CAS号 [3771-14-0] 生产工艺。  1-萘酚-3-磺酸

CAS名：2-Naphthalenesulfonic acid, 4-hydoxy-     历史参考文献：Beil. 11. 待检索。

用途：酸性红431。 直接蓝127, 138。 LookChem网登录生产与经营单位5家，钠盐9家。 反应类别：氨基加压水解。

BIOS 1152, 13-14.（=胶卷PB 81027）。  1-Naphthol-3-sulphonic acid. (Leverkusen).  英国人译自德文，无资料来源。

反应式：本人有加注，德文原件未抄录。

Plant details:  设备： 

1.  Homogeneously lead-lined steel autoclave, lined with “Maxielsteinen”(Maxiel-tiles) of 65 mm. thickness.  Hoescht Cement, S.W. 10.

Capacity, 5,400 l.  For 12 atm. pressure.  Copper stirrer.

2.  Filter presses and Montejus.

Materials:  投料量：1-Naphthylamine-3-sulphonic acid (in paste form) ≈275 kg. as 100% NaNO2.  Equivalent H2SO4 by analysis.

Hydrolysis:  水解：

    1-Naphthylamine-3-sulphonic acid paste, equivalent to 275 kg. NaNO2, is mixed with 500 l. of water.  A titration is carried out to determine the amount of free H2SO4 and then sufficient H2SO4 of 400Be’ is added to bring the H2SO4 up to 20 kg. at 100%.  High pressure steam is now introduced directly to the closed vessel which raises the pressure to 10 atm. inside and this pressure in maintained for 20-25 hours.

Test: 250 cc. of the mixture from the kettle is made up to 1,000 cc. of this, 250 cc. is neutralized with soda and coupled with diazobenzene to determine the coupling value.  Another 500 cc. is acidified further and diazotized.  It should not show more than 1.5 g. NaNO2 per 100 g. NaNO2 of the 1-naphthylamine-3-sulphonic acid.

After the test has been found satisfactory, the kettle is cooled to 90℃. and the excess H2SO4 neutralized with soda ash.  The neutral solution is cleared with activated charcoal and filtered.  The solution is taken directly by truck to the azo shed.

Yield as solution = 86-88% theory.

Isolation: 离析：

If this is required, it is treated with salt.  For 1,000 l. clear neutral solution 280-300 kg. of salt are required.  Cooled to 25℃. and filter off.  The press cake is washed with conc. 230Be’ salt until the filtrate becomes light yellow in colour.  The press cake can be directly after hydraulic pressing.  Dry and grind.

Yield after isolation:  82-84% of theory.

张澍声 《精细化工中间体工业生产技术》。（染料工业）编辑部 出版。 1996年。P.196.  1-萘酚-3-磺酸。译自BIOS 1152, 13.

相当于275 kg亚硝酸钠量的1-萘胺-3-磺酸滤饼与500 L水混合，先分析其中游离硫酸含量，然后加入足够的48% 硫酸，使总酸量达20 kg 100% 硫酸。向密闭的压力锅中通高压直接蒸汽，使内压达10巴，在此压力保持20-25小时。

取样分析：取样250毫升，稀释至1000毫升，取出250毫升，用碳酸钠中和后，用苯胺重氮盐偶合，测定其偶合值。另取500毫升酸化后也重氮化。对于每100克样品，其亚硝酸钠硝化量应不大于1.5克。

取样测试合格后，冷却到90℃，用碳酸钠中和硫酸，加活性炭脱色，过滤，溶液装槽车直接制备偶氮染料。收率86-88%。

离析：

如需分离，每1000 L中性清液应加280-300 kg食盐，冷却到25℃，过滤，滤饼用比重1.19的食盐水洗涤，直至滤液变为浅黄色，再经干燥，研磨。分离后的收率82-84%。

何岩彬 主编 《染料品种大全》。沈阳出版社 出版。2018年。 P. 1924.  1-萘酚-3-磺酸。

陈忠源 2019年11月22日星期五。