CAS号 [5855-78-7] 生产工艺。   2-氯-5-氨基-4-磺酸基苯甲酸

CAS名：Benzoic acid, 5-amino-2-chloro-4-sulfo-     历史参考文献：Beil. 待检索

用途：有机合成，染料中间体等。 LookChem网登录生产与经营单位10家。 反应类别：硝基还原。

FIAT 1313, 92-95.（=胶卷PB 85172）。2-Chloro-5-amino-4-sulfobenzoic acid = CA Säure. (Hoechst). 美国人译自德文，无资料来源。

反应式：本人有加注，德文原件未抄录。硝基CA酸，暂未找到其CAS号，如有读者可以提供，本人还可以再立项上网。

Used for dyestuffs for lacquers.  漆用染料。  Plant capacity: 8 tons.  设备生产能力：8吨。

Equipment:  设备：

1) 1 brick-lined dissolving vessel for the“Nitro-CA-acid”.  Working volume, about 6 cu. m.

2) 1 Wooden vat, 6 cu. m., for the dissolved CA-acid。  3) 1 brick-lined reducing vessel with a working volume of about 8 cu. m.

4) 1 precipitating vat, 12 cu. m., with cooling coil, for the finished product。 

5) 1 iron sludge“Monstre”press, capable of being washed out, with 30 chamber 1200 X 1200。

6) 1 acid-proof suction filter with receiver。  7) 1 storage vessel and 1 measuring vessel for crude 200Be’ hydrochloric acid。

Materials used per ton: 每吨原料用量：

Nitro CA-acid, M.W. 281.5   1197 kg。  Iron turnings sieved   715 kg。

Sodium carbonate about   380 kg。    Hydrochloric acid crude of 200Be’ about   900 kg。

Service requirements per ton of product:  每吨公用工程单耗：

Electricity   340 kwh。   Steam   14 tons。   Water   260 cu. m.。   Compressed air   4800 cu. m.

Procedure:  操作步骤：

670 kg of“Nitro CA-acid”(100%), molecular weight 281.5, as a moist acid product of about 60 – 65% strength are stirred in 2000 l of water in the brick-lined reducing apparatus which contains ca. 400 kg of screened iron turnings cauterized in about 1.5 cu. m. of water or wash liquor (from the proceeding operation) with ca. 10 kg of acetic acid.

The mass is reduced boiling and tested with Mohrs salt（抄注：Ferrous ammonium sulfate = [1185-57-5]）for completion of the reaction.  When the reduction is finished, the mass is made alkaline with about 200 – 220 kg of sodium carbonate and filtered boiling from the iron sludge.  The iron sludge is washed with boiling water, the first part of the wash liquor being combined with the mother liquor and the second part – about 1.5 cu. m. – is introduced into the reducer for the next reduction.  In the precipitating vat the CA-acid is precipitated from the mother liquor combined with the first wash liquor, in the form of a well crystallized product by adding about 500 kg of crude hydrochloric acid of 200Be’.  The whole is cooled to water temperature and the precipitated CA-acid is filtered on the suction filter.  The product analyzes 75 – 80%; molecular weight 251.5.

Yield: 560 kg of CA-acid, 100%, M. W. 251.5 = 93.6% of the theoretical amount.

Control: 生产控制分析：

Test for the completion of the reduction with Mohrd’ salt (Ferrous ammonium sulfate).  Test of the iron sludge has been well washed.  Determination of the content of CA-acid by titration with n/1-nitrite solution (good potassium iodide starch paper!).  In the laboratory of the Dyestuffs Plant the quality of the CA-acid is tested by formation of dyestuff.

Quality: 原料及产品质量分析：

The Nitro CA-acid（抄注：暂未找到其CAS号）is well crystallized product with adhering acid, analyzing 60 – 65%, molecular weight 281.5.  The iron turnings have to be free form coarse constituents.  Hydrochloric acid crude of 200Be’; usual commercial product.  Sodium carbonate; usual commercial product.

The finished product is a well crystallized light substance analyzing 75 – 80%, M. W. 251.5.

抄录说明：以下为从甲苯磺化开始到氯化和硝化的产品质量分析要求。其中 [104-15-1] 和 [51084-27-6] ，本人已上网，英文译文，不再抄录。

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. 163.  2-氯-5-氨基-4-磺酸基苯甲酸。

2-氯-5-氨基-4-磺酸基苯甲酸又名CA 酸。在8000 L衬砖还原锅中，加入约400 kg铁粉与1500 L水（或洗水）打浆，再加入约10 kg醋酸，670 kg 100% 硝基CA 酸（2-氯-5-硝基-4-磺酸基苯甲酸，为湿的酸产品，含量60 – 65%）与2000 L水搅拌加入，进行沸腾还原，并用莫尔盐检验反应的完成。当还原结束，反应物用约200 kg碳酸钠调节为碱性。沸腾过滤出铁泥，并用沸水洗涤铁泥，洗水的第一部分与母液合并，第二部分（约1500 L）送入还原锅供下次反应。在沉淀槽中加入约500 kg 32% 粗盐酸，使CA酸从母液和第一部分洗水中以很好的结晶产品沉淀出来。冷却至室温，抽滤出CA 酸，为75 – 80% 滤饼。得到560 kg 100% 2-氯-5-氨基-4-磺酸基苯甲酸，收率93.6%。

PB 70361, 6837. “CA-acid”(2-Chloro-5-amino-4-sulfo-1-benzoic acid). By Waldmueller.  May 13, 1937. In German. 未抄录。

PB 73377, 2429-2431.  CA-acid. 这是美国人编写的英文战地考察报告，未抄录。

国内出版物：本人手头资料有限，暂未见到有报导！

何岩彬 主编 《染料品种大全》。沈阳出版社 出版。2018年。P. 1879.  中文名称：5-氨基-2-氯-4-磺酸基苯甲酸。

【可合成的染料】C.I. 活性黄13；C.I. 颜料红68。

【预告】作为一名“技术资料抄编者”，历史文献抄录上网已进入第五年，由于手头资料有限，所以准备进入正常日期上网！不再是“全年无休”，请读者谅解！

陈忠源 2020年6月11日星期四。