CN105694861A - 发光材料[Mn(tibc)2]n及合成方法 - Google Patents
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- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 4
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- FMCUPJKTGNBGEC-UHFFFAOYSA-N 1,2,4-triazol-4-amine Chemical compound NN1C=NN=C1 FMCUPJKTGNBGEC-UHFFFAOYSA-N 0.000 abstract 1
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000003446 ligand Substances 0.000 abstract 1
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Abstract
本发明公开了一种荧光材料[Mn(tibc)2]n及合成方法。单体分子式为：C18H10MnBr4N8O2，分子量为：744.88g/mol,Htibc为3,5-二溴水杨醛缩4-氨基-1,2,4三氮唑希夫碱。将分析纯的3,5-二溴水杨醛和分析纯的4-氨基-1,2,4-三氮唑，溶于分析纯乙醇溶液中，加热回流并搅拌得到配体Htibc。将干燥后的Htibc和分析纯乙酸镉溶于分析纯N,N’-二甲基甲酰胺中，再加入蒸馏水，在80℃烘箱中静置三天。[Mn(tibc)2]n在450nm的入射光照射下产生1980a.u.强度的479nm的荧光；在800V的光电倍增管，3倍的放大系数下，置于1mol/L过硫酸钾溶液中，产生3010a.u.强度的发光，且在此条件下，能持续而稳定发光。本发明工艺简单、成本低廉、化学组分易于控制、重复性好且产量高。
Description
技术领域
本发明涉及一种稳定的发光材料[Mn(tibc)2]n,(Htibc为3,5-二溴水杨醛缩4-氨基-1,2,4三氮唑希夫碱)及合成方法。
背景技术
现代发光材料历经数十年的发展，己成为信息显示、照明光源、光电器件等领域的支撑材料，为社会发展和技术进步发挥着日益重要的作用。特别是能源紧缺的现在，开发转化效率高的发光材料是解决能源紧缺问题方法之一。
发明内容
本发明的目的就是为设计合成发光性质优异的功能材料，利用微瓶反应方法合成[Mn(tibc)2]n。
本发明涉及的[Mn(tibc)2]n的分子式为：C18H10MnBr4N8O2，分子量为：744.88g/mol,Htibc为3,5-二溴水杨醛缩4-氨基-1,2,4三氮唑希夫碱，晶体结构数据见表一,键长键角数据见表二。
表一:[Mn(tibc)2]n的晶体学参数
aR1＝Σ||Fo|–|Fc||/Σ|Fo|.bwR2＝[Σw(|Fo 2|–|Fc 2|)2/Σw(|Fo 2|)2]1/2
表二:[Mn(tibc)2]n的键长和键角°
| Br16—C15 | 1.903(5) | C4—C6 | 1.431(6) |
| Mn5—O3i | 2.050(3) | C4—C2 | 1.428(7) |
| Mn5—O3 | 2.050(3) | N9—N1 | 1.390(5) |
| Mn5—N11 | 2.407(4) | N9—C10 | 1.304(6) |
| Mn5—N11i | 2.407(4) | N1—C8 | 1.292(6) |
| Mn5—N1 | 2.251(4) | C12—C13 | 1.359(7) |
| Mn5—N1i | 2.251(4) | C15—C14 | 1.356(6) |
| Br17—C13 | 1.897(5) | C15—C2 | 1.413(6) |
| O3—C2 | 1.280(5) | C13—C14 | 1.385(7) |
| N11—C6 | 1.286(6) | N7—N11iii | 1.428(5) |
| N11—N7ii | 1.428(5) | N7—C10 | 1.351(6) |
| C4—C12 | 1.403(6) | N7—C8 | 1.358(6) |
| O3—Mn5—O3i | 164.43(19) | C10—N9—N1 | 107.1(4) |
| O3—Mn5—N11 | 78.35(12) | N9—N1—Mn5 | 127.0(3) |
| O3—Mn5—N11i | 92.00(12) | C8—N1—Mn5 | 124.2(3) |
| O3i—Mn5—N11 | 92.00(12) | C8—N1—N9 | 107.1(4) |
| O3i—Mn5—N11i | 78.35(12) | C13—C12—C4 | 121.2(5) |
| O3—Mn5—N1 | 104.00(13) | C14—C15—Br16 | 117.4(4) |
| O3—Mn5—N1i | 87.80(13) | C14—C15—C2 | 125.3(4) |
| O3i—Mn5—N1 | 87.79(13) | N11—C6—C4 | 127.3(5) |
| N11i—Mn5—N11 | 103.9(2) | C12—C13—Br17 | 121.2(4) |
| N1—Mn5—N11i | 161.44(14) | C12—C13—C14 | 120.3(4) |
| N1i—Mn5—N11 | 161.44(14) | C14—C13—Br17 | 118.3(4) |
| N1—Mn5—N11 | 88.75(14) | C10—N7—N11iii | 127.2(4) |
| N1i—Mn5—N11i | 88.75(14) | C10—N7—C8 | 105.3(4) |
| N1—Mn5—N1i | 82.6(2) | C8—N7—N11iii | 127.5(4) |
| C2—O3—Mn5 | 137.0(3) | C15—C14—C13 | 118.5(4) |
| C6—N11—Mn5 | 122.6(3) | O3—C2—C4 | 123.3(4) |
| C6—N11—N7ii | 111.6(4) | O3—C2—C15 | 122.7(4) |
| N7ii—N11—Mn5 | 124.9(3) | C15—C2—C4 | 114.0(4) |
| C12—C4—C6 | 116.1(4) | N9—C10—N7 | 110.0(5) |
| C12—C4—C2 | 120.6(4) | N1—C8—N7 | 110.4(4) |
| C2—C4—C6 | 123.3(4) |
Symmetrycodes:(i)y,x,-z+1；(ii)y+1,x,-z+1；(iii)y,x-1,-z+1.
所述[Mn(tibc)2]n的合成方法具体步骤为：
(1)将2.79g分析纯的3,5-二溴水杨醛和0.841g分析纯的4-氨基-1,2,4-三氮唑，溶于30mL分析纯乙醇溶液中，加热回流并搅拌两个小时后有固体析出，过滤，用10mL分析纯乙醇洗涤三次，放置50℃下干燥，得到配体Htibc。将0.056-0.112g干燥后的Htibc和0.050-0.100g分析纯乙酸锰溶于5mL分析纯N,N’-二甲基甲酰胺溶剂中，置于微反应瓶中，再加入5mL蒸馏水，在80℃烘箱中静置三天，有暗红色晶体生成即[Mn(tibc)2]n。通过单晶衍射仪测定[Mn(tibc)2]n的结构，晶体结构数据见表一,键长键角数据见表二。
(2)取步骤(1)所得[Mn(tibc)2]n溶于分析纯N,N’-二甲基甲酰胺溶剂中配成浓度为5.0×10-6mol/L的溶液，进行荧光测试，[Mn(tibc)2]n在450nm的入射光照射下产生1980a.u.强度的479nm的荧光；在800V的光电倍增管，3倍的放大系数下，取100μL上述配好的溶液置于1mol/L过硫酸钾溶液(导电介质)中，产生了3010a.u.强度的发光，且在此条件下，能持续而稳定发光。
本发明具有工艺简单、成本低廉、化学组分易于控制、重复性好并产量高等优点。
附图说明
图1为本发明[Mn(tibc)2]n的结构图。
图2为本发明[Mn(tibc)2]n的二维平面图。
图3为本发明[Mn(tibc)2]n的三维结构图。
图4为本发明[Mn(tibc)2]n荧光光谱图。
图5为本发明[Mn(tibc)2]n的电化学发光光谱图。
具体实施方式
实施例1：
本发明涉及的[Mn(tibc)2]n的分子式为：C18H10MnBr4N8O2，分子量为：744.88g/mol,Htibc为3,5-二溴水杨醛缩4-氨基-1,2,4三氮唑希夫碱，晶体结构数据见表一,键长键角数据见表二。
[Mn(tibc)2]n的合成方法具体步骤为：
(1)将2.79g分析纯的3,5-二溴水杨醛和0.841g分析纯的4-氨基-1,2,4-三氮唑，溶于30mL分析纯乙醇溶液中，加热回流并搅拌两个小时后有固体析出，过滤，用10mL分析纯乙醇洗涤三次，放置50℃下干燥，得到配体Htibc。产量：2.641g，产率96％。将0.056g干燥后的Htibc和0.050分析纯乙酸锰溶于5mL分析纯N,N’-二甲基甲酰胺中，置于微反应瓶中，再加入5mL蒸馏水，在80℃烘箱中静置三天，有暗红色晶体生成即[Mn(tibc)2]n。产量：0.059g，产率63％。通过单晶衍射仪测定[Mn(tibc)2]n的结构，晶体结构数据见表一,键长键角数据见表二。
(2)取步骤(1)所得[Mn(tibc)2]n溶于分析纯N,N’-二甲基甲酰胺溶剂中配成浓度为5.0×10-5mol/L的溶液，进行荧光测试，[Mn(tibc)2]n在450nm的入射光照射下产生1980a.u.强度的479nm的荧光；在800V的光电倍增管，3倍的放大系数下，取100μL上述配好的溶液置于1mol/L过硫酸钾溶液(导电介质)中，产生了3010a.u.强度的发光，且在此条件下，能持续而稳定发光。
实施例2：
本发明涉及的[Mn(tibc)2]n的分子式为：C18H10MnBr4N8O2，分子量为：744.88g/mol,Htibc为3,5-二溴水杨醛缩4-氨基-1,2,4三氮唑希夫碱，晶体结构数据见表一,键长键角数据见表二。
[Mn(tibc)2]n的合成方法具体步骤为：
(1)将2.79g分析纯的3,5-二溴水杨醛和0.841g分析纯的4-氨基-1,2,4-三氮唑，溶于30mL分析纯乙醇溶液中，加热回流并搅拌两个小时后有固体析出，过滤，用10mL分析纯乙醇洗涤三次，放置50℃下干燥，得到配体Htibc。产量：2.641g，产率96％。将0.112g干燥后的Htibc和0.108g分析纯乙酸锰溶于5mL分析纯N,N’-二甲基甲酰胺中，置于微反应瓶中，再加入5mL蒸馏水，在80℃烘箱中静置三天，有暗红色晶体生成即[Mn(tibc)2]n。产量：0.109g，产率57％。通过单晶衍射仪测定[Mn(tibc)2]n的结构，晶体结构数据见表一,键长键角数据见表二。
(2)取步骤(1)所得[Mn(tibc)2]n溶于分析纯N,N’-二甲基甲酰胺溶剂中配成浓度为5.0×10-5mol/L的溶液，进行荧光测试，[Mn(tibc)2]n在450nm的入射光照射下产生1980a.u.强度的479nm的荧光；在800V的光电倍增管，3倍的放大系数下，取100μL上述配好的溶液置于1mol/L过硫酸钾溶液(导电介质)中，产生了3010a.u.强度的发光，且在此条件下，能持续而稳定发光。
Claims (1)
1.一种发光材料[Mn(tibc)2]n，其特征在于[Mn(tibc)2]n的单体分子式为：C18H10MnBr4N8O2，分子量为：744.88g/mol,Htibc为3,5-二溴水杨醛缩4-氨基-1,2,4三氮唑希夫碱，晶体结构数据见表一,键长键角数据见表二；在450nm的入射光照射下产生1980a.u.强度的479nm的荧光；在800V的光电倍增管，3倍的放大系数下，置于1mol/L过硫酸钾溶液中，产生3010a.u.强度的发光，且在此条件下，能持续而稳定发光；
表一:[Mn(tibc)2]n的晶体学参数
aR1＝Σ||Fo|–|Fc||/Σ|Fo|.bwR2＝[Σw(|Fo 2|–|Fc 2|)2/Σw(|Fo 2|)2]1/2
表二:[Mn(tibc)2]n的键长和键角°
Symmetrycodes:(i)y,x,-z+1；(ii)y+1,x,-z+1；(iii)y,x-1,-z+1.
所述[Mn(tibc)2]n的合成方法具体步骤为：
将2.79g分析纯的3,5-二溴水杨醛和0.841g分析纯的4-氨基-1,2,4-三氮唑，溶于30mL分析纯乙醇溶液中，加热回流并搅拌两个小时后有固体析出，过滤，用10mL分析纯乙醇洗涤三次，放置50℃下干燥，得到配体Htibc；将0.056-0.112g干燥后的Htibc和0.050-0.100g分析纯乙酸锰溶于5mL分析纯N,N’-二甲基甲酰胺溶剂中，置于微反应瓶中，再加入5mL蒸馏水，在80℃烘箱中静置三天，有暗红色晶体生成即[Mn(tibc)2]n。
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