化学研究
化學研究
화학연구
CHEMICAL RESEARCHES
2013年
3期
303-306
,共4页
磷酸钛固载磷钨酸%非均相催化剂%催化%异戊酸己酯%合成
燐痠鈦固載燐鎢痠%非均相催化劑%催化%異戊痠己酯%閤成
린산태고재린오산%비균상최화제%최화%이무산기지%합성
titanium phosphate-supported phosphotungstic acid%heterogeneous catalyst%cataly-sis%hexyl isovalerate%synthesis
通过在300℃下焙烧2 h制备了磷酸钛固载15%磷钨酸H3 PW12 O40(简记为 H PW )非均相酯化催化剂H PW/T i3(PO4)4;采用红外光谱仪分析了催化剂的结构;基于异戊酸与正己醇的酯化反应考察了催化剂用量、n (正己醇)∶ n(异戊酸)、反应时间、带水剂种类和催化剂重复使用性能等因素对酯化率的影响.结果表明,该催化剂催化合成异戊酸己酯的适宜反应条件为:0.2mol异戊酸,催化剂用量0.6g,n(正己醇)∶ n(异戊酸)=1.6∶1,反应时间4.5h,环己烷10mL ;相应的酯化率达95.1%.与此同时,该催化剂循环利用6次后酯化率不低于84%.
通過在300℃下焙燒2 h製備瞭燐痠鈦固載15%燐鎢痠H3 PW12 O40(簡記為 H PW )非均相酯化催化劑H PW/T i3(PO4)4;採用紅外光譜儀分析瞭催化劑的結構;基于異戊痠與正己醇的酯化反應攷察瞭催化劑用量、n (正己醇)∶ n(異戊痠)、反應時間、帶水劑種類和催化劑重複使用性能等因素對酯化率的影響.結果錶明,該催化劑催化閤成異戊痠己酯的適宜反應條件為:0.2mol異戊痠,催化劑用量0.6g,n(正己醇)∶ n(異戊痠)=1.6∶1,反應時間4.5h,環己烷10mL ;相應的酯化率達95.1%.與此同時,該催化劑循環利用6次後酯化率不低于84%.
통과재300℃하배소2 h제비료린산태고재15%린오산H3 PW12 O40(간기위 H PW )비균상지화최화제H PW/T i3(PO4)4;채용홍외광보의분석료최화제적결구;기우이무산여정기순적지화반응고찰료최화제용량、n (정기순)∶ n(이무산)、반응시간、대수제충류화최화제중복사용성능등인소대지화솔적영향.결과표명,해최화제최화합성이무산기지적괄의반응조건위:0.2mol이무산,최화제용량0.6g,n(정기순)∶ n(이무산)=1.6∶1,반응시간4.5h,배기완10mL ;상응적지화솔체95.1%.여차동시,해최화제순배이용6차후지화솔불저우84%.
A heterogeneous esterification catalyst ,titanium phosphate-supported phosphotung-stic acid (denoted as HPW) with an HPW content of 15% (mass fraction) ,was prepared by clacination at 300 ℃ for 2 .0 h .The structure of as-synthesized HPW/Ti3 (PO4 )4 catalyst was analyzed by means of infrared spectrometry .Moreover ,the effects of catalyst dosage ,molar ratio of alcohol to acid ,reaction time ,deaquation reagents and reusability of the catalyst on the esterification rate were investigated in relation to the esterification reaction of isopentanoic acid with n-hexanol .Results indicate that as-synthesized heterogeneous catalyst can be well used to catalytically synthesize hexyl isovalerate at an isovaleric acid dosage of 0 .2 mol ,an alcohol to acid molar ratio of 1 .6∶1 ,a catalyst dosage of 0 .6 g ,a cyclohexane dosage of 10 mL ,and a reaction time of 4 .5 h .Corresponding esterification rate is as much as 95 .1% .Besides ,the catalyst retains an esterification rate of above 84% after it is recycled for six cycles .