CAJ | 학술논문

;合成了一系列具有Keggin结构的P-V-Mo-W四元杂多化合物(Cpyr)_(3+x)PV_xMo_yW_(12-x-y)O_(40)·nH_2O[其中,Cpyr=(C_(16)H_(32)C_5H_4N)~+,x=0、1、2和3],采用傅里叶变换红外光谱和X射线衍射等方法表征了杂多化合物的结构;以磷钒钼钨杂多化合物为相转移催化剂,用m(H_2O_2)=30%双氧水氧化苯甲醇制备苯甲醛.考察了催化剂的种类、溶剂的类型和反应条件(催化剂用量、反应温度、反应时间、H_2O_2用量)对苯甲醇氧化反应的影响.在优化条件下,即苯甲醇0.1 mol、催化剂(Cpyr)_5PV_2Mo_5W_5O_(40)0.04 mmol、m(H_2O_2)=30%H_2O_2 0.1 mol、在100℃反应8 h、溶剂水10 mL,苯甲醇的转化率达88.51%、笨甲醛的选择性达96.06%.
;합성료일계렬구유Keggin결구적P-V-Mo-W사원잡다화합물(Cpyr)_(3+x)PV_xMo_yW_(12-x-y)O_(40)·nH_2O[기중,Cpyr=(C_(16)H_(32)C_5H_4N)~+,x=0、1、2화3],채용부리협변환홍외광보화X사선연사등방법표정료잡다화합물적결구;이린범목오잡다화합물위상전이최화제,용m(H_2O_2)=30%쌍양수양화분갑순제비분갑철.고찰료최화제적충류、용제적류형화반응조건(최화제용량、반응온도、반응시간、H_2O_2용량)대분갑순양화반응적영향.재우화조건하,즉분갑순0.1 mol、최화제(Cpyr)_5PV_2Mo_5W_5O_(40)0.04 mmol、m(H_2O_2)=30%H_2O_2 0.1 mol、재100℃반응8 h、용제수10 mL,분갑순적전화솔체88.51%、분갑철적선택성체96.06%.
Multicomponent heteropoly compounds (Cpyr)_(3+x)PV_xMo_yW_(12-x-y)O_(40)·nH_2O with Keggin structure were synthesized and proved by FTIR and X-ray spectroscopies. With 30% aqueous hydrogen peroxide as oxidant, benzyl alcohol was efficiently oxidized to benzaldehyde over reaction-controlled phase-transfer catalysts (Cpyr)_(3+x)PV_xMO_yW_(12-x-y)O_(40). Effects of the type of catalyst, the amount of catalyst and H_2O_2, the kind of solvent, reaction temperature and time were investigated. Under the optimal conditions, i.e., with 0.1 mol of benzyl alcohol, 0.04 mmol of(Cpyr)_5PV_2Mo_5W_5O_(40) catalyst and 0.1mol of 30% H_2O_2, reaction temperature 100℃, 10 mL water as the solvent, 88.51% conversion of benzyl alcohol and 96.06% selectivity for benzaldehyde were achieved within 8h.