有色金属科学与工程
有色金屬科學與工程
유색금속과학여공정
JIANGXI NONFERROUS METALS
2014年
6期
21-27
,共7页
舒庆%刘宝%宋胜海%张志武%陈培德
舒慶%劉寶%宋勝海%張誌武%陳培德
서경%류보%송성해%장지무%진배덕
杂多酸盐%酯化反应%催化剂%钨钼
雜多痠鹽%酯化反應%催化劑%鎢鉬
잡다산염%지화반응%최화제%오목
heteropoly acid salt%esterification reaction%catalyst%tungsten and molybdenum
以Na2WO4·2H2O和 Na2MoO4·2H2O为原料,通过硝酸酸化-乙醚萃取法制备了一种钨钼混配型杂多酸盐催化剂(Na4SiMoW12O40·xH2O).应用X射线荧光光谱对合成的催化剂的元素组成进行了分析;通过红外光谱对其的官能团结构进行了分析;借助热重分析对其的热稳定性进行了研究.并以正丁醇和乙酸为反应物,研究了所制备的钨钼混配型杂多酸盐在催化酯化反应时的活性和稳定性.通过正交试验[L9(3)4]对影响乙酸正丁酯收率的关键影响参数进行了优化,包括催化剂与反应物的质量比、反应时间和温度、以及正丁醇与乙酸的摩尔比.结果表明:当反应时间为120 min,反应温度为90℃,催化剂用量为0.4 g,醇酸摩尔比为2∶1,酯化效果最好,达到93.24 wt%.
以Na2WO4·2H2O和 Na2MoO4·2H2O為原料,通過硝痠痠化-乙醚萃取法製備瞭一種鎢鉬混配型雜多痠鹽催化劑(Na4SiMoW12O40·xH2O).應用X射線熒光光譜對閤成的催化劑的元素組成進行瞭分析;通過紅外光譜對其的官能糰結構進行瞭分析;藉助熱重分析對其的熱穩定性進行瞭研究.併以正丁醇和乙痠為反應物,研究瞭所製備的鎢鉬混配型雜多痠鹽在催化酯化反應時的活性和穩定性.通過正交試驗[L9(3)4]對影響乙痠正丁酯收率的關鍵影響參數進行瞭優化,包括催化劑與反應物的質量比、反應時間和溫度、以及正丁醇與乙痠的摩爾比.結果錶明:噹反應時間為120 min,反應溫度為90℃,催化劑用量為0.4 g,醇痠摩爾比為2∶1,酯化效果最好,達到93.24 wt%.
이Na2WO4·2H2O화 Na2MoO4·2H2O위원료,통과초산산화-을미췌취법제비료일충오목혼배형잡다산염최화제(Na4SiMoW12O40·xH2O).응용X사선형광광보대합성적최화제적원소조성진행료분석;통과홍외광보대기적관능단결구진행료분석;차조열중분석대기적열은정성진행료연구.병이정정순화을산위반응물,연구료소제비적오목혼배형잡다산염재최화지화반응시적활성화은정성.통과정교시험[L9(3)4]대영향을산정정지수솔적관건영향삼수진행료우화,포괄최화제여반응물적질량비、반응시간화온도、이급정정순여을산적마이비.결과표명:당반응시간위120 min,반응온도위90℃,최화제용량위0.4 g,순산마이비위2∶1,지화효과최호,체도93.24 wt%.
A tungsten and molybdenum mixed heteropoly acid salt catalyst(Na 4SiMoW12O40·xH2O) is prepared by using Na2WO4·2H2O and Na2MoO4·2H2O as raw materials through the combination of nitric acid acidification and ether extraction technique. The resulting catalyst is characterized by X-ray fluorescence spectrometer (XRF) for the investigation of its elemental composition. The infrared spectroscopy (FTIR) is used to analyze its functional group structure. The thermogravimetric analysis (TGA) is used to study its thermal stability. The catalytic activity and stability of the tungsten and molybdenum mixed heteropoly acid salt catalyst are studied during the process of esterification reaction of butanol and acetic acid. The key reaction parameters that influence the yield of n-butyl acetate are optimized by employing an orthogonal experiment [L 9(3)4], including the mass loading of catalyst, reaction time and reaction temperature, as well as the molar ratio of butanol to acetic acid. Results show that esterification reaction effect of 93.24 wt%is obtained when the reaction time is 120 minutes, reaction temperature is 90 ℃and catalyst loading is 0.4 g with the molar ratio of butanol to acetic acid of being 2:1.