CN107056824A - 对苯二甲酸锌配合物的制备、结构及荧光性质 - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- KYQCOXFCLRTKLS-UHFFFAOYSA-N Pyrazine Chemical compound C1=CN=CC=N1 KYQCOXFCLRTKLS-UHFFFAOYSA-N 0.000 claims abstract description 52
- PCNDJXKNXGMECE-UHFFFAOYSA-N Phenazine Natural products C1=CC=CC2=NC3=CC=CC=C3N=C21 PCNDJXKNXGMECE-UHFFFAOYSA-N 0.000 claims abstract description 26
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000011701 zinc Substances 0.000 claims abstract description 15
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 4
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
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- 229910021645 metal ion Inorganic materials 0.000 claims description 9
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 5
- 125000004429 atom Chemical group 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N Formic acid Chemical group OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 3
- 229910007541 Zn O Inorganic materials 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 150000001455 metallic ions Chemical class 0.000 claims description 3
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 241000040710 Chela Species 0.000 claims description 2
- NHXLWAPIFFWMRV-UHFFFAOYSA-N formic acid;pyrazine Chemical compound OC=O.C1=CN=CC=N1 NHXLWAPIFFWMRV-UHFFFAOYSA-N 0.000 claims 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 229910052723 transition metal Inorganic materials 0.000 abstract description 2
- 150000003624 transition metals Chemical class 0.000 abstract description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 239000013110 organic ligand Substances 0.000 description 2
- KUCOHFSKRZZVRO-UHFFFAOYSA-N terephthalaldehyde Chemical compound O=CC1=CC=C(C=O)C=C1 KUCOHFSKRZZVRO-UHFFFAOYSA-N 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- -1 benzene Dioctyl phthalate pyrazine Chemical compound 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
本发明公开了对苯二甲酸吡嗪锌配合物的制备、结构及其荧光性质。该配合物属于单斜晶系，空间群为P21/c，对苯二甲酸的两个羧基一个以单齿的形式与Zn(II)离子配位，另一个以螯合的形式与Zn(II)离子配位，吡嗪以桥联的形式参与配位。室温下测定了对苯二甲酸和配合物的荧光性能。对苯二甲酸在280nm的波长激发下，最大荧光发射在385nm处。配合物在290nm激发波长下，最大荧光发射为382nm。相比配体有3nm蓝移，荧光强度减弱。本发明利用对苯二甲酸、吡嗪为配体和硝酸锌通过水热法获得对苯二甲酸吡嗪锌配合物，具有工艺简单、成本低廉、重复性好等优点，为合成过渡金属的配合物提供了一定的依据。
Description
技术领域
本发明属于配合物制备技术领域，特别涉及一种对苯二甲酸锌配合物的制备、结构及其荧光性质。
背景技术
金属与羧酸类有机配体所形成的配位化合物结构多样，用途广泛，越来越受到人们的重视，它的研究涉及到无机配位化学、有机化学、晶体化学及材料化学等诸多领域，已成为当今化学研究领域的热点之一。羧酸类配体由于它具有单齿配位，双齿配位，桥联，螯合等多样的配位模式和氢键等弱相互作用的大量存在，是一种被广泛应用的配体，对苯二甲酸便是其中的一种良好的配体。另外，对于吡嗪，它具有分子内共轭大π键，能够作为十分有效的生色团来测定产物，并且具有很好的分子内电子传递和能量传递性质，是一种良好的辅助配体。
发明内容
本发明的目的是提供一种对苯二甲酸锌配合物的制备、结构及其荧光性质。
本发明的思路：利用对苯二甲酸、吡嗪为配体和硝酸锌通过水热法获得对苯二甲酸吡嗪锌配合物。
对苯二甲酸吡嗪锌配合物的结构见附图1。该配合物属于单斜晶系，空间群为P21/c，在该配合物中，对苯二甲酸的两个羧基一个以单齿的形式与金属离子Zn(II)配位，另一个以螯合的形式与金属离子Zn(II)配位。吡嗪以桥联的形式参与配位，水中的氧通过孤对电子与金属离子Cd(II)形成配位键参与配位。中心金属离子Zn(II)分别与来自两个不同的对苯二甲酸配体上的三个氧原子(O1、O3A、O4A)，一个吡嗪的一个氮原子(N1)配位，水分子中的氧原子(O5)配位。五个配位原子在Zn(II)离子周围以畸变三角双锥形式排布。Zn-O键长在之间，Zn-N键长是
该对苯二甲酸吡嗪锌配合物的制备方法为：
(1)称量0.5～1毫摩尔硝酸锌溶解于2～4毫升蒸馏水中，制得硝酸锌溶液；
(2)称量0.5～1毫摩尔对苯二甲酸溶解于5～10毫升蒸馏水中，制得对苯二甲酸溶液；
(3)称量0.5～1毫摩尔吡嗪溶解于2～4毫升蒸馏水中，制得吡嗪溶液；
(4)将上述溶液混合并加入1～2毫摩尔三乙胺；
(5)将上述制得的溶液加入到聚四氟乙烯反应釜内胆中，在室温下磁力搅拌0.5～1小时，套上不锈钢反应釜外套放入90摄氏度反应48～72小时，反应完成后以每小时10摄氏度梯度降至室温，静置12～24小时后开釜得无色溶液，过滤得无色透明块状晶体，即为对苯二甲酸吡嗪锌配合物。
本发明具有工艺简单、成本低廉、重复性好等优点，成功的合成了对苯二甲酸吡嗪锌配合物，为合成过渡金属的配合物提供了一定的依据。
该配合物具有良好的发光性能，在室温下对有机配体对苯二甲酸和配合物进行了荧光性能的测试。如附图2所示，对苯二甲酸在280nm的波长激发下，最大荧光发射波长在385nm处，可归属于π*→π或π*→n的跃迁。配合物在290nm激发波长下，最大荧光发射波长为382nm。相比配体最大荧光发射波长有3nm蓝移，荧光强度减弱。
附图说明
图1是本发明的对苯二甲酸吡嗪锌配合物的分子结构图。
图2是本发明的对苯二甲酸和配合物室温固态荧光发射光谱。
具体实施方式
实施例：
(1)称量0.5毫摩尔(0.1487克)硝酸锌溶解于3毫升蒸馏水中，制得硝酸锌溶液；
(2)称量0.5毫摩尔(0.0831克)对苯二甲酸溶解于5毫升蒸馏水中，制得对苯二甲酸溶液；
(3)称量0.5毫摩尔(0.0400克)吡嗪溶解于2毫升蒸馏水中，制得吡嗪溶液；
(4)将上述溶液混合并加入1毫摩尔(0.1012克)三乙胺；
(5)将上述制得的溶液加入到聚四氟乙烯反应釜内胆中，在室温下磁力搅拌0.5小时，套上不锈钢反应釜外套放入90摄氏度反应72小时，反应完成后以每小时10摄氏度梯度降至室温，静置12小时后开釜得无色溶液，过滤得无色透明块状晶体，即为对苯二甲酸吡嗪锌配合物。
该配合物属于单斜晶系，空间群为P21/c，在该配合物中，对苯二甲酸的两个羧基一个以单齿的形式与金属离子Zn(II)配位，另一个以螯合的形式与金属离子Zn(II)配位。吡嗪以桥联的形式参与配位，水中的氧提供孤对电子与金属离子Cd(II)形成配位键参与配位。中心金属离子Zn(II)分别与来自两个不同的对苯二甲酸配体上的三个氧原子(O1、O3A、O4A)，一个吡嗪的一个氮原子(N1)配位，水分子中的氧原子(O5)配位。五个配位原子在Zn(II)离子周围以畸变三角双锥形式排布。Zn-O键长在之间，Zn-N键长是
Claims (3)
1.一种对苯二甲酸吡嗪锌配合物的结构。该配合物属于单斜晶系，空间群为P21/c，在该配合物中，对苯二甲酸的两个羧基一个以单齿的形式与金属离子Zn(II)配位，另一个以螯合的形式与金属离子Zn(II)配位。吡嗪以桥联的形式参与配位，水中的氧通过孤对电子与金属离子Cd(II)形成配位键参与配位。中心金属离子Zn(II)分别与来自两个不同的对苯二甲酸配体上的三个氧原子(O1、O3A、O4A)，一个吡嗪的一个氮原子(N1)配位，水分子中的氧原子(O5)配位。五个配位原子在Zn(II)离子周围以畸变三角双锥形式排布。Zn-O键长在之间，Zn-N键长是
2.根据权利要求1所述的对苯二甲酸吡嗪锌配合物的制备方法，其特征在于具体步骤为：
(1)称量0.5～1毫摩尔硝酸锌溶解于2～4毫升蒸馏水中，制得硝酸锌溶液；
(2)称量0.5～1毫摩尔对苯二甲酸溶解于5～10毫升蒸馏水中，制得对苯二甲酸溶液；
(3)称量0.5～1毫摩尔吡嗪溶解于2～4毫升蒸馏水中，制得吡嗪溶液；
(4)将上述溶液混合并加入1～2毫摩尔三乙胺；
(5)将上述制得的溶液加入到聚四氟乙烯反应釜内胆中，在室温下磁力搅拌0.5～1小时，套上不锈钢反应釜外套放入90摄氏度反应48～72小时，反应完成后以每小时10摄氏度梯度降至室温，静置12～24小时后开釜得无色溶液，过滤得无色透明块状晶体，即为对苯二甲酸吡嗪锌配合物。
3.配合物的荧光性质
在室温下对配体对苯二甲酸和配合物进行了荧光性能的测试。对苯二甲酸在280nm的波长激发下，最大荧光发射波长在385nm处。配合物在290nm激发波长下，最大荧光发射波长为382nm。相比配体最大荧光发射波长有3nm蓝移，荧光强度减弱。
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