应用化工
應用化工
응용화공
APPLIED CHEMICAL INDUSTRY
2015年
4期
771-774,778
,共5页
异丙苯间二甲苯%3 ,5-二甲基苯酚%合成%应用
異丙苯間二甲苯%3 ,5-二甲基苯酚%閤成%應用
이병분간이갑분%3 ,5-이갑기분분%합성%응용
isopropyl-m-xylene%3,5-dimethyl phenol%synthesis%application
以间二甲苯和异丙醇为原料，经过烷基化、氧化、酸解反应合成3，5-二甲基苯酚。对反应产物结构进行了表征，并通过不断优化，确定了反应总收率在50％左右的反应工艺条件。烷基化工艺条件：原料摩尔比n （间二甲苯）∶n（异丙醇）∶n（三氯化铝）＝8∶1∶1，反应温度为70℃，反应时间为7 h，在此工艺下产品收率为75％，纯度为90％；氧化工艺条件：5-异丙基间二甲苯30 g，NHPI 3．26 g，AIBN 1．0 g，乙腈200 mL，空气流速为600 mL／min，反应温度50℃，反应时间16 h；酸解工艺条件：氧化反应液20 g，浓硫酸与丙酮混合液50 g（浓硫酸质量分数为5％），反应温度为50℃，反应时间为2 h。最终通过实验得出适合整个反应的最优化工艺条件，完成了3，5-二甲基苯酚的实验室合成，同时为工业化开发3，5-二甲基苯酚新型合成路线提供了依据。
以間二甲苯和異丙醇為原料，經過烷基化、氧化、痠解反應閤成3，5-二甲基苯酚。對反應產物結構進行瞭錶徵，併通過不斷優化，確定瞭反應總收率在50％左右的反應工藝條件。烷基化工藝條件：原料摩爾比n （間二甲苯）∶n（異丙醇）∶n（三氯化鋁）＝8∶1∶1，反應溫度為70℃，反應時間為7 h，在此工藝下產品收率為75％，純度為90％；氧化工藝條件：5-異丙基間二甲苯30 g，NHPI 3．26 g，AIBN 1．0 g，乙腈200 mL，空氣流速為600 mL／min，反應溫度50℃，反應時間16 h；痠解工藝條件：氧化反應液20 g，濃硫痠與丙酮混閤液50 g（濃硫痠質量分數為5％），反應溫度為50℃，反應時間為2 h。最終通過實驗得齣適閤整箇反應的最優化工藝條件，完成瞭3，5-二甲基苯酚的實驗室閤成，同時為工業化開髮3，5-二甲基苯酚新型閤成路線提供瞭依據。
이간이갑분화이병순위원료，경과완기화、양화、산해반응합성3，5-이갑기분분。대반응산물결구진행료표정，병통과불단우화，학정료반응총수솔재50％좌우적반응공예조건。완기화공예조건：원료마이비n （간이갑분）∶n（이병순）∶n（삼록화려）＝8∶1∶1，반응온도위70℃，반응시간위7 h，재차공예하산품수솔위75％，순도위90％；양화공예조건：5-이병기간이갑분30 g，NHPI 3．26 g，AIBN 1．0 g，을정200 mL，공기류속위600 mL／min，반응온도50℃，반응시간16 h；산해공예조건：양화반응액20 g，농류산여병동혼합액50 g（농류산질량분수위5％），반응온도위50℃，반응시간위2 h。최종통과실험득출괄합정개반응적최우화공예조건，완성료3，5-이갑기분분적실험실합성，동시위공업화개발3，5-이갑기분분신형합성로선제공료의거。
Using m-xylene and isopropyl alcohol as raw materials ,through alkylation ,oxidation,acidolysis reaction to obtain 3,5-dimethyl phenol .The structure of reaction product was characterized ,and through continuous optimization ,determine the reaction process conditions that the total yield of 3 ,5-dimethyl phe-nol can over 50%.The best conditions of preparation of the alkylation reaction were got as follows:the molar ratio of n(m-xylene)∶n(isopropyl alcohol )∶n(aluminum chloride)=8∶1∶1,the reaction tempera-ture of 70℃,the reaction time of 7 h,in these conditions ,the yield of product is 75%,the purity is 90%;The best conditions of preparation of the oxidation reaction were got as follows:5-isopropyl-m-xylene 30 g,NHPI 3.26 g,AIBN 1.0 g,acetonitrile 200 mL,air velocity is 600 mL/min,the reaction tempera-ture of 50 ℃,the reaction time of 16 h;and the best conditions of preparation of the acidolysis reaction were got as follows:the liquid of oxidation reaction 20 g,the miscible liquids of concentrated sulfuric acid and acetone ( mass fraction of concentrated sulfuric acid is 5%) ,the reaction temperature of 50℃,the re-action time of 2 h.Finally,the optimum process conditions of the reaction was selected through experi-ment,completed the synthesis of 3,5-dimethyl phenol in the laboratory .At the same time,it provide the basis for the new synthetic route of 3 ,5-dimethyl phenol in industry .
