CN104263352B - Fluorescent material Zn (hfoac)2(phen) H2o and synthetic method - Google Patents
Fluorescent material Zn (hfoac)2(phen) H2o and synthetic method Download PDFInfo
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- CN104263352B CN104263352B CN201410454852.8A CN201410454852A CN104263352B CN 104263352 B CN104263352 B CN 104263352B CN 201410454852 A CN201410454852 A CN 201410454852A CN 104263352 B CN104263352 B CN 104263352B
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Abstract
The invention discloses a kind of fluorescent material Zn (hfoac)2(phen)H2O and synthetic method.Fluorescent material Zn (hfoac)2(phen)H2The molecular formula of O is: C26H18F2N2O7Zn, molecular weight is: 573.81, H2Foac is 4 fluorosalicylic acids, and phen is Phen.By analytically pure to analytically pure for 0.108g 0.43g 4 fluorosalicylic acids, the 0.099 analytically pure Phen of 0.396g and 0.11 0.438g two acetate hydrate zinc mixing, it is dissolved in 10 40mL analytical pure methanol solutions, adding analytical pure triethylamine regulation pH after stirring 10 minutes is 7.5, after continuing stirring 20 minutes, being put in the baking oven of 120 DEG C by the solution obtained after standing 120 hours, cooling obtains colourless bulk crystals i.e. Zn (hfoac)2(phen)H2O;Zn(hfoac)2(phen)H2O produces the fluorescence of the 377nm of 182 a.u. intensity under the incident illumination of 280nm irradiates.Present invention process is simple, with low cost, chemical constituent is easily controllable, reproducible and yield is high.
Description
Technical field
The present invention relates to a kind of fluorescent material Zn (hfoac)2(phen)H2O(H2Foac is 4-fluorosalicylic acid, and phen is adjacent
Phenanthroline) and synthetic method.
Background technology
The development of many decades gone through by modern fluorescence material, oneself become information show, the field such as lighting source, photoelectric device
Backing material, plays the effect become more and more important for social development and technological progress.Particularly energy scarcity is present, and exploitation turns
Changing the high fluorescent material of efficiency is to solve one of energy scarcity problem method.
Summary of the invention
The purpose of the present invention is exactly the functional material for design synthesis photoluminescent property excellence, utilizes solvent thermal process to synthesize Zn
(hfoac)2(phen)H2O。
The Zn (hfoac) that the present invention relates to2(phen)H2The molecular formula of O is: C26H18F2N2O7Zn molecular weight is: 573.18,
H2Foac is 4-fluorosalicylic acid, and phen is Phen, and crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
Table one: Zn (hfoac)2(phen)H2The crystallographic parameter of O
Table two: Zn (hfoac)2(phen)H2The bond distance of OWith bond angle (°)
Table three: Zn (hfoac)2(phen)H2The hydrogen-bond length of OWith bond angle (°)
D-H···A | D-H | H···A | D···A | D-H···A |
O1-H1A···O3 | 0.85 | 2.34 | 2.911(4) | 125 |
O1-H1B···O6 | 0.85 | 1.93 | 2.690(4) | 148 |
O4-H4···O3 | 0.82 | 1.81 | 2.535(3) | 147 |
O7-H7···O6 | 0.82 | 1.82 | 2.550(4) | 147 |
Described Zn (hfoac)2(phen)H2The synthetic method of O concretely comprises the following steps:
(1) by analytically pure for 0.108g-0.43g 4-fluorosalicylic acid, the analytically pure Phen of 0.099-0.396g and
The analytically pure two acetate hydrate zinc mixing of 0.11-0.438g, are dissolved in 10-40ml analytical pure methanol solution, after stirring 10 minutes
Adding analytical pure triethylamine regulation pH is 7.5, after continuing stirring 20 minutes, is put in the baking oven of 120 DEG C quiet by the solution obtained
After putting 120 hours, cooling obtains colourless bulk crystals i.e. Zn (hfoac)2(phen)H2O。
(2) step (1) gained Zn (hfoac) is taken2(phen)H2O is dissolved in analytical pure N, joins in N '-dimethyl formamide solvent
Becoming concentration is 4.0 × 10-6The solution of mol/l, carries out fluorometric investigation, Zn (hfoac)2(phen)H2O is at the incident illumination of 280nm
Penetrate the fluorescence of the 377nm of lower generation 182a.u. intensity.
The present invention has that technique is simple, with low cost, chemical constituent is easily controllable, reproducible and yield advantages of higher.
Accompanying drawing explanation
Fig. 1 is Zn of the present invention (hfoac)2(phen)H2The structure chart of O.
Fig. 2 is Zn of the present invention (hfoac)2(phen)H2The two-dimensional layer figure of O
Fig. 3 is Zn of the present invention (hfoac)2(phen)H2O fluorescence spectrum figure.
Detailed description of the invention
Embodiment 1:
The Zn (hfoac) that the present invention relates to2(phen)H2The molecular formula of O is: C26H18F2N2O7Zn, molecular weight is:
573.18,H2Foac is 4-fluorosalicylic acid, and phen is Phen, and crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table
Two.
Zn(hfoac)2(phen)H2The synthetic method of O concretely comprises the following steps:
(1) by analytically pure for 0.108g 4-fluorosalicylic acid, the analytically pure Phen of 0.099g and 0.11g analytically pure two
Acetate hydrate zinc mixes, and is dissolved in 10ml analytical pure methanol solution, adds analytical pure triethylamine regulation pH and be after stirring 10 minutes
7.5, after continuing stirring 20 minutes, the solution obtained is put in the baking oven of 120 DEG C after standing 120 hours, cooling obtains colourless
Bulk crystals i.e. Zn (hfoac)2(phen)H2O.Zn (hfoac) is measured by single crystal diffractometer2(phen)H2The structure of O, brilliant
Body structured data is shown in Table one, and bond distance's bond angle data are shown in Table two.Yield: 0.097g, productivity: 67.69%.Surveyed by single crystal diffractometer
Determine Zn (hfoac)2(phen)H2The structure of O, crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
(2) step (1) gained Zn (hfoac) is taken2(phen)H2O is dissolved in analytical pure N, and N '-dimethyl Methanamide (DMF) is molten
Being made into concentration in agent is 4 × 10-6The solution of mol/l, carries out fluorometric investigation, obtains fluorescent spectrum curve such as accompanying drawing 3, Zn
(hfoac)2(phen)H2O produces the fluorescence of the 377nm of 182a.u. intensity under the incident illumination of 280nm irradiates.
Embodiment 2:
The Zn (hfoac) that the present invention relates to2(phen)H2The molecular formula of O is: C26H18F2N2O7Zn molecular weight is: 573.18,
H2Foac is 4-fluorosalicylic acid, and phen is Phen.
Zn(hfoac)2(phen)H2The synthetic method of O concretely comprises the following steps:
(1) by analytically pure for 0.43g 4-fluorosalicylic acid, the analytically pure Phen of 0.396g and 0.438g analytically pure two
Acetate hydrate zinc mixes, and is dissolved in 40ml analytical pure methanol solution, adds analytical pure triethylamine regulation pH and be after stirring 10 minutes
7.5, after continuing stirring 20 minutes, the solution obtained is put in the baking oven of 120 DEG C after standing 120 hours, cooling obtains colourless
Bulk crystals i.e. Zn (hfoac)2(phen)H2O.Zn (hfoac) is measured by single crystal diffractometer2(phen)H2The structure of O, brilliant
Body structured data is shown in Table one, and bond distance's bond angle data are shown in Table two.Yield: 0.388g, productivity: 67.69%.Surveyed by single crystal diffractometer
Determine Zn (hfoac)2(phen)H2The structure of O, crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
(2) step (1) gained Zn (hfoac) is taken2(phen)H2O is dissolved in analytical pure N, and N '-dimethyl Methanamide (DMF) is molten
Being made into concentration in agent is 4.0 × 10-6The solution of mol/l, carries out fluorometric investigation, obtains fluorescent spectrum curve such as accompanying drawing 3, Zn
(hfoac)2(phen)H2O produces the fluorescence of the 377nm of 182a.u. intensity under the incident illumination of 280nm irradiates.
Claims (1)
1. a fluorescent material Zn (hfoac)2(phen)H2O, it is characterised in that Zn (hfoac)2(phen)H2The molecular formula of O is:
C26H18F2N2O7Zn, molecular weight is: 573.81, H2Foac is 4-fluorosalicylic acid, and phen is Phen, and crystal structural data is shown in
Table one, bond distance's bond angle data are shown in Table two;Zn(hfoac)2(phen)H2It is strong that O produces 182a.u. under the incident illumination of 280nm irradiates
The fluorescence of the 377nm of degree;
Described Zn (hfoac)2(phen)H2The synthetic method of O concretely comprises the following steps:
By analytically pure for 0.108g-0.43g 4-fluorosalicylic acid, the analytically pure Phen of 0.099-0.396g and 0.11-
The analytically pure two acetate hydrate zinc mixing of 0.438g, are dissolved in 10-40mL analytical pure methanol solution, add and divide after stirring 10 minutes
Analysing pure triethylamine regulation pH is 7.5, after continuing stirring 20 minutes, the solution obtained is put in the baking oven of 120 DEG C standing 120 little
Shi Hou, cooling obtains colourless bulk crystals i.e. Zn (hfoac)2(phen)H2O;
Table one: Zn (hfoac)2(phen)H2The crystallographic parameter of O
Table two: Zn (hfoac)2(phen)H2The bond distance of OWith bond angle °
Table three: Zn (hfoac)2(phen)H2The hydrogen-bond length of OWith bond angle °
。
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CN105801503B (en) * | 2016-03-23 | 2018-09-11 | 桂林理工大学 | Luminescent material [Zn (tidc)2]nAnd synthetic method |
CN107698610B (en) * | 2017-10-01 | 2020-07-31 | 桂林理工大学 | Europium complex red luminescent material and synthetic method thereof |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101434617A (en) * | 2008-08-20 | 2009-05-20 | 西北大学 | Energetic coordination complex based on azo tetrazole azotetrazole and use thereof |
CN101787043A (en) * | 2010-02-10 | 2010-07-28 | 河北工业大学 | Novel light-emitting transition metal organic framework structured compound and preparation method thereof |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN101434617A (en) * | 2008-08-20 | 2009-05-20 | 西北大学 | Energetic coordination complex based on azo tetrazole azotetrazole and use thereof |
CN101787043A (en) * | 2010-02-10 | 2010-07-28 | 河北工业大学 | Novel light-emitting transition metal organic framework structured compound and preparation method thereof |
Non-Patent Citations (2)
Title |
---|
Self-assembly of two zinc(II) supramolecular architectures with carboxylate and chelating aromatic amine ligands: [Zn(nba)2(phen)(H2O)] and [Zn(nip)(phen)]n (nba = 4-nitrobenzoic acid, nip = 5-nitroisophthalic acid);Hong Ren等;《Transition Metal Chemistry》;20061130;第31卷;992-998 * |
Synthesis, crystal structures, and anti-convulsant activities of ternary [ZnII(3,5-diisopropylsalicylate)2], [ZnII(salicylate)2] and [ZnII(aspirinate)2] complexes;Pascale Lemoine 等;《Journal of Inorganic Biochemistry》;20040908;第98卷;1734-1749 * |
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Effective date of registration: 20180912 Address after: 530022 Nanning District, Qingxiu District, Guangxi, No. 141, No. 17, D Patentee after: China Aluminum Guangxi nonferrous Rare Earth Development Co., Ltd. Address before: No. 12, Jian Gong Road, Guilin, the Guangxi Zhuang Autonomous Region Patentee before: Guilin University of Technology |