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C.I.颜料红68 (C.I. 15525) 生产工艺

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C.I.颜料红68 (C.I. 15525) 生产工艺   CAS号:[5850-80-6] 

	CAS名： Benzoic acid, 2-chloro-5-[(2-hydroxt-1-naphthalenyl)azo]-4-sulfo-, calcium sodium salt (2:1:2) 
 

	发明者：  I.G. 
 

	生产工艺文献：BIOS 1548, 209-210.  英文，译自德文，二手货。见抄录文。 
  FIAT 764 – Permanentrottoner NCR Plv.  “Colour Index”  未说明PB号。 
  FIAT 1313,III, 490-493. Permanent Red Tonner NCR。1942年12月1日。英文，见抄录文。 
  PB 73607, 6307-6354. Permanentrottoner NCR 1943年。未抄录。 
  PB 74067, 709-711. Permanentrottoner NCR 1。5美元。未抄录。 
  PB 74753  Pa. – Po.  品种卡片。 未抄录。 
以上二战后的产物，英文是二手货，德文是原件。 
 

	 
 

	项 斌 高建荣 编“颜料”。Be 009. P. 273-274. C.I.颜料红68.  2008年。未注明资料来源。 
 

	中国化工大全，有机颜料。Fn 0022. P. 787. C.I.颜料红68. 2012年。同上。可能译自BIOS或FIAT。 
 

	化妆品品用：  Kosmetische Faerbemittel. C-ext. Rot 59 (3 pp). (1984).   Coloring of Foods, Drugs and Cosmetics. p. 135 (1999) 
 

	 
 

	Be 009  C.I. 颜料红68    可能译自英文，如果是，译文有错！抄录如下： 
  【制法】 反应釜中加入800 L水及115 L 33%的苛性碱溶液，加入252 kg 重氮组分，使反应液呈亮黄色，pH值约为7.0，然后加入131 L 40%亚硝酸钠溶液，过滤，并把滤液加入已加入500 L 5 mol/L 盐酸及300 kg 冰的反应釜中进行重氮化反应，温度7-100C亚硝酸微过量并补水350 L, 调整温度100C 备用。 
  在3000 L 250C 水中加入950 L 33% 苛性钠溶液，加入150 kg β-萘酚搅拌，使溶解调整体积至5000 L备用。 
  将重氮后的乳浮液在45 min内加入到β-萘酚液中，终点β-萘酚微过量搅拌2 h, 加入413 kg 硫化钠及300 L水，进行盐析，并搅拌过夜。压滤可得到1200 – 1300 kg 滤饼。将滤饼加入1500 L 600C水中。搅拌并降温至540C，过滤得溶液体积2500 L，加冰降温至290C. 
 

	在另一釜中加入1500 L水，170 kg 氯化钙及700 kg盐，并调整体积至2700 L，于在180C过滤澄清，在40 min加入已制备好的染料溶液，温度升至240C，并搅拌过夜，加热至700C过滤， 55-600C烘干，得200 kg 产品。 
 

	反应式：  本人有加注。 
<img alt="" src="http://www.陈忠源化学文库.cn//chenzhongyuan/Upload/ArticlePicture/IMG_07042016_095129.png" /> 
 
 

	 
 

	 
 

	BIOS 1548, 209 抄录文。 
 

	BIOS 1548, 209 (= PB 85593, 209.   Permanent Red Toner NCR   (Hoechst). 
 

	2-Chloro-5-amino-4-sulphobenzoic acid (CA saure)  à  β-Naphthol. 
Scale:   1 kg. mol. 
  CA acid (252 kg.) is dissolved in 800 l. water with caustic soda (115 l. 33%) at room temperature. Add sodium nitrite solution (131 l. 40%) and ice to 7-100C. Add Kiesulguhr (10 kg.)(译注：硅藻土) and screen into a mixture of 500 l. water, 600 l. HCl 5N and 7 kg. ice. Volume of diazo 3,500 l. Temperature 100C. 
β-Naphthol (150 kg.) is dissolved at 220C. in 3,000 l. water and 95 l. 33% caustic soda solution. Adjust volume to 5,200 l. at 220C. and add 103 kg. soda. 
  Run diazo under the surface of the naphthol solution over 3/4 hour. The dyestuff is almost completely in solution. Add over 2 hours 1,300 l. clarified saturated salt solution. Good agitation must be maintained throughout this addition the batch being very thick at first but then breaking up. Stir overnight. Test of filtrate should next day show 6 to 6.50Be’. Run into an agitated blow-egg and blow to filter press (Do not use a pump). 
  Yield = 1,200-1300 kg. Paste. 
Divide this paste into two equal parts and treat each part successively as follows:- 
Charge paste slowly into 1,800 l. water at 600C. The temperature falls to 540C. Add Kiesulguhr and screen. Volume of filtrate 2,500 l. Temperature 440C. Add ice and water to give a temperature of 290C. and a volume of 3,050 l. 
Dissolve 170 kg. calcium chloride in 15,00 l. water and add 700 kg. salt. Adjust volume to 2,700 l. and clarify at 180C. 
  Add 31/2 kg. glacial acetic acid to the filtrate. Then run in the dyestuff sodium salt solution over 40 minutes maintaining a temperature of 240C.  Stir rapidly overnight. 
  Next morning heat slowly (over 11/2 hours) to 700C. and maintain this temperature 1/4 hour. Dilute with cold water to adjust temperature to 35-400C. Filter and wash with water.  Dry at 55-600C. 
Yield = 200 kg. dry  (No dilution is necessary). 
  The remaining half of the paste is then similarly dealt with. 
 

	Note :  The preparation of this colour was stated to be very difficult and often part of the manufacture was sold at a lower price – sometimes because of blueness and thinness and sometimes because of Yellowness in shade. 
 

	 
 

	FIAT 1313,III, 490-493. 抄录文。 
 

	FIAT 1313,III, 490-493.     Permanent Red Toner NCR       Dec. 1, 1942 
 

	Process:   Diazo  800 l. H2O and 115 l. NaOH 33% are added to the diazo vat. To this solution 252 kg. CA Saeure (2-chloro-4-sulfo-5-amino-benzoic acid) 100% are added and stirred to complete solution. A definite reaction on Brilliant Yellow should be obtained. 20 l. of this solution is taken out and retained for later correcting the nitrite value (usage). Then, 131 l. NaNO2 40% by weight are added and then 10 kg Kiesselgur. The solution is filtered thru a clarifying press during 3/4 hr. at 7-80C. and the clarified solution run into 600 l. HCl 5 N in 500 l. H2O and 300 kg Ice, 300 kg additional ice are added during this time. The HNO2 reaction should be weak at the end of diazotization. Volume diazo suspension = 3500 l. Temperature = 100C. 
 

	Naphthol Solution   To a solution of 3000 l. H2O at 250C and 95 l. NaOH 33% by weight in the coupling vat. 150 kg BN are added and and completely dissolved by stirring 1/2 hr. To ths is added 103 kg Na2CO3. Volume is made to 5200 l. at 220C. 
 

	Coupling   The diazo suspension is run over 3/4 hr. into the BN solution under the surface. At the end of coupling the dye is completely in solution. It is tested for excess BN and excess diazo, the former with o-Dianisidine tetrazo. After stirring 1/3 hr. a clear solution of saturated  413 kg NaCl in 1300 l. H2O is run in over 2 hrs. The dye precipitates and the mass thickens (eventually all the dye salts out). Then the dye is stirred overnight. A sample is filtered next day and the filtrate should run about 6 to 6.50Be’. The dye is filtered in a press, requiring 24-28 hrs. The Yield of Na salt = 1200 to 1300 kg (wet cake). The Na salt is laked in 1/2 mol size by two different procedures. 
 

	Cold Laking – 0.5 m   The presscake of half the charge of Na salt is dissolved in 1800 l. H2O at 600C with stirring. To this is added at 540C. 10 kg Kieselgur and the dye solution clarified by filtration thru a filter press over 3/4 hr. Volume = 2500 l. at 440C. ±300 kg of ice (1 wagon load) is added. Volume = 3050 l., temperature is then adjusted to 290C.  In a separate vat 170 kg CaCl2 solid are dissolved in 1500 l. H2O, then 700 kg NaCl are added and the volume adjusted to 2700 l. and this solution clarified. Volume = 2700 l. temperature 180C. 3.5 kg Acetic acid glacial are added to the CaCl2-NaCl solution and the soda salt dye solution is added to this over 40 minutes. Temperature should be 240C. (In summer the CaCl2 solution is made up at lower temperature.) The pigment is stirred overnight with rapid agitation. The formation of the orange yellow di-Ca salt requires about 3 hours. Next A. M. the temperature is about 250C.. The pigment is slowly heated to 700C and held at 700C for 15 minutes, flooded and pressed (3 hrs.) and press washed 4 hours, then dried at 55-600C. 
 

	Yield: ± 200 kg dry = 159% of original quantity of C.A Acid. Plant material is somewhat stronger, slightly bluer and slightly darker in color than standard. 
 

	Hot Laking – 0.5 mol   上面是冷色淀化，这是热色淀化。 
 

	    The other half batch of Na salt is stirred to solution in 2100 l. H2O at 700C. To this is added 10 kg Kieselgur.  The solution is then 
 

	Filtered. Volume = 3100 l.; temperature = 470C.  Then a solution of 22.5 kg “Leonil S” * dissolved in 200 l. H2O at 500C are added. In a 
 

	separate  170 kg CaCl2 are dissolved in 1500 l. H2O  700 kg NaCl are added and the volume adjusted to 2700 l. with H2O. The solution 
 

	 is stirred for 10 minutes and clarified by filtration. The solution is heated to 730C and 10 kg Cycanon L ** in 50 l. warm H2O are added 
 

	under rapid agitation and then the laking is carried out at 73-750C as described above. The lake is stirred 1/4 hr., filtered in 1/2 hr., 
 

	washed 4 hrs., and dried at 55-600C. 
 

	Yield: ± 200 kg = 159% of the original quantity of C.A.Acid. Plant material is definitely stronger, slightly yellow and somewhat darker 
 

	in color than standard. 
 

	Notes: 
 

	    (For both laking processes.) 
 

	    Large (1 mol) batches gave poorer results because of less satisfactory mechanical conditions, such as agiyation. 
 

	    3 Cold and 2 hot lakings are prepared and these are mixed to obtain the desired shade of standard product. The hot laking which 
 

	requires only 12 hrs. is the simpler and more rapid process and yields a stronger (70 to 75:100) product. The tendency, therefore, was 
 

	to use the hot laking process. 
 

	l    “Leonil S” = benzylnaphthalene sulfonic acid sodium salt. 应是一种分散剂。 
 

	**   Cyclanon L = alcoholate of stearic acid. 
 

	 
 

	以上请读者对照中文译文！ 
 

	 
 

	编注： 
 

	    为什么说，BIOS，FIAT是二手货？德国人编写生产工艺规程，能用英文吗？当然不能。为什么说BIOS 
 

	和FIAT不可靠？因为它是靠人翻译的，而翻译人员，不一定专业，各人理解也有不同，另外也可能有笔误， 
 

	所以科技人员应看原件。这是我多次对照得出的结论。 
 

	 
 

	    为什么说是二战后的产物？因为德国人是战败国，美国人可以把它公开，而且可以出售，因为资料大 
 

	多，只能采用缩微胶卷的方法，其中拿出一部分翻译成英文，出书，这就是BIOS和FIAT。这些书同时保留 
 

	有缩微胶卷，所以日本人用PB号表示。国内为什么不用？ 
 

	 
 

	    目前提倡精准，创新，诚信，为什么不认真出书？抄来的，就应注上是哪里抄的，有错不怕，要改正。 
 

	所谓新，一定是在旧的基础上，了解产品历史，了解过去是有用的，而且要认真看，有哪些经验可以借鉴 
 

	参考，目前又提倡环保，所以过去的方法不能用，但要了解过去是怎么做的？ 
 

	 
 

	    为什么要建立“化学文库”？这里首先要感谢公司的领导和同志们，其次是我的爱好，别人是周游世 
 

	界，我是游览各种有关资料，而且我还有精力。我应该回报社会，因为我是国家培养的技术人员，上大学 
 

	是拿国家补贴工资的，今天不是要名，也不要利。过去收集的资料不用就会变成废纸。拿出来对大家应该 
 

	有用吧！我的文库主要是战前的德国资料。以上供参考！ 
 

	 
 

	陈忠源   2016年4月5日。   于 无锡 明辉国际 
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