新型钛可溶阳极电解产物后处理实验研究

New experimental study on the post-treatment of products from titanium soluble anode electrolysis

针对钛可溶阳极电解产物后处理带来的产品污染和电解质回收难的问题,采用无水乙醇选择性溶出、不溶固体产物热态溶解——冷态结晶的方法实现电解产物中KCl的回收和钛粉获得;滤液经氯化、蒸馏实现钛酸乙脂制备和乙醇的回收。结果表明:无水乙醇与电解质液固比为10∶1,即可完全浸出低价钛氯化物。NaCl/KCl溶液与不溶物的液固比为5∶1时可完全溶出不溶物中的KCl,1L滤液可得127.3g结晶物,其成分为KCl 96.62%、NaCl 3.38%,所得的钛粉质量明显优于传统洗涤获得的钛粉。经氯化后的滤液完全生成钛酸乙脂需5倍体积量的氨气,乙醇回收率平均能达到96.3%,1L醇液能得47mL钛酸乙脂。

Aiming at problems of product pollution and difficult - to - recovery of electrolyte in the post - treatment process of electrolysis products from titanium soluble anode, a new method of using anhydrous alcohol selective dissolution and hot state dissolution ＆ cold state crystallization dealing with the insoluble solid product to recover KC1 from electrolyte and acquire titanium powder was proposed in this paper. Tetraethyl titanate could be prepared and alcoholic could be recovery by filtrate chloration and distillation. The experiment results show that： low valence titanium chlorides can be completely leached when the solid -liquid ratio of anhydrous ethanol to electrolyte is 10：1 ; KCI in the insoluble solid can completely dissolve out when the liquid - solid ratio of NaCI/KC1 solution to insoluble solid is 5： 1, and 127.3g crystal, which contains KC196. 62% and NaC13.38%, could be acquired from IL filtrate; The titanium powder quality is obviously superior to the traditional washing obtained; the filtrate after chlorination can completely generate tetraethyl titanate when ammonias flow is 5 times volume than its theory demand; alcohol recovery rate is 96. 3% and about 47mL tetraethyl titanate could be acquired from 1 L alcohol liquid.