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CAS号 [84-67-3] 生产工艺。 2,2’-二甲基联苯胺

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CAS号 [84-67-3] 生产工艺。  2,2’-二甲基联苯胺
 

	CAS名：[1,1’-Biphenyl]-4,4’-diamine, 2,2’-dimethyl-      历史参考文献：Beil. 13, 255.
 

	用途：有机合成，染料：酸性黄68, 86。酸性橙49, 79。酸性红99, 111, 164, 173。酸性黑70。颜料黄70, 90。颜料红62。
 

	LookChem网登录生产与经营单位75家。  反应类别：还原，转位。
 

	BIOS 1153, 266-268.（=胶卷PB 85687）。 m-Tolidine sulphate.
(Leverkusen).  英国人译自德文，无资料来源。
 

	反应式：本人有加注，暂未找到德文原件。 
<img src="http://www.陈忠源化学文库.cn//chenzhongyuan/Upload/ArticlePicture/QQ图片20200327093405.png" alt="" /> 
 

	Plant:  设备； 
 

	2  Reducers, 1000 l. capacity.。  
2  Dezincing vats with brine
cooling.。   Disintegrator.。   Pump.。  
Nutsche with receiver.。
 

	Conversion vat with brine cooling.。  
Solution vat.。   Press with blow egg.。  
Crystallisation vat。   Nutsche and blow egg.。
 

	Process:  操作步骤：含还原和转位。
 

	The well-dried reduction vessel is charged with 230 kg. of
m-nitrotoluene (≈116 kg. NaNO2) and 2 l. of 50% caustic liquor, and heated to
80-850.  At this temperature 235 kg. of
zinc dust (90%) are added during 9-10 hours with the simultaneous addition of
17 l. of 50% caustic liquor.
 

	It is then tested for completion of reduction to the azo stage,
stirred a further 1 hour, and then diluted during 5 hours with 100 l. of
water.  At 78-800, 100 kg. of zinc dust
(90%) are added slowly.
 

	The hydrazo-toluene floats as a deep, yellow thick oil and on adding
water to the 3/4 mark this is changed to a homogeneous deep grey paste.  It is cooled to 200 and, without grinding,
blown to the desincing vat.
 

	Here it is cooled to 00 with brine and hydrochloric acid added until
faintly acid; temperature 5℃. 
Without stopping the agitator it is then pumped through a disintegrator
into a second vat, the temperature being maintained at 0℃. to prevent partial melting of the hydrazo-compound.  From here it is dropped to a nutsche and
casked up.  The nutsche must be cleaned
between each batch.
 

	The nutsche cake is charged into 1000 l. of water and 435 l. of 190Be’
hydrochloric acid cooled to 0℃.  The
temperature is held at 5-100 during the first day then allowed to rise to 150
during the second day.  When conversion
is complete the batch is run to the dissolving vat.
 

	The volume is adjusted to 4000 l. and solution effected by heating to
90-950.  Terrana and carbon are added,
and sulphide run in to precipitate lead. 
The batch is screened through a small press (nitro-cloth) and the
filtrate run to the crystallization vat into which are charged 300 kg. of
sodium sulphate at 80-850.  After 2 hours
the mass is cooled slowly to 200 and filtered. 
The mother liquor (after a test for completion of precipitation) is run
to drain.
 

	The crystallization vat is now charged with 3000 l. of water and 100
kg. of sodium sulphate and heated to 80-850. 
The tolidine sulphate is charged in, stirred 3 hours at 80-850, cooled
to 200 and filtered on anutsche,  The
mother liquor runs to drain.
 

	The residue from the screening operation is collected from 6-8 batches
and worked up as a separate batch.
 

	Yield: 70-78% theory.
 

	抄注：德文原件，按Leverkusen = Bayer ，应该有：A. 
Chemischer Teil: Konstitution, Einsatz, Ausbeute, Arbeitsweise（操作步骤）, Erfahrengen.
 

	B.  Technischer Teil:  Apparatur. 
 

	 
 

	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。未见有报导。
 

	 
 

	【单元反应】还原和转位。按CAS号，已上网有: [119-90-4] – 2019/5/24. [119-93-7] –
2019/6/11.
 

	 
 

	何岩彬 主编 《染料品种大全》。沈阳出版社 出版。 2018年。 P. 1994.  2,2’-二甲基联苯胺。只列有合成的染料。
 

	 
 

	陈忠源 2020年2月17日星期一。非常时期。 2020年3月26日星期四。
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