CAS号 [6407-95-0] 生产工艺。  1-(2’,5’-二氯苯甲酰氨基)-8-萘酚-4,6-二磺酸

CAS名：1,7-Naphthalenedisulfonic acid, 4-[(2,5-dichlorobenzoyl)amino]-5-hydroxy-,  CAS号[6407-95-0].

        1,7-Naphthalenedisulfonic acid, 4-[(2,4-dichlorobenzoyl)amino]-5-hydroxy-,  CAS号[6528-49-0].

用途：染料中间体。LookChem网登录数：[6407-95-0] 1家；[6528-49-0] 3家。反应类别：氨基酰化。

BIOS 986, 412.（=胶卷PB 77764）。1-(2’,5’-Dichlorobenzoylamino)-8-naphthol-4,6-disulphonic acid (Dichloryl K säure 25).

    I. G. Ludwigshafen.   英国人译自德文，无资料来源。  反应式：本人有加注。（抄录文为2,5-体，CAS号 [6407-95-0]）。

Manufactured by the condensation of 2,5-dichlorbenzoyl chloride with K acid in the presence of soda.  Yield: 82.4%. 

The materials usage per 1,000 kg. of product is :-

790 kg. K acid;  510 kg. 2,5-dichlorbenzoyl chloride;  150 kg. 30% hydrochloric acid;  205 kg. soda;  95 kg. caustic soda 100%;  266 kg. salt (for cooling).

The average monthly production during the years 1938 – 1944 inclusive was nil, nil, 0.2, nil, 1.1, nil, nil tones.

BIOS 1152, 106-107.（=胶卷PB 81027）。2,5-Dichlorobenzoyl-K-Acid (1-(2’,5’-Dichlorobenzoylamino)-8-naphthol-4,6-disulphonic acid.)

(Ludwigshafen).  英国人译自德文，无资料来源。

Outline: K acid is condensed with 2,5-dichlorobenzoyl chloride.

Plant: 设备：抄录不再分项。

1 wrought iron, rubber-lined stirred vessel, with rubber covered blade agitator, 30 r. p. m. 2.2 kw. Motor.  7.8 m3。   1 Filter press with wooden frames. 1.1 m3。   1 Homogeneously lead-lined wrought iron blow-egg, 7.5 m3。   1 Rubber-lined wrought iron stirred vessel with tile-lining on top.  Blade agitator, 25 r. p. m.  Motor 3.7 kw.  Hot and cold water coils, 17 m3。   2 Iron nutsche, kerasolither and tiled, 8 m2, 6 m3。

Materia;s: 所投物料：抄录不再分项。

K acid moist (M.W. 319);   2,5-Dichlorobenzoyl chaloride (M.W. 209.5);   Caustic soda liquor 34.5%;   Soda ash；  Hydrochloric acid 200Be’;   Rock salt in solution。

Process:  操作步骤：

2000 kg. of K acid (at 100%) as a 44 – 46% moist technical product (= 4300 – 4500 kg. act. wt.) are stirred into 2450 kg. of water.  34.5% caustic liquor is pumped in until a brown colour is just not showing on Congo Red paper.  At this stage a little of the K acid has not dissolved (test in laboratory).

The batch is then pumped through the screening press into the benzoylation vessel and diluted with 2700 l. of water.  111 kg. of soda ash are then added.

The 2,5-dichlorobenzoyl chloride (1300 kg.) is added at 35 – 400 during 17 hours; further additions of soda ash made from time to time (total 400 kg.) so that the batch remains alkaline throughout to Brilliant Yellw paper.

The batch is now heated carefully to 900 during 2.5 hours (a strong effervescence begins at 700 !), held at 900 for 1 hour, and then acidified at 600 with 360 – 400 kg. of hydrochloric acid 200Be’.  The acid must be run in during 14 hour.  The end point is when a weakly acid reaction is given to litmus paper.

The batch is cooled to 350 and dropped to nutsches A and B in two parts.  Each part is washed with 1400 l. of 15% salt solution in 14 parts of 100 l. each (2800 l. for both nutsches), and pulled as dry as possible.

The nutsche-cake weights ca. 31oo kg. and is 40 – 45%.  Mother liquor 14 – 14.50Be’.   Final wash liquor 15 – 160Be’.

1000 cc. ≈ 1.6 – 2.2 cc. N/1 NaNO2.

Yield = 2560 kg. 100% (from 2 nutsches) as 40 – 45% cake estimated by coupling with p-nitrodiazobenzene in acetic acid solution.

Theory yield ; 154.2% by wt. on K acid.  Works yield 128% by wt. = 83% theory.   Quality: The batch is tested by colour preparation.

PB 25602, 553-557. “2,5-Dichloroyl K säure”=1-(2’,5’-Dichlorobenzoylamino)-8-naphthol-4,6-disulfonic acid).德文原件，未抄录。

PB 70058, 8807- 8810. “2,5-Dichloroyl K säure”. 1945年德文生产工艺原件，未抄录。

张澍声 《精细化工中间体及产品生产工艺》。沈阳院 出版。 2006年。P. 572.  1-(2’,5’-二氯苯甲酰氨基)-8-萘酚-4,6-二磺酸。

K酸与2,5-二氯苯甲酰氯缩合而得，又名2,5-二氯苯甲酰基K 酸。（译自BIOS 1152，106）。

在7800 L锻铁橡胶衬里搅拌锅（装有包橡胶浆式搅拌器，转速30转/分）中，加入2450 kg水，再搅拌加入2000 kg 100% 1-氨基-8-萘酚-4,6-二磺酸（实际重量4300 – 4500 kg，为含水44 – 46% 工业品）。用泵压入34.5% 氢氧化钠溶液，直至刚果红试纸的棕色刚刚消失。在此阶段有少量K酸还没有溶解（在实验室检测）。

反应物经滤清压滤机过滤，滤液流入17 m3 橡胶衬里锻铁搅拌锅（顶部衬砖，25转/分浆式搅拌器，加热和冷却蛇管）中，用2700 L水稀释，然后加入111 kg碳酸钠。

在35 – 40℃于17小时内加入1300 kg 2,5-二氯苯甲酰氯，再随时加入总量为400 kg 的碳酸钠，要使反应物对亮黄试纸始终保持碱性。

加完后，于2.5小时内将反应物加热到90℃（在70℃开始产生强烈泡沫），在90℃保持1小时，然后在60℃用360 – 400 kg 31% 盐酸酸化，酸的加入必须在14小时内，当石蕊试纸呈弱酸性反应时即为终点。

反应物冷却到35℃，投入2台抽滤槽抽滤，每台用1400 L 15%盐水洗涤，分为14次，每次100 L，即总计用2800 L水，并尽可能抽干。

得到约3100 kg 1-(2’,5’-二氯苯甲酰氨基)-8-萘酚-4,6-二磺酸滤饼，由两台抽滤槽得到2560 kg 100% 产品。以K酸计，收率83%。

何岩彬 主编《染料品种大全》。沈阳出版社 出版。2018年。P. 2021.  中文名称：8-(2,5-二氯苯甲酰氨基)-1-萘酚-3,5-二磺酸。

CAS号：6407-95-0. 【可合成的染料】C.I. 酸性红161.

何岩彬 主编《染料品种大全》。沈阳出版社 出版。2018年。P. 2012. 中文名称：8-(2,4-二氯苯甲酰氨基)-1-萘酚-3,5-二磺酸。

CAS号：6528-49-0. 【可合成的染料】C.I. 酸性红107；C.I. 酸性红110；C.I. 酸性蓝68； C.I. 颜料红65；C.I. 颜料红67。

同上。P. 2012.  中文名称：8-(2,5-二氯苯甲酰氨基)-1-萘酚-3,5-二磺酸。

CAS号：6407-95-0. 【可合成的染料】C.I. 酸性红161.

【抄注】本产品未见国内有报导，考虑到反应类别相同，所以将两者合并在一起，供读者参考！

陈忠源 2020年。2021年5月23日星期日。