Luminescent material [Cd (tidc)2]nAnd synthetic method
Technical field
The present invention relates to a kind of luminescent material of stabilization [Cd (tidc)2]n, (Htidc is 3,5- dichloro-salicylaldehyde's contracting 4- ammonia
The triazole of base -1,2,4 schiff bases) and synthetic method.
Background technology
Development of the modern luminescent material after many decades, oneself turns into the fields such as presentation of information, lighting source, photoelectric device
Backing material, the effect to become more and more important is played for social development and technological progress.Particularly energy scarcity is present, and exploitation turns
The luminescent material for changing efficiency high is that solve the problems, such as one of energy scarcity method.
The content of the invention
The purpose of the present invention is exactly to synthesize the excellent functional material of luminosity for design, utilizes micro- bottle of reaction method to synthesize
[Cd(tidc)2]n。
[Cd (tidc) of the present invention2]nMonomer molecule formula be:C18H10CdCl4N8O2, molecular weight is: 624.55,
Htidc is 3,5- dichloro-salicylaldehyde's contracting 4- amino -1,2,4 triazole schiff bases, and crystal structural data is shown in Table one, bond distance's bond angle number
According to being shown in Table two.
Table one:[Cd(tidc)2]nCrystallographic parameter
aR1=Σ | | Fo|–|Fc||/Σ|Fo|.b wR2=[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) |
|
|
Symmetry codes:(i)y,x,-z+1;(ii)x+1,y,z;(iii)y,x+1,-z+1;(iv)x-1,y,z.
[the Cd (tidc)2]nSynthetic method concretely comprise the following steps:
(1) by analytically pure 3, the 5- dichloro-salicylaldehydes of 1.91g and the analytically pure 4- amino -1,2 of 0.841g, 4- triazoles,
It is dissolved in 30mL analysis straight alcohol solution, is heated to reflux and has solid precipitation after stirring two hours, filter, is analyzed with 10mL pure
Ethanol washs three times, places and is dried at 50 DEG C, obtains part Htidc.By the dried Htidc of 0.056-0.112g and
0.054-0.108g, which analyzes pure cadmium acetate and is dissolved in 5mL, analyzes pure N, in N '-dimethyl formamide, is placed in micro- reaction bulb, then add
Enter 5mL distilled water, three days are stood in 80 DEG C of baking ovens, there are yellow crystals to generate i.e. [Cd (tidc)2]n- cross single crystal diffractometer measure
[Cd(tidc)2]nStructure, crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
(2) [Cd (tidc) obtained by step (1) is taken2]nThe pure N of analysis is dissolved in, concentration is made into N '-dimethyl formamide solvent
For 5.0 × 10-6Mol/L solution, carry out fluorometric investigation, [Cd (tidc)2]nProduced under 450nm incident light irradiation
The 512nm of 1316a.u. intensity fluorescence;Under 800V photomultiplier, 3 times of amplification coefficient, take 100 μ L are above-mentioned to prepare
Solution be placed in 1mol/L potassium persulfate solutions (conducting medium), generate the luminous of 3262a.u. intensity, and in this condition
Under, it can continue and stabilized illumination.
The present invention has the advantages that technique is simple, cost is cheap, chemical constituent is easily controllable, reproducible and yield is high.
Brief description of the drawings
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 spectra.
Fig. 5 is the present invention [Cd (tidc)2]nElectrochemical luminescence spectrogram.
Embodiment
Embodiment 1:
[Cd (tidc) of the present invention2]nMolecular formula be:C18H10CdCl4N8O2, molecular weight is:624.55,
Htidc is 3,5- dichloro-salicylaldehyde's contracting 4- amino -1,2,4 triazole schiff bases, and crystal structural data is shown in Table one, bond distance's bond angle number
According to being shown in Table two.
[Cd(tidc)2]nSynthetic method concretely comprise the following steps:
(1) by analytically pure 3, the 5- dichloro-salicylaldehydes of 1.91g and the analytically pure 4- amino -1,2 of 0.841g, 4- triazoles,
It is dissolved in 30mL analysis straight alcohol solution, is heated to reflux and has solid precipitation after stirring two hours, filter, is analyzed with 10mL pure
Ethanol washs three times, places and is dried at 50 DEG C, obtains part Htidc.Yield:2.641g yield 96%.0.056g is dried
The pure cadmium acetate of the analyses of rear Htidc and 0.054 is dissolved in 5mL and analyzes pure N, in N '-dimethyl formamide, is placed in micro- reaction bulb,
5mL distilled water is added, three days are stood in 80 DEG C of baking ovens, there are yellow crystals to generate i.e. [Cd (tidc)2]n.Yield:0.059g,
Yield 63%.[Cd (tidc) is determined by single crystal diffractometer2]nStructure, crystal structural data is shown in Table one, bond distance's bond angle data
It is shown in Table two.
(2) [Cd (tidc) obtained by step (1) is taken2]nThe pure N of analysis is dissolved in, concentration is made into N '-dimethyl formamide solvent
For 5.0 × 10-5Mol/L solution, carry out fluorometric investigation, [Cd (tidc)2]nProduced under 450nm incident light irradiation
The 512nm of 1316a.u. intensity fluorescence;Under 800V photomultiplier, 3 times of amplification coefficient, take 100 μ L are above-mentioned to prepare
Solution be placed in 1mol/L potassium persulfate solutions (conducting medium), generate the luminous of 3262a.u. intensity, and in this condition
Under, it can continue and stabilized illumination.
Embodiment 2:
[Cd (tidc) of the present invention2]nMolecular formula be:C18H10CdCl4N8O2, molecular weight is:624.55,
Htidc is 3,5- dichloro-salicylaldehyde's contracting 4- amino -1,2,4 triazole schiff bases, and crystal structural data is shown in Table one, bond distance's bond angle number
According to being shown in Table two.
[Cd(tidc)2]nSynthetic method concretely comprise the following steps:
(1) by analytically pure 3, the 5- dichloro-salicylaldehydes of 1.91g and the analytically pure 4- amino -1,2 of 0.841g, 4- triazoles,
It is dissolved in 30mL analysis straight alcohol solution, is heated to reflux and has solid precipitation after stirring two hours, filter, is analyzed with 10mL pure
Ethanol washs three times, places and is dried at 50 DEG C, obtains part Htidc.Yield:2.641g yield 96%.0.112g is dried
Rear Htidc and 0.108g, which analyzes pure cadmium acetate and is dissolved in 5mL, analyzes pure N, in N '-dimethyl formamide, is placed in micro- reaction bulb
In, 5mL distilled water is added, three days are stood in 80 DEG C of baking ovens, there are yellow crystals to generate i.e. [Cd (tidc)2]n.Yield:
0.118g, yield 63%.- [Cd (tidc) is determined by single crystal diffractometer2]n- structure, crystal structural data is shown in Table one, bond distance
Bond angle data are shown in Table two.
(2) [Cd (tidc) obtained by step (1) is taken2]nThe pure N of analysis is dissolved in, concentration is made into N '-dimethyl formamide solvent
For 5.0 × 10-5Mol/L solution, carry out fluorometric investigation, [Cd (tidc)2]nProduced under 450nm incident light irradiation
The 512nm of 1316a.u. intensity fluorescence;Under 800V photomultiplier, 3 times of amplification coefficient, take 100 μ L are above-mentioned to prepare
Solution be placed in 1mol/L potassium persulfate solutions (conducting medium), generate the luminous of 3262a.u. intensity, and in this condition
Under, it can continue and stabilized illumination.