精细与专用化学品
精細與專用化學品
정세여전용화학품
FINE AND SPECIALTY CHEMICALS
2012年
11期
47-49
,共3页
吴梅%叶明琰%段云丽%喻莉%吕宝兰%杨水金
吳梅%葉明琰%段雲麗%喻莉%呂寶蘭%楊水金
오매%협명염%단운려%유리%려보란%양수금
苹果酯%硅钨钼酸%二氧化硅%催化
蘋果酯%硅鎢鉬痠%二氧化硅%催化
평과지%규오목산%이양화규%최화
2-methyl-2-ethoxycarbonylmethyl-1%3-dioxolane%H4SiW6Mo6O40 /SiO2%catalysis
采用溶胶-凝胶法制备了二氧化硅负载硅钨钼酸催化剂。以其为催化剂,以乙酰乙酸乙酯和乙二醇为原料合成了苹果酯,探讨二氧化硅负载硅钨钼酸对苹果酯合成反应的催化活性。用正交实验法较系统地研究了反应物料配比、催化剂用量、带水剂用量、反应时间等因素对产物收率的影响。实验表明,二氧化硅负载硅钨钼酸是合成苹果酯的良好的催化剂,固定乙酰乙酸乙酯的用量为0.20mol,在n(乙酰乙酸乙酯):n(乙二醇)=1:1.5,催化剂用量为反应物料总质量的1.0%,带水剂环己烷8mL,反应时间60min的优化条件下,苹果酯的收率可达72.8%。
採用溶膠-凝膠法製備瞭二氧化硅負載硅鎢鉬痠催化劑。以其為催化劑,以乙酰乙痠乙酯和乙二醇為原料閤成瞭蘋果酯,探討二氧化硅負載硅鎢鉬痠對蘋果酯閤成反應的催化活性。用正交實驗法較繫統地研究瞭反應物料配比、催化劑用量、帶水劑用量、反應時間等因素對產物收率的影響。實驗錶明,二氧化硅負載硅鎢鉬痠是閤成蘋果酯的良好的催化劑,固定乙酰乙痠乙酯的用量為0.20mol,在n(乙酰乙痠乙酯):n(乙二醇)=1:1.5,催化劑用量為反應物料總質量的1.0%,帶水劑環己烷8mL,反應時間60min的優化條件下,蘋果酯的收率可達72.8%。
채용용효-응효법제비료이양화규부재규오목산최화제。이기위최화제,이을선을산을지화을이순위원료합성료평과지,탐토이양화규부재규오목산대평과지합성반응적최화활성。용정교실험법교계통지연구료반응물료배비、최화제용량、대수제용량、반응시간등인소대산물수솔적영향。실험표명,이양화규부재규오목산시합성평과지적량호적최화제,고정을선을산을지적용량위0.20mol,재n(을선을산을지):n(을이순)=1:1.5,최화제용량위반응물료총질량적1.0%,대수제배기완8mL,반응시간60min적우화조건하,평과지적수솔가체72.8%。
A novel catalyst,H4SiW6Mo6O40 /SiO2 was synthesized by a sol-gel technique,and characterized by FTIR and XRD.2-Methyl-2-ethoxycarbonylmethyl-1,3-dioxolane was synthesized from ethyl acetoacetate and ethylene glycol in the presence of H4SiW6Mo6O40 /SiO2 as catalyst.The factors influencing the synthesis were discussed and the best reaction conditions were found out.Experimental results showed that H4SiW6Mo6O40 /SiO2 is an excellent catalyst.Under the exeperimental conditions as follows:molar ratio of ethyl acetoacetate to ethylene glycol is 1:1.5,the mass ratio of the catalyst is 1.0% of all the reactants,volume of cyclohexane is 8mL,and the reaction time is 60 min,the yield of 2-methyl-2-ethoxycarbonylmethyl-1,3-dioxolane can reach 72.8 %.