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N,N,N’,N’-四(β-羟丙基)己二酰胺的合成探索
The Exploration for Synthesis of N,N,N’,N’-tetra-(β-Hydroxypropyl) Hexadiamide
【摘要】 N,N,N’,N’-四(β-羟丙基)己二酰胺(简称“1260”)是一种新型的粉末涂料固化剂,其性能优于N,N,N’,N’-四(β-羟乙基)己二酰胺(简称“552”)。用己二酸二甲酯和二异丙醇胺一步反应合成“1260”,反应转化率100%,反应纯度80.6%。本文设计正交试验,通过HPLC检测研究了温度、投料比、催化剂用量及反应时间等参数对反应的影响;同时对后处理工艺进行研究。结果表明,最优反应条件为己二酸二甲酯∶二异丙醇胺投料比1.0∶3.4、催化剂添加量6%、反应时间16 h、反应温度140℃,通过结晶纯化获得白色固体产品,收率58.9%;产物结构经1H NMR和LC-MS确证。
【Abstract】 N,N,N’,N’-tetra(β-hydroxypropyl) hexanediamide(referred to as “1260”) is a new kind of curing agent for powdercoatings,and its properties are better than N,N,N’,N’-tetra(β-hydroxyethyl)hexanediamide(referred to as “552”).“1260” was synthesized by one-step reaction of dimethyl adipate and diisopropanolamine with the reaction conversion rate of 100% and reaction purity of 80.6%.The effects of temperature,material ratio,catalyst dosage,contact time and other parameters on the reaction were studied by HPLC,and orthogonal experiments was designed in this paper.Meanwhile,the post-treatment technology is studied,the results show that under the optimal reaction conditions(the ratio of feeding dimethyl adipate and diisopropanolamine is 1.0 to 3.4,dosage of catalyst 6%,reaction time 16 h,reaction temperature 140 ℃),the white solid product was obtained by crystallization and purification,with a crystallization yield of 58.9%.The structure of the product was confirmed by 1 H NMR and LC-MS.
【Key words】 N,N,N’,N’-tetra(β-hydroxypropyl) hexanediamide; orthogonal design; crystal; by-product;
- 【文献出处】 生物化工 ,Biological Chemical Engineering , 编辑部邮箱 ,2022年01期
- 【分类号】TQ225.261;TQ630.493
- 【下载频次】68