C.I. 溶剂紫12 = C.I. 分散紫4（C.I. 61105）生产工艺。   CAS号 [1220-94-6]

CAS名：9,10-Anthracenedione, 1-amino-4-(methylamino)-   历史参考资料：Beil. 待检索。

用途：化纤染色，塑料着色等。LookChem网登录生产与经营单位12家。 反应类别：氨基烷化。

BIOS 1484, 61.（=胶卷PB 86139）。 Celliton Fast Violet 6B (Partislly methlated 1,4-diaminoanthraquione). (Ludwigshafen).

英国人译自德文，无资料来源。反应式：本人有加注：

An iron pressure vessel is charged with 1200 kg. sulphuric acid 96% and leuco 1,4-diaminoanthraquinone (M. Pt. 258-260℃. with decomposition) (300 kg. 100%) introduced, causing the temperature to rise to 75-80℃.  The temperature is raised to 103-105℃. and 200-250 kg. chlorine passed through at the rate of 15 kg. per hour.  The exit pipe on the pan leads to a wash bottle 1 m. high containing sulphuric acid so that a pressure of 0.2 atmospheres is obtained inside the pan.  The oxidation is satisfactory when a sample shaken with excess ammonia and filtered off does not give a yellow filtrate.  (Yellow colour is due to leuco diaminoanthraquinone.) .  Excessive chlorination, however, causes chlorine to enter molecule, resulting in a dyestuff which has much less colouring power.  The excess chlorine and hydrochloric acid blown out with a current of dry air for 2-3 hours, then the melt cooled to 20℃. 

336 kg. methanol are run in over 3 hours with cooling, keeping temperature below 60℃.  The pan is then closed, heated to 133℃. and held at this temperature for 2-2.5 hours.  The batch is tested by neutralizing a small sample with soda, dissolving in acetone and comparing with a solution of standard.  As too long a heating during the methylation causes a duller and greener shade, the batch is cooled immediately and blow slowly on to 6000 kg. water, 300 kg. caustic soda 400Be’, and 3000 kg. ice.  The temperature should not exceed 40℃.  Filtered, washed free and dried.

Yield = 360 kg.

FIAT 1313, II, 205-206.（=胶卷PB 85172）。 Celliton Fast Violet 6B. (Lidwigshafen).  美国人译自德文，无资料来源。

This color was made by partial methylation of 1,4-diamino anthraquinone to the approximate formula given above.

The process: To 1200 kg. 96% sulfuric acid in an iron kettle, add 300 kg. leuco 1,4-diamino anthraquinone allowing the temperature to go to 75-80℃.  Heat to 103-105℃ and at this temperature pass in chlorine at 15 kg. per hour until oxidation is complete by test.  200-250 kg. chlorine is required.  The test: Drown sample in water, make ammoniacal, and filter.  Oxidation is complete when filtrate is no longer yellowish in color.

Blow out the dissolved chlorine and hydrogen chloride with dry air (2-3 hours).  Cool to 20℃ and during 3 hours, add 336 kg. 96-100% methanol at temperature (2-2.5 hours).  Test: Drown sample in water, add excess soda ash, filter.  Dissolve sample of solid in acetone and compare with standard.

When satisfactory, cool at once and drown in mixture of 8 cbm. water, 3000 kg. 400Be’ sodium hydroxide, and 3000 kg. ice. Keeping the temperature below 40℃ during drowning.  The charge is alkaline.  Filter.  Wash neutral with cold water.   The yield is 360 kg. paste.

In this case the paste is converted directly to the dispersible powder.

细田豊 《理论制造染料化学》。技報當 出版。 1957年。 P. 689.  セリトヲファスト バイオレット 6B. 译自FIAT 1313.

96% 硫酸1.2 tにリウコ1,4-ジアミノアントラキノン300 kgを加えれば75-800に上リ，103-1050に上げてCl2を每时15 kgの割で200-250 kg通ずる。空气を吹入んでCl2 + HCl を追出し，200で96-100% メタノ-ル336 kgを600以下3 hで加え，1330に上げ2-2.5 h保温する。冷して水8 t + NaoH 400Be’ 3 t + 冰3 tに400 以下で排出，滤過水洗する。360 kg paste。

张澍声《精细化工中间体工业生产技术》。《染料工业》编辑部 出版。1996年 P. 239.  1-甲氨基-4-氨基蒽醌。译自FIAT 1313,II,305.

在铁锅中向1200 kg 96% 硫酸加入300 kg 1,4-二氨基蒽醌隐色体，让温度升至75-80℃。加热到103-105℃，在此温度通氯15 kg/小时，直至氧化完全，需要200-205 kg氯。（取样投入水中，氨化并过滤，当滤饼不再有黄色，氧化完全）。

用干空气吹除溶解的氯和氯化氢约2-3小时。冷至20℃，在60℃以下于3小时内加入336 kg 96-100% 甲醇，加热到133℃，保持至反应完全，约2-2.5小时。检验是取国体样品溶于丙酮，与标准样进行比色。

检验满意，立即冷却，投入8 m3 水，3000 kg 35% 氢氧化钠溶液和3000 kg 冰的混合物，在投入时温度保持40℃以下。物料呈碱性，过滤，水洗至中性，得360 kg滤饼，直接转变为可分散性粉末。

PB 25628.  Methods for production of dyestuffs as disclosed through T.E.A. Büro documents. 1928-1937年。共1090页。6美元。

PB 25628, 4090-4091.  Manufacturing directions for preparing finely powdered Celliton Fast Blue Green B and Celliton Fast Violet 6B by means of a Kraus drying apparatus.  美国人介绍如下：

    The nonacidic dye cake is treated with definite quantities of a dispersing agent and“Dekol”.  The resulting paste is placed on a Krause drying apparatus,

Where it is reduced to a fine powder.  In German. 其中有C.I. 分散紫4，商品染料的加工。未抄录。

PB 25628, 4207-4213.  Cellitonechtviolett 6B. 德文生产工艺原件，共7页，未抄录。

美国人介绍胶卷内容，未抄录。

《日本化药染料便览》。 日本化药株式会社 出版。 1982年。P. 176.  Kayalon Fast Violet BB. 有织物染色数据。不再抄录。

染料专业历史出版物。

1.  The society of dyers and colourists. 《Colour Index》. Second Edition 1956. P. 3494.  C.I. 61105.  C.I. Disperse Violet 4.

Discoverer – I.G.  BIOS 1484, 61; FIAT 1313, 2, 205;  FIAT 764 – Cellitonechtviolett 6B.

2.  编写者：丁忠传 史献平 等。《染料品种指南》。中国化工信息中心 出版。1995年。 P. 428.  C.I. 分散紫4（C.I. 61105）.

【主要参考文献】BIOS 1484, 61; FIAT 1313, 2, 205;  FIAT 764 – Cellitonechtviolett 6B.

3.  《世界染料品种 – 2000年》。《世界染料品种 – 2000年》编写组 编写。 P. 1061.  C.I. 分散紫4 .

【参考文献】BIOS 1484, 61; FIAT 1313, 2, 205;  FIAT 764 – Cellitonechtviolett 6B.

4.   肖 刚  杨新玮 等 主编《世界染料品种 – 2005年》。全国染料工业信息中心 出版。 P. 568.  C.I. 分散紫4 。

【参考文献】BIOS 1484, 61; FIAT 1313, 2, 205;  FIAT 764 – Cellitonechtviolett 6B.

5.   何岩彬 主编 《染料品种大全》。沈阳出版社 出版。 2018年。 P. 882.  C.I. 分散紫4 。

     【参考文献】日本化药染料便览（第四版）。 1982: 170.  PB 25628, 4207-13; PB 73726, 269-99.（抄注：这是本人的差错！）。

     BIOS 1484, 61; FIAT 1313. 2, 205;  FIAT 764 – Cellitonechtviolett 6B.

陈忠源 2020年1月5日星期日。