摘要
采用氧化精馏方法,对过氧乙酸预精制俄罗斯工业级乙腈的工艺条件(包括过氧乙酸用量、固体氧化剂过硫酸钾用量及精馏时间进行了考察;并采用紫外分光光度法对乙腈精制过程进行在线检测,结合GC、GC-MS、水分测定及FTIR分析对乙腈中的杂质组成及除杂效果进行了探讨。实验结果表明,俄罗斯工业级乙腈中的主要杂质是丙腈和烯丙醇,其中丙腈影响产品纯度,但对其紫外吸光度影响较小;而烯丙醇不仅影响产品纯度,且对其紫外吸光度影响较大。过氧乙酸能选择性环氧化烯丙醇中的双键,可获得紫外吸光度和纯度达HPLC级乙腈的精制产品。最佳精制条件为:V(乙腈)∶V(过氧乙酸)=100∶6,m(乙腈)∶m(过硫酸钾)∶m(氢氧化钾)=100∶1.5∶0.5,精馏时间4 h。
The purification of Russia industrial-grade acetonitrile was carried out by oxidation and rectification. The process conditions, such as amount of peracetic acid, amount of solid oxidant potassium persulfate and rectification time, in the pre-purification of the Russia industrial-grade acetonitrile with peracetic acid were studied. The purification process was analyzed by means of UV spectrophotometer on-line. The impurity composition in the Russia industrial-grade acetonitrile and their removal were investigated by means of GC, GC-MS, moisture meter and FTIR. The results show that the main impurities were propionitrile and allylalcohol, in which propionitrile influences the purity of the Russian industrial-grade acetonitrile but plays the small role in the UV absorbance and allylalcohol impacts not only the purity but also the UV absorbance. By selectively epoxydizing the double bonds of allylalcohol with peracetic acid, the purity of the Russia industrial-grade acetonitrile can be improved and meet the requirement of HPLC grade acetonitrile. The optimum process parameters of the purification are as follows： V（CH3CN） ： V（CH3CO3H） 100 ： 6, m（CH3CN） ： m（K2S2O8） ： m（KOH） 100 ： 1.5 ： 0.5 and rectification time 4 h.
出处
《石油化工》
CAS
CSCD
北大核心
2013年第2期175-180,共6页
Petrochemical Technology
关键词
俄罗斯工业级乙腈
过氧乙酸
过硫酸钾
精制
除杂
Russia industrial-grade acetonitrile
peracetic acid
potassium persulfate
purification
impurity removal
