摘要
以PS树脂固载的季铵盐为相转移催化剂,硫脲和叔丁基溴为原料,水为反应溶剂,经成盐和水解两步反应制得叔丁基硫醇,并运用FT-IR、1H-NMR等现代分析手段确定了产物结构。然后以性能优良的PS树脂固载三正丁铵盐(PS-C3)为代表,考察了其在叔丁基硫醇制备中的最佳应用工艺,并讨论了成盐温度、成盐时间、碱液用量、水解时间等因素对叔丁基硫醇收率的影响。实验结果表明,叔丁基硫醇制备的优化条件为(以0.1 mol叔丁基溴计),成盐反应:n(硫脲)=0.105 mol,n(叔丁基溴)=0.1 mol,PS-C3 1 g,H2O 30 mL,反应温度50℃,反应时间4 h;水解反应:20%(w/w)的NaOH 30 g,60℃温和回流2 h。在此条件下,叔丁基硫醇的最终收率可达73.9%,催化剂回收简单并可重复使用4次以上,且催化性能无明显下降。
Using thiourea and tert-butyl bromide as raw materials,water as solvent and several different PS grafted quaternary ammoniums as catalyst respectively;the tert-butyl mercaptan（t-BM） was prepared via salification and hydrolyzation reactions.The structure of the prepared t-BM was identified by FT-IR and 1H-NMR.It was found that,among all the used catalysts,the catalyst of tributylamine quaternized bead（PS-C3） has the best catalytic performance for the synthesis of t-BM,and then the optimum conditions for t-BM synthesis with PS-C3 as catalyst were studied in detail.The results show that the main factors affecting the yield of t-BM are salification temperature and time,amount of NaOH solution and hydrolyzation time.The optimal conditions for salification and hydrolyzation reactions are as follows（based on 0.1 mol tert-butyl bromide）： the dosage of thiourea 0.105 mol and that of tert-butyl bromide 0.1 mol,amount of PS-C3 1 g,volume of water 30 mL,salfication reaction temperature 50℃ and time 4 h,then during hydrolyzation reaction,the 20%NaOH aqueous solution used 30 g and the reflux time 2 h at temperature 60℃.Under above optimal conditions,the yield of t-BM is about 73.9%,and the catalyst can be recovered easily and can be reused for four times or even more with no evident decline in its catalytic performance.
出处
《高校化学工程学报》
EI
CAS
CSCD
北大核心
2011年第4期627-631,共5页
Journal of Chemical Engineering of Chinese Universities
关键词
绿色化学
叔丁基硫醇
三相转移催化
硫脲
叔丁基溴
green chemistry
tetra-butyl mercaptan
triphase transfer catalysis
thiourea
tert-butyl bromide
