高校化学工程学报
高校化學工程學報
고교화학공정학보
Journal of Chemical Engineering of Chinese Universities
2015年
5期
1126-1132
,共7页
游佳勇%张天永%刘艳凤%李彬%赵振东%黄俊浩
遊佳勇%張天永%劉豔鳳%李彬%趙振東%黃俊浩
유가용%장천영%류염봉%리빈%조진동%황준호
HKUST-1%超声辅助法%合成%金属有机框架
HKUST-1%超聲輔助法%閤成%金屬有機框架
HKUST-1%초성보조법%합성%금속유궤광가
HKUST-1%ultrasonic assisted method%synthesis%metal-organic framework
采用超声波辅助法用一水合醋酸铜、五水合硫酸铜、二水合氯化铜、三水合硝酸铜四种铜盐分别和均苯三酸反应快速制备金属有机框架化合物HKUST-1,探讨了铜盐、三乙胺、超声波作用功率、反应时间、溶剂的配比、加料顺序等因素对HKUST-1产率的影响。结果表明,适宜的反应条件为:醋酸铜8.62 mmol,均苯三酸4.76 mmol,分别溶解于24 mL体积比为1:1:1的水、N,N-二甲基甲酰胺、乙醇的混合溶剂中,将两种反应物混合后,添加1 mL三乙胺,在300 W超声功率间歇式(超声2 s,关3 s)作用下反应30 min,可得到产率为99.1%的HKUST-1,所得产物通过XRD、IR进行表征并验证。
採用超聲波輔助法用一水閤醋痠銅、五水閤硫痠銅、二水閤氯化銅、三水閤硝痠銅四種銅鹽分彆和均苯三痠反應快速製備金屬有機框架化閤物HKUST-1,探討瞭銅鹽、三乙胺、超聲波作用功率、反應時間、溶劑的配比、加料順序等因素對HKUST-1產率的影響。結果錶明,適宜的反應條件為:醋痠銅8.62 mmol,均苯三痠4.76 mmol,分彆溶解于24 mL體積比為1:1:1的水、N,N-二甲基甲酰胺、乙醇的混閤溶劑中,將兩種反應物混閤後,添加1 mL三乙胺,在300 W超聲功率間歇式(超聲2 s,關3 s)作用下反應30 min,可得到產率為99.1%的HKUST-1,所得產物通過XRD、IR進行錶徵併驗證。
채용초성파보조법용일수합작산동、오수합류산동、이수합록화동、삼수합초산동사충동염분별화균분삼산반응쾌속제비금속유궤광가화합물HKUST-1,탐토료동염、삼을알、초성파작용공솔、반응시간、용제적배비、가료순서등인소대HKUST-1산솔적영향。결과표명,괄의적반응조건위:작산동8.62 mmol,균분삼산4.76 mmol,분별용해우24 mL체적비위1:1:1적수、N,N-이갑기갑선알、을순적혼합용제중,장량충반응물혼합후,첨가1 mL삼을알,재300 W초성공솔간헐식(초성2 s,관3 s)작용하반응30 min,가득도산솔위99.1%적HKUST-1,소득산물통과XRD、IR진행표정병험증。
Cu(OAc)2·H2O, CuSO4·5H2O, CuCl2·2H2O and Cu(NO3)2·3H2O were individually reacted with benzenetricarboxylic acid under ultrasonication for rapid synthesis of metal-organic framework HKUST-1. The effects of cupric salts, triethylamine, ultrasonic power, reaction time, solvent ratio and reactant addition sequence on the yield of HKUST-1 were investigated. The optimized condition for the preparation of HKUST-1 was found as: Cu(OAc)2·H2O (8.62 mmol) and benzenetricarboxylic acid (4.76 mmol) were firstly individually dissolved in the mixtures of H2O, DMF and ethanol (volume ratio 1:1:1), and the resulted solutions were then mixed together and triethylamine (1 mL) was added. The mixture was then ultrasonicated for 30 min under intermittent ultrasonication(work 2 s, pause 3 s) to generate HKUST-1 with a yield of 99.1%. The samples were characterized by XRD and IR.