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C.I. 还原橙4 = C.I. 颜料红216 (C.I. 59710) 生产工艺 CAS号[1324-33-0]

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C.I. 还原橙4 = C.I. 颜料红216 (C.I. 59710) 生产工艺 CAS号[1324-33-0] 

	CAS名:  8,16-Pyranthrenedione, tribromo- 发明者：  R. H. Scholl and M. H. Isler  1909年。 
	
		生产工艺文献：以下抄录文，请读者比较。多学点外文是好的。（如需学德文请看原资料） 
		
			BIOS 987, 62.  (= 胶卷 PB 75860).  Indanthrene Orange 4R.   英国人译自德文。 未说明年份，资料来源？抄录如下。 
			
				反应式：  本人有加注。 
<img alt="" src="http://www.陈忠源化学文库.cn//chenzhongyuan/Upload/ArticlePicture/QQ图片20160809113555.png" /> 
				
					200 kg. Indanthrene Gold Orange G Powder.   2,000 kg. Chlorosulphonic acid. 
					
						4 kg. Iodine.   124 kg. Bromine. 
						
							The Orange G is dissolved in the chlorosulphonic acid together with the iodine and the bromine then added. The whole is stirred at room temperature for 2 hours. The temperature is now raised to 620 and held for 10 hours. The melt is now diluted with 2,000 kg. of 96% H2SO4 and poured into excess of ice and water. Filtered and washed. 
							
								The dyestuff is somewhat dirty and is yellower than type. It is therefore necessary to clean one batch in every three and then mix two dirty and one clean batches to give the correct shade, 
								
									Cleaning process:The press cake of one charge is stirred with  10,000 litres of water.   80 kg. sodium carbonate. 
									
										20 kg.  NaOH 460 Be’.  500 kg. sodium hypochlorite.   Heated to 1000 and boiled 4 hours.   Filtered and washed. 
										
											Yield = 290 kg. Indanthrene Orange 4R.  = 91% of theory. 
											
												FIAT 1313,II, 116-7. (= 胶卷 PB 85172)。Indanthrene Golden Orange 4R. 美国人译自德文。未说明年份，资料来源。抄录如下。 
												
													200 kilograms of Indanthrene Golden Orange G (Dry 100%).  2000 kilograms of chloro sulfonic acid. 
													
														4 kilograms of iodine.  124 kilograms of bromine. 
														
															The Golden Orange G crude is dissolved in the chlorosulfonic acid at room temperature and the iodine and bromine then added, after which the temperature is raised to 620 and this temperature held for 10 hours, or until a sample shows an analysis of 36 – 37% bromine. When the analysis is correct, the mixture is cooled to 300 and 2,000 kilograms of sulfuric acid (96%) is run in slowly, after which the mixture is agitated until the hydrogen chloride has been driven off and the mixture is run into 20,000 liters of water. 
															
																The precipitated dyestuff is filtered off, washed acid free and the press cakes dyetested. 
																
																	In case the color is duller than standard, which happens frequently, about every third charge is given a bleaching treatment as follows:  The press cakes from one charge are slurried in  10,000 liters of water  and  20 kilograms of caustic soda solution (460Be’) 
																	
																		80 kilograms of soda ash are added and then  500 kilograms of sodium hypochlorite solution (12%). 
																		
																			This mixture is heated to the boil and held until the bleach has disappeared, after which the slurry is filtered, washed alkali-free and the filter cakes dyetested.  日文摘译文，见细田豊 《理论制造染料化学》  1957年。  P. 703. 
																			
																				Yield = 290 kilograms Indanthrene Golden Orange 4R (100% equiv.) = 90% of theory from the Golden Orange G used. 
																				
																					PB 73726, 96.   Indanthrenorange 4R.  德文生产工艺。1933年3月28日。抄录。译文如下。 
																					
																						设备：3.2立方米铁溴化锅。22立方米稀释锅。压滤机。22立方米次氯酸钠处理锅。压滤机。 
																						
																							操作步骤：   溴化锅内先加入2000公斤氯磺酸，随后加入4公斤碘，搅拌下加入200公斤金橙G粉（100%），在室温溶解1小时，然后加入124公斤（33罐）溴，室温搅拌2.5小时，再在2.5小时加热到450，最后在2小时加热到620，保温10小时，冷却到250，取样与标准品打样比较，微黄色时，加入2000公斤96%硫酸，搅拌2小时，压入预先加有5000公斤冰和8000公斤水的稀释锅内，过滤析出的染料，洗到中性，所得染料略暗，需用次氯酸钠精制。将粗染料置于10立方米水中，加80公斤碳酸钠和20公斤460波美苛性钠，随后加入500公斤次氯酸钠溶液（12%），加热到95-1000，煮沸4小时，取样证明尚有活性氯，加入亚硫氢酸钠，除去多余的次氯酸钠，过滤。 得量：290 公斤。生产要点：  等。 略。 
																							
																								陈忠源    2016年8月8日          于 无锡  明辉国际。 
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