic method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109503856A true CN109503856A (en) | 2019-03-22 |
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ID=65755865
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811649867.4A Withdrawn CN109503856A (en) | 2018-12-31 | 2018-12-31 | Polymer 4- (bis- (4- carboxyl phenyl) amino of N, N ' -) benzene sulfonic acid lead and synthetic method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109503856A (en) |
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2018
- 2018-12-31 CN CN201811649867.4A patent/CN109503856A/en not_active Withdrawn
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Application publication date: 20190322 |