荧光增白剂CBS的合成及性能

Synthesis and Properties of Fluorescent Brightener CBS

以对氯氯苄、亚磷酸三乙酯和邻磺酸钠苯甲醛为原料,经3步反应制得荧光增白剂4,4'-双-(2-磺酸钠苯乙烯基)联苯(CBS),并对其结构进行了IR、1HNMR表征。采用紫外光谱和荧光光谱,研究了产物的光致异构化和荧光浓度自猝灭现象,考察了p H和光照时间对其荧光强度的影响,同时对滤纸和棉布进行了增白性能检测。通过单因素实验确定了最佳反应条件:4-氯-二苯乙烯-2'-磺酸钠的合成,n(对氯氯苄)∶n(甲醇钠)=1∶1.1,温度45℃;CBS的合成,温度80℃,m(催化剂)/m(4-氯-二苯乙烯-2'-磺酸钠)=0.04,催化剂配比n(Ni Cl2)∶n(PPh3)∶n(Zn)=1∶3∶2。结果表明,CBS总收率可达66.7%;光照使CBS反式异构体向顺式异构体转换,荧光性能下降;CBS在碱性条件下的荧光性能优于在酸性条件下的荧光性能;荧光淬灭的质量浓度为10 mg/L。

Fluorescent brightener 4,4 ＇-bis （ 2-sulfostryl ） biphenyl disodium salt （ CBS ） was synthesized through a three-step reaction by using 4-chlorobenzyl chloride, trimethyl phosphite and benzaldehyde-2- sulfonie acid sodium salt as starting materials. The chemical structure was characterized by means of IR and NMR. The photoindueed isomerization phenomena and fluorescence emission properties were studied. In addition, the effects of concentration, pH and light irradiation time on fluorescence properties were investigated. The whiteness measurement was conducted through dyeing filter paper and cotton. The optimized reaction conditions were as follows： reaction temperature for sodium 2-（4- chlorostyry） benzenesulfonate synthesis was 45 ~C, n （4-chlorobenzyl chloride ） ： n （ sodium methoxide ） = 1.0 ： 1.1, reaction temperature for CBS synthesis was 80 ℃, m （ catalyst ） /m [ sodium 2-（4- ehlorostyry） benzenesulfonate ] = 0. 04 and n （ NiCl2 ） ： n （ PPh3 ） ： n （ Zn ） = 1 ： 3：2. The results show that the overall yield of CBS was 66.7%. With the increasing of light irradiation time, trans-isomers were transformed into eis-isomers, and fluorescence intensity was reduced. The fluorescence intensity of CBS under alkaline condition was higher than that under acidic condition. The fluorescence quenching mass concentration of CBS was 10 mg/L.