CAS号 [83-55-6] 生产工艺。   1-氨基-5-萘酚

CAS名：1-Naphthalenol, 5-amino-    历史参考文献：Beil. 13, 670; E1, 273; E2, 411; E3, 1885; E4, 2090.

用途：酸性蓝70。 硫化棕16。 LookChem网登录生产与经营单位52家。 反应类别：碱熔。

BIOS 986, 42-45.（=胶卷PB 77764）。 1-Amino-5-naphthol (Purpurol). I.G. Mainkur.  英国人译自德文（无资料来源）。

反应式：本人有加注。德文原件未抄录。

Materials charge per Batch.  每批投料量：

669 kg. 1-aminonaphthalene-5-sulphonic acid M.W. 223 = about 1,030 kg. paste (ex Leverkusen and essentially free from 1:8- ).

1,065 kg.  Caustic soda 100%.    2,000 kg.  Hydrochloric acid.

Services Consumptions: 公用工程单耗：略。

Plant Description:  设备：共6项。略。

Process Description:  操作步骤：

Into the cast steel autoclave charge 150-200 l. of water according to the water content of the 1-aminonaphthalene-5-sulphonic acid paste, and 1,065 kg. of caustic soda in small pieces and heat without agitation by direct gas firing.  As soon as all the caustic soda has dissolved start the agitator.  An inner temperature of 200℃.  Lower the gas flame and during 1 hr. charge 1,030 kg. 1-aminonaphthalene-5-sulphonic acid paste = 669 kg. M.W. 223.  When the addition is complete heat during 2-3 hr. to 225-230℃. and then reduce the gas heating to the minimum or shut it off completely according to the progress of the reaction.  In about 1 hr. the temperature rises on its own to 245-250℃.  At this temperature the reaction is often very vigorous.

Test: Dissolve 5 g. of the melt in about 50 c.c. hot water in an Erlenmeyer flask, make exactly neutral with concentrated hydrochloric acid, filter and cool.  By acidulating with concentrated hydrochloric acid no aminonaphthalene sulphonic acid should precipitate and the solution must remain completely clear.

The progress of the reaction is followed by the testing of sample at frequent intervals in the laboratory.  Finally no aminonaphthalene sulphonic acid should be detectable.  The course of the fusion takes 2-3 hr. at 250℃.

Dilute very carefully by slow addition of hot water until a volume of 3,000 l. is reached – there is vigorous frothing at this stage.  Then dilute with cold water to 4,000 l.  The diluted melt is stirred long enough to break up any lumps and give a homogeneous solution in the kettle.  The diluted melt is blown in two halves to the neutralizing kettle, item (2).  Each half is adjusted to 2,500 l.  600 l. of hydrochloric acid run in under the surface and the liquor allowed to stand for several hours so as to allow the residue to settle.  After standing overnight the temperature is about 70-75℃.  The half batch is then filtered through ten chambers of iron press without agitation and the press washed with 400-500 l. of water from the kettle with agitation.  The filtrate and the was water are run into the precipitation kettle where each half is adjusted to exact neutrality with about 400 l. hydrochloric acid (Betagelb and litmus).  The precipitated batch is blown into two lead-lined troughs and after cooling to atmospheric pressure, filtered.  Each filter cake is washed with 300 l. water and sucked as dry as possible.  Each batch gives 4 nutsche loads.   Yield: 430-450 kg. = 85-90% theory.

Remarks: 备注：

    1.  The wash of the final product is restricted to about 300 l. of water per nutsche load because the product has a slight solubility in water.  The presence of inorganic salts in the product is not deleterious from the point of view of colour manufacture.

2.  The product is unstable to drying is unnecessary for the purpose of colour manufacture.

3.  The following control tests are used: (a) 100 c.c. of the batch in the neutralisation kettle adjusted to 2,500 l., is treated with 100 c.c. hydrochloric acid and 100 c.c. water and boiled for 1 hr.  The volume is then adjusted to 1,000 c.c. and 50 c.c. titrated at 5-10℃. with a standard solution of m-nitraniline.  20-25 c.c. of m-nitraniline solution is run in initially, about 50 g. sodium acetate added and titration continued until there is no reaction to nitrodiazobenzene.

(b) The strength of the product is estimated by dissolving 100 g. of the paste in water adding 50 c.c. of hydrochloric acid and boiling for 1/2 hr. until the evolution of sulphur dioxide is complete.  A sample is then filtered, adjusted to one litre and 25 c.c. titrated as above with m-nitraniline solution.

4.  与生产硫化染料有关，略。   5.  生产单耗。略。

抄注：英国人就是这么翻译德文的！这已是历史！这类资料。在国外出版的《化工大全》中是没有的！

细田豊 《理论制造染料化学》1957年。 P. 526.  1-アミノ-5-ナフト- ル.  译自PB 77764.

4.9 m3オ- トクレ- フに水150-200 l，NaOH 1065 kgを装入し，ガス加热で溶し2000で搅拌しながわ，ロ- レント酸669 kg (ペ- ススト1030 kg) を1 hで加え，2-3 hで225-2300に上げ，さらやに1 hで245-250に上げて2-3 h保温する。

湯を徐徐に加えて3 m3にし,水でにうすめて排出し，5 m3にして盐酸1.2 m3を液面下に加えて70-750で1夜静置後滤過し，滤液に盐酸约800 l を加えて正确に中性にしアミノナフト- ルを滤過水洗し，ペ- ストトのまま硫化染料の原料とする。430-450 kg，收率85-90%。

张澍声 《精细化工中间体工业生产技术》1996年。  P. 191.  1-氨基-5-萘酚。 译自BIOS 986, 42.

在铸铁高压釜中加入150-200 L水（根据1-萘胺-5-磺酸滤饼中的水含量）和1065 kg小片状氢氧化钠，在不搅拌下加热。当所有氢氧化钠完全溶解，立即开始搅拌。当内部温度达200℃时，减慢加热速度，于1小时内加入1030 kg 1-氨基萘-5-磺酸滤饼，相当于669 kg干品。加完后于2-3小时内加热到225-230℃，然后主要由反应热于约1小时内升温至245-250℃。在此温度反应往往是很强烈的，熔融在250℃进行约2-3小时，直至检测不出氨基磺酸。

缓慢而仔细地加入热水进行稀释，直至体积达到3000 L，在此阶段会有激烈的泡沫产生。然后用冷水稀释至4000升。稀释的碱熔物要充分搅拌至破碎所有的小块，得到均匀的溶液。将一半加水至2500 L，在表面以下加入600 L盐酸，静置数小时使沉降完全。放置过夜，温度约70-75℃。过滤，用400-500 L水洗涤，滤液和洗水流入沉降锅中，加400 L盐酸调节至中性，冷却，过滤用300升水洗涤，尽可能处理干。得到430-450 kg 1-氨基-5-萘酚为理论量的85-90%。

产品对干燥是不稳定的，通常用于染料的制造可不需干燥。

抄注：本资料未非正式出版物，大学一般不收藏。

PB 74181.  Instructions on the production of dyes. 1930-1946年。上海染料研究所有放大本。

    这是研究所专门到北京中科院放大复制的书本式资料，但是后来去，已看不到了！

PB 74181, 2315-2321.  1-Amino-5-naphthol (purpurol) 德文生产工艺原件。未抄录。

国内出版物：

侯乐山 主编 《中国精细化工产品集 – 原料及中间体10396种》2006年。 P. 45.  1-氨基-5-萘酚。

中国化工信息中心  全国精细化工原料及中间体行业协作组 出版 《版权所有  未经允许  不得翻印》。

1-氨基-5-萘酚

英文名：5-Amino-1-naphthol

分子式：C10H9NO     分子量：159.19

CAS：83-55-6     物质登记状态：已登记

生产厂：山东平原忠臣化工有限公司。网址：www. zhongchen-chem. Com

抄注：资料就这么简单！当然，国内已能生产，上述抄录的资料仅供参考！

何岩彬 主编 《染料品种大全》。 沈阳出版社 出版。 2018年。 P. 1851-2038.  染料中间体及可合成染料。

 P. 1929.  5-羟基-1-萘胺。读者可将上述资料补充在内。

不用多说。老有所乐，乐在其中。

陈忠源 2019年2月18日星期一。