一步法合成氨基磺酸镍工艺的研究

Research on synthesis of nickel sulfaminate by one-step method

采用适宜的活化剂,可实现氨基磺酸与镍的直接、快速反应,通过一步法合成氨基磺酸镍,避免了多步法对产品的污染。研究了预活化时间、活化剂、反应温度、pH、反应时间对反应的影响。结果表明,活化预处理4 h,使用自行研制的氧化性活化剂,在30～50℃、pH为3.0～4.0、反应时间为72 h的条件下,能够完成合成反应,并有效控制氨基磺酸水解的发生。产品满足GB/T 23847—2009《电镀用氨基磺酸镍》优等品指标要求,硫酸根和游离氨仅为优等品指标的1/6。该产品已顺利实现产业化。

Direct, rapid response of sulfamic acid and nickel can be achieved by using the suitable activator and nickel sulfaminate can be prepared with one-step method, so that it can avoid the pollution of product that synthesized by multi-step method.Effects of pre-activation time, activator, reaction temperature, pH, and reaction time on the reaction were studied.Resuits showed that under the conditions of 4 h activation pretreatment, using self-developed oxidative activation agent, reaction temperature of 30-50 ℃, pH of 3.0-4.0, and reaction time of 72 h, the synthesis reaction could be completed, and the hydrolysis of sulfamic acid could also be effectively controlled.The quality indexes of the obtained product met the requirements of the high-class products stipulated in the national standard of Nickel Sulfaminate for Electroplating （GB/T 23847-2009）, especially for SO4^2- and free ammonia contents are only 1/6 of the national standard.Now the product has been successfully put into industrialization.