酯基有机硅季铵盐柔软整理剂的合成与表征
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TQ649

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Synthesis and Characterization of siloxane quaternary
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    摘要:

    以硬脂酸和N-甲基二乙醇胺为原料进行酯化反应得到硬脂酸甲基二乙醇胺酯,再与γ-氯丙基甲基二甲氧基硅烷季铵化反应制备酯基有机硅季铵盐。通过单因素和正交试验,考察了反应温度、反应时间、反应物摩尔比及催化剂用量等对酯化反应的影响。酯化反应优化工艺条件:反应温度为180℃,反应时间为8h,反应物摩尔比n(硬脂酸): n(MDEA)= 1.6:1.0,次磷酸催化剂用量为0.9%;二甲基亚砜作为季铵化反应的溶剂。通过溴酚蓝显色反应以及红外光谱分析中间体和产物,测定了产物在298K下的表面活性以及柔软性能。结果表明产物表面张力为19.65 mN/m,临界胶束浓度CMC为0.197g/L,柔软性能优于同类市售产品。

    Abstract:

    Stearic acid methyl diethanolamine ester was synthesized from stearic acid and N-methyl diethanolamine, and then the intermediate was quaternized by γ-chloropropyl methyl dimethoxysilane to get the product siloxane quaternary ammonium salt containing ester group in this study. The effect of molar ratios of raw materials, reaction temperature, reaction time and catalyst dosage on the conversion of stearic acid were investigated by the orthogonal experiment. The optimal reaction conditions for the esterification were found to be 180℃ for 6h with hypophosphorous acid as ascatalyst at 1.6:1.0 molar ratio.The maximum yield of product was 56.42% in dimethyl sulfoxide. The intermediate and product were characterized by FTIR. The surface chemical properties were investigated at 298 K. The result show that the cmc is 0.197g/L, the γcmc is 24.25 mN/m, surface tension is 19.65mN/m and the softening performance of the sample is superior to general commercial products.

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郑成.酯基有机硅季铵盐柔软整理剂的合成与表征[J].精细化工,2012,29(12):

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  • 收稿日期:2012-08-12
  • 最后修改日期:2012-10-18
  • 录用日期:2012-10-19
  • 在线发布日期: 2012-11-30
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