化学试剂
化學試劑
화학시제
CHEMICAL REAGENTS
2010年
3期
251-254
,共4页
异辛醇%马来酸酐%异辛基正丁基琥珀酸双酯磺酸钠%磺化
異辛醇%馬來痠酐%異辛基正丁基琥珀痠雙酯磺痠鈉%磺化
이신순%마래산항%이신기정정기호박산쌍지광산납%광화
iso-octanol%maleic anhydride%sodium iso-octyl n-butyl sulfosuccinate%sulfonation
以异辛醇、马来酸酐、正丁醇和亚硫酸氢钠为原料,通过单酯化、双酯化和磺化反应合成了标题化合物,通过FT-IR表征了产物的结构.对各步反应的条件进行了考察.异辛醇与马来酸酐单酯化反应的适宜条件为:n(马来酸酐)∶n(异辛醇)=1.05,反应温度80 ℃,反应时间90 min;异辛醇马来酸单酯与正丁醇双酯化反应的适宜条件为:n(正丁醇)∶n(异辛醇马来酸单酯)=1.5,催化剂对甲苯磺酸的用量(基于总反应物的质量)为0.20%,反应温度130 ℃,反应时间150 min;异辛基正丁基马来酸双酯与亚硫酸氢钠磺化反应的适宜条件为:n(亚硫酸氢钠)∶n(异辛基正丁基马来酸双酯)=1.1,反应时间150 min,反应温度95 ℃.在此优化反应条件下,异辛基正丁基琥珀酸双酯磺酸钠盐的总收率为91.38%.
以異辛醇、馬來痠酐、正丁醇和亞硫痠氫鈉為原料,通過單酯化、雙酯化和磺化反應閤成瞭標題化閤物,通過FT-IR錶徵瞭產物的結構.對各步反應的條件進行瞭攷察.異辛醇與馬來痠酐單酯化反應的適宜條件為:n(馬來痠酐)∶n(異辛醇)=1.05,反應溫度80 ℃,反應時間90 min;異辛醇馬來痠單酯與正丁醇雙酯化反應的適宜條件為:n(正丁醇)∶n(異辛醇馬來痠單酯)=1.5,催化劑對甲苯磺痠的用量(基于總反應物的質量)為0.20%,反應溫度130 ℃,反應時間150 min;異辛基正丁基馬來痠雙酯與亞硫痠氫鈉磺化反應的適宜條件為:n(亞硫痠氫鈉)∶n(異辛基正丁基馬來痠雙酯)=1.1,反應時間150 min,反應溫度95 ℃.在此優化反應條件下,異辛基正丁基琥珀痠雙酯磺痠鈉鹽的總收率為91.38%.
이이신순、마래산항、정정순화아류산경납위원료,통과단지화、쌍지화화광화반응합성료표제화합물,통과FT-IR표정료산물적결구.대각보반응적조건진행료고찰.이신순여마래산항단지화반응적괄의조건위:n(마래산항)∶n(이신순)=1.05,반응온도80 ℃,반응시간90 min;이신순마래산단지여정정순쌍지화반응적괄의조건위:n(정정순)∶n(이신순마래산단지)=1.5,최화제대갑분광산적용량(기우총반응물적질량)위0.20%,반응온도130 ℃,반응시간150 min;이신기정정기마래산쌍지여아류산경납광화반응적괄의조건위:n(아류산경납)∶n(이신기정정기마래산쌍지)=1.1,반응시간150 min,반응온도95 ℃.재차우화반응조건하,이신기정정기호박산쌍지광산납염적총수솔위91.38%.
Sodium iso-octyl n-butyl sulfosuccinate was synthesized via monoesterification,diesterification and sulfonation reactions using iso-octanol,maleic anhydride,n-butanol and sodium bisulfite as starting materials.Its structure was characterized by means of FT-IR spectroscopy.The effects of reaction conditions on monoesterification,diesterification and sulfonation were studied.The optimum conditions for monoesterification between iso-octanol and maleic anhydride were:a mole ratio of maleic anhydride to iso-octanol at 1.05,a reaction temperature of 80 ℃ and a reaction time of 90 min.The optimum conditions for diesterification between iso-octanol maleic monoester and n-butanol were:a mole ratio of n-butanol to iso-octanol maleic monoester at 1.5,a p-toluenesulfonic acid catalyst mass fraction of 0.20%(based on total mass of reaction materials),a reaction temperature of 130 ℃ and a reaction time of 150 min.The optimum conditions for sulfonation between NaHSO_3 and iso-octyl n-butyl maleate were:a mole ratio of NaHSO_3 to iso-octyl n-butyl maleate at 1.1,a reaction temperature of 95 ℃ and a reaction time of 150 min.The overall yield of sodium iso-octyl n-butyl sulfosuccinate was around 91.38% obtained under the optimized reaction conditions.
