六次甲基四胺基多季铵盐的合成与表征
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摘要
以环氧氯丙烷和六次甲基四胺为原料,通过季铵化反应制备一种具有多取代环氧基结构的季铵盐。研究了反应溶剂、原料摩尔比、原料浓度、反应温度、反应时间等因素对季铵化反应程度及产物环氧值的影响。结果表明,在以水为溶剂、六次甲基四胺和环氧氯丙烷物质的量比1∶4、六次甲基四胺用量为0.04 mol、反应温度45℃、反应时间2 h时,转化率为68.50%,环氧值为62.04%。高效液相色谱、红外光谱和氢核磁谱图等表征手段表明,所得结果与预期目标一致,取代度为3.5,产物具有环氧基团,且环氧开环可以引入碳氯键,为下一步合成提供了基础。
A new epoxy propyl quaternary ammonium salt with multi-substituted epoxide group and high charge density was synthesized by hexamethylenetetramine and epichlorohydrin though quaternization reaction. The influences of reaction solvent, raw material concentration, reaction temperature and reaction time, molar ratio of raw materials on the degree of quaternization reaction and the epoxy value of product were studied systematically. The results showed that the conversion rate and the epoxy value could reach to 68.50% and 62.04% respectively, when the molar ratio of hexamethylenetetramine to epichlorohydrin was 1∶ 4 and the concentration of hexamethylenetetramine was 0.04 mol using water as solvent at 45 ℃ for 2 h. The structures of raw materials and product were characterized by FT-IR, HPLC, NMR, respectively. The result showed that the structure of product are consistent with the expected results, of which substitution degree is 3.5. The product has epoxy group and the carbon-chlorine bond could be introduced into the opening epoxy ring, which could provide the basis for the following synthesis.
A new epoxy propyl quaternary ammonium salt with multi-substituted epoxide group and high charge density was synthesized by hexamethylenetetramine and epichlorohydrin though quaternization reaction. The influences of reaction solvent, raw material concentration, reaction temperature and reaction time, molar ratio of raw materials on the degree of quaternization reaction and the epoxy value of product were studied systematically. The results showed that the conversion rate and the epoxy value could reach to 68.50% and 62.04% respectively, when the molar ratio of hexamethylenetetramine to epichlorohydrin was 1∶ 4 and the concentration of hexamethylenetetramine was 0.04 mol using water as solvent at 45 ℃ for 2 h. The structures of raw materials and product were characterized by FT-IR, HPLC, NMR, respectively. The result showed that the structure of product are consistent with the expected results, of which substitution degree is 3.5. The product has epoxy group and the carbon-chlorine bond could be introduced into the opening epoxy ring, which could provide the basis for the following synthesis.
引文
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[2] 张利利,岳智毅,李沅,等.端基为C—Br键新型聚季铵盐的合成与表征[J].大连工业大学学报,2017,36(1):37-40.
[3] 于俊杰,马希晨,曹亚峰.新型季铵烷基阳离子单体YJJ的合成[J].大连轻工业学院学报,2003,22(2):94-96.
[4] 杨心督,张其清.聚乙二醇单甲醚接枝壳聚糖取代度测定方法与分析[J].河北医药,2015,37(12):1885-1886.
[5] 张毅民,鲍锋,张志飞,等.紫外光谱法测定羟丙基-β-环糊精平均取代度[J].分析化学简报,2007,35(7):1055-1058.
[6] 马希晨,于俊杰,宋辉,等.新型季铵烷基淀粉醚的研制[J].精细石油化工,2004(5):46-68.