贵金属
貴金屬
귀금속
PRECIOUS METALS
2014年
4期
19-25
,共7页
晏彩先%李艳%姜婧%常桥稳%赵婧%雷婧%刘伟平%陈家林
晏綵先%李豔%薑婧%常橋穩%趙婧%雷婧%劉偉平%陳傢林
안채선%리염%강청%상교은%조청%뢰청%류위평%진가림
有机化学%磷光材料%FIrpic%批量合成%结构%光物理性能
有機化學%燐光材料%FIrpic%批量閤成%結構%光物理性能
유궤화학%린광재료%FIrpic%비량합성%결구%광물이성능
organic chemistry%photoluminescence material%bis(4,6-difluorophenyl-pyridine)-(picolinate)iridium(III)%batch production%structure%light-physical property
以水合三氯化铱和 dfppy 为原料,在乙二醇单乙醚溶剂中反应得氯桥二聚体(dfppy)2Ir(μ-Cl2)Ir(dfppy)2,然后在碱性条件下与2-吡啶甲酸反应合成出 FIrpic。通过核磁共振谱(1HNMR、13CNMR)、质谱、红外光谱和单晶X射线衍射等确定了分子结构,高效液相色谱法(HPLC)测试了纯度,利用紫外-可见吸收光谱和光致发光光谱对其光物理性能进行了测试。结果表明:FIrpic为电中性八面体配合物,在476 nm处出现了较强的蓝光发射,其合成产率大于90%,纯度为99.22%,该方法适于FIrpic的批量制备。
以水閤三氯化銥和 dfppy 為原料,在乙二醇單乙醚溶劑中反應得氯橋二聚體(dfppy)2Ir(μ-Cl2)Ir(dfppy)2,然後在堿性條件下與2-吡啶甲痠反應閤成齣 FIrpic。通過覈磁共振譜(1HNMR、13CNMR)、質譜、紅外光譜和單晶X射線衍射等確定瞭分子結構,高效液相色譜法(HPLC)測試瞭純度,利用紫外-可見吸收光譜和光緻髮光光譜對其光物理性能進行瞭測試。結果錶明:FIrpic為電中性八麵體配閤物,在476 nm處齣現瞭較彊的藍光髮射,其閤成產率大于90%,純度為99.22%,該方法適于FIrpic的批量製備。
이수합삼록화의화 dfppy 위원료,재을이순단을미용제중반응득록교이취체(dfppy)2Ir(μ-Cl2)Ir(dfppy)2,연후재감성조건하여2-필정갑산반응합성출 FIrpic。통과핵자공진보(1HNMR、13CNMR)、질보、홍외광보화단정X사선연사등학정료분자결구,고효액상색보법(HPLC)측시료순도,이용자외-가견흡수광보화광치발광광보대기광물이성능진행료측시。결과표명:FIrpic위전중성팔면체배합물,재476 nm처출현료교강적람광발사,기합성산솔대우90%,순도위99.22%,해방법괄우FIrpic적비량제비。
A new chemical technique was developed for batch synthesis of bis(4,6-difluorophenyl-pyridine)(picolinate)iridium(III), an organometallic light-emitting molecule for OLED. The process involves cycometalation of IrCl3·nH2O with 2-(2,4-difluorophenyl)pyridine and cleavage of chloride-bridged dimer by 2-pyridinecarboxylic acid to produce the desired compound in a 20~30 gram batch scale. The yield was more than 90%, and the purity was determined by HPLC to be 99.22%. The chemical structure of bis(4,6-difluorophenyl-pyridine)(picolinate)iridium(III) was verified by NMR (1H and 13C), MS and FT-IR along with single crystal X-ray diffraction data. The synthesized FIrpic is an electrically neutral octahedral complex. A strong blue-emission at 476 nm was observed in ultraviolet-visible and photoluminescence absorption spectra of the compound.