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C.I. 媒介红19(C.I. 18735)生产工艺 CAS号[1934-24-3]

C.I. 媒介红19C.I. 18735)生产工艺  CAS[1934-24-3]

CASBenzenesulfonic 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schnellover 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. 19401月。未抄录。

PB 73561, 1995-7. Palatinechtrot RN.  Kupplung. 194362日。已抄录。

PB 73607, 6913-6929 .(17Metachromrot 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。



文章作者:陈忠源