林产化学与工业
林產化學與工業
림산화학여공업
CHEMISTRY AND INDUSTRY OF FOREST PRODUCTS
2014年
5期
115-121
,共7页
马艾华%胡庭维%陕绍云%贾庆明
馬艾華%鬍庭維%陝紹雲%賈慶明
마애화%호정유%협소운%가경명
α-蒎烯%环氧化反应%金属Salen催化剂%分子筛负载型催化剂%微波
α-蒎烯%環氧化反應%金屬Salen催化劑%分子篩負載型催化劑%微波
α-파희%배양화반응%금속Salen최화제%분자사부재형최화제%미파
α-pinene%epoxidation%matal-Salen catalyst%molecular sieve loaded metal catalyst%microwave
采用普通热溶剂法和微波加热法将SalenMnCl成功负载于NaY分子筛的超笼中,通过FT-IR、XRD、TG和比表面分析方法对催化剂进行了表征。以此负载型催化剂催化低浓度过氧乙酸氧化α-蒎烯制备α-环氧蒎烷,比较了2种方法制备的催化剂性能,然后用响应曲面法探索最佳反应条件,并在该条件下研究负载型催化剂循环使用情况。结果表明,2种方法制备的分子筛负载型SalenMnCl催化剂均可催化α-蒎烯环氧化反应,且催化效果微波法优于普通热溶剂法。微波法制备的SalenMnCl/Y-MW催化剂催化反应的最优条件为:过氧乙酸与α-蒎烯物质的量之比值为1.43,反应温度为10℃,反应时间为3.75 h,在此条件下产物产率达91.60%。同时,该负载型催化剂重复使用5次,产物产率仍达76%以上,其具有较好的稳定性,可循环利用。
採用普通熱溶劑法和微波加熱法將SalenMnCl成功負載于NaY分子篩的超籠中,通過FT-IR、XRD、TG和比錶麵分析方法對催化劑進行瞭錶徵。以此負載型催化劑催化低濃度過氧乙痠氧化α-蒎烯製備α-環氧蒎烷,比較瞭2種方法製備的催化劑性能,然後用響應麯麵法探索最佳反應條件,併在該條件下研究負載型催化劑循環使用情況。結果錶明,2種方法製備的分子篩負載型SalenMnCl催化劑均可催化α-蒎烯環氧化反應,且催化效果微波法優于普通熱溶劑法。微波法製備的SalenMnCl/Y-MW催化劑催化反應的最優條件為:過氧乙痠與α-蒎烯物質的量之比值為1.43,反應溫度為10℃,反應時間為3.75 h,在此條件下產物產率達91.60%。同時,該負載型催化劑重複使用5次,產物產率仍達76%以上,其具有較好的穩定性,可循環利用。
채용보통열용제법화미파가열법장SalenMnCl성공부재우NaY분자사적초롱중,통과FT-IR、XRD、TG화비표면분석방법대최화제진행료표정。이차부재형최화제최화저농도과양을산양화α-파희제비α-배양파완,비교료2충방법제비적최화제성능,연후용향응곡면법탐색최가반응조건,병재해조건하연구부재형최화제순배사용정황。결과표명,2충방법제비적분자사부재형SalenMnCl최화제균가최화α-파희배양화반응,차최화효과미파법우우보통열용제법。미파법제비적SalenMnCl/Y-MW최화제최화반응적최우조건위:과양을산여α-파희물질적량지비치위1.43,반응온도위10℃,반응시간위3.75 h,재차조건하산물산솔체91.60%。동시,해부재형최화제중복사용5차,산물산솔잉체76%이상,기구유교호적은정성,가순배이용。
Immobilization of Mn( salen) complex into the super-cage of Zeolite Y was achieved via traditional solvothermal method ( SalenMnCl/Y) and microwave heating method ( SalenMnCl/Y-MW) , respectively. And FT-IR, XRD, TG and Specific surface area analysis were used to characterize the catalysts which were employed to catalyze the epoxidation of α-pinene to getα-poxypiene by peracetic acid under the low catalyst concentration. Comparative study of the performance of catalysts prepared by two methods was carried out. The optimal reaction condition was investigated by response surface methodology and used to evaluate the performance of the recycle catalyst . The results showed that although the catalysts prepared by two methods can both successfully catalyse α-pinene epoxidation, microwave heating method however is priority to traditional solvothermal method. The yield can reach 91. 60% with the catalyst of SalenMnCl/Y-MW under the following conditions,i. e. , peroxide andα-pinene mole ratio 1. 43, the reaction temperature 10 ℃ and the reaction time 3. 75 h. Meanwhile, this type of catalyst can be recycled for 5 times and the yield also can reach 76 %. It indicates that this type of catalyst has good stability and can be recycled.