林产化学与工业
林產化學與工業
림산화학여공업
CHEMISTRY AND INDUSTRY OF FOREST PRODUCTS
2014年
1期
43-48
,共6页
丁玉秋%刘绍刚%李龙%丁玉波%刁开盛
丁玉鞦%劉紹剛%李龍%丁玉波%刁開盛
정옥추%류소강%리룡%정옥파%조개성
脱氢枞胺%氧化叔胺%表面活性%吸附性能
脫氫樅胺%氧化叔胺%錶麵活性%吸附性能
탈경종알%양화숙알%표면활성%흡부성능
dehydroabietylamine%tertiary amine oxide%surface activity%adsorption performance
利用纯度99%的脱氢枞胺原料经烷基化和氧化两步反应合成了一种含松香基三元菲环结构的N,N-二甲基脱氢枞基氧化叔胺。采用红外光谱(FT-IR)、核磁(1H NMR)对其结构进行表征,并通过L16(45)正交试验,对双氧水氧化法合成氧化叔胺的工艺条件进行了优化研究,制备反应的最佳工艺条件:双氧水与叔胺的物质的量比为1.5:1,反应时间12 h,催化剂用量1.5%,反应温度80℃。在优化的工艺条件下重复试验,氧化叔胺的产率为80%,GC含量均大于70%。产物的临界胶束浓度( CMC)为0.2 g/L,表面张力为22.75 mN/m,并且经此氧化叔胺改性得到的新型沸石吸附剂对一定浓度的腐殖酸、刚果红等环境污染物具有较佳的吸附效果,当初始质量浓度达到40 mg/L左右时吸附基本达到平衡,去除率分别为51.1%和91.0%。
利用純度99%的脫氫樅胺原料經烷基化和氧化兩步反應閤成瞭一種含鬆香基三元菲環結構的N,N-二甲基脫氫樅基氧化叔胺。採用紅外光譜(FT-IR)、覈磁(1H NMR)對其結構進行錶徵,併通過L16(45)正交試驗,對雙氧水氧化法閤成氧化叔胺的工藝條件進行瞭優化研究,製備反應的最佳工藝條件:雙氧水與叔胺的物質的量比為1.5:1,反應時間12 h,催化劑用量1.5%,反應溫度80℃。在優化的工藝條件下重複試驗,氧化叔胺的產率為80%,GC含量均大于70%。產物的臨界膠束濃度( CMC)為0.2 g/L,錶麵張力為22.75 mN/m,併且經此氧化叔胺改性得到的新型沸石吸附劑對一定濃度的腐殖痠、剛果紅等環境汙染物具有較佳的吸附效果,噹初始質量濃度達到40 mg/L左右時吸附基本達到平衡,去除率分彆為51.1%和91.0%。
이용순도99%적탈경종알원료경완기화화양화량보반응합성료일충함송향기삼원비배결구적N,N-이갑기탈경종기양화숙알。채용홍외광보(FT-IR)、핵자(1H NMR)대기결구진행표정,병통과L16(45)정교시험,대쌍양수양화법합성양화숙알적공예조건진행료우화연구,제비반응적최가공예조건:쌍양수여숙알적물질적량비위1.5:1,반응시간12 h,최화제용량1.5%,반응온도80℃。재우화적공예조건하중복시험,양화숙알적산솔위80%,GC함량균대우70%。산물적림계효속농도( CMC)위0.2 g/L,표면장력위22.75 mN/m,병차경차양화숙알개성득도적신형비석흡부제대일정농도적부식산、강과홍등배경오염물구유교가적흡부효과,당초시질량농도체도40 mg/L좌우시흡부기본체도평형,거제솔분별위51.1%화91.0%。
A new dehydroabietylamine derivative, i. e. , N, N-dimethyl dehydroabietylamine oxide, was synthesized from dehydroabietylamine (99 %) via alkylation and oxidation. Its structure was identified by FT-IR and 1H NMR spectra. The oxidation conditions were optimized by the L16 (45 ) orthogonal test. The results showed that suitable synthesis reaction conditions of the titled compound were as follows:N,N-dimethyl dehydroabietylamine oxide and H2 O2 molar ratio of 1. 5:1, reaction time of 12 h, EDTA of 1. 5 % and reaction temperature of 80 ℃. The GC content of the tertiary amine oxide were above 70 % in repetitive experiments. The surfactivity experiment showed that the critical micelle concentration ( CMC ) can be as low as 0. 2 g/L, and the surface tension is 22. 75 mN/m. And a new type of adsorbent prepared from amine oxide-modified zeolite has better adsorption effect on a certain concentration of humic acid and Congo red. When the initial concentration of 40 mg/L reached equilibrium, the removal rates were 51. 1% and 91. 0 %, respectively.