C.I.颜料红163 (c.I. 12455) 生产工艺 CAS号: [6410-37-3]
CAS名： 2-Naphthalenecarboxamide, N-(2,3-dimethylphenyl)-3-hydroxy-4-[[2-methoxy-5-[(phenylmethyl)sul-
-fonnyl]phenyl]azo]-
发明者： I.G.
生产工艺文献： BIOS 1661, 97 (= PB 91693, 97). Lithol fast Red Toner R. 德文摘要英译文，二手货。未收藏。
FIAT 1313,III, 488-491. 德文工艺英译文。1942年12月1日。 抄录如下。
PB 74067, 637-639. Litholechtrottoner R 未注明年份。 1.5美元。未抄录。
PB 74123, 5878-5880. Litholechtrottoner R 1945年。德文原生产工艺规程。未抄录。
PB 74744. Le – ku. 品种卡片。未抄录。
项 斌 高建荣 编：化工产品手册，第五版“颜料” 2008年。Bf 039. C.I. 颜料红163. P. 322-3.
化学工业出版社 出版： 中国化工产品大全，第四版“有机颜料” 2012年。Fo 0039. 同上。P. 800.
以上二书未注明资料来源，对照书中所述，应是译自FIAT 1313,III, 488-491. 抄录如下。
Lithol Fast Red Toner R Jan. 21, 1942. （注：译文按德文格式，我改动了。）
Trade Name: Litholechtrot toner R (Hoe.) - 这是德文。
Composition: 我改成反应式：
2-氨基-4-苄基磺酰基苯甲醚 à à 3-羟基-2’,3’-二甲基-2-萘甲酰苯胺 à C.I.颜料红163 (C.I. 12455)
Principal uses: Printing ink. Batch size: 0.3 mol Process: Diazo
800 l. H2O and 36.9 kg (译文，漏了) HCl (202 l. 5 N HCl) are run into diazo vat and heated to 250C (文中是750C，错了), then 83.1 kg (文中是83 kg) Orthosinsulfobenzyl (1-methoxy-3-aminophenyl-4-benzyl sulfone) are Added. The base dissolves very quickly. 1300 kg ice are added and temperature adjusted to 00C. To this is added immediately and rapidly under the suface 39.4 l. (文中是39.5 L) 40% NaNO2 solution (20.7 kg NaNO2 100%) Stirring is continued for 1 1/2 hrs (未译) and the temperature held at 00C. Reaction should be weak on starch KI paper (未译). Volume diazo is made to 2400 l. and temperature to 00C. 6 kg Carboraffin * is added and the diazo stirred for 1/4 hr. Agitation of the diazo is discontinued during coupling.
Coupling Component
1000 l. H2O and 105 l. 33% NaOH solution (47 kg NaOH) are heated to 850C. To this is added 96 kg meta-xylidide of BON and the temperature held at 80-850C for 10 minutes. 6 kg Kieselgur are added and the solution is clarified thru a press and filtrate run to the coupling vat. The solution vat is washed with 300 l. H2O thru the press. Volume in coupling vat is made to 2000 l. and 18 kg Igepon T ** Dissolved in 200 l H2O are added. (译文不清，不是膏状物). The solution is cooled with ±1600 kg ice to 20C and precipitated with 250 l. HCl 5 N over 1/4 hr. under agitation. Reaction definite on Congo Red. 200 kg Sodium acetate crystals are then added.
Coupling
The precipitate of the arylide is heated to 420C and at this temperature the diazo solution is run in under the surface, after first clarifying thru a filter press – over 21/2 hrs.(不是2-2.5 h). The temperature is held at 420C. No excess diazo solution is permissible. The pigment is stirred for 15 minutes, filtered and washed 2 hrs. * Carboraffin = clarifying carbon 88 Igepon T = CAS No.:[137-20-2]
陈忠源 2016年4月5日。