化工进展
化工進展
화공진전
CHEMICAL INDUSTRY AND ENGINEERING PROGRESS
2015年
1期
229-233
,共5页
周宝强%宋林林%张楠%高瑞昶
週寶彊%宋林林%張楠%高瑞昶
주보강%송림림%장남%고서창
溴代异戊烯%3-甲基-2-丁烯-1-醇%水解%精馏
溴代異戊烯%3-甲基-2-丁烯-1-醇%水解%精餾
추대이무희%3-갑기-2-정희-1-순%수해%정류
brominatedisoamylene%3-methyl-2-buten-1-ol%hydrolysis%distillation
研究了以溴代异戊烯水解工艺和精馏分离工艺为基础来制备3-甲基-2-丁烯-1-醇的新工艺。通过优化溶剂种类得到当水解溶剂为偶极类溶剂乙腈时,得到产物的选择性最高。并通过进一步优化实验操作条件,得到当溶剂加入量为 v(乙腈):v(溴代异戊烯)=1∶1,水解温度为70℃,碱用量为 n(NaOH)∶n(溴代异戊烯)=1.2∶1和反应时间为25min时,水解部分3-甲基-2-丁烯-1-醇的转化率最高可达63.35%。水解后的料液通过间歇精馏得到纯的3-甲基-2-丁烯-1-醇,最终的3-甲基-2-丁烯-1-醇总收率达到57.4%。
研究瞭以溴代異戊烯水解工藝和精餾分離工藝為基礎來製備3-甲基-2-丁烯-1-醇的新工藝。通過優化溶劑種類得到噹水解溶劑為偶極類溶劑乙腈時,得到產物的選擇性最高。併通過進一步優化實驗操作條件,得到噹溶劑加入量為 v(乙腈):v(溴代異戊烯)=1∶1,水解溫度為70℃,堿用量為 n(NaOH)∶n(溴代異戊烯)=1.2∶1和反應時間為25min時,水解部分3-甲基-2-丁烯-1-醇的轉化率最高可達63.35%。水解後的料液通過間歇精餾得到純的3-甲基-2-丁烯-1-醇,最終的3-甲基-2-丁烯-1-醇總收率達到57.4%。
연구료이추대이무희수해공예화정류분리공예위기출래제비3-갑기-2-정희-1-순적신공예。통과우화용제충류득도당수해용제위우겁류용제을정시,득도산물적선택성최고。병통과진일보우화실험조작조건,득도당용제가입량위 v(을정):v(추대이무희)=1∶1,수해온도위70℃,감용량위 n(NaOH)∶n(추대이무희)=1.2∶1화반응시간위25min시,수해부분3-갑기-2-정희-1-순적전화솔최고가체63.35%。수해후적료액통과간헐정류득도순적3-갑기-2-정희-1-순,최종적3-갑기-2-정희-1-순총수솔체도57.4%。
A new technology for the preparation of 3-methyl-2-butene-1-ol was investigated based on the hydrolysis of brominated isoamylene and distillation separation technology. By choosing a dipolar solvent,acetonitrile,for the hydrolysis the products showed the highest selectivity. And through further the optimization of experimental operating conditions,hydrolysis yield of 3-methyl-2-butene-1-ol reached 63.35%under the condition of the solvent amount v(acetonitrile)∶v(bromo-3-ene)=1∶1, hydrolysis temperature 70℃,base amount n(NaOH)∶n(bromo-3-ene)=1.2∶1 and reaction time 25 minutes. The pure 3-methyl-2-butene-1-ol was made of the feed liquid after hydrolysis by batch distillation operation,and the final total yield of 3-methyl-2-butene-1-ol reached 54%.