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CAS号 [19479-88-0] 生产工艺。 5-亚磺基水杨酸

CAS号 [19479-88-0] 生产工艺。   5-亚磺基水杨酸

CAS名：Benzoic acid, 2-hydroxy-5-sulfino-    历史参考文献：待检索。

用途：有机合成。 LookChem网登录生产与经营单位2家。 反应类别：磺酰氯还原。

BIOS 1153, 256-257.（=胶卷PB 85687）。 Salicylsulphinic acid (5-Sulphinosalicylic acid).  英国人译自德文，无资料来源。

反应式：本人有加注。德文原件 Salicylsulfinsäure 暂未找到。

Outline:  Salicyl-5-sulphonyl chloride is reduced with zinc dust. 

Materials: 426 kg. 100% Salicyl-5sulphonyl chloride.。   160 kg. Sodium acetate.。   200 kg. Zinc dust.。   600 kg. Soda ash.。   3,000 kg. Ice.。

Plant:  1  Iron vat of 10,000 l. capacity.。   1  Iron Montejus of 80,000 l. capacity with scraper type agitator.

       1  Screening press.。   1  Iron vat of 10,000 l. capacity fitted with copper coil.。

Process: 操作步骤：

The vat is charged with 1,000 l. of water and 1,900 kg. of finely crushed ice followed by 426 kg. of 100% salicylsulphonyl chloride.  In addition, 160 kg. of sodium acetate are added and a further 600 kg. of ice.  The temperature is reduced to 40℃.（抄注：译文有错！请看美国人的译文）。

During half an hour 200 kg. of zinc dust are added slowly together with 500 kg. of ice.  The batch is stirred for 6 hours after which the volume is brought up to 6,000 l.  The whole is now stirred for 8 hours and then sufficient soda ash is added to produce a weak Congo acid reaction.  Direct steam heating is now applied to raise the temperature to 20-30℃. after which soda ash is again added to bring alkaline to phenolphthalein paper.  At the same time it is heated to 93-95℃. with direct steam.

The batch is then run down to the Montejus and filtered through the press to remove zinc carbonate.  The liquors are returned to the vat containing the copper coil and concentrated down to 4,500 l. with steam.  Yield: 90% theory as total liquor.

 

FIAT 1313, 76-77.（=胶卷PB 85172）。 3-Carboxy-4-hydroxybenzenesulfinic acid (Salicylsulfinsäure). (I.G. Leverkusen). 美国人的译文。

Apparatus:  1 – brick-lined cast iron vessel, 10000 l.。   1 – iron blow case (monojo) 8000 l.。  1 – residue press.。

           1 – brick-lined vessel with copper coil, 10000 l.

Materials:  1 – 426 kg. 100% salylsulfochlorid (3-carboxy-4-hydroxybenzenesulfone chloride).。   2 – 160 kg Nacl.。、

           3 – 200 kg. Zinc dust.。   4 – 600 kg Na2CO3.。    5 – 3000 kg. ice.。

Procedure: 操作步骤：

Into the brick-lined vessel charge 1000 l. water and blow in 1900 kg. of very fine ice.  Add 426 kg. of (1).  Add (2) and 600 kg. ice.  Temperature, minus 4℃.  In 1/2 hour, add (3) and 500 kg. more ice.  Stir 6 hours and dilute to 6000 l.  Stir 8 hours longer.  Add (4) to make neutral to Congo.  Heat to 20-30℃. with direct steam and add (4) to make weakly alkaline on phenolphthalein.  At the same time heat to 93-95℃. with direct steam.  Put the charge in the Monjo and filter off ZnCO3 in press.  Liquor runs to tub with coil where it is evaporated to 4500 l.  Yield: 90% of theoretical.

 

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. 104.  水杨酸-5-亚磺酸。译自BIOS 1153,255.

1000 L铁锅中加入1000 L水和1900 kg碎冰，随后加入426 kg 100%水杨酸-5-磺酰氯。再加入160 kg醋酸钠和600 kg冰，温度降到40℃。（抄注：英文有错，所以译文也错了，请看美国人的译文 = Minus 4℃ = - 4℃.）。

0.5小时内缓缓加入200 kg锌粉和500 kg冰，反应物搅拌6小时，然后将体积充满至6000 L。再搅拌8小时，然后加入足够的碳酸钠，使对刚果红为弱酸性，用直接蒸汽加热，使温度达20-30℃，在加入碳酸钠，使对酚酞试纸为碱性，同时用直接蒸汽加热到93-95℃。

过滤除去碳酸锌，滤液浓缩至4500 L。收率90%，为溶液。

张大国 编 《精细有机单元反应合成技术手册》。化学工业出版社 出版。 2014年。

书中无此类单元反应，也无此化合物报导。 CAS大号：[19479-88-0] ，至少说明有人在使用或者在研究！

 

陈忠源 2020年2020年2月3日 – 2020年3月4日 上网。



文章作者：陈忠源