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。