液体荧光增白剂制备的研究

以DSD酸和三聚氯氰为主要原料,通过三步缩合反应得到四磺酸盐型液体荧光增白剂产品.研究了不同分散剂对反应速度及反应转化率的影响,并通过盐析,添加增溶剂改善产品性能.实验结果表明:丁酮为分散剂效果最佳,与平平加为分散剂和未加分散剂比,二步缩合反应合计时间均缩短了45min;并且反应转化率比后者高出6%.以丁酮为分散剂,经盐析精制,加入10%三乙醇胺和一缩二丙二醇复合助溶剂,得到了高质量的四磺酸型液体荧光增白剂.产品为澄清透明的液体,固含量高达40%,强度为55分,并且保持1个月性质不发生变化.另外,采用电子喷雾质谱仪对产品进行测定,经解析确定为四磺酸钠盐目标化合物.

Research on the preparation of liquor fluorescent whitening agent

The fluorescent whitening agents 4,4'-bis (4-p-sulfoanilino-6-isopropanolamino-s-triazin-2-ylamino)-2,2'-stilbenedisulfonic acid tetrasodium salts (tetra-sulfonate compound) were prepared using DSD acid and cyanuric chloride as the primary materials by the three step condensation reaction. Effects of different dispersants on the reaction rate and conversion rate were studied, and the properties of the products were improved by salting out and adding the complex cosolvents. The results showed that the dispersing effect was optimized with butanone as dispersant, and the total time of two-step condensation reaction shortened by 45min compared with adding polyoxyethylene alkyl ether and not adding any dispersants, and the conversion ratio increased by 6% than the latter. The product with high quality was obtained by using butanone as the dispersant, adding 10% of triethanolamine-dipropylene glycol complex cosolvents (w/w%), and purifying with salting out. The product was a transparent liquid and its solid content and the fluorescence strength were 40% and 55% respectively. Furthermore, its properties did not change within one month. With the ESI-MS analysis, the main component of this product was determined as tetra-sulfonate compound.