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C.I. 酸性橙33 = C.I.酸性橙95 (C.I. 24780) 生产工艺 CAS号 [6507-77-3]

C.I. 酸性橙33 = C.I.酸性橙95 (C.I. 24780) 生产工艺  CAS号 [6507-77-3]

CAS名:  1,3-Naphthalenedisulfonic acid, 7-hydroxy-8-[[4-1-[(4-hydroxyphenyl)azo]phenyl]cyclohexyl]phenyl]--azo]-,  disodium salt. 发明者:  R. Schuele and E. Korten 1928年

生产工艺文献：

BIOS 1548, 45.  (= 胶卷PB 85593)  Supranol Orange GS. （Leverkusen）. 英国人摘译自德文。 抄录如下。

反应式: 本人有加注。本工艺未指明译自哪个PB报告？

à  (1) 2-Naphthol-6:8-disulphonic acid

4:4’-Diaminodiphenyl-1:1’-cyclohexane à à  (2)  Phenol.

50 kg. Nitrite 4:4’-Diaminodiphenyl-1:1’-cycloxane (M. 266 = 138 nitrite) and 180 l. HCl 19.50Be’ are charged with good stirring into 700 l. water at 50-600C. When solution is complete, cool to 00C. with ice and tetrazotise with 50 kg. NaNO2 as 30% solution.

31 kg. Nitrite 2-naphthol-6:8-disulphonic acid (M. 304) as Potassium Salt is charged into a solution of 120 kg. soda ash in 650 l. water at 350C. When solution is complete, cool to 00C. with Ice.

Run the tetrazo into the coupling vat, add 750 kg. salt and, ready for the first coupling, a solution of 45 kg. soda ash in 200 l. water. Then run in the potassium salt solution of 2-naphthol-6:8-disulphonic acid over 11/2 – 2 hours. Add slowly 1,500 kg. salt to ensure that the monoazo dyestuff is precipitated. Stir 4 hours at a temperature of 1-30C. when the first coupling is complete as shown by absence of tetrazo.

27 kg. Nitite Phenol (M. 94) is dissolved in 550 l. water at 850C. and the solution cooled with ice to 50C. Add this solution to the first coupling and stir 10 hours. Warm to 200C. and maintain this temperature for 1 hour and then warm to 350C. for 1 hour,  Filter.

The dyestuff paste is dissolved in 4,400 l. water at 80-900C. Add 40 kg. chalk and stir for 1 hour at 80-900C.

Filter through a filter press into a second vat. Salt with 25% salt at 60-650C. maintaining good stirring during the addition.

Filter. Dry in a Tunnel stove at 50-550C.

Standardise with 2% Soda Ash and the remainder Glauber’s Salt.   Yield = 380 kg. dry = 550 kg. Type.

日文译文。细田豊《理论制造染料化学》1957年。 P. 581-2.  请见原书。

PB 74025, 1183. Supranolorange GS. 德文生产工艺。 未抄录。

PB 82232, 151. Supranolorange GS. 1946年。德文生产工艺。2美元。未抄录。

天津染料工业汇编。136-8（1980）

    1. 重氮化: 将100% 4,4’-二氨基二苯环己烷盐酸盐203.4公斤，加入重氮罐中放水3000升，开动搅拌加入100%盐酸54。75公斤，搅拌至4,4’-二氨基二苯环己烷盐酸盐完全溶解。用制冷盐水降温至00C 以下，在1小时内加入亚硝酸钠100%84.12公斤，进行重氮化反应，温度控制在0-50C, 终点控制碘化钾淀粉试纸变蓝。

2. 一步偶合：将100%G盐335公斤，碱面180公斤，加入化料罐，加水至2700升，搅拌溶透，温度10-150C备用。将重氮液放入偶合罐，开动搅拌加盐900公斤，再加入78公斤碱（碱要加快，以防沫）然后将G盐碱液细流加入用2-2.5小时加完，

在G盐加入一半时，开始陆续加入1300公斤盐，与G盐同时加完，其pH 为8，温度为100C.  搅拌1小时后加碱180公斤，调pH 至9，然后搅拌至重氮物消失（约用4小时）温度100C.

    3. 二步偶合：将100%苯酚39.5公斤，加水100公斤，化成乳液，细流加入偶合罐内，搅拌4小时后用1小时升温至350C,再搅拌3小时，然后进行过滤，烘干。

染料工业 1975,1, 57. 酸性橙GS 扩大试验。染料工业 1977,5,11-13. 酸性橙GS试验总结 。

陈忠源  2016年9月23日    于 无锡  明辉国际。




文章作者：陈忠源