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文章编号： 16726987（2019）04004608； DOI： 10.16351/j.16726987.2019.04.005
丁军委， 程秋振， 于文龙， 毛康成(青岛科技大学 化工学院，山东 青岛 266042）
摘要： 以4-氨基二苯胺和甲基异戊基甲酮为原料合成橡胶抗氧剂7PPD，对比了1%Pd/C、1%Pt/C和1%Pt-S/C 3种催化剂，得Pt-S/C催化剂的催化效果最好；以Pt-S/C为催化剂，对抗氧剂7PPD的合成工艺条件进行优化，得最佳工艺条件：催化剂加入量2%（以干基对4-氨基二苯胺的质量分数计），投料比n（甲基异戊基甲酮）∶n（4-氨基二苯胺）=6.0∶1，反应温度110 ℃，反应压力3.0 MPa，搅拌转速500 r·min-1；在此条件下，催化剂可重复使用18次，4-氨基二苯胺转化率可达99.5%以上，抗氧剂7PPD的收率可达98.5%以上；通过TEM、ICP、BET等手段对新鲜和失活的Pt-S/C催化剂进行表征，对比发现，催化剂载体部分孔道堵塞与晶粒长大是催化剂失活的主要原因。
关键词： 抗氧剂7PPD； Pt-S/C催化剂； 工艺优化； 失活分析
中图分类号： TQ 246.3文献标志码： A
引用格式： 丁军委， 程秋振， 于文龙， 等. PtS/C催化剂用于合成橡胶抗氧剂7PPD\[J\]. 青岛科技大学学报（自然科学版）， 2019， 40（4）： 4653.
DING Junwei, CHENG Qiuzhen, YU Wenlong, et al. Synthesis of rubber antioxidant 7PPD by PtS/C catalyst\[J\]. Journal of Qingdao University of Science and Technology（Natural Science Edition), 2019, 40(4)： 4653.
Synthesis of Rubber Antioxidant 7PPD by Pt-S/C Catalyst
DING Junwei, CHENG Qiuzhen, YU Wenlong, MAO Kangcheng
(College of Chemical Engineering，Qingdao University of Science and Technology，Qingdao 266042,China)
Abstract: Rubber antioxidant 7PPD was synthesized with 4-Amino diphenylamine and methyl isoamyl ketone. Three catalysts (1%Pd/C, 1%Pt/C and 1%Pt-S/C) were compared. The catalytic performance of Pt-S/C was the best. The optimal reaction conditions using Pt-S/C were obtained as follows, the quantity of catalyst 2% for 4-Amino diphenylamine, the mole ratio n(methyl isoamyl ketone)∶n(4-Amino diphenylamine) =6.0∶1, reaction temperature 110℃, reaction pressure 3.0 MPa, stirring speed 500 rpm. Under aforementioned conditions, the catalyst can be reused 18 times. The conversion rate of 4-amino diphenylamine reached 99.5% and the yield of antioxidant 7PPD reached 98.5%. The fresh and deactivated Pt-S/C were characterized by TEM, ICP, BET, etc. It was found that the main reason for catalyst deactivation was that part of the pores of the catalyst carrier was blocked and the crystal grains had grown.
Key words: antioxidant 7PPD; Pt-S/C catalyst; process optimization; inactivation
收稿日期： 20180820
基金项目： 山东省自然科学基金重大基础研究项目(ZR2017ZC0630).
作者简介： 丁军委(1970—)，男，教授.
