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CAS号 [98-33-9] 生产工艺 2-氨基甲苯-5-磺酸

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CAS号 [98-33-9] 生产工艺 2-氨基甲苯-5-磺酸 
 

	CAS名:  Benzenesulfonic acid, 4-amino-3-methyl-, 参考文献: Beil. 14, 726; E2, 448; E3, 2216; E4, 2776. 
 

	用途: 酸性橙8。酸性棕3, 143, 425。直接橙118。直接红24, 62, 85。媒介黄60。
 

	生产工艺参考文献: 
 

	BIOS 986, 427-428. (=胶卷PB 77764) o-Toluidine-5-sulphonic acid
(o-Toluidinsaeure) I.G.
Ludwigshafen. 英国人译自德文。 
 

	反应式:  本人有加注，译者未说明译自哪个德文原件。 
<img src="http://www.陈忠源化学文库.cn//chenzhongyuan/Upload/ArticlePicture/QQ图片20170309095805.png" alt="" /> 
 

	o-Toluidine is charged to 98% sulphuric acid with
initial cooling. The temperature is raised to 1500C and water and
excess o-toluidine distilled off. The sulphate is then heated in a static baker to 235-2550C. The
baker product is purified by solution in caustic soda in the presence of chalk,
treated with soda and screened after the addition of carboraffin. A sodium salt
paste brand was also prepared by allowing this solution to crystallize, the
mother liquors also being utilized as sodium salt liquor.
 

	Yield 98.6% crude.  97% sodium salt total liquor from crude.  53% from crude plus 44% liquor (sodium salt
paste)
 

	Materials usage per 1,000 kg. of 
 

	Crude: 580 kg. o-Toluidine. 590 kg. 98% sulphuric acid per 1,000 kg.
total liquor. 1,030 kg. crude.
 

	270 kg. caustic soda 100%. 130 kg. soda. 38 kg. carboraffin.
 

	Sodium salt paste:1,30 kg.
crude. 260 kg. caustic soda 100%. 20 kg. soda. 45 kg.carboraffin.
 

	The average monthly production in tones for the years
1938 – 1944 inclusive were:-
 

	Crude: 5.6, 8, 10.1, 9.6, nil, 2.5,
nil. Sodium salt total liquor: 5.9, 6.2, 8.1, 7.4, 0.4, 1.1, 0.6. Sodium salt paste: 0.3, 0.5, 略。 
 

	BIOS 1153, 173-174. (=胶卷PB 85687) o-Toluidine-5-sulphonic acid. (Ludwigshafen) 英国人译自德文。抄录如下。 
 

	Plant: 设备: 本译文比上面详细，仍未说明译自哪个德文原件。
 

	1  Cast iron agitated vessel fitted with reflux
condenser, capacity 3 cu.m. Blade type agitator 28 r.p.m., driven by motor 2.2
kw. Fitted with jacket for heating and cooling.
 

	1  Cast iron measuring vessel for sulphuric
acid. 1  Oven fitted with gas heating.
 

	Materials: Sulphuric acid
98%. o-Toluidine.
 

	Process: 
 

	    The agitated vessel is charged with 1495
kg. of 98% H2SO4 which is then diluted with 100 l. of
water with cooling. Slowly 1542 kg. of
 

	o-toluidine are then added. The
temperature is raised to 1500C., at which temperature water and
toluidine reflux.  The  resulting
 

	o-toluidine sulphate is put on
to trays, 12-13 trays being required per batch.
 

	    The trays are put into the gas heated oven
and heated for 11/4 – 11/2 hours at
235-2550C., the heating being by means of hot air
 

	From a Schilde burner. The hot air is drawn out and recycled to keep a
constant temperature. After 11/4 – 11/2 hours the material  is
 

	drawn out, cooled and stored for
completion of the whole batch, which is then ground.
 

	    Yield:  172% by wt. from o-toluidine = 98.5%
theory.   Strength:  95% as
o-toluidine sulphuric acid.
 

	    The crude product can be purified as
described in BIOS Final Report No. 986 (page 441) to give total liquor sodium
salt or isolated
 

	Sodium salt paste. 
 

	中文译文。张澍声《精细化工中间体工业生产技术》 1996年。P.41.2-氨基甲苯-5-磺酸。译自BIOS 1153/ 986.  抄录如下。 
 

	    在3000 L铸铁搅拌釜中加入1495 kg 98% 硫酸，再在冷却下用100 L水稀释，缓缓加入1542 kg邻甲苯胺，温度升至1500C,
 

	在此温度下水和邻甲苯胺沸腾回流。生成的邻甲苯胺硫酸盐放入盘中，每锅需要12-13个盘。
 

	    盘送进煤气加热炉中，在235-2550C加热75-90分钟，加热是用Schilde燃烧器来的热空气进行，热空气出来后再循环进入
 

	燃烧器，以保持恒定温度。75-90分钟后取出物料，冷却，粉碎。  收率98.5%。 邻甲苯胺-5-磺酸含量95%
 

	    精制:  在CaCO3存在下将2-氨基甲苯-5-磺酸溶解于Na2CO3水溶液，加入活性炭后进行过滤，滤液是磺酸钠浆状物，直接应
 

	用，其收率为97%。或者将浆状物结晶，母液仍以钠盐应用，结晶为53%，母液为44%，总收率97%。
 

	PB 25602, 847-851.  No. 4105-1 
“o-Toluidinsaeure”.  Na-salt
in solution 未抄录。 
 

	PB 25602, 852-854.  No. 4105-2 
“o-Toluidinsaeure”.  Na-salt
in solid. 未抄录。 
 

	PB 25602, 855-858.  No. 4105-o 
“o-Toluidinsaeure”.  Crude.  未抄录。 
 

	    以上说明德文生产工艺原件共有12页。 
 

	PB 25624, 1103-1105.   o-Toluidinsaeure. 未抄录。   
 

	PB 70063, 304-305. Manufacture of 2-toluidine-5-sulfonic
acid. By Heinze. 1945年9月18日。德文生产工艺摘要。  未抄录。 
 

	PB 70063, 306-307, Manufacture of sodium
2-toluidine-5-sulfate. By Heinze 1945年9月10日。同上。未抄录。 
 

	PB 73616, 1505-1506.  Sodium 2-toluidine-5-sulfonate. 未抄录。 
 

	加注: 
 

	    从上面抄录的资料可以看出，同一资料，译者不同，所叙述的内容也就有不同，因为译者未说明资料
 

	来源，所以很难说明其完整性和可靠性。
 

	    PB 25602, 847-858. 共有12页，国内有胶卷，上海染料研究所是复印件，读者感兴趣，可以看一下。
 

	    PB 70063. 上海图书馆有收藏，其编号是 F-643。 PB 73616. 只有北京有收藏。 
 

	今天是三八妇女节，祝女读者节日快乐！ 
 

	陈忠源  2017年3月8日        于 无锡   明辉国际
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