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C.I. 颜料红37 (C.I. 21205) 生产工艺

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C.I. 颜料红37 (C.I. 21205) 生产工艺  CAS号:[6883-91-6] 

	CAS名：3H-Pyrazol-3-one, 4,4’-[(3,3’-dimethoxy[1,1’-biphenyl]-4.4’-diyl)bis(azo)bis[2,4-dihydro-5-methyl- 
 

	-2-(4-methylphenyl)- 发明者：  I.G. 
 

	生产工艺文献：  BIOS 1661, 160. Vulcan fast Red GF paste. 未抄录。 
 

	    FIAT 764 – Vulcanechtrot G. “Colour Index” 未注明PB号。 
 

	FIAT 1313,III, 501-503. Vulcan fast Red GF. 德文生产工艺规程，英译。抄录如下。 
 

	PB 74067, 779-784. Vulcanechtrot GF & GK. 3美元。 德文生产工艺规程。未抄录。 
 

	PB 74771. Vul.  品种卡片  未抄录。 
 

	项 斌 高建荣 编“颜料” Bh 005. P. 388-389. C.I.颜料红37.  2008年。 请见原书，它未注明资料来源。 
 

	中国化工产品大全，有机颜料。Fq 0004. P. 816. C.I.颜料红37. 2012年。同上。可能译自FIAT 1313.III, 501-3. 
 

	             C.I. 颜料红37 生产工艺规程    抄自FIAT 1313,III, 501-503 
 

	Vulcan fast Red GF  Oct. 1, 1940年。 
 

	Trade Name:    Vulcanechtrot GF 
 

	Composition:   改成反应式： 
<img alt="" src="http://www.陈忠源化学文库.cn//chenzhongyuan/Upload/ArticlePicture/IMG_07042016_095712.png" /> 
 
 

	3,3’-二甲氧基二苯胺  à  à   1-(4-甲基苯基)-3-甲基-5-吡唑啉酮   à  C.I. 颜料红 37. 
 

	Pricipal Uses;  Rubber, as factis color.  Printing ink and vinyl plastics.   Batch Size:  0.2 mols 
 

	Process:  Tetrazo 
  52 kg 0-Dianisidine (special Mol. 244) are stirred with 100 l. HCl 5N (= 18.25 kg 100% Hcl) and 1500 l. H2O at 500C. for 1 hr., then 10 kg Carboraffin are added, stirring continued for ±1/2 hr. at 500C and the solution clarified by filtration. To the clarified solution are added 100 l. HCl 5N (=18.25 kg 100% HCl) and then 1000 kg ice. The temperature is adjusted to 00C. 52.6 l. NaNO2 40% (by wt.)= 27.7 kg 100% NaNO2 are immediately and rapidly added under the surface at 00C. HNO2 reaction definitely positive but weak on Diaminodiphenyl sulfone after 1/2 hr. stirring. Volume is then adjusted to 3000 l.  3 kg Kieselgur are then added and the solution filtered and run directly from press into the Tolyl MP suspension which is prepared as follows:-       Tolyl MP Suspension 
  80 kg Tolylpyrazolon 100% (Mol. 188) are slowly scattered into a solution of 25.7 kg NaOH 100% (=39.4 l. 65% by vol. or 57.3 l. 33% by wt. caustic solution) in 3000 l. H2O at 200C over 3/4 hr. Stirring is continued until solution is complete.10 kg Kieselgur are added and the solution clarified by filtration. The Tolyl MP is then precipitated in not less than 1/2 hr. (not quicker) with ±150 l. HCl 5N（=28.5 可供100% HCl）until just positive reaction on Congo Red is obtained. 128 kg chalk are then added and 350 kg ice. The volume is adjusted to 4000 l. at 100C. The dye is coupled in 2 hrs. by running the diazo under the surface of the TMP suspension. Stirring is continued 1 hr. after end of coupling and the dye then made acid by slow addition (because mass foams badly) of  420 to 430 l. HCl 5N (=76.5 to 78.5 kg HCl 100%). After 1 hr. stirring a small quantity 2 kg chalk are then added in order to neutralize the acidity. The pigment suspension is heated over 1 hr. to the boil and boiled for 1 hr. It is then pressed immediately and washed well with water as hot as possible. The presscake is mixed in the “Draisapparat” (paste mixer) after which it can be used for preparation of the GF (factis) brand as Vulcanechtrot GF Paste. For the powder brand the paste is dried at 50 to 550C. It is ground on a Plathmill No. 11, 12 or 13. The pulverized material is used for Coloring Igelit (Polyvinyl resin) and in the U.S.A. principally for printing inks. 
Yield:  Wet presscake =±635 kg of 20% solids. Dry = ± 127 kg.   Preparation of Vulcanosol Red G paste (10%)   略！ 
加注：  按德文原件是一次文献，那么FIAT是二次文献，颜料一书又是摘译，应该是三次文献了。又是未注明资料来源，读者如何看清资料是否正确，所以请作者一定要注明文献出处。 
 

	陈忠源   2016年4月6日。 
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