C.I.溶剂绿4 = C.I.荧光增白剂74 (C.I. 45550)    CAS号[81-37-8]

CAS名:  Naphtho[3,2,1-kl]xanthenes, 2,8-dimethyl-

发明者：  Badische Co.

生产工艺文献：

BIOS 987, 185, 186. Dimethyl-ceroxen. Fluorol 5G Pulver.     英文，无具体工艺。

BIOS 1433, 107-109. Fluorol 5G.  英文，生产工艺，译自德文，但未说哪个PB报告号。

FIAT 1313, 2, 61.  Fluorol 5G (anthraquinone color for use in lubricating oils).     英文，工艺简述。

FDX 885 – Fluorol 5G.  品种卡片。 未抄录。

PB 25624, 1309-1312. Fabrikationsvorschrift fuer Dimethylfluoran.  见CAS号[125-14-4]。  已上网。

PB 70057, 8441-8444.  同上。

PB 70057, 8422-8426. “ Coeren“ = 2,7-Dimethylcoeroxene  Kirchner  1937年8月21日。

这是德文原件（35毫米缩微胶卷）。    未抄录。

BIOS 1433, 107-109.  Fluorol 5G     原文部分抄录。这是因为德文原件未抄录。

(2)  Coerene Dry.  2:7-dimethyl Coeroxene,  C₂₂H₁₆O, M.W. 296.

Dimethylfluorane is converted by dissolving in oleum to dimethylcoeroxonol (Coerol) which is reduced under pressure with zinc dust and ammonia to Coerene.  CAS号为本人加注。
 

500 kg. Oleum 24% are cooled to 10⁰C. in a 600 litre iron vessel and 100 kg. dimethylfluorane powder added slowly through a sieve. The temp. must not exceed 20⁰C. The batch is stirred one hour and a test taken to determine whether the batch dissolves completely in 25% H₂SO₄ It is then precipitated in a mixture of 8000 litres water and 2000 kg. Ice. The temp. rise to about 7⁰C. About 1300 kg. Caustic 40⁰Be’ are added till the filtrate from a test filtration is only a pale reddish colour. The temp. rises to about 15-20⁰C. The faintly acid precipitate is filtered through a wooden press and blown dry without washing.

The press cake (about 350-450 kg.) is charged into the stirred autoclave (2 cu.m. horizontal, iron) and filled with water to 480 kg. 75 kg. zinc dust (90%) stirred with 20 litres water, are added with good agitation, followed by 100 kg. Ammonia 30% and 200 kg. caustic 34%.

The autoclave is closed and deairated by blowing through 30-45 lbs/sq. in. pressure nitrogen, twice, and carefully releasing the gas on account of froth. The contents are heated in 3 hours to 120⁰C. and maintained at this temp. 5 hours. They are then cooled with cooling water to 35⁰C. and blown through an iron press.  Since the melt is too strongly alkaline for the cotton filter cloth, and since the autoclave on account of the froth generated is still under pressure and cannot be opened for dilution, water is forced into the blow out pipe during the blowing out to dilute the melt. The water pipe must be fitted with a good check valve, and a slight glass inserted in the line so that it is possible to see that no Coerene goes up the water pipe by an alteration of water pressure. The cake is washed neutral with hot water and dried at 100⁰C.

Yield. 150 kg. Coerene at 47% (sublimation value). = about 70 kg. at 100%.

It contains zinc and zink salts which remain behind in the residue of the sublimation.

Sublimation.  以下，略。  

抄注：  以上是部分抄录，说明有此文献，如有需要，可参见原文。

陈忠源   2016年5月4日               于  无锡  明辉国际。