CAS号 [81-06-1] 生产工艺 - 1-萘胺-2-磺酸

CAS名：2-Naphthalenesulfonic acid, 1-amino-

用途：染料中间体，用于C.I.直接紫11；C.I.活性红250.  LookChem网登录生产与经营单位7家。 反应式：如下。

BIOS 986, 424.（=胶卷PB 77764）。 α-Naphthylamine sulphonic acid (mixture) (α-Naphtaminsäure V). 英国人译自德文。 

I.G. Ludwigshafen:  α-Naphthylamine is charged into 98% sulphuric acid at 70℃, the solution cooled to 45℃, 24% oleum added and the sulphonation finished at 100℃.  The sulphonation mass is diluted with water and screened at 25 – 30℃.   Yield:  88.4% theory.

The materials usage per 1,000 kg of product is :

725 kg.  α-naphthylamine,  

1,445 kg. 98% sulphuric acid,  

525 kg.  24% sulphuric acid.

The average monthly production for the years 1938 – 1944 inclusive was 3.8,  1.3,  3.6,  nil,  1.3,  3.3,  nil tones.

BIOS 1152, 27-28.（=胶卷PB 81027）。 1-Naphthylamine-2-sulphonic acid. (Leverkusen).  英国人译自德文，

Plant/设备：

1. 16000 l. vacuum baker.  

2. 16000 l. iron agitated vessels.  

3. 13000 l. tiled agitated vats.

4. 6 sq.m. tiled box nutsches  

5. 10000 l. tiled blow-eggs.

Process/操作步骤：Sodium naphthionate (522 kg. ≈143 kg. NaNO2) is charged into the previously heated baker drum, placed under vacuum and heated up to 2040.  After 8 hours the batch is finished.  The baker is allowed to stand for 4 hours to cool and then emptied.

Each of two batches of crude dry product (ca. 1000 kg. ≈ ca. 272 kg. NaNO2) are charged into 5000 l. of cold water, and 5 kg. of soda added.  The solution is heated slowly to 800, stirred 10hours at this temperature, salted with 250 kg. of rock salt, cooled, filtered, and washed with a little water.

1500 kg. of this paste, corresponding to 190 kg. NaNO2, are heated with 9000 l. of water and direct steam to 1000, and stirred at this temperature until all has gone into solution.  Then 450 l. of milk of lime (= 100 kg. CaO) are charged, the mixture is boiled for 2 hours, filtered (press) and the clear solution decomposed with 70 kg. of soda.  100 kg. of carbon are added, the batch screened, and the filtrate salted with 650 kg of NaCl and cooled to 180.

The carbon residue is boiled up, filtered and the liquor used as charge for the next batch. The cooled batch is nutsched and pulled as dry as possible.  Yield: 900 kg. moist paste = 132 kg. NaNO₂. The chalk residue from 3 batches is slurried with 7000 l. of hot water, made acid with 600 l. of hydrochloric acid and then precipitated with 500 kg. of soda.  100 kg. of carboraffin are added, the batch screened and the clear solution salted with 650 kg. of salt.  The product is filtered and pulled as dry as possible.  Yield:  600 kg  moist paste ≈111 kg NaNO₂.

Note:  It is not clear whether the 1500 kg paste referred to for the purification is the entire batch.  If it is, the final overall yield from 2 batches is equivalent to (132 + 111/3) = 169 kg. NaNO₂.  This represents 59% 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. 195. 1-萘胺-2-磺酸，译自BIOS 1152, 27. ℃

在16 m3真空烘焙釜中加入522 kg 4-氨基萘-1-磺酸钠（相当于143 kg NaNO2，真空釜经预热），抽真空，加热到204℃，8小时后反应完毕，烘焙釜放冷4小时，然后倾出。

两批烘焙釜的干的粗品约1000 kg（相当于272 kg NaNO2）加到5000 L冷水中，加入5 kg 碳酸钠溶液缓缓加热到80℃，在此温度搅拌10小时，用250 kg 食盐盐析，冷却，过滤，少量水洗涤。

1500 kg 该滤饼（相当于190 kg NaNO2）与9000 L水用直接蒸汽加热到100℃。在此温度搅拌至完全溶解。然后加入450 L石灰乳（相当于100 kg CaO），煮沸2小时，压滤。清滤液用70 kg Na2CO3转化为钠盐，加100 kg活性炭脱色，过滤，滤液用650 kg食盐盐析，并冷却到18℃。

活性炭滤渣煮沸，过滤，该滤液用于下批配料。 盐析后反应物抽滤至尽可能干，得900 kg湿滤饼，相当于132 kg NaNO2。

三批钙滤饼用7000 L热水打浆，用600 L盐酸酸化，然后用500 kg Na2CO3 沉淀。加入100 kg活性炭，反应物过滤，清溶液用650 kg食盐盐析，产品抽滤。得600 kg湿滤饼，相当于111 kg NaNO2。两者合计，相当于169 kg NaNO2，收率为59%。

何岩彬 主编《染料品种大全》。沈阳出版社 出版。2018年。P. 1930.  中文名称：1-氨基萘-2-磺酸。

【可合成的染料】C.I. 直接紫11；C.I. 活性红250.等，不再全部抄录。

陈忠源 2020年。/ 2021年6月17日星期四。