癸二胺的合成工艺及其应用分析-synthesis process and application analysis of decylenediamine.docxVIP

癸二胺的合成工艺及其应用研究摘要1，10-二氨基癸烷（癸二胺）是合成聚酰胺和共聚酰胺的重要原材料。癸二胺的合 成与开发源于尼龙 1010 树脂的生产需要，而尼龙 1010 树脂可以广泛应用在服装面料、 表面活性剂、化工各类树脂等行业，因而癸二胺作为一种用途广泛的精细化工中间体， 在服装热熔胶行业用量增加较快。本文主要研究了癸二酸氨化脱水合成癸二腈，癸二腈加氢合成癸二胺，癸二酸和癸 二胺熔融缩聚合成尼龙 1010 等三个过程。运用红外光谱（IR）、气质联用（GC-MS）、 核磁共振氢谱（1HNMR）、差示扫描量热法（DSC）等检测手段对其进行了结构表征和 性能测试，主要内容包括以下几个方面：1、以癸二酸、氨气为原料，使用复合催化剂，加压催化合成癸二腈。最佳合成条 件为：将反应分为高低两个温区，低温区酰胺化反应温度为 140～210℃，8 小时；高温 区脱水温度为 210～265℃，5 小时；复合型催化剂 ZnO/Al2O3（2:1），相应的质量分数 为 6%显示最好的催化效果，癸二腈收率为 83%。反应在两个温区进行，前期充分进行 酰胺化反应，避免物质多元化。后期强化温度充分脱水，避免了长时间单一强化温度的 炭化和副产物增多。2、以癸二腈和氢气为原料、乙醇为溶剂、氢氧化钾为助催化剂、雷尼镍为催化剂， 采用间歇式催化加氢生产合成癸二胺，最佳合成条件为：反应温度范围在 80~85℃，反 应压力范围 2.1~2.4MPa，800r/min 的搅拌速度，抑制剂氢氧化钾 0.6~0.8%（癸二腈的 质量分数），催化剂选取 20μm 雷尼镍相应质量分数为 15%显示效果最好，癸二胺的 收率为 92%。3、以纯化的癸二胺和癸二酸为单体、水为溶剂，采用一步熔融缩聚法合成了尼龙1010，采用特性粘度测试和差示扫描量热法对产物进行结构和热性能表征，熔融温度为202℃，结晶温度为173℃，PA1010的在340℃开始热分解，验证了癸二胺的实用性与市 售相似。关键词：癸二酸；氨化；癸二腈；氢化；癸二胺；尼龙 1010The synthesis and application of Decane diamine from sebacic acidAbstractDecane diamine was an important raw material of synthetic polyamides and polyamide, which was also known as 1,10-diamino decane or 1,10 a decamethylenediamine. The synthesis and development of decane diamine was derived from the production needs of 1010 nylon resin. PA1010 resin were widely used in apparel fabrics, surfactants, all kinds of resin, chemical and other industries, and so decane diamine as a versatile chemical intermediates, which was applied in clothing hot melt adhesive especially.This paper mainly studied three reactions processes: firstly, the sebaconitrile was prepared by amide dehydration from sebacic acid, and then sebaconitrile hydrogenation synthesis decanediamine, finally, nylon 1010 were obtained by sebacic acid and decane diamine melt polycondensation reaction. Structure and performance of sebacic acid and sebaconitrile were investigated by Fourier transform infrared (IR), nuclear magneticresonance spectroscopy (1HNMR), differential scanning calorimetry (DSC) and otherdetection means. The main results obtained