双三嗪氨基二苯乙烯类液体荧光增白剂的合成与应用研究

Studies on the synthesis of liquid fluorescent whitening agents and its application

以三聚氯氰(CC)、对氨基苯磺酸(Sulfanilic acid)和DSD酸(DSD acid)等为主要原料,经过三步缩合反应合成了双三嗪氨基二苯乙烯类液体荧光增白剂,采用纳滤技术对其脱盐精制,得到纯度为99.8%的液体荧光增白剂溶液。对三步缩合工艺中时间、温度、pH值、原料配比等因素进行正交实验。在最佳工艺条件下,第一步缩合反应转化率为99.4%,第二步缩合反应转化率为93.2%,第三步缩合反应液消光值为0.760,三步总转化率达到92.6%。经过纳滤脱盐精制后,NaCl的浓度由0.31mol/L降到0.0088mol/L,液体荧光增白剂的增白率由10.3%提高到15.9%,产品在0℃下放置6个月保持澄清透明和良好的流动性。采用电喷雾质谱对产物进行了表征。

The liquid fluorescent whitening agents were synthesized by the reaction of cyanuric chloride （CC）, sulfanilic acid, DSD acid. Then the fluorescent whitening agents＇ aqueous solutions were desalinated and concentrated by nanofiltration membrane. The purity of 99.8% liquid fluorescent whitening can be got. The optimal conditions were confirmed by orthogonal experiments, and the conversion rate of the first step of amino-group was 99.4%, the conversion rate of the second step of amino-group was 93.2%, the extinction value of the last solutions was 0.760. The total conversion rate of three steps was 92.6%. After the processes of desalinating and concentrating, the concentration of NaCl decreased from 0.31mol/L to 0.0088mol/L, the whitening rate increased from 10.3% to 15.9%. The liquid fluorescent whitening agent can be kept transparent under 0℃ for 6 months with good mobility.