陕西科技大学学报(自然科学版)
陝西科技大學學報(自然科學版)
협서과기대학학보(자연과학판)
JOURNAL OF SHAANXI UNIVERSITY OF SCIENCE & TECHNOLOGY
2015年
4期
75-79
,共5页
李运涛%郝文强%关琳%党蓓君
李運濤%郝文彊%關琳%黨蓓君
리운도%학문강%관림%당배군
2-甲基萘%过硫酸铵%2-甲萘醌%亚硫酸氢钠甲萘醌
2-甲基萘%過硫痠銨%2-甲萘醌%亞硫痠氫鈉甲萘醌
2-갑기내%과류산안%2-갑내곤%아류산경납갑내곤
2-methylnaphthalene%ammonium persulphate%2-methylnaphthoquinone%mena-dione sodium bisulfite
以过硫酸铵为引发剂,双氧水为氧化剂,冰乙酸为溶剂,将2‐甲基萘氧化为2‐甲萘醌,进而制得亚硫酸氢钠甲萘醌.研究了反应时间、反应温度、引发剂的用量及反应物与氧化剂、溶剂的物料比等因素对产品收率的影响.确定了最佳的反应条件是2‐甲萘醌的合成条件为:反应时间3 h ,反应温度85℃,引发剂的用量为反应物总量的2%,n(2‐甲基萘)∶ n(冰乙酸)∶ n (双氧水)=1∶15∶11.5.亚硫酸氢钠甲萘醌的合成条件为:反应温度45℃,反应时间1 h ,n (2‐甲萘醌)∶ n(亚硫酸氢钠)=1∶1.5.在以上条件下,2‐甲萘醌的收率为54%,亚硫酸氢钠甲萘醌的收率为70%.
以過硫痠銨為引髮劑,雙氧水為氧化劑,冰乙痠為溶劑,將2‐甲基萘氧化為2‐甲萘醌,進而製得亞硫痠氫鈉甲萘醌.研究瞭反應時間、反應溫度、引髮劑的用量及反應物與氧化劑、溶劑的物料比等因素對產品收率的影響.確定瞭最佳的反應條件是2‐甲萘醌的閤成條件為:反應時間3 h ,反應溫度85℃,引髮劑的用量為反應物總量的2%,n(2‐甲基萘)∶ n(冰乙痠)∶ n (雙氧水)=1∶15∶11.5.亞硫痠氫鈉甲萘醌的閤成條件為:反應溫度45℃,反應時間1 h ,n (2‐甲萘醌)∶ n(亞硫痠氫鈉)=1∶1.5.在以上條件下,2‐甲萘醌的收率為54%,亞硫痠氫鈉甲萘醌的收率為70%.
이과류산안위인발제,쌍양수위양화제,빙을산위용제,장2‐갑기내양화위2‐갑내곤,진이제득아류산경납갑내곤.연구료반응시간、반응온도、인발제적용량급반응물여양화제、용제적물료비등인소대산품수솔적영향.학정료최가적반응조건시2‐갑내곤적합성조건위:반응시간3 h ,반응온도85℃,인발제적용량위반응물총량적2%,n(2‐갑기내)∶ n(빙을산)∶ n (쌍양수)=1∶15∶11.5.아류산경납갑내곤적합성조건위:반응온도45℃,반응시간1 h ,n (2‐갑내곤)∶ n(아류산경납)=1∶1.5.재이상조건하,2‐갑내곤적수솔위54%,아류산경납갑내곤적수솔위70%.
Synthesis of 2‐methylnaphthoquinone with ammonium persulfate as initiator in the acetic‐H202 system by oxidation of 2‐methylnaphthalene was researched .The effects of reac‐tion temperature ,reaction time ,amount of initiator ,reactant and solvent material ratio and other factors on β‐methylnaphthoquinone yeild were investigated .The best performences were achieved .The synthesis conditions of 2‐methylnaphthoquinone:reaction time 3 h ,reac‐tion temperature 85 ℃ ,molar ratio of 2‐methylnaphthalene to acetic acid and Hydrogen per‐oxide 1∶11 .5∶15 ,amoout of initiator is 2% of the total amount of reactant .The synthesis conditions of menadione sodium bisulfite:reaction time 1 h ,reaction temperature 45 ℃ ,molar ratio of 2‐methylnaphthoquinone to sodium bisulfite 1∶1 .5 .In these conditions ,the yelid of 2‐methylnaphthoquinone was 54% ,the yelid of menadione sodium bisulfite was 70% .