C.I. 媒介红19(C.I. 18735)生产工艺 CAS号[1934-24-3]
CAS名:Benzenesulfonic acid, 5-chloro-3-[(4,5-dihydro-3-methyl-5-oxo-1-phenyl-1H-pyrazol-4-yl)azo]-2-hydroxy-,
monosodium salt.
生产工艺文献:
BIOS 961, 42, 73. (=胶卷PB 60905) metachrome Red 5G, Palatine fast Red RN, Coupling, 英国人摘译自德文。未收藏。
BIOS 1548, 24-5. (=胶卷PB 85593) Palatin fast Red RN. Coupling. 英国人译自德文。抄录如下。
反应式:本人有加注。它摘译自PB 73561,195-7. 本文于原件比,有一些差错。
1. Coupling:
134 kg.
4-chloro-2-aminophenol-6-sulphonic acid (= 223.5 kg. dry at 60%) is stirred in 1,000 l. water and dissolved with 50 kg. caustic soda 50%. Add 180 l. 23% nitrite solution, adjust
with 800 kg. ice and water to a
volume of 2,800 l. at a temperature
of 50C. and diaotise by
adding 200 l. dilute HCl (M.
200). Temp. 7-90C. Vol. 3,000 l. Stir 2 hours maintaining an excess nitrite.
115 kg. at 100%
1-phenyl-3-methyl-5-pyrazolone (technical, strength 98-99%) is dissolved with 125 kg. caustic soda
50% in 500 l. water at 450C. Dilute with 1,500 l. water, add 80
kg. sodium bicarbonate and adjust with ice and water to a volume of 3,200 l. at a temperature of 120C.
220 l. β-salt solution (= 66 kg.β-salt 100%) (抄注:这是2-萘磺酸) is added to the diazo, stir 1/4 hour and then run slowly (德文是schnell)over 15 to 20
minutes into the pyrazolone solution. Vol. 6,200 l.
Approximately 15
minutes after addition of the diazo, a test sample spotted on filter paper
shows no diazo with alkaline resorcinol solution.
Stir 2 hours and
then add 800 kg. salt and stir
overnight. Filter next day – filtration taking approximately 10 hours.
Yield = approximately 1,100 kg. paste.
中文译文。张兆麟 张玉珍。《金属络合染料》1986年。 P. 118-9. 请见原书。
PB 25625, 984-6. Palatinechtrot
RN. Kupplung. 1940年1月。未抄录。
PB 73561, 1995-7. Palatinechtrot
RN. Kupplung. 1943年6月2日。已抄录。
PB 73607, 6913-6929 .(共17页) Metachromrot
5G. C.I. 媒介红19 生产工艺规程,德文。未抄录。
用途:
钠盐:CAS号 [1394-24-3] 是媒介红19.
酸式:CAS号 [25746-81-0], 它经铬络合可生产酸性红180;362.
加注:2-萘磺酸,是作为重氮盐的稳定剂使用。
知识就是力量!
陈忠源 2016年9月7日 于 无锡 明辉国际。