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作 者:李文骁[1] 李付刚[1] 闫士杰[1] 鄢冬茂[1] 白雪松[1]
出 处:《染料与染色》2014年第3期29-33,共5页Dyestuffs and Coloration
基 金:"十二五"科技支撑项目:荧光增白剂与直接染料重要中间体清洁生产新技术开发及示范。(课题编号2011BAE07B07)
摘 要:本文研究了4,4'-二硝基二苯乙烯-2,2'-二磺酸(DNS酸),在Pt/C催化剂存在下,Zn和Cu为抑制剂,水相体系中液相催化加氢制备DSD酸。Pt-Cu-Zn/C催化剂制备DSD酸具有很好的活性和选择性,能有效抑制苄基物及影响色度的杂质的生成。较佳的工艺条件为:DNS酸钠盐质量浓度为12~20%、Pt/C催化剂量为硝基物的0.5~0.7%,反应温度40~60℃、pH4~6、氢气压力1.0 MPa。DNS酸转化率100%,DSD酸选择性98.5%以上,收率98%,DSD酸含量均达到95%以上(氨基值法),苄基物含量低于0.1%(外标法),色度低于0.2。新工艺生产每吨DSD酸产生废水12吨,废水COD值为24 mg/L,无色透明。DSD acid was prepared from DNS acid by liquid phase catalytic hydrogenation in the presence of Pt-Cu-Zn /C catalyst. The catalyst could effectively inhibit benzyl compound and the by-productions which affected the chrominance of DSD acid. The optimum conditions were: concentration of the DNS sodium salt 12%- 20%,the amount of catalyst 0. 5%- 0. 7%( in DNS acid),reaction temperature was 40℃- 60℃,pH4- 6,and hydrogen pressure 1. 0 MPa. Through the study on liquid phase catalytic hydrogenation,we found the content of benzyl compound was contrary to the chrominance. In this new process: the conversion of DNS acid was100%; the regioselectivity was 98. 5%; the yield was 98%; the concentration purity of product was more than 95%( the value of amino-group was detected). The benzyl compound was less than 0. 1%; the chrominance was less than 0. 2,and other targets were reached sector standard. The new process generated 11 ton wastewater per 1 ton DSD acid,the wastewater was colorless and transparent,and COD volue was 24 mg /L.
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