石油化工
石油化工
석유화공
PETROCHEMICAL TECHNOLOGY
2009年
11期
1225-1229
,共5页
胡应燕%郭睿%窦蓓蕾%高于涵
鬍應燕%郭睿%竇蓓蕾%高于涵
호응연%곽예%두배뢰%고우함
酯基%季铵盐%杀菌剂%十二烷基二甲基叔胺%环氧氯丙烷%月桂酸
酯基%季銨鹽%殺菌劑%十二烷基二甲基叔胺%環氧氯丙烷%月桂痠
지기%계안염%살균제%십이완기이갑기숙알%배양록병완%월계산
ester group%quaternary ammonium salt%bactericide%N%N dimethyl dodecylamine%epichlorohydrin%lauric acid
以十二烷基二甲基叔胺、环氧氯丙烷、月桂酸为原料,经两步反应合成了一种新型含酯基季铵盐杀菌剂(2-羟基-3-月桂酰氧基丙基)十二烷基二甲基氯化铵(HFAC).第一步的最佳合成条件为:n(环氧氯丙烷):n(十二烷基二甲基叔胺)=1.2、反应温度25 ℃、反应时间4 h,此时中间体十二烷基-(2,3-环氧丙基)二甲基氯化铵(HYAC)的收率为82.54%.第二步的最佳合成条件为:n(月桂酸):n(HYAC)=1.2、反应温度60 ℃、反应时间6 h,此时目标产物HFAC的收率为92.58%.用傅里叶变换红外光谱、元素分析、氢核磁共振和飞行时间质谱对中间体和产物进行了结构表征.同时将HFAC用于处理造纸污水,当污水中HFAC的质量分数为0.010%、杀菌时间为18 h时,HFAC能达到很好的杀菌效果.
以十二烷基二甲基叔胺、環氧氯丙烷、月桂痠為原料,經兩步反應閤成瞭一種新型含酯基季銨鹽殺菌劑(2-羥基-3-月桂酰氧基丙基)十二烷基二甲基氯化銨(HFAC).第一步的最佳閤成條件為:n(環氧氯丙烷):n(十二烷基二甲基叔胺)=1.2、反應溫度25 ℃、反應時間4 h,此時中間體十二烷基-(2,3-環氧丙基)二甲基氯化銨(HYAC)的收率為82.54%.第二步的最佳閤成條件為:n(月桂痠):n(HYAC)=1.2、反應溫度60 ℃、反應時間6 h,此時目標產物HFAC的收率為92.58%.用傅裏葉變換紅外光譜、元素分析、氫覈磁共振和飛行時間質譜對中間體和產物進行瞭結構錶徵.同時將HFAC用于處理造紙汙水,噹汙水中HFAC的質量分數為0.010%、殺菌時間為18 h時,HFAC能達到很好的殺菌效果.
이십이완기이갑기숙알、배양록병완、월계산위원료,경량보반응합성료일충신형함지기계안염살균제(2-간기-3-월계선양기병기)십이완기이갑기록화안(HFAC).제일보적최가합성조건위:n(배양록병완):n(십이완기이갑기숙알)=1.2、반응온도25 ℃、반응시간4 h,차시중간체십이완기-(2,3-배양병기)이갑기록화안(HYAC)적수솔위82.54%.제이보적최가합성조건위:n(월계산):n(HYAC)=1.2、반응온도60 ℃、반응시간6 h,차시목표산물HFAC적수솔위92.58%.용부리협변환홍외광보、원소분석、경핵자공진화비행시간질보대중간체화산물진행료결구표정.동시장HFAC용우처리조지오수,당오수중HFAC적질량분수위0.010%、살균시간위18 h시,HFAC능체도흔호적살균효과.
A novel quaternary ammonium salt bactericide containing ester structure (2 hydroxy 3 lauryl acyloxypropyl) dodecyl dimethyl ammonium chloride (HFAC) was prepared from N,N dimethyl dodecylamine, epichlorohydrin and lauric acid by two step synthesis. The intermediate dodecyl (2,3 epoxypropyl) dimethyl ammonium chloride(HYAC)was first prepared from N,N dimethyl dodecylamine and epichlorohydrin by nucleophilic substitution reaction. Under the optimized reaction conditions for HYAC synthesis: n(epichlorohydrin):n(N,N dimethyl dodecylamine) 1.2, reaction time 4 h and reaction temperature 25 ℃, the yield of HYAC was 82.54%. The target product HFAC was obtained by reacting the intermediate HYAC with lauric acid. Under the optimized reaction conditions for HFAC synthesis: n(lauric acid):n(HYAC) 1.2, reaction time 6 h and reaction temperature 60 ℃, the yield of HFAC was 92.58%. Both the intermediate and the target product were characterized by means of FTIR, EA, ~1H NMR, TOF MS, etc.. The HFAC had been applied in treatment of paper making wastewater and had promising sterilization property under appropriate conditions: HFAC mass fraction (based on mass of the wastewater) 0.010% and sterilizing time 18 h.