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苯并咪唑酮-二噁嗪颜料(P.B.80)的合成及其颜料化(二)
引用本文:张合杰,张东江,刘建胜.苯并咪唑酮-二噁嗪颜料(P.B.80)的合成及其颜料化(二)[J].上海染料,2010,38(1):25-29.
作者姓名:张合杰  张东江  刘建胜
作者单位:上海捷虹颜料化工有限公司
摘    要:该文以2,4-二硝基氯苯(MZ)为起始原料与乙胺盐酸盐在无水乙醇中缩舍得到2,4-二硝基-N-乙基苯胺(MZ-1)。MZ—1与硫化钠在热水中还原为N1-乙基-4一硝基苯一1,2二胺(MZ-2)。MZ-2同尿素经固相缩合得到了1-乙基-5-硝基-1H-苯并d]咪唑-2(3H)-酮(MZ-3)。以MZ-3为起始原料,经铁粉还原得到了5-氨基-1-乙基-1H-苯并d]d咪唑-2(3H)-酮(MZ-4)。它们的结构均通过质谱、核磁共振等手段加以表征,纯度用高效液相色谱(HPLC)进行了测定。通过MZ一4与四氯苯醌在二氯苯溶剂中缩合,然后在浓硫酸中在闭环剂的作用下得到了苯并咪唑酮一二噁嗪颜料(P.B.80)粗品,经过颜料化得到了精品颜料。

关 键 词:苯并咪唑酮  二嗯嗪(咔唑)  颜料  颜料化

Synthesis & Finishing of Bezimidazolone-dioxazine Pigment(P.B.80)(Ⅱ)
ZHANG He-jie,ZHANG Dong-jiang,LIU Jian-sheng.Synthesis & Finishing of Bezimidazolone-dioxazine Pigment(P.B.80)(Ⅱ)[J].Shanghai Dyestuffs,2010,38(1):25-29.
Authors:ZHANG He-jie  ZHANG Dong-jiang  LIU Jian-sheng
Affiliation:ZHANG He-jie ZHANG Dong-jiang LIU Jian-sheng
Abstract:In this paper, the starting material of 2,4--dinitrochlorobenzene (MZ) in the solvent of ethanol was treated with ethylamine hydrochloride to prepare 2,4-dinitro-N-ethylaniline (MZ- 1 ). MZ- 1 was then reduced with sodium sulfide in the hot water into N l - ethyl - 4 - nitrophenyl-1,2-diamine (MZ-2) . MZ-2 further reacted with urea in the solid- phase to result in 1 -ethyl-5- nitro-- 1 H-benzo d] imidazole-2 (3H) -one (MZ -3 ) . Finally, the intermediate of bezimidazolone- dioxazine pigment, 5- amino- 1- ethyl- 1Hbenzo d] imidazole- 2 (3H) - one (MZ- 4) , was obtained with the reduction of MZ- 3 using iron powder as reducing agent. The crude pigment of benzimidazolone-dioxazine (P.B. 80) was prepared via two steps: ①by the condensation of MZ-4 with tetrachlorobenzoquinone (chloranil) in the solvent of dichlorobenzene; ②ring-closed in concentrated sulfuric acid. Also the pigment finishing process was studied. All chemical structures of intermediates and the targent pigment were chacterized by 1H NMR, MS, and HPLC.
Keywords:benzimidazolone dioxazine (carbazole) pigments finishing
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