CN105694860A - Luminescent material [Cd(tidc)2]n and synthetic method - Google Patents
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- CN105694860A CN105694860A CN201610171128.3A CN201610171128A CN105694860A CN 105694860 A CN105694860 A CN 105694860A CN 201610171128 A CN201610171128 A CN 201610171128A CN 105694860 A CN105694860 A CN 105694860A
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- C07D249/02—Heterocyclic compounds containing five-membered rings having three nitrogen atoms as the only ring hetero atoms not condensed with other rings
- C07D249/08—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
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Abstract
The invention discloses a fluorescent material [Cd(tidc)2]n and a synthetic method. The molecular formula of a monomer is C18H10CdCl4N8O2; a molecular weight is 624.55g/mol; Htidc is 3,5-dichlorosalicylidene-4-amino-1,2,4-triazole schiff base. Analytically pure 3,5-dichlorosalicylaldehyde and analytically pure 4-amino-1,2,4-triazole are dissolved in analytically pure ethanol; an obtained first mixture is heated, refluxed, agitated and filtered; an obtained substance is washed for three times by using the analytically pure ethanol; the obtained substance is dried, so as to obtain the ligand Htidc. The dried Htidc and analytically pure cadmium acetate are dissolved in analytically pure N,N'-dimethyl formamide; distilled water is added into an obtained second mixture; an obtained third mixture is stood for three days in a drying oven at 80 DEG C. The [Cd(tidc)2]n generates 512nm fluorescent light with intensity of 1316a.u. (astronomical unit) when being irradiated by 450nm incident light, and under an 800V photomultiplier and a 3 times of amplification coefficient, generates emergent light which has intensity of 3262a.u. and is further stable in a potassium peroxodisulfate solution. The fluorescent material [Cd(tidc)2]n and the synthetic method are simple in process, low in cost, easy in the control of chemical components, good in repeatability and further high in yield.
Description
Technical field
The present invention relates to a kind of stable luminescent material [Cd (tidc)2]n, (Htidc is 3,5-dichloro-salicylaldehyde's contracting 4-amino-1,2,4 triazole schiff bases) and synthetic method。
Background technology
The development of many decades gone through by modern luminescent material, oneself become information show, the backing material in the field such as lighting source, photoelectric device, play the effect become more and more important for social development and technological progress。Particularly energy scarcity is present, and the luminescent material that exploitation transformation efficiency is high 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 luminosity excellence, utilizes micro-bottle of reaction method synthesis [Cd (tidc)2]n。
[the Cd (tidc) that the present invention relates to2]nMonomer molecule formula be: C18H10CdCl4N8O2, molecular weight is: 624.55, Htidc is 3,5-dichloro-salicylaldehyde contracting 4-amino-1, and 2,4 triazole schiff bases, crystal structural data is in Table one, and bond distance's bond angle data are in Table two。
Table one: [Cd (tidc)2]nCrystallographic parameter
aR1=Σ | | Fo|–|Fc||/Σ|Fo|.bwR2=[Σ w (| Fo 2|–|Fc 2|)2/Σw(|Fo 2|)2]1/2
Table two: [Cd (tidc)2]nBond distanceWith bond angle °
| Cd1—O1 | 2.190(7) | C6—C5 | 1.293(18) |
| Cd1—O1i | 2.190(7) | C2—C3 | 1.403(15) |
| Cd1—N2ii | 2.288(9) | C7—N4 | 1.305(13) |
| Cd1—N2iii | 2.288(9) | N2—Cd1iv | 2.288(9) |
| Cd1—N4 | 2.443(10) | N2—N1 | 1.397(15) |
| Cd1—N4i | 2.443(10) | N2—C9 | 1.314(15) |
| Cl2—C5 | 1.747(12) | N1—C8 | 1.323(18) |
| Cl1—C3 | 1.706(13) | C5—C4 | 1.432(18) |
| O1—C2 | 1.261(12) | C4—C3 | 1.386(16) |
| C1—C6 | 1.387(15) | N4—N3 | 1.393(13) |
| C1—C2 | 1.462(16) | C9—N3 | 1.354(15) |
| C1—C7 | 1.427(15) | N3—C8 | 1.337(14) |
| Cd1—O1 | 2.190(7) | C6—C5 | 1.293(18) |
| O1—Cd1—O1i | 162.5(5) | C3—C2—C1 | 114.9(10) |
| O1i—Cd1—N2iii | 84.0(3) | N4—C7—C1 | 127.3(11) |
| O1i—Cd1—N2ii | 109.2(3) | N1—N2—Cd1iv | 124.6(7) |
| O1—Cd1—N2iii | 109.2(3) | C9—N2—Cd1iv | 126.3(8) |
| O1—Cd1—N2ii | 84.0(3) | C9—N2—N1 | 107.8(10) |
| O1i—Cd1—N4i | 76.0(3) | C8—N1—N2 | 104.8(10) |
| O1i—Cd1—N4 | 93.0(3) | C6—C5—Cl2 | 124.3(11) |
| O1—Cd1—N4 | 76.0(3) | C6—C5—C4 | 121.1(12) |
| O1—Cd1—N4i | 93.0(3) | C4—C5—Cl2 | 114.5(10) |
| N2iii—Cd1—N2ii | 84.1(5) | C3—C4—C5 | 117.0(11) |
| N2iii—Cd1—N4i | 156.3(3) | C2—C3—Cl1 | 117.2(9) |
| N2ii—Cd1—N4 | 156.3(3) | C4—C3—Cl1 | 118.7(10) |
| N2iii—Cd1—N4 | 90.4(4) | C4—C3—C2 | 124.1(12) |
| N2ii—Cd1—N4i | 90.4(4) | C7—N4—Cd1 | 124.0(7) |
| N4i—Cd1—N4 | 103.2(5) | C7—N4—N3 | 111.1(10) |
| C2—O1—Cd1 | 135.8(7) | N3—N4—Cd1 | 123.8(7) |
| C6—C1—C2 | 119.3(10) | N2—C9—N3 | 110.0(11) |
| C6—C1—C7 | 116.9(11) | C9—N3—N4 | 129.7(10) |
| C7—C1—C2 | 123.8(10) | C8—N3—N4 | 124.8(11) |
| C5—C6—C1 | 123.6(12) | C8—N3—C9 | 105.3(11) |
| O1—C2—C1 | 122.7(10) | N1—C8—N3 | 111.9(13) |
| O1—C2—C3 | 122.4(11) |
Symmetrycodes:(i) y, x ,-z+1；(ii) x+1, y, z；(iii) y, x+1 ,-z+1；(iv) x-1, y, z.
Described [Cd (tidc)2]nSynthetic method concretely comprise the following steps:
(1) by analytically pure for 1.91g 3,5-dichloro-salicylaldehyde and the analytically pure 4-amino-1 of 0.841g, 2,4-triazole, is dissolved in 30mL analytical pure alcoholic solution, is heated to reflux and has solid to precipitate out after stirring two hours, filter, by 10mL analytical pure washing with alcohol three times, dry at placing 50 DEG C, obtain part Htidc。Dried for 0.056-0.112g Htidc and 0.054-0.108g analytical pure cadmium acetate is dissolved in 5mL analytical pure N, in N '-dimethyl Methanamide, it is placed in micro-reaction bulb, adds 5mL distilled water, 80 DEG C of baking ovens stand three days, has yellow crystals to generate i.e. [Cd (tidc)2]n-cross single crystal diffractometer mensuration [Cd (tidc)2]nStructure, crystal structural data is in Table one, and bond distance's bond angle data are in Table two。
(2) step (1) gained [Cd (tidc) is taken2]nBeing dissolved in analytical pure N, being made into concentration in N '-dimethyl formamide solvent is 5.0 × 10-6The solution of mol/L, carries out fluorometric investigation, [Cd (tidc)2]nThe fluorescence of the 512nm of 1316a.u. intensity is produced under the incident illumination of 450nm irradiates；Under the photomultiplier tube of 800V, the amplification coefficient of 3 times, take the 100 above-mentioned solution prepared of μ L and be placed in 1mol/L potassium persulfate solution (conducting medium), create the luminescence of 3262a.u. intensity, and with this understanding, can continue and stabilized illumination。
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 the present invention [Cd (tidc)2]nStructure chart。
Fig. 2 is the present invention [Cd (tidc)2]n2 d plane picture。
Fig. 3 is the present invention [Cd (tidc)2]nTomograph。
Fig. 4 is the present invention [Cd (tidc)2]nFluorescence spectrum figure。
Fig. 5 is the present invention [Cd (tidc)2]nElectrochemiluminescence spectrogram。
Detailed description of the invention
Embodiment 1:
[the Cd (tidc) that the present invention relates to2]nMolecular formula be: C18H10CdCl4N8O2, molecular weight is: 624.55, Htidc is 3,5-dichloro-salicylaldehyde contracting 4-amino-1, and 2,4 triazole schiff bases, crystal structural data is in Table one, and bond distance's bond angle data are in Table two。
[Cd(tidc)2]nSynthetic method concretely comprise the following steps:
(1) by analytically pure for 1.91g 3,5-dichloro-salicylaldehyde and the analytically pure 4-amino-1 of 0.841g, 2,4-triazole, is dissolved in 30mL analytical pure alcoholic solution, is heated to reflux and has solid to precipitate out after stirring two hours, filter, by 10mL analytical pure washing with alcohol three times, dry at placing 50 DEG C, obtain part Htidc。Yield: 2.641g, productivity 96%。Dried for 0.056g Htidc and 0.054 analytical pure cadmium acetate is dissolved in 5mL analytical pure N, in N '-dimethyl Methanamide, it is placed in micro-reaction bulb, adds 5mL distilled water, 80 DEG C of baking ovens stand three days, has yellow crystals to generate i.e. [Cd (tidc)2]n。Yield: 0.059g, productivity 63%。[Cd (tidc) is measured by single crystal diffractometer2]nStructure, crystal structural data is in Table one, and bond distance's bond angle data are in Table two。
(2) step (1) gained [Cd (tidc) is taken2]nBeing dissolved in analytical pure N, being made into concentration in N '-dimethyl formamide solvent is 5.0 × 10-5The solution of mol/L, carries out fluorometric investigation, [Cd (tidc)2]nThe fluorescence of the 512nm of 1316a.u. intensity is produced under the incident illumination of 450nm irradiates；Under the photomultiplier tube of 800V, the amplification coefficient of 3 times, take the 100 above-mentioned solution prepared of μ L and be placed in 1mol/L potassium persulfate solution (conducting medium), create the luminescence of 3262a.u. intensity, and with this understanding, can continue and stabilized illumination。
Embodiment 2:
[the Cd (tidc) that the present invention relates to2]nMolecular formula be: C18H10CdCl4N8O2, molecular weight is: 624.55, Htidc is 3,5-dichloro-salicylaldehyde contracting 4-amino-1, and 2,4 triazole schiff bases, crystal structural data is in Table one, and bond distance's bond angle data are in Table two。
[Cd(tidc)2]nSynthetic method concretely comprise the following steps:
(1) by analytically pure for 1.91g 3,5-dichloro-salicylaldehyde and the analytically pure 4-amino-1 of 0.841g, 2,4-triazole, is dissolved in 30mL analytical pure alcoholic solution, is heated to reflux and has solid to precipitate out after stirring two hours, filter, by 10mL analytical pure washing with alcohol three times, dry at placing 50 DEG C, obtain part Htidc。Yield: 2.641g, productivity 96%。Dried for 0.112g Htidc and 0.108g analytical pure cadmium acetate is dissolved in 5mL analytical pure N, in N '-dimethyl Methanamide, it is placed in micro-reaction bulb, adds 5mL distilled water, 80 DEG C of baking ovens stand three days, has yellow crystals to generate i.e. [Cd (tidc)2]n。Yield: 0.118g, productivity 63%。By single crystal diffractometer mensuration-[Cd (tidc)2]n-structure, crystal structural data is in Table one, and bond distance's bond angle data are in Table two。
(2) step (1) gained [Cd (tidc) is taken2]nBeing dissolved in analytical pure N, being made into concentration in N '-dimethyl formamide solvent is 5.0 × 10-5The solution of mol/L, carries out fluorometric investigation, [Cd (tidc)2]nThe fluorescence of the 512nm of 1316a.u. intensity is produced under the incident illumination of 450nm irradiates；Under the photomultiplier tube of 800V, the amplification coefficient of 3 times, take the 100 above-mentioned solution prepared of μ L and be placed in 1mol/L potassium persulfate solution (conducting medium), create the luminescence of 3262a.u. intensity, and with this understanding, can continue and stabilized illumination。
Claims (1)
1. a luminescent material [Cd (tidc)2]n, it is characterised in that [Cd (tidc)2]nMonomer molecule formula be: C18H10CdCl4N8O2, molecular weight is: 624.552g/mol, Htidc are 3,5-dichloro-salicylaldehyde contracting 4-amino-1, and 2,4 triazole schiff bases, crystal structural data is in Table one, and bond distance's bond angle data are in Table two；[Cd (tidc)2]nUnder the incident illumination of 450nm irradiates, produce the fluorescence of the 512nm of 1316a.u. intensity, under the photomultiplier tube of 800V, the amplification coefficient of 3 times, in conducting medium potassium persulfate solution, produce 3262a.u. intensity and stable luminescence；
Table one: [Cd (tidc)2]nCrystallographic parameter
aR1=Σ | | Fo|–|Fc||/Σ|Fo|.bwR2=[Σ w (| Fo 2|–|Fc 2|)2/Σw(|Fo 2|)2]1/2
Table two: [Cd (tidc)2]nBond distanceWith bond angle °
Symmetrycodes:(i) y, x ,-z+1；(ii) x+1, y, z；(iii) y, x+1 ,-z+1；(iv) x-1, y, z.
Described [Cd (tidc)2]nSynthetic method concretely comprise the following steps:
By analytically pure for 1.91g 3,5-dichloro-salicylaldehyde and the analytically pure 4-amino-1 of 0.841g, 2,4-triazole, is dissolved in 30mL analytical pure alcoholic solution, is heated to reflux and has solid to precipitate out after stirring two hours, filter, by 10mL analytical pure washing with alcohol three times, dry at placing 50 DEG C, obtain part Htidc；Dried for 0.056-0.112g Htidc and 0.054-0.108g analytical pure cadmium acetate is dissolved in 5mL analytical pure N, in N '-dimethyl Methanamide, it is placed in micro-reaction bulb, adds 5mL distilled water, 80 DEG C of baking ovens stand three days, has yellow crystals to generate i.e. [Cd (tidc)2]n。
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503963A (en) * | 2011-09-13 | 2012-06-20 | 江西师范大学 | Zinc metal-organic coordination polymer and preparation method thereof |
| JP2014152114A (en) * | 2013-02-05 | 2014-08-25 | Nippon Shokubai Co Ltd | Organometallic complex |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503963A (en) * | 2011-09-13 | 2012-06-20 | 江西师范大学 | Zinc metal-organic coordination polymer and preparation method thereof |
| JP2014152114A (en) * | 2013-02-05 | 2014-08-25 | Nippon Shokubai Co Ltd | Organometallic complex |
Non-Patent Citations (2)
| Title |
|---|
| MUHAMMAD HANIF等: "Design, spectral characterization and biological studies of transition metal(II) complexes with triazole Schiff bases", 《SPECTROCHIMICA ACTA PART A: MOLECULAR AND BIOMOLECULAR SPECTROSCOPY》 * |
| ZAHID H. CHOHAN等: "Synthesis and characterization of biologically active new Schiff bases containing 3-functionalized 1,2,4-triazoles and their zinc(II) complexes:crystal structure of 4-bromo-2-[(E)-(1H-1,2,4-triazol-3-ylimino)- methyl]phenol", 《APPL. ORGANOMETAL. CHEM.》 * |
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Effective date of registration: 20191107 Address after: 531105 floor 1-2, building 1, No.146, Wuhua Avenue, Guangxi ASEAN Economic and Technological Development Zone, Nanning City, Guangxi Zhuang Autonomous Region (excluding the top floor) Patentee after: Guangxi baolixing Lighting Technology Co., Ltd Address before: 541004 the Guangxi Zhuang Autonomous Region Guilin Construction Road No. 12 Patentee before: Guilin University of Technology |
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