CAS号 [83-31-8] 生产工艺 1,8-萘磺内酯 

CAS名：1,8-Naphthosultone      Beil. 19. E^3/4, 323. 

用途：染料中间体。LookChem网登录生产与经营单位40家。

PB 74197.  Reports on dyes and dye intermediates.  共868页。

PB 74197,817.  Naphtosulton. 德文生产工艺，未抄录。反应式如下，本人有加注。

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. 199 1,8-萘磺内酯，译自PB 74197,817。

反应釜内加入4.5 m³水或上批的洗涤水，230 L 96% 硫酸和1.5 – 1.6吨周位酸滤饼（相当于280 kg亚硝酸钠），加热至50 – 55℃。于约16小时内加入1000 L 30% 亚硝酸钠溶液，在80℃短时间加热，冷却过滤，以磺内酯形式分离出来，即以此形式使用。 

BIOS 1152,14.（=胶卷PB 81027）。 !-Naphthol-8-sulphonic acid. (Leverkusen).  英国人译自德文，暂未找到德文原件。

General: Naphthalenesultone (BIOS Report 1157) is heated with dilute NaOH（抄注：其钠盐CAS号[20215-36-5]）.

Plant: 

1*15,000 l. vat, rubber-lined, homogeneous lead-lined coil;

1*Pitch pine agitator;

1*Nutsche and Monteju.

Materials:

Naphthalenesultone ≈ 530 kg

nitrite 720 kg

50% caustic soda liquor 1,300 kg

salt 300 kg

hydrochloric acid 19.5⁰Be’. 40 kg Na₂SO_3。

Process:  The vat is charged with 4,000 l. of water and two batches (≈530 kg. nitrite) sultone then fed in and the contents of the vat heated to 80℃.  The 720 kg. of 30% caustic soda liquor are added, and heating is then continued to 100℃. and the whole diluted to 12,000 l. 

Test: 500 cc. are diluted with water and filtered.  There should be no residue left on the paper. 

If this test is satisfactory, the solution is treated with 40 kg. of sodium sulphite and solidified whilst hot with hydrochloric acid to congo acid. 10% salt is then added and the whole cooled with stirring. 

Test: The solid and filtrate are estimated with nitrite.  The solid should give a yield around 95% nitrite.  Filter and dry. Yield: 94-95%. 

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. 198.  1-萘酚-8-磺酸，译自BIOS 1152,14。

在15 m³的槽中加入4000 L水和相当于530 kg的亚硝酸钠的萘磺内酯，加热到80℃。加入720 kg 30% NaOH，继续加热到100℃，整个稀释到12000 L。取样稀释后过滤，滤纸上应无残渣。

加入40 kg Na₂SO₃，趁热用盐酸酸化至对刚果红呈酸性。加10% 食盐，搅拌冷却，过滤，干燥。收率94 – 95%。 

侯乐山 主编《中国精细化工产品集 – 原料及中间体10396种》。中国化工信息中心 出，版2006年。P. 943 1,8-萘磺酸内酯。

CAS：83-31-8. 【产品性状】淡黄色针状晶体。【生产厂】山东平原永恒染料化工有限公司。 

周位酸重氮化：

PB 25627, 2264. 周位酸重氮化，1938年9月德文生产工艺，1美元，美国人介绍如下。

    1-Naphthylamine-8-sulfonic acid is diazotized and thereby precipitated except for 2 – 3% as the diazonium compound is difficultly soluble. 未抄录。 

FIAT 1313,II, 93.（=胶卷PB 85172）。 The amino group in Peri acid is diazotized as follows: 美国人译自德文，未说明资料来源。

1227 kilograms of Peri acid (approximately 60% paste),  730 kilograms of Peri acid (100% equivalent) are charged into 1500 literts of water in a 22,000 liter, acid proof brick lined tub, equipped with wooden agitator.  After mixing well 690 kilograms of hydrochloric acid (31.5%) are run in, followed by 5000 to 6000 kilograms of ice.

760 liters od sodium nitrite solution (40%) are now added slowly over a period of 20 hours, the temperature being maintained between 5 and 8℃ by the addition of ice as needed.  When all the nitrite has been added, the charge is allowed to agitate for 6 – 7 hours longer to complete the diazotization.  The end point is determined by the permanence of a slight excess of nitrous acid when teats with starch iodide paper and the absence of free Peri acid, which is determined by spotting upon filter paper adjacent to a spot of diluted aqueous pyridine, which produces a blue violet color, if free Peri acid is still present, due to coupling with the diazo compound.

When finished, the diazo compound is filtered off in a wooden filter press, dressed with nitro or polyvinyl filter colth, the diazo compound being fairly insoluble.  The loss amounts to about 3%.

细田豊《理论制造染料化学》。技報當 出版。1957年。P. 729. 周位酸重氮化，译自FIAT 1313.

    ペリ酸730 kgをペ-ストの形で22 m³ 槽に水1.5 tとまぜ盐酸690 kg，冰5 – 6 tを加えた後NaNO₂ 40%液760 lを5 - 8⁰ で20 hで加6 – 7 h搅拌しジアゾ化が终つたなら不溶性のジアゾ化合物を滤過する。 

BIOS1152, 119.（=胶卷PB 81027）。周位酸重氮化。英国人译自德文，未说明资料来源。

Materials:  Peri acid (free acid)  740 kg. = 3.32 mol.   Hydrochloric acid 20⁰Be’  690 kg.    Sodium nitrite   295 kg.

Procedure:  (a) Diazotisation:  操作步骤：重氮化。

The Peri acid is pasted with 1500 l. water and 690 kg. hydrochloric acid.  Sodium nitrite (295 kg.) is then added with the temperature maintained at 5 – 8℃ by the addition of ice.  The diazotization takes 1 day to complete and 5 – 6 tones of ice are required.

The insoluble diazo compound is filtered off (press).

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. 575  周位酸重氮化，译自BIOS 1152,119。

740 kg周位酸（1-氨基萘-8-磺酸）用1500 L水和690 kg 30% 盐酸打浆。然后加入295 kg 亚硝酸钠，同时加冰保持温度在5 – 8℃，重氮化进行1天才完成，需要加入5 – 6 t冰。 压滤出不溶解的重氮物。 

A.B.Eльцова《染料及中间体实验室合成方法》。1985年。§2.3  还原亮橙KX，其中1-磺酸-8-萘重氮盐的合成。[20653-35-4]。

将装有搅拌，温度计和滴液漏斗的200毫升瓷杯，置于冰浴，固定在卡圈内。加入30毫升水，12毫升32% 盐酸和14.8克8-氨基-1-萘磺酸，搅拌冷却至5℃，滴加由5.9克亚硝酸钠和10毫升水配成的亚硝酸钠溶液，于5 – 8℃搅拌30分钟，定期用刚果红试纸测反应物酸度（pH ＜3），用碘淀粉试纸测亚硝酸，以控制重氮化反应，当碘淀粉试纸变蓝即为重氮化终点。重氮盐可用2-萘酚或H-酸碱性溶液测渗圈检出。用布氏漏斗过滤出不溶性重氮盐，滤饼用100毫升冷水（5 – 10℃）洗涤（每次25毫升），然后用50毫升冷乙醇和50毫升冷乙醚洗涤，产品置于培养皿中，于暗处空气中干燥约20分钟。

得量：14.6克（96%），浅灰色粉末，遇光变黑，可用深色瓶存放。 

何岩彬 主编《染料品种大全》。沈阳出版社 出版，2018年，P. 1921 中文名称：1,8-萘磺内酯。 未列入。 

陈忠源  2021年6月20日星期日