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。