CN105622649A - 蒽环双***间苯二甲酸包结二甲基乙酰胺锌配合物单晶及应用 - Google Patents
蒽环双***间苯二甲酸包结二甲基乙酰胺锌配合物单晶及应用 Download PDFInfo
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- 239000013078 crystal Substances 0.000 title claims abstract description 20
- QWENRTYMTSOGBR-UHFFFAOYSA-N 1H-1,2,3-Triazole Chemical compound C=1C=NNN=1 QWENRTYMTSOGBR-UHFFFAOYSA-N 0.000 title abstract 3
- VONQHBNZVVGNAO-UHFFFAOYSA-N N,N-dimethylacetamide zinc Chemical compound [Zn].CN(C)C(C)=O VONQHBNZVVGNAO-UHFFFAOYSA-N 0.000 title abstract 3
- 229940045799 anthracyclines and related substance Drugs 0.000 title abstract 3
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000975 dye Substances 0.000 claims abstract description 20
- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 6
- 239000012046 mixed solvent Substances 0.000 claims abstract description 6
- 150000003852 triazoles Chemical class 0.000 claims description 15
- WFKAJVHLWXSISD-UHFFFAOYSA-N isobutyramide Chemical compound CC(C)C(N)=O WFKAJVHLWXSISD-UHFFFAOYSA-N 0.000 claims description 14
- 150000001454 anthracenes Chemical class 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 230000005260 alpha ray Effects 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 230000005855 radiation Effects 0.000 claims description 3
- 238000001914 filtration Methods 0.000 abstract description 5
- 239000011701 zinc Substances 0.000 abstract 3
- CPIYEXXYOQSGAM-UHFFFAOYSA-N 1-[10-(1,2,4-triazol-1-yl)anthracen-9-yl]-1,2,4-triazole Chemical compound C1=NN(C=N1)C1=C2C=CC=CC2=C(N2C=NC=N2)C2=CC=CC=C12 CPIYEXXYOQSGAM-UHFFFAOYSA-N 0.000 abstract 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 18
- NSPMIYGKQJPBQR-UHFFFAOYSA-N 4H-1,2,4-triazole Chemical compound C=1N=CNN=1 NSPMIYGKQJPBQR-UHFFFAOYSA-N 0.000 description 13
- BRUOAURMAFDGLP-UHFFFAOYSA-N 9,10-dibromoanthracene Chemical compound C1=CC=C2C(Br)=C(C=CC=C3)C3=C(Br)C2=C1 BRUOAURMAFDGLP-UHFFFAOYSA-N 0.000 description 11
- 239000000243 solution Substances 0.000 description 11
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 229910000027 potassium carbonate Inorganic materials 0.000 description 9
- 239000005751 Copper oxide Substances 0.000 description 7
- 229910000431 copper oxide Inorganic materials 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 3
- 238000000113 differential scanning calorimetry Methods 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- -1 and after filtration Substances 0.000 description 2
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical class C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 150000002460 imidazoles Chemical class 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000002798 polar solvent Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241001597008 Nomeidae Species 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000019771 cognition Effects 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000005564 crystal structure determination Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 230000001795 light effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000001455 metallic ions Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000003217 pyrazoles Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- GRONZTPUWOOUFQ-UHFFFAOYSA-M sodium;methanol;hydroxide Chemical compound [OH-].[Na+].OC GRONZTPUWOOUFQ-UHFFFAOYSA-M 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/003—Compounds containing elements of Groups 2 or 12 of the Periodic Table without C-Metal linkages
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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Abstract
本发明公开了蒽环双***间苯二甲酸包结二甲基乙酰胺锌配合物单晶及应用,其结构:[Zn(L)(ipa)(H2O)]·2.25DMAC,其中,L=1-[9-(1H-1,2,4-三氮唑-1-基)蒽-10-基]-1H-1,2,4-三氮唑;ipa=间苯二甲酸;DMAC=N,Nˊ-二甲基乙酰胺。它是采用常温挥发法,即Zn(NO3)2·6H2O、ipa和L在DMAC和水的混合溶剂中搅拌半小时后过滤,滤液常温挥发一周后得到适合X-射线单晶衍射的无色棒状晶体。其中,Zn(NO3)2·6H2O:ipa:L的摩尔比为1:1:1。本发明进一步公开了蒽环双***间苯二甲酸包结二甲基乙酰胺包结二甲基乙酰胺锌配合物作为潜在荧光材料在检测染料或发光剂的吸附量方面的应用。
Description
本发明得到国家自然科学基金面上项目(21471113)、天津市教委面上项目(20140506)和天津师范大学中青年教师学术创新推进计划项目(52XC1401)的资助。
技术领域
本发明属于有机和无机合成技术领域,涉及述蒽环双***间苯二甲酸包结二甲基乙酰胺锌配合物[Zn(L)(ipa)(H2O)]·2.25DMAC的制备方法及作为潜在的荧光材料的应用,其中,L=1-[9-(1H-1,2,4-三氮唑-1-基)蒽-10-基]-1H-1,2,4-三氮唑;ipa=间苯二甲酸;DMAC=N,N'-二甲基乙酰胺。
背景技术
1,2,4-***及其衍生物兼有吡唑和咪唑的配位特点,是配位能力较强的桥连配体,目前已合成并表征了大量的单核、多核和多维化合物。这些配体能够以1,2位上的氮原子与金属离子配位形成N1,N2-桥连模式,对于4位未取代的1,2,4-***衍生物能通过2,4位上的氮原子形成N2,N4-桥连模式,这种N2,N4-桥连模式同金属酶中咪唑的N1,N3-桥连模式类似。对于***类化合物的特殊用途还表现在分子器件化的设计上,合成具有不同维数的金属配合物乃是完成器件化至关重要的一步。
本发明即是采用常温挥发法,即Zn(NO3)2·6H2O、ipa和L在DMAC和水的混合溶剂中搅拌半小时后过滤,滤液常温挥发一周后得到适合X-射线单晶衍射的无色棒状晶体[Zn(L)(ipa)(H2O)]·2.25DMAC,其中,L=1-[9-(1H-1,2,4-三氮唑-1-基)蒽-10-基]-1H-1,2,4-三氮唑;ipa=间苯二甲酸;DMAC=N,N'-二甲基乙酰胺。该配合物还可作为潜在的荧光材料方面得以应用。
发明内容
为此本发明人提供了如下的技术方案:
一种蒽环双***间苯二甲酸包结二甲基乙酰胺锌配合物的单晶,其特征在于该单晶结构采用APEXIICZN单晶衍射仪,使用经过石墨单色化的Mokα射线,λ=0.71073?为入射辐射,以ω-2θ扫描方式收集衍射点,经过最小二乘法修正得到晶胞参数,从差值傅立叶电子密度图利用SHELXL-97直接法解得单晶数据:
其结构如下:
[Zn(L)(ipa)(H2O)]·2.25DMAC,其中
L=1-[9-(1H-1,2,4-三氮唑-1-基)蒽-10-基]-1H-1,2,4-三氮唑;
ipa=间苯二甲酸;
DMAC=N,N'-二甲基乙酰胺。
本发明进一步公开了蒽环双***间苯二甲酸包结二甲基乙酰胺锌配合物单晶的制备方法,其特征在采用常温挥发法,将Zn(NO3)2·6H2O、ipa和L在DMAC和水的混合溶剂中搅拌半小时后过滤,滤液常温挥发一周后得到适合X-射线单晶衍射的无色棒状晶体;其中Zn(NO3)2·6H2O:ipa:L的摩尔比为1:1:1;
蒽环双***间苯二甲酸包结二甲基乙酰胺锌配合物单晶的结构为[Zn(L)(ipa)(H2O)]·2.25DMAC;其中L=1-[9-(1H-1,2,4-三氮唑-1-基)蒽-10-基]-1H-1,2,4-三氮唑;ipa=间苯二甲酸;DMAC=N,N'-二甲基乙酰胺;
Lipa。
本发明更进一步公开了蒽环双***间苯二甲酸包结二甲基乙酰胺锌配合物单晶作为潜在荧光材料在检测染料或发光剂的吸附量方面的应用,实验结果显示:
(1)实施例2中的配合物单晶对染料具有很好的选择性和灵敏性,检测限达到0.1ppm。
(2)能够检出痕量的发光剂,检出限达到5.0μg/L。
(3)实施例2制备的配合物单晶对于染料的吸附量为1.4×10-3mol/cm2。
本发明一个优选的例子:
1-[9-(1H-1,2,4-三氮唑-1-基)蒽-10-基]-1H-1,2,4-三氮唑(L)的制备
9,10-二溴蒽:1H-1,2,4-***:碳酸钾:氧化铜的摩尔比为2:10:30:1
在装有磁子、回流冷凝器和温度计的50mL三口圆底烧瓶内分别加入CuO(0.0398mg,0.5mmol),碳酸钾(2.0731g,15mmol),1H-1,2,4-***(0.345mg,5mmol),9,10-二溴蒽(0.3360g,1mmol)和20mLDMF。开动搅拌在100oC,反应24小时。反应结束后,将反应液降至室温,过滤,滤液加入100mL水,析出大量沉淀,抽滤,收集滤饼,收率60%。元素分析(C18N6H12)理论值(%):C,69.22;H,3.87;N,26.91。实测值:C,69.26;H,3.99;N,26.95;
9,10-二溴蒽1H-1,2,4-***
本发明优选9,10-二溴蒽:1H-1,2,4-***:碳酸钾:氧化铜的摩尔比为2:10:30:1;反应温度80-200℃,反应时间12-120小时。在极性溶剂中,采用“一锅法”,将9,10-二溴蒽,1H-1,2,4-***,碳酸钾和氧化铜在加热条件下制备1-[9-(1H-1,2,4-三氮唑-1-基)蒽-10-基]-1H-1,2,4-三氮唑(L)。
本发明另一个优选的实施例
1-[9-(1H-1,2,4-三氮唑-1-基)蒽-10-基]-1H-1,2,4-三氮唑(L)(0.1mmol)、ipa(0.1mmol)和Zn(NO3)2·6H2O(0.1mmo)在10mL水和6mLDMAC混合溶剂中搅拌半小时后产生少量无色沉淀,过滤后,滤液呈无色。常温挥发一周后有适合X-射线单晶衍射的无色棒状晶体。产率:35%。元素分析(C140H145N33O25Zn4)理论值(%):C,56.97;H,4.95;N,15.66。实测值:C,56.92;H,4.94;N,15.62。
本发明公开的一种蒽环双***间苯二甲酸包结二甲基乙酰胺锌配合物单晶所具有的优点和特点在于:
(1)反应操作简便易行。
(2)反应收率高,所得产品的纯度高。
(3)本发明所制备的蒽环双***间苯二甲酸包结二甲基乙酰胺锌配合物单晶,生产成本低,方法简便,适合大规模生产。在染料或发光剂应用方面可以解决拓宽染料的光电响应范围问题。
附图说明
图1:配合物单晶的晶体结构图;
图2:配合物单晶的二维层状结构图。
具体实施方式
下面结合实施例对本发明做进一步的说明,实施例仅为解释性的,决不意味着它以任何方式限制本发明的范围。所用原料9,10-二溴蒽、1H-1,2,4-三氮唑、碳酸钾和氧化铜等均有市售,直接购买,没有经过继续提纯而直接使用。
实施例1
1-[9-(1H-1,2,4-三氮唑-1-基)蒽-10-基]-1H-1,2,4-三氮唑(L)的制备
9,10-二溴蒽:1H-1,2,4-***:碳酸钾:氧化铜的摩尔比为2:10:30:1
在装有磁子、回流冷凝器和温度计的50mL三口圆底烧瓶内分别加入CuO(0.0398mg,0.5mmol),碳酸钾(2.0731g,15mmol),1H-1,2,4-***(0.345mg,5mmol),9,10-二溴蒽(0.3360g,1mmol)和20mLDMF。开动搅拌在100oC,反应24小时。反应结束后,将反应液降至室温,过滤,滤液加入100mL水,析出大量沉淀,抽滤,收集滤饼,收率60%。元素分析(C18N6H12)理论值(%):C,69.22;H,3.87;N,26.91。实测值:C,69.26;H,3.99;N,26.95;
9,10-二溴蒽1H-1,2,4-***
本发明优选9,10-二溴蒽:1H-1,2,4-***:碳酸钾:氧化铜的摩尔比为2:10:30:1;反应温度80-200℃,反应时间12-120小时。在极性溶剂中,采用“一锅法”,将9,10-二溴蒽,1H-1,2,4-***,碳酸钾和氧化铜在加热条件下制备1-[9-(1H-1,2,4-三氮唑-1-基)蒽-10-基]-1H-1,2,4-三氮唑(L)。
实施例2
1-[9-(1H-1,2,4-三氮唑-1-基)蒽-10-基]-1H-1,2,4-三氮唑(L)(0.1mmol)、ipa(0.1mmol)和Zn(NO3)2·6H2O(0.1mmo)在10mL水和6mLDMAC混合溶剂中搅拌半小时后产生少量无色沉淀,过滤后,滤液呈无色。常温挥发一周后有适合X-射线单晶衍射的无色棒状晶体。产率:35%。元素分析(C140H145N33O25Zn4)理论值(%):C,56.97;H,4.95;N,15.66。实测值:C,56.92;H,4.94;N,15.62。
实施例3
晶体结构测定采用APEXIICZN单晶衍射仪,使用经过石墨单色化的Mokα射线,λ=0.71073?为入射辐射,以ω-2θ扫描方式收集衍射点,经过最小二乘法修正得到晶胞参数,从差值傅立叶电子密度图利用软件解出晶体结构,并经洛仑兹和极化效应修正。所有的H原子由差值傅立叶合成并经理想位置计算确定。详细的晶体测定数据:
实施例4
染料或发光剂使用的实际例子
方法:染料溶液的微分脉冲伏安(DPV)曲线通过美国普林斯顿应用研究所研制的PARSTAT2273电化学工作站测量。溶液的DPV测试采用三电极体系,玻碳电极为工作电极,辅助电极为铂片电极,自制的Ag/AgNO3电极为参比电极;电解液为0.1mol·L-1TBAP的乙腈溶液。以二茂铁氧化还原可逆点对为内标,得到测试体系与标准氢电极体系之间的校正值。
单色入射光光电转换效率(IPCE)描述DSCs在单色光作用下的光电转换效率,是转移到外电路的电子数与入射光子数之比。测量时,使用500W氙灯作为光源,入射光经过WDS-5型组合式多功能光栅光谱仪得到不同波长λ下的单色光;单色光照射于电池的光阳极,由Keithley2400数字源表读取电流值I。单色光的福照度由USB4000plug-and-play微型光线光谱仪测量。
步骤:为了确切了解染料在TiO2膜上的吸附量,将实施例2制备的配合物单晶染料敏化TiO2纳米晶膜(几何面积约为1cm2)浸泡在10mL0.01mol·L-1的氢氧化钠的甲醇溶液中过夜,待染料完全解附后测定溶液的吸光度。根据吸光度和摩尔吸光洗漱可以计算出单位面积纳米晶膜上染料的吸附量。该配合物单晶的吸附量为1.4×10-3mol/cm2。
结果:与染料的甲醇溶液相比,配合物单晶染料在TiO2膜上的吸收光谱均明显变宽和红移。这表明染料分子在TiO2形成了首并尾的J-聚集体。从DSCs的工作原理讲,染料聚集引起的光谱宽化和红移对于染料的光电响应范围的拓宽是十分有利的。但与此同时,染料聚集体会大大降低其电子注入效率,从而导致DSCs的性能低下。所以,通常在染料溶液中加入共吸附剂来抑制染料的聚集。该配合物单晶在甲醇溶液中及其在TiO2膜电极上的紫溶液的荧光测试采用2.5×10-5mol/L的甲醇溶液,最大荧光发射波长位于500nm。
实施例5
蒽环双***间苯二甲酸包结二甲基乙酰胺锌配合物单晶作为制备发光材料的应用。
方法:通过荧光分光光度计,分别进行该化合物单晶(实施例2)的激发波长和发射波长的扫描,选择并确定最佳波长。
结论:该化合物的激发波长和发射波长分别为340nm和500nm。
步骤:将蒽环双***间苯二甲酸包结二甲基乙酰胺锌配合物单晶研磨压片成外径为27mm、厚度约3mm的片状样品,放入MPF-4荧光光谱仪的样品池进行测量。
结果:该化合物的激发波长λex=340nm,发射波长λem=500nm。
在详细说明的较佳实施例之后,熟悉该项技术人士可清楚地了解,在不脱离上述申请专利范围与精神下可进行各种变化与修改,凡依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均属于本发明技术方案的范围。且本发明亦不受说明书中所举实例实施方式的限制。
Claims (3)
1.一种蒽环双***间苯二甲酸包结二甲基乙酰胺锌配合物的单晶,其特征在于该单晶结构采用APEXIICZN单晶衍射仪,使用经过石墨单色化的Mokα射线,λ=0.71073?为入射辐射,以ω-2θ扫描方式收集衍射点,经过最小二乘法修正得到晶胞参数,从差值傅立叶电子密度图利用软件解出单晶数据:
其结构如下:
[Zn(L)(ipa)(H2O)]·2.25DMAC,其中
L=1-[9-(1H-1,2,4-三氮唑-1-基)蒽-10-基]-1H-1,2,4-三氮唑;
ipa=间苯二甲酸;
DMAC=N,N'-二甲基乙酰胺。
2.权利要求1所述蒽环双***间苯二甲酸包结二甲基乙酰胺锌配合物单晶的制备方法,其特征在于它是采用常温挥发法,即Zn(NO3)2·6H2O、ipa和L在DMAC和水的混合溶剂中搅拌半小时后过滤,滤液常温挥发一周后得到适合X-射线单晶衍射的无色棒状晶体;其中Zn(NO3)2·6H2O:ipa:L的摩尔比为1:1:1;
蒽环双***间苯二甲酸包结二甲基乙酰胺锌配合物单晶的结构为[Zn(L)(ipa)(H2O)]·2.25DMAC,其中,L=1-[9-(1H-1,2,4-三氮唑-1-基)蒽-10-基]-1H-1,2,4-三氮唑;ipa=间苯二甲酸;DMAC=N,N'-二甲基乙酰胺;
Lipa。
3.权利要求1所述蒽环双***间苯二甲酸包结二甲基乙酰胺锌配合物单晶作为潜在荧光材料在检测染料或发光剂的吸附量方面的应用。
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