摘要
以n(葡萄糖):n(十二胺)=1:1.3合成了中间体N-十二烷基葡萄糖亚胺。中间体在35～45℃,压力为3.5MPa,Raney-Ni作催化剂条件下高压催化加氢合成了N-十二烷基葡萄糖胺,纯化后产率为55.7%;中间体在氧化剂H2O2和缓冲剂NaHCO3存在下,N2环境0～5℃反应3h后,55℃无水条件下反应20h合成了硝酮类化合物N-氧自由基-N-十二烷基葡萄糖亚胺,纯化后产率为60.2%。通过IR,元素分析和1HNMR对产品和中间体进行了结构表征。测定了N-十二烷基葡萄糖胺和N-氧自由基-N-十二烷基葡萄糖亚胺对钙、镁离子的键合能力,分别为157.40mgCaO.g-1、252.30mgMgO.g-1和154.75mgCaO.g-1、283.4mgMgO.g-1。考察了两者的生物降解性能,在10d内降解度分别为96.1%、98.5%,达到了欧盟议会和欧盟委员会关于洗涤剂的(EC)No648/2004法规对表面活性剂生物降解性的要求,属于易降解表面活性剂。
The intermediate N-dodecylglucosimine was synthesized using glucose and dodecylamine in molar ratio 1：1. 3. Then, catalyzed by Raney-Ni, the intermediate was hydrogenated at 35 - 45 ℃ under 3.5 MPa. The yield of N-dodecylglucosamine after purification was 55.7%. The intermediate was treated with oxidizing agent H2O2 and buffering agent NaHCO3 under the protection of N2. The reaction temperature should be controlled between 0 -5 ℃ for 3 h, then controlled bellow 55 ℃ for 20 h in the anhydrous condition. The yield of oxidized N-dodecylglucosimine nitrone after purification was 60.2%.Structures of the target products and the key intermediate were characterized with IR,^1HNMR and elementary analysis. The capability of N-dodecylglucosamine and N-dodecylglucosimine nitrone for complexometry of calcium ion and magnesium ion was determined as 57.40 mg CaO .g^-1,252.30 mg MgO . g^-1 and 154.75 mg CaO . g^-1,283.4mg MgO . g^-1 ,respectively. The biodegradability of two target products were 96.1% and 98.5 %, respectively. Such results meet the requirement of regulation （EC） No 648/2004 of the European Parliament and of the Council of 31 March 2004 on Detergents,and these surfactants are all belong to easily biodegradable surfactants.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2008年第5期454-458,共5页
Fine Chemicals
作者简介
徐爱忠（1982-），男，江苏苏州人，硕士研究生，师从王建新教授，主要从事精细化学品合成与应用，电话：（0）13485040913，E—mail：aizhongnight@163．com。
联系人：王建新（1949-），男，江苏无锡人，教授，主要从事天然有机物的合成与应用，电话（0510）89880711，E—mail：agkist@sina．com。
