Azo Carboxylic Acid Ester And Water-soluble Azo Initiator Synthesis Research

Azo compound is an imporpant chemical compound which is used as initiator,vesicant, commonly used for producing polymer,organic synthesis and so on.This degree thesis consists of two parts, the synthesis of azocarboxylic esters as well as the synthesis and characteristics of aqueous azo-initiator.The first part is about the synthesis of azocarboxylic esters. azocarboxylic esters are commonly used as the initiator in the synthesis of polymer and vesicant. They do not contain cyano, are soluble somewhat in the water and their outcome of decomposition is innoxious, So they can be used for producing innoxious polymer . The research is done on the process of AzobisIsoButyroNitrile, AzobismethyButyroNitrile, AzobisdimethylValeroNitrile in 1,2—dichloroethane. At the same time ,the optimum condition for the synthesis of azocarboxylic esters is discussed. It is discovered that at the temperature of twenty centigrade when azonitrile and alcohol dissolved in proportition of 1:2.5 in 1,2—dichloroethane. Azoiminodimethlyether hydrochloride is obtained by ventilating dry HCl. azonitrile and azonitrile,alcohol,HCl dissolved in proportition of 1:2.5:2.6 ,Finally, azocarboxylic esters is obtained by hydrolyzing azoiminomethylether hydrochloride ,extracting, drying, decompression and distillation. By comparison, it is discovered that the synthesis of azocarboxylic esters from the reaction of azonitrile in 1,2-dichloroethane is economical , convenient to operate , recover and of high purity and productivity. Based on this, 2,2/—azobis(2—methyl—propanoic acid) dimethyl ester;2,2/—azobis(2—methyl—propanoicacid)diethylester;2,2/—azobis(2—methyl—propanoicacid)dipropylester;2,2/—azobis(2—methyl—propanoicacid)dibutylester;2,2/—azobis(2—methyl—propanoicacid)diisobutylester;2,2/—azobis(2—methyl—butanoicacid)dimethylester;2,2/—azobis(2,4—dimethyl—valeric acid) dimethyl ester are synthesized and the content of the chemical compound are measured by heating ,decomposition,and measuring the volume of N2.Meantime the decomposition temperature of these chemical compound are measured and they are also indicated by IR,1HNMR,elementary analysis.