C.I. 酸性蓝9 =C.I. 食品蓝2 (C.I. 42090) 生产工艺  CAS号[2650-18-2]

CAS名:  Benzenemethanaminium, N-ethyl-N-[4-[[4-[ethyl[(3-sulfophenyl)methyl]amino]phenyl](2-sulfophenyl)methylene]-2,5- -cyclohexadien-1-ylidene]-3-sulfo-,innersalt,diammonium salt.

发明者:  Sandmeyer  1896年。 参考文献:  Beil. 14, 855.

生产工艺文献:

BIOS 1433, 20-1.  (=胶卷 PB 81029)  Patent Blue AE.  英国人摘译自德文，但未注明资料来源。抄录如下。

反应式: 本人有加注。

From 1 mol. O-Sulphobenzaldehyde and 2 mol. Ethylbenzylaniline sulphonic acid.

1.  Leuco Acid  (Plant.) 略。2.  Dyestuff. (Plant.) 略。

 Leuco Acid:

   1400 l. Water, 2200 kg. Ethylbenzylaniline sulphonic acid 100% (Gruensaeure, M.W. 281) and 720 kg. o-sulphobenzaldehyde 100% (“Sulfal” M.W. 186) (= theory + 2.35%) are charged into the condensation montejus. The violume is made up to 4800 l. with water, and the solution heated at 100-103⁰C for 24 hrs. It is then tested in the Lab. for completion of the condensation. For this purpose three samples 500 gms. (about 200 gms. Of dry material) are withdrawn and worked up as follows: Test 1. 500 gms. Of solution.  Test 11. 500 gms. Of solution + 9.4 gms. Gruensaeure 10.  Test 111. 500 gms. of solution 9.3 gms. Sulfal.

These are heated for 48 hrs. on the water bath with stirring, then diluted in each case to 1000 cc. 1060 cc. and 1060 cc. respectively.

Three oxidations are made of each preparation, using 24 cc. of soln. ( = 5 gm Leuco acid). The colour is filtered off, diluted to 3100 cc. and dyed up against 200 cc. Patent Blue soln. (1 gm. Type in 200 cc. water).

According to the best oxidation reault, more Gruensaeure or Sulfal is added to the batch and heating continued at 100-103⁰C. for a further 48 hrs. An excess of Sulfal is harmless, but too much Gruensaeure leads to a duller shade. The batch is then diluted and blown into the storage vessel.

Dyestuff:

Three tests are made by taking 100 gms. Of the Leuco soln. and oxidizing with the same amount of oxalic acid and sulphuric acid present, but using slightly different amounts of Bichromate, e.g. 12, 13, and 14 gms. The oxidation is worked up and dyed against a standard soln. as before.

850 l. of the Leuco soln. ( = 300 kg. 100%) are run from the storage tank via. The measuring vessel into the oxidation vat, diluted to 2000 l. and made slightly alkaline to Brilliant Yellow with 70 kg. Caustic Soda 40⁰Be’. Bout 39 kg. Sodium bichromate (exact weight according to the oxidation test), as 55 l. of soln., are run in, and then after a few seconds the following mixture is tipped in –

54 kg. Oxalic acid crystals dissolved in 150 l. Water, 66 kg. Sulphuric acid 60⁰Be’. 50 kg. Ice.  Temperature may rise to 37⁰C. It is stirred for ¹/₂ hr at 30-34⁰C.  22 l. Ammonia 25% added and also 3 kg. Kieselguhr to improve the filtration. The dyestiff soln. goes through the screening press into the conical salting out vessel, where two such batches are isolated together with 2400 kg Sulphate to 34⁰Be’ at 40-45⁰C. 70-80 kg. Soda, dissolved in water, are added gradually, the batch stirred a sort while, and allowed to stand overnight. The mother-liquor is run off through the settiling box, and the sticky colour dried under vacuum at 90-100⁰C.

Yield:  From 300 kg. Leuco Acid 360 kg. F ware, about 40=100 (应是40%)

i.e. about 900 kg. Patent Blue AE type.

PB 25627, 3129-3131.  Neptune Blue BR. 1930年4月。3页。1美元。其说明如下。原件未抄录。

   The leuco compound of this dye is produced by the condensation of ethylbenzylaniline-sulfonic acid and benzaldehydre-o-sulfonic acid. It is then oxidized with manganese dioxide. The process is described. A modification for obtaining a manganese-free product is added.  In English. 工艺用二氧化锰氧化！国内至今未见有人引用此文献。

PB 74067, 139-141.   Patent Blue AE.  问答式调査报告。 未抄录。

国内研究动态：

大连工学院。食用色素概况及食品蓝2合成中缩合剂对反应率的影响。染料工业  1987,2,1-4（14）  引用BIOS 1433,20.

潘国光。 二氧化锰氧化法合成酸性翠蓝AE。染料与染色  2003, 5, 253-5.  引用上述文献。

中国专利。 CN 104327533. 2015, 2, 4. 7页。

用途：

DFG.  Kosmetische Faerbemittel / Colours for Cosmetics. C-Blau 21. (共6页) 1984年。

Axel Mixa.  Coloring of Foods, Drugs and COSMETICS.  p. 206-8.  1999年。

有关产物CAS号和EC号：

分子式           CAS号       EC号        产品名

C₃₇H₃₆N₂O₉S₃.       25305-78-6

-----“ ---------. 2 H₃N      2650-18-2   220-168-0      酸性蓝9 / 食品蓝2

-----“ ---------. 2 Na      3844-45-9   223-339-8      食品蓝2

-----“ ---------. 2 K        71701-18-3   275-866-8

-----“ ---------. K.Na       71701-19-4   275-867-3

-----“ ---------. Ba       6548-12-5   229-466-5   颜料蓝24

-----“ ---------. ²/₂ Al     15792-67-3   239-897-0   食品蓝2:1

-----“ ---------. x Al      68921-42-6   272-939-6   颜料蓝78

-----“ ---------. x Al x Na   84473-85-8   282-940-3   食品蓝2:2

-----“ ---------. 2 C₆H₁₅NO₃   82910-94-9

酸性蓝9 + 酸性黄23    147975-82-2       Daiwa oil melon

                                    910-238-5     复配

                                    910-510-2     复配

知识就是力量！

陈忠源     2016年8月29日       于 无锡   明辉国际。