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| C.I. 溶剂黄14=C.I. 分散黄97（C.I. 12055）生产工艺。 CAS号[842-07-9] |
C.I. 溶剂黄14=C.I. 分散黄97（C.I. 12055）生产工艺。 CAS号[842-07-9]
CAS名：2-Naphthalenol, 1-(phenylazo)-
Beil. 16, 162; E1, 254; E2, 70; E3, 129; E4, 228.
原版Colour Index: 发明者：C. Liebermann. 1883年。生产工艺参考文献：FIAT 764 – Sudanorange R.
用途：织物染色，油品，树脂，塑料，木器着色。 LookChem网登录生产与经营单位105家。
FIAT 1313, II, 258.（=胶卷PB 85172）。 Sudan Orange R. 美国人译自德文，反应式本人有加注，如下：
2 mole charge size: Aniline à β-naphthol. 2公斤分子投料量：苯胺重氮化与2-萘酚偶合。（国内未见有译文！）
In diazo tub charge 1000 l. water and 870 kg. of 120Be’ hydrochloric
acid. The solution is cooled to 00 and
188 kg. of aniline is added from a weighing tank. By the addition of ice, the solution is
cooled to -2℃. and at this temperature is dusted in 140
kg. of solid sodium nitrite during which the temperature is maintained below 3℃. For this diazotization 2700
kg. of ice is used. The solution is
agitated for an additional 2 hours maintaining a distinct excess of
nitrite. The final diazo solution is
made up to 7000 l. and the excess nitrite is destroyed by the same method as is
used for Sudan Yellow 3G and allowed to stir during the following 3 hours. （这是苯胺重氮化，[100-34-5]）。
In the coupling tub is charged 3000 l. of water and 405 kg. of 380Be’
caustic soda solution and in this is dissolved 300 kg. of β-naphthol at room
temperature.（这是制备2-萘酚钠盐 [875-83-2]）。 The naphthol solution at the beginning of the coupling is cooled to 00
by the addition of approximately 1200 kg. of ice and then diluted to 5500
l. During the addition of the above
diazo solution to 5500 l. During the
addition of the above diazo solution, the temperature is allowed to rise
somewhat so that no further adition of ice is required. （这是偶合反应）。
After the addition of the diazo solution, the combination is stirred
for 0.5 hour; thereupon is added an additional 50 kg. of 380Be’ caustic soda
solution（= 57 kg. 350Be’ caustic soda solution）。 The mixture is then heated to 30℃. and agitated one to two hours or overnight. It is filtered in a press, washed until
neutral and blown dry. The color is
dried at 60℃.
Yield : 2500 kg. presscake, 500 kg. dry.
PB 73067, 6751-6753.
Sudanorange R. 德文生产工艺，未抄录。
PB 74027, 3497-3498.
Sudanorange R. 德文生产工艺，为不同年份，未抄录。
上海市有机化学工业公司 《染料生产工艺汇编》。1976年。P. 524-525.
油溶黄。 操作方法。
1. 重氮化：[100-34-5]。
在重氮桶内放水1,800升，盐酸100% 160.6公斤，搅拌中将100% 苯胺160.8公斤徐徐加入，再降温至3 – 4℃，体积3,000升，然后将100% 亚硝酸钠（配成30% 的溶液）119.2公斤于30分钟内均匀加入重氮桶进行重氮反应，终点刚果红试纸呈蓝色，碘淀粉试纸呈淡蓝色不退，搅拌20分钟，备偶合用。
2. 乙萘酚钠盐的制备：[875-83-2]。
在溶解桶内放水1,500升，加液碱100% 116.1公斤，磺化蓖麻油100% 15.6公斤，升温至60℃，在搅拌下加入100% 乙萘酚245.7公斤，使之完全溶解，然后放入偶合桶中，调整体积6,500升，温度20℃备偶合用。
3. 偶合：[842-07-9]。
在搅拌下将反应好的重氮盐液于30分钟平均流入偶合液中进行反应，终点pH值为8.5 – 9，乙萘酚微过量，然后搅拌1小时，徐徐升温至70℃，过滤。然后用自来水漂洗，终点以漂洗液用1% 硝酸银溶液测定与自来水相比近似即可，滤饼在70℃烘干。 得量：450公斤。
【加注】成品用乙醇为溶剂，可用苯为展开剂，可以看出主产品的斑点。
何岩彬 主编《染料品种大全》。沈阳出版社 出版。2018年。P. 780. C.I. 分散黄97；P. 1257. C.I. 溶剂黄14.
陈忠源 2020年10月20日星期二。
文章作者：陈忠源 |
