C.I. 酸性黄117 (C.I. 24820) 生产工艺   CAS号 [6459-70-7]

CAS名:  Benzenesulfonic acid, 4,4’-[(phenylmethylene)bis[4,1-phenyleneazo(4,5-dihydro-3-methyl-5-oxo-1H-

                           -pyrazol-4,1-diyl)]]bis-, disodium salt.

发明者：   H. Wagner and J. Erber  1913年。

生产工艺文献：

BIOS 961, 57.   (=胶卷PB 60905)  英文生产工艺，摘译自德文。                         本人未收藏。

BIOS 1548, 40-1. (=胶卷PB 85593)  Milling Yellow HG. (Hoechst)  英文生产工艺，摘译自德文。   抄录如下。

反应式：    本人有加注。

4,4’-Diaminotriphenylmethane  à à 2 mols. 1-(4’-sulphophenyl)-3-methyl-5-pyrazolone  -à

Plant:  Diazotisation vat 6 cu.m.          Coupling vat 18 cu.m.

       Measuring vessels for hydrochloric acid, nitrite and sodium carbonate solution.

       Filter press with 37 chambers (110 x 110 cm.)

Method:

4,4’-Diaminotriphenylmethane (0.6 mol.) is dissolved in the diazotization vat in approximately 3,000 l. water and HCl (324 kg. 30%). Add ice to cool to 0⁰ and diazotize at this temperature with 160 l. 40% nitrite solution. The tetrazo is clear and no screening is necessary.

1-(4’-Sulphophenyl)-3-methyl-5-pyrazolone (1.26 mol.) is slurried in the coupling vat in approximately 2,000 l. water, dissolved with sodium carbonate (133 kg. in solution) and iced to 0⁰C. The tetrazo is runin as rapidly as possible. Add soda ash solution till alkaline to Brilliant Yellow Paper (approximately 70 kg. required). Coupling is then complete and shows excess pyrazolone on testing with diazo sulphanilic acid. The dyestuff is partially precipitated.   Heat to 90⁰C., add 2,400 kg. salt and filter at 80⁰C.     Dry at 70-80⁰C.

Yield = 658 kg. at 56=100.    Diluent  Common Salt. = 80.9% theory.

PB 70407, 7451-7459.  Fulling Yellow HG.  Made by coupling diazotized diamino-triphenylmethane with

1-(4’-sulfophenyl)-3-methyl-5-pyrazolone (=pyrazolic acid 4).  1935年。1.5美元。共9页未抄录。

它是完整的生产工艺规程。  该胶卷主题：  Instructions for the preparation of Dyes.   1922 – 1945.

PB 74024, 432-434.  Walkgelb HG.   德文生产工艺。                                     未抄录。

上海染料生产工艺汇编，365-367 （1976年）                                         请见原书。

加注：

本人抄录目的，是针对利用BIOS出新书而未指明资料来源者，其次要说明BIOS是二次文献。以上产品历史生产工艺，仅供参考。

陈忠源    2016年6月7日                                               于 无锡  明辉国际。