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CAS号 [96-93-5] 生产工艺 2-氨基-6-硝基苯酚-4-磺酸

CAS [96-93-5] 生产工艺  2-氨基-6-硝基苯酚-4-磺酸

CAS:Benzenesulfonic acid,3-amino-4-hydroxy-5-nitro-参考文献:Beil.14,816; E1,746; E2,488.

用途: 酸性橙72。酸性红214。酸性蓝184。酸性绿45。酸性棕122。直接蓝184。媒介橙35。媒介红67。

媒介棕22, 30。媒介黑15, 51。

生产工艺参考文献: 以下按本人手头资料整理如下:反应类别: 硝化。

BIOS 1153, 232-233.=胶卷PB 85687 6-Nitro-2-aminophenol-4-sulphonic acid. (Leverkusen). 英国人译自德文。抄录如下。

反应式: 本人有加注,译者未说明译自哪个德文原件。经核对,本译文是摘译自PB 25623, 235-237.的德文原件。
 

Outline:  2-Aminophenol-4-sulphonic acid is nitrated with mixed acid O in a mixture of H2SO4 and Oleum.

Plant:  1  3000 l. cast iron nitration vessel, fitted with lead coils and brine cooling. 1 8000 l. Montejus.

1 Filter press; rubber covered plates and frames, 1.2 x 1.2 m.

Materials: 638 kg. 2-Aminophenol-4-sulphonic acid ≌ 220 kg. NaNO2. 1650 kg. H2SO4 98%.

500 kg. Oleum 26%. 610 kg. Mixed acid O (33% HNO3, 67% H2SO4). ≌ 201 kg. HNO3 = 101% theory.

Process:

The nitration vessel is charged with 1650 kg. of 98% sulphuric acid and 500 kg. of 26% oleum, followed at 10-200C. by 638 kg. of 2-aminophenol-4-sulphonic acid. The 2-aminophenol4-sulphonic acid should have a strength equivalent to approx. 34% NaNO2 and should be free from salt. After the addition, which occupies 2 hours, it is stirred for a further 2 hours.

After this, and during 12 hours, the mixed acid (610 kg.) is run in at 0-20C. Speed of agitation45 r.p.m. It is stirred a further 1 hour and thenrun to a vat containing 4,800 l. of water. The temperature is kept below 150C. by means of the cooling coil. It is further cooled to 50C. and filtered via the Montejus through the press with good air pressure.

Yield: 775 kg. 81% theory as bright yellow plates.

细田豊。《理论制造染料化学》1957年。P. 479. 译自PB 85687. 6-ニトロ-2-アミノフエノ--4-スルホン酸 抄录如下。

    98%硫酸1650 kg + 26%发烟硫酸500 kgに10-2002-アミノフエノ-ル-4-スルホン酸638 kg (NaNO2 220 kg) を2 hて加え,2 h 搅拌,混酸(33% HNO3,67% H2SO4)610 kgを0-20 12 hて加え1 h搅拌,水4.8 m3に150以下て排出,50滤過する。775 kg,收率81% 

张澍声。《精细化工中间体工业生产技术》 1996年。P. 82.  译自BIOS 1153, 233, 6-硝基-2-氨基苯酚-4-毫升 抄录如下。

在3000 L铸铁硝化锅中加入1650 kg 98% 硫酸和500 kg 26% 发烟硫酸,然后在10-200C加入638 kg 2-氨基苯酚-4-磺酸,相 当于220 kg NaNO2,并且不含盐,约2小时加完,再搅拌2小时。

然后在0-20C于12小时内加入混酸O (33% 硝酸,67% 硫酸,硝酸为理论量的101%),搅拌速度45 转/分。再搅拌1小时,

然后流入装有4800 L水的桶中,通过冷却保持温度低于150C。再冷却到50C,压滤,得到775 kg 6-硝基-2-氨基苯酚-4-磺酸的亮黄

色片状结晶产品。收率81% 

PB 25623, 235-237. 6-Nitro-2-aminophenol-4-sulfonic acid = Nitraminzsaeure SF. 德文生产工艺原件。未抄录。

本胶卷,中科院收藏编号Mo 7657, 上海染料研究所为放大复印本(由中科院复制)。

加注: 从德文原件(未抄录),英国人摘译文,日本人再摘译到国内摘译文,抄录仅供读者参考! 

陈忠源  2017年6月22日           于 无锡   明辉国际。



文章作者:陈忠源