南通大学学报:自然科学版
南通大學學報:自然科學版
남통대학학보:자연과학판
Journal of Nantong University (Natural Science Edition)
2012年
3期
11-17
,共7页
朱国华%叶俊%华平%戴宝江%方略韬
硃國華%葉俊%華平%戴寶江%方略韜
주국화%협준%화평%대보강%방략도
Gemini表面活性剂%磺酸盐型Gemini表面活性剂%乙二醇双子琥珀酸2-甲基戊基酯磺酸钠%碳基固体酸
Gemini錶麵活性劑%磺痠鹽型Gemini錶麵活性劑%乙二醇雙子琥珀痠2-甲基戊基酯磺痠鈉%碳基固體痠
Gemini표면활성제%광산염형Gemini표면활성제%을이순쌍자호박산2-갑기무기지광산납%탄기고체산
Gemini surfactant%sulfonate Gemini surfactant%ethylene glycol Gemini sodium 2-methyl-l-pentanol sul- fosuccinate%carbonyl solid acid
采用酯化反应无需有机溶剂为介质、以碳基固体酸作酯化反应催化剂、磺化反应不外加相转移催化剂在常压下反应的新方法合成了乙二醇双子琥珀酸2-甲基戊基酯磺酸钠,最佳工艺条件为:单酯化反应,n(乙二醇):n(顺酐):l_00:2.10,催化剂碳基固体酸用量为顺酐质量的2%,于100℃反应4.7h,酯化率99.02%(质量分数);双酯化反应。n(2-甲基-l-戊醇):n(顺酐)=1-30:1.00,于210℃反应1.2h,酯化率95.34%(质量分数);磺化反应,n(亚硫酸氢钠):n(顺酐):1.05:1.00。于油浴120℃反应3.2h,磺化率100.64%(质量分数).对产物结构进行了IR光谱表征,测定了产物性能:CMC为2.5×10。mol/L,7cMc为27.79mN/m,乳化力为11.5min,渗透力为6s,耐硬水力为13.5min.比较了碳基固体酸和无水乙酸钠、对甲苯磺酸对酯化反应的催化效果,结果表明:碳基固体酸对酯化反应的催化效果好.且易于分离.
採用酯化反應無需有機溶劑為介質、以碳基固體痠作酯化反應催化劑、磺化反應不外加相轉移催化劑在常壓下反應的新方法閤成瞭乙二醇雙子琥珀痠2-甲基戊基酯磺痠鈉,最佳工藝條件為:單酯化反應,n(乙二醇):n(順酐):l_00:2.10,催化劑碳基固體痠用量為順酐質量的2%,于100℃反應4.7h,酯化率99.02%(質量分數);雙酯化反應。n(2-甲基-l-戊醇):n(順酐)=1-30:1.00,于210℃反應1.2h,酯化率95.34%(質量分數);磺化反應,n(亞硫痠氫鈉):n(順酐):1.05:1.00。于油浴120℃反應3.2h,磺化率100.64%(質量分數).對產物結構進行瞭IR光譜錶徵,測定瞭產物性能:CMC為2.5×10。mol/L,7cMc為27.79mN/m,乳化力為11.5min,滲透力為6s,耐硬水力為13.5min.比較瞭碳基固體痠和無水乙痠鈉、對甲苯磺痠對酯化反應的催化效果,結果錶明:碳基固體痠對酯化反應的催化效果好.且易于分離.
채용지화반응무수유궤용제위개질、이탄기고체산작지화반응최화제、광화반응불외가상전이최화제재상압하반응적신방법합성료을이순쌍자호박산2-갑기무기지광산납,최가공예조건위:단지화반응,n(을이순):n(순항):l_00:2.10,최화제탄기고체산용량위순항질량적2%,우100℃반응4.7h,지화솔99.02%(질량분수);쌍지화반응。n(2-갑기-l-무순):n(순항)=1-30:1.00,우210℃반응1.2h,지화솔95.34%(질량분수);광화반응,n(아류산경납):n(순항):1.05:1.00。우유욕120℃반응3.2h,광화솔100.64%(질량분수).대산물결구진행료IR광보표정,측정료산물성능:CMC위2.5×10。mol/L,7cMc위27.79mN/m,유화력위11.5min,삼투력위6s,내경수력위13.5min.비교료탄기고체산화무수을산납、대갑분광산대지화반응적최화효과,결과표명:탄기고체산대지화반응적최화효과호.차역우분리.
Ethylene glycol Gemini sodium 2-methyl-l-pentanol sulfosuccinate is synthesized by the methed of using carbonyl solid acid as the catalyst without organic solvents in esterification and any extra phase transfer catalysts in sulfonation. The optimal synthetic conditions are as follows: in the single-esterification, n (ethylene glycol):n (maleic anhydride) = 1.00:2.10, the amount of carbonyl solid acid is 2% of the amount of maleic anhydride, and reacted un- der 100 ~C for 4.7 h with the esterification rate of 99.02%(Mass fraction). In the di-esterification, n(2-methyl-1- pentanol):n(maleic anhydride) = 1.30:1.00, and reacted under 210 ~C for 1.2 h with the esterification rate of 95.34% (Mass fraction). In the sulfonation, n (sodium hydrogen sulfite) :n (maleic anhydride) = 1.05:1.00, and reacted under 120 ~C for 3.2 h with the sulfonation rate of 100.64% (Mass fraction). The structure of the product is characterized by IR. And its properties are measured: CMC = 2.5x10mol/L, Yc = 27.79 mN/m. Emulsifying power is 11.5 rain, permeability is 6 s and the ability of hard water resistance is 13.5 min. Compared with sodium acetate anhydrous andtoluenesulfonic acid, the carbonyl solid acid is more catalytic efficiency and easily to be separated.