Research On Synthetical Technology And Reaction Mechanism Of Curing Agents Of Amide

The curing agents ofβ-hydroxyalkylamides are widely used in polyesters which contain carboxyl and anhydride groups because of their non toxicity,high efficiency,economy and ecology.Firstly,this paper focused on synthesis and technology of N,N,N',N'-tetra (β-hydroxyethyl)adipamide based on single factor experiments,orthogonal experiments and choice of auxiliaries under ratio of stoichiometric coefficient.The yield reached 90.7%with melting point meeting requirement.Moreover,two-step synthesis and gradient temperaturereducing synthesis were studied.By-product was identified by ~1HNMR in order to explore reaction mechanism.Secondly,N,N-bis(β-hydroxyethyl)benzoylamide was synthesized first by aminolysis of methyl benzoate with diethanolamine using a method of preparing N,N,N',N'-tetra (β-hydroxyethyl)adipamide.Synthetical technology was studied with help of GC and optimal reaction condition was obtained.Under this condition,yield was about 87.8%.Liquid- liquid continuous extractor which was designed in person was used to separate target product.Thirdly,yellowing of N,N,N',N'-tetra(β-hydroxyethyl)adipamide limits its application. In this paper,synthesis of N,N,N',N'-tetra(acryloxyethyl)adipamide(Ⅰ)and N,N,N',N'-tetra (epoxy propyloxyethyl)adipamide(Ⅱ)as its derivatives were explored to expand its new use. Methods of "acrylic acid","methyl acrylate" and "acryloyl chloride" were tried to synthesize I.Results revealed that method of acryloyl chloride had low reaction temperature and degree of polymerization which gave high yield compared to methods of acrylic acid and methyl acrylate.Two-step method under catalyst of acid and one-step method under catalyst of base were studied to prepareⅡ.Results revealed that no low polar ingredient was found in two-step method which was inferior to one-step method.Finally,photo curing agent of N,N'-diallyladipamide and N-allyl benzoylamide were prepared both with a yield of over 90%.