CN105694867B - Fluorescent material [Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nAnd synthetic method - Google Patents

Fluorescent material [Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nAnd synthetic method Download PDF

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CN105694867B
CN105694867B CN201610221790.5A CN201610221790A CN105694867B CN 105694867 B CN105694867 B CN 105694867B CN 201610221790 A CN201610221790 A CN 201610221790A CN 105694867 B CN105694867 B CN 105694867B
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mtyp
coo
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CN105694867A (en
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甘爱城
张淑华
覃玲
欧燕翠
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Guangxi baolixing Lighting Technology Co., Ltd
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Guilin University of Technology
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    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/06Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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    • C09K2211/00Chemical nature of organic luminescent or tenebrescent compounds
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    • C09K2211/00Chemical nature of organic luminescent or tenebrescent compounds
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    • C09K2211/00Chemical nature of organic luminescent or tenebrescent compounds
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Abstract

The invention discloses a kind of fluorescent material [Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nAnd synthetic method.[Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nMonomer molecule formula is:C22H26Cu2N10Na2O11, molecular weight is:779.59g/mol, H2Mtyp is 3 methoxysalicyl aldehydes, 5 amino of contracting, 1 hydrogen, 1,2,3,4 tetrazole schiff bases.3 methoxysalicyl aldehydes and 5 amino, 1 hydrogen, 1,2,3,4 tetrazole are dissolved in analysis straight alcohol solution, is heated to reflux and stirs to get H2mtyp.By the H after drying2Mtyp, the pure copper acetate of analysis and analysis pure cerium hydroxide sodium are dissolved in analysis straight alcohol, are added the pure acetonitrile of analysis, are stood three days at normal temperatures, obtained [Cu2Na2(mtyp)2(CH3COO)2(H2O)2]nFluorometric investigation is carried out, under the wavelength excitation of 416nm, maximum emission wavelength generates shining for 660a.u. fluorescence intensities at 508nm.Present invention process is simple, of low cost, chemical constituent is easily controllable, reproducible and yield is high.

Description

Fluorescent material [Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nAnd synthetic method
Technical field
The present invention relates to a kind of fluorescent material [Cu of stabilization2Na2(mtyp)2(CH3COO)2(H2O)3]n(H2Mtyp is 3- Methoxysalicyl aldehyde contracting -5- amino -1- hydrogen -1,2,3,4- tetrazoles schiff bases) and synthetic method.
Background technology
Development of the modern luminescent material after many decades, oneself becomes the fields such as presentation of information, lighting source, photoelectric device Backing material plays the effect to become more and more important for social development and technological progress.Especially now, there is a energy deficiency exploitation turns It is to solve one of energy deficiency method to change efficient luminescent material.
Invention content
The purpose of the present invention is exactly to synthesize the excellent functional material of luminosity for design, and micro- bottle of reaction method is utilized to synthesize [Cu2Na2(mtyp)2(CH3COO)2(H2O)3]n
Of the present invention-[Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nMolecular formula be: C22H26Cu2N10Na2O11, molecular weight is:779.59g/mol, H2Mtyp is hydrogen -1 3- methoxysalicyl aldehyde contracting -5- amino -1-, 2,3,4- tetrazole schiff bases, crystal structural data are shown in Table one, and bond distance's bond angle data are shown in Table two.
Table one:[Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nCrystallographic parameter
Table two:[Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nBond distanceWith bond angle °
[the Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nSynthetic method the specific steps are:
(1) by the analytically pure 3- methoxysalicyl aldehydes of 1.521g and analytically pure hydrogen -1,2,3 5- amino -1- 0.851g, 4- tetrazoles are dissolved in 30mL analysis straight alcohol solution, are heated to reflux and have solid precipitation after stirring two hours, filter, use 10mL analyzes straight alcohol washing three times, places drying at 50 DEG C, obtains ligand H2mtyp.After 0.110-0.220g is dried H2Mtyp, 0.100-0.200g analyze pure copper acetate and 0.02-0.04g analysis pure cerium hydroxide sodium is dissolved in 7-14mL analysis straight alcohols In, it is placed in micro- reaction bulb, adds 3-6mL and analyze pure acetonitrile, stand three days at normal temperatures, there is kermesinus crystal to generate i.e. [Cu2Na2(mtyp)2(CH3COO)2(H2O)3]n.[Cu is measured by single crystal diffractometer2Na2(mtyp)2 (CH3COO)2(H2O)3]n Structure, crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
(2) [Cu obtained by step (1) is taken2Na2(mtyp)2(CH3COO)2(H2O)3]nIt is dissolved in the pure N of analysis, N '-dimethyl formyl A concentration of 5.0 × 10 are made into amine solvent-6The solution of mol/L carries out fluorometric investigation, [Cu2Na2(mtyp)2(CH3COO)2 (H2O)3]nUnder the wavelength excitation of 416nm, maximum emission wavelength generates shining for 660a.u. fluorescence intensities at 508nm.
The present invention has many advantages, such as that simple for process, of low cost, chemical constituent is easily controllable, reproducible and yield is high.
Description of the drawings
Fig. 1 is the present invention [Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nMonomer structure figure.
Fig. 2 is the present invention [Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nOne-dimensional chain figure.
Fig. 3 is the present invention [Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nTomograph.
Fig. 4 is the present invention [Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nFluorescence spectra.
Specific implementation mode
Embodiment 1:
[Cu of the present invention2Na2(mtyp)2(CH3COO)2(H2O)3]nMolecular formula be:C22H26Cu2N10Na2O11, point Son is measured:779.59g/mol, H2Mtyp is 3- methoxysalicyl aldehyde contracting -5- amino -1- hydrogen -1,2,3,4- tetrazole Schiffs Alkali, crystal structural data are shown in Table one, and bond distance's bond angle data are shown in Table two.
[Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nSynthetic method the specific steps are:
(1) by the analytically pure 3- methoxysalicyl aldehydes of 1.521g and analytically pure hydrogen -1,2,3 5- amino -1- 0.851g, 4- tetrazoles are dissolved in 30mL analysis straight alcohol solution, are heated to reflux and have solid precipitation after stirring two hours, filter, use 10mL analyzes straight alcohol washing three times, places drying at 50 DEG C, obtains ligand H2mtyp.H after 0.110g is dried2mtyp、 0.100g analyzes pure copper acetate and 0.02g analysis pure cerium hydroxide sodium is dissolved in 7mL analysis straight alcohols, is placed in micro- reaction bulb, then 3mL is added and analyzes pure acetonitrile, stands three days at normal temperatures, has kermesinus crystal to generate i.e. [Cu2Na2(mtyp)2(CH3COO)2 (H2O)3]n.Yield:0.119g, yield 61%.[Cu is measured by single crystal diffractometer2Na2(mtyp)2(CH3COO)2(H2O)3]n's Structure, crystal structural data are shown in Table one, and bond distance's bond angle data are shown in Table two.
(2) [Cu obtained by step (1) is taken2Na2(mtyp)2(CH3COO)2(H2O)3]nIt is dissolved in the pure N of analysis, N '-dimethyl formyl A concentration of 5.0 × 10 are made into amine solvent-6The solution of mol/L carries out fluorometric investigation, [Cu2Na2(mtyp)2(CH3COO)2 (H2O)3]nUnder the wavelength excitation of 416nm, maximum emission wavelength generates shining for 660a.u. fluorescence intensities at 508nm.
Embodiment 2:
[Cu of the present invention2Na2(mtyp)2(CH3COO)2(H2O)2]nMolecular formula be:C22H26Cu2N10Na2O11, point Son is measured:779.59g/mol, H2Mtyp is 3- methoxysalicyl aldehyde contracting -5- amino -1- hydrogen -1,2,3,4- tetrazole Schiffs Alkali, crystal structural data are shown in Table one, and bond distance's bond angle data are shown in Table two.
[Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nSynthetic method the specific steps are:
(1) by the analytically pure 3- methoxysalicyl aldehydes of 1.521g and analytically pure hydrogen -1,2,3 5- amino -1- 0.851g, 4- tetrazoles are dissolved in 30mL analysis straight alcohol solution, are heated to reflux and have solid precipitation after stirring two hours, filter, use 10mL analyzes straight alcohol washing three times, places drying at 50 DEG C, obtains ligand H2mtyp.H after 0.220g is dried2mtyp、 0.200g analyzes pure copper acetate and 0.04g analysis pure cerium hydroxide sodium is dissolved in 14mL analysis straight alcohols, is placed in micro- reaction bulb, It adds 6mL and analyzes pure acetonitrile, stand three days at normal temperatures, there is kermesinus crystal to generate i.e. [Cu2Na2(mtyp)2 (CH3COO)2 (H2O)3]n.Yield:0.226g, yield 58%.[Cu is measured by single crystal diffractometer2Na2 (mtyp)2(CH3COO)2(H2O)3]n Structure, crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
(2) [Cu obtained by step (1) is taken2Na2(mtyp)2(CH3COO)2(H2O)3]nIt is dissolved in the pure N of analysis, N '-dimethyl formyl A concentration of 5.0 × 10 are made into amine solvent-6The solution of mol/L carries out fluorometric investigation, [Cu2Na2(mtyp)2(CH3COO)2 (H2O)3]nUnder the wavelength excitation of 416nm, maximum emission wavelength generates shining for 660a.u. fluorescence intensities at 508 nm.

Claims (1)

1. a kind of fluorescent material [Cu2Na2(mtyp)2(CH3COO)2(H2O)3]n, it is characterised in that [Cu2Na2(mtyp)2 (CH3COO)2(H2O)3]nMolecular formula be:C22H26Cu2N10Na2O11, molecular weight is:779.59,H2Mtyp is 3- methoxyl group water Poplar aldehyde contracting -5- amino -1- hydrogen -1,2,3,4- tetrazole schiff bases;Crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table Two;[Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nUnder the wavelength excitation of 416nm, maximum emission wavelength generates at 508nm 660a.u. fluorescence intensities shine;
Table one:[Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nCrystallographic parameter
Table two:[Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nBond distanceWith bond angle °
[the Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nSynthetic method the specific steps are:
(1) by the analytically pure 3- methoxysalicyl aldehydes of 1.521g and analytically pure four nitrogen of 5- amino -1- hydrogen -1,2,3,4- of 0.851g Azoles is dissolved in 30mL analysis straight alcohol solution, ligand H is obtained after being heated to reflux two hours2mtyp;0.110-0.220g is done H after dry2Mtyp, 0.100-0.200g analyze pure copper acetate and 0.02-0.04g analysis pure cerium hydroxide sodium is dissolved in 7-14mL analyses It in straight alcohol, is placed in micro- reaction bulb, adds 3-6mL and analyze pure acetonitrile, stand three days at normal temperatures, there is the life of kermesinus crystal At i.e. [Cu2Na2(mtyp)2(CH3COO)2(H2O)3]n
(2) [Cu obtained by step (1) is taken2Na2(mtyp)2(CH3COO)2(H2O)3]nIt is dissolved in the pure N of analysis, N '-dimethyl formamide is molten A concentration of 5.0 × 10 are made into agent-6The solution of mol/L carries out fluorometric investigation, [Cu2Na2(mtyp)2(CH3COO)2(H2O)3]n Under the wavelength excitation of 416nm, maximum emission wavelength generates shining for 660a.u. fluorescence intensities at 508nm.
CN201610221790.5A 2016-04-08 2016-04-08 Fluorescent material [Cu2Na2(mtyp)2(CH3COO)2(H2O)3]nAnd synthetic method Expired - Fee Related CN105694867B (en)

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CN104031639A (en) * 2014-06-25 2014-09-10 桂林理工大学 Fluorescent material [ZnNa(ehbd)2N3]n and synthetic method thereof
CN104194772A (en) * 2014-08-25 2014-12-10 桂林理工大学 Fluorescent material [CuNa(ehbd)2(dca)(CH3OH)] and synthesis method thereof

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CN104031639A (en) * 2014-06-25 2014-09-10 桂林理工大学 Fluorescent material [ZnNa(ehbd)2N3]n and synthetic method thereof
CN104194772A (en) * 2014-08-25 2014-12-10 桂林理工大学 Fluorescent material [CuNa(ehbd)2(dca)(CH3OH)] and synthesis method thereof

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