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C.I. 媒介黄8 (C.I. 18821) 生产工艺 CAS号[6359-83-7]

C.I. 媒介黄8 (C.I. 18821) 生产工艺  CAS号[6359-83-7]

CAS名:  Benzoic acid, 2-[[4,5-dihydro-3-methyl-5-oxo-1(4-sulfophenyl)-1H-pyrazol-4-yl]azo]-, disodium salt.

生产工艺文献：

BIOS 961, 57.  (=胶卷PB 60905)  未收藏。

BIOS 1548, 83.  (=胶卷 PB 85593)    Acid Alizarine Flavine R  (Hoechst)  英国人译自德文。抄录如下。

反应式：本人有加注。它是摘译自PB 73067,6878-6894.
 

Anthranilic acid  à  1-(4’-Sulphophenyl)-3-methyl-5-pyrazolone.

Plant:  Diazotisation vat cu.m. with measuring vessels for hydrochloric acid (2 cu.m.) and nitrite solution (o.5 cu.m.)

      Coupling vat 20 cu.m.   Centrifugal pump.   Wooden filter press with 38 frames  (110 x 110 cm.).

Method:

Anthranilic acid (2 mols.) is slurried overnight in approximately 3,000 l. water and 500 l. 5N HCl. Next day ice to 00C. and diazotize at this temperature with 262 l. nitrite solution (40%).

1-(4’-Sulphophenyl)-3-methyl-5-pyrazolone (2.07 mols) is slurried in approximately 2,000 l. water and dissolved to a neutral solution with caustic soda solution 33%. Add 150 kg. soda ash and adjust the temperature of 250C.

Run the diazo under the surface of the pyrazolone solution over 11/2 hours. Coupling is immediate and a test with diazo sulphanilic acid shows excess pyrazolone. The dyestuff is in complete solution. Heat to 500C. Volume 10,000 l. approximately. Salt slowly 20% w/v. Stir overnight and then filter from clear mother liquors at 21Be’. Dry at 800C. and standarise with sodium sulphate.

Yield = 1,150 kg. at 74/100.   这里原文打成74=100，错了。

Note:  1.  Appreciable variation in colour strength is experienced with this colour.

      2.  When higher strength material is required only 10% w/v. salt is used and the mother liquors from the filtration are used in the next batch.

    Strength then 64/100.  And Yield is 970 kg. 

PB 25625, 178-9.  Saeurealizarinflavin R.  1932年6月生产工艺。 德文。 1美元。 未抄录。 

PB 73607, 6878-6894.（共7页）  Saeurealizarinflavin R.  德文生产工艺规程。未抄录。 

用途：

酸式：[54480-58-9].  钠盐：媒介黄8 =[6359-83-7]

钙盐：C.I. 颜料黄142.  C17H12CaN4O6S = 440.44.  商品名：Kayaset Yellow E-L2R.

酸式与不带磺酸基的单偶氮染料铬络合：C.I. 酸性黄259.  CAS号[84682-44-0]

酸式2:1铬络合与有机胺成盐：C.I. 溶剂黄13.  CAS号 [72479-91-5] 

陈忠源  2016年8月25日                 于 无锡   明辉国际。



文章作者：陈忠源