副品红的合成、提纯及生产废水处理  

Synthesis,purification and wastewater treatment of parafuchsin

作　　者：徐习习 顾贵洲[1] 蒋林时[1] 李政[1] XU Xixi;GU Guizhou;JIANG Linshi;LI Zheng(School of Environmental and Safety Engineering,Liaoning Petrochemical University,Fushun 113001,Liaoning,China)

机构地区：[1]辽宁石油化工大学环境与安全工程学院,辽宁抚顺113001

出　　处：《精细化工》2023年第5期1149-1154,共6页Fine Chemicals

基　　金：辽宁省教育厅科研项目(2021-510-000-2691)。

摘　　要：采用两步催化法合成副品红。首先,对硝基甲苯与多硫化钠在无水乙醇为有机溶剂、N,N-二甲基乙酰胺(DMA)为胺基催化剂条件下生成对氨基苯甲醛,得到最佳n(DMA)∶n(对硝基甲苯)=3∶13,其中,对硝基甲苯用量为25 g(0.18 mol),下同。然后,对氨基苯甲醛在聚乙二醇400(PEG-400)催化下与苯胺和盐酸反应生成副品红粗品,考察了物料比、反应温度和反应时间对副品红粗品产率的影响。结果表明,在n(PEG-400)∶n(对硝基甲苯)=2∶300、n(对硝基甲苯)∶n(苯胺)∶n(盐酸)=1∶5.9∶2.8、110℃下反应4 h,副品红粗品产率为85.6%。最后,考察了蒸馏温度和时间对副品红质量分数的影响。发现在130℃下蒸馏3 h,副品红的质量分数达到91.3%。副品红生产废水主要为苯胺,精馏后苯胺回收率达89.3%。Parafuchsin was synthesized by two-step catalytic method.Firstly,p-nitrotoluene and sodium polysulfide were reacted with ethyl alcohol absolute as organic solvent and N,N-dimethylacetamide(DMA)as amine catalyst to form p-aminobenzaldehyde,and the best n(DMA)∶n(p-nitrotoluene)=3∶13 was obtained,herein,p-nitrotoluene dosage 25 g(0.18 mol),the same below.Then,p-aminobenzaldehyde reacted with aniline and hydrochloric acid under the catalysis of polyethylene glycol 400(PEG-400)to produce crude parafuchsin.The effects of material ratio,reaction temperature and reaction time on the yield of crude parafuchsin were investigated.The results showed that n(PEG-400)∶n(p-nitrotoluene)=2∶300,n(p-nitrotoluene)∶n(aniline)∶n(hydrochloric acid)=1∶5.9∶2.8,reaction temperature of 110℃and reaction time of 4 h,the crude product yield of parafuchsin was 85.6%.Finally,the effects of distillation temperature and time on the mass fraction of parafuchsin were investigated.It was found that the mass fraction of parafuchsin reached 91.3%after distillation at 130℃for 3 h.The wastewater from parafuchsin production was mainly aniline,and the recovery rate of aniline reached 89.3%after rectification.

关 键 词：副品红 胺基催化剂 醇基催化剂 水共沸精馏 工艺改进 精细化工中间体 

分 类 号：TQ246.31[化学工程—有机化工] X78[环境科学与工程—环境工程]