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作 者:华平[1] 叶俊[2] 喻红梅[1] 戴宝江[3] 方略韬[2]
机构地区:[1]南通大学化学化工学院,江苏南通226019 [2]南通大学纺织服装学院,江苏南通226019 [3]南通江山农药化工股份有限公司,江苏南通226006
出 处:《精细化工》2012年第8期742-745,共4页Fine Chemicals
基 金:"十二五"国家科技支撑计划重大项目(2011BAE06A06-9);江苏高校科研成果产业化推进项目(JHB2011-46);南通市科技创新计划项目(AS2009006)~~
摘 要:采用碳基固体酸作酯化反应催化剂于常压下反应的方法合成了乙二醇双子琥珀酸2-乙基丁基酯磺酸钠,酯化反应无需有机溶剂,磺化反应不外加相转移催化剂。最佳工艺条件为:单酯化反应,n(乙二醇)∶n(顺酐)=1.00∶2.10,催化剂碳基固体酸用量为顺酐质量的2%,100℃反应4.7 h,酯化率99.21%(质量分数);双酯化反应,n(2-乙基-1-丁醇)∶n(顺酐)=1.30∶1.00,于210℃反应1 h,酯化率95.17%(质量分数);磺化反应,n(亚硫酸氢钠)∶n(顺酐)=1.05∶1.00,于120℃反应1 h,磺化率100.65%(质量分数)。对产物结构进行了IR和1HNMR光谱表征,对产物性能进行了测定:CMC为2.99×10-3mol/L,γCMC为27.96 mN/m,乳化力4.35 min,渗透力为11.6 s,耐硬水力为13.3 min。Ethylene glycol Gemini sodium 2-ethyl-l-butanol sulfosuccinate was synthesized by the method of using carbonyl solid acid as the catalyst and esterification without organic solvents and sulfonation without any extra phase transfer catalysts at normal atmospheric pressure. The optimal synthetic conditions were as follows: in the single-esterification, n (ethylene glycol):n (maleic anhydride) = 1.00:2. 10 ,the amount of carbonyl solid acid was 2% of the amount of maleic anhydride, and the reaction took place at 100 ℃ for 4.7 h,with the esterification rate of 99.21% (mass fraction). In the di-esterification, n (2-ethyl-I -butanol) : n ( maleic anhydride) = 1.30:1.00, and the reaction took place at 210 ℃ for 1 h, with the esterification rate of 95.17% (mass fraction). In the sulfonation, n ( sodium hydrogen sulfite) : n ( maleic anhydride) = 1.05 : 1.00, and the reaction took place at 120 ~C for 1 h, with the sulfonation rate of 100.65% (mass fraction). The structure of the product was characterized by means of IR and ^1HNMR. Its properties were measured: CMC = 2.99 × 10^-3 mol/L, YCMC = 27.96 mN/m. The emulsifying power was 4.35 min, permeability was 11.6 s and the ability of hard water resistance was 13.3 min.
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