合成硝基麝香溶液结晶分离研究

为了开发低共熔组成酮麝香、二甲苯麝香混合物溶液结晶新过程,计算得到酮麝香、二甲苯麝香、溶剂三元相图。在此基础上研究了麝香混合物溶液结晶分离方法,提出了轮流加入乙腈和庚烷从低共熔组成麝香混合物中,分级冷却结晶分离得到2种产品的过程。由三元相图得到理论产量并进行试验验证,结果表明加入乙腈一级结晶可得到纯度为97.5%的二甲苯麝香,加入庚烷二级结晶后酮麝香的纯度为98.1%。

Study on crystallization of synthetic nitro-musks solution

In order to develop a new solution crystallization process to separate the eutectics of musk ketone and musk xylene,the ternary phase diagrams of musk ketone,musk xylene and solvent were calculated.On the basis of these diagrams,the methods of musk separation by solution crystallization were studied.A new cooling and fractional crystallization process was proposed to separate musk ketone and musk xylene from the eutectics by adding acetonitrile and heptane in turn,which was depicted by ternary phase diagrams and verified by experiments.The experimental results show that musk xylene with a purity of 97.5% is obtained by adding acetonitrile in one-stage crystallization and musk ketone with a purity of 98.1% was obtained by adding heptane in two-stage crystallization.