碘仿电解合成的工艺研究

Technological Study of Iodoform Electrosynthesis

开发了一种以石墨为阳极、铅为阴极、采用旋转阳极和离子膜分隔电解槽的碘仿电解合成的先进工艺 ,经过 5因素 4水平的正交试验 ,发现影响电流效率的各工艺因素中 ,阳极电流密度的影响最大 ,其次分别为阳极液温度 ,阳极液 p H值 ,阳极液中碘化钾的浓度和阳极转速。优化得到碘仿电合成的最佳工艺条件为 :碘化钾浓度 2 0 0 g· L- 1 ,阳极电流密度 2 5 A· dm- 2 ,阳极液温度为 2 0℃ ,阳极液 p H值为 9.5,阳极转速为2 0 0 r· min- 1 ,在此最佳工艺条件下 ,电流效率可达 97.2 3%。

The technology of preparation of iodoform by electrochemical synthesis was investigated. The electro synthesis of iodoform is realized by basic aqueous 0.1mol·L -1 Na 2CO 3 solution in which there is certain amount of acetone and KI. The electrochemical cell is a kind of ion exchange membrane divided tri chamber cell in which the anode is set in the middle. The anode material is graphite and the cathode is lead. The anode is designed as rotating one whose speed can be controlled.It was found that several parameters would influence the current efficiency such as: pH value of anolyte, temperature of anolyte, potassium iodide concentration in anolyte, speed of anode rotation and anode current density. Furthermore the orthogonal test was designed and carried out in which included 5 factors and 4 indices. According to the experimentally results of orthogonal test,the optimized experimental conditions for the preparation of iodoform were given as follows: anode current density being 25A·dm -2 ,pH value of anolyte being 9.5,temperature of anolyte being 20℃,potassium iodide concentration being 200 g·L -1 and speed of anode rotation being 200 r·min -1 .Very high current efficiency (97.23%) was obtained under optimized experimental conditions.ould influence the curren