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1. 发明授权

US4338261A Process for the preparation of 1-naphthylamine-4,6-disulphonic acid and 1-naphthylamine-2,4,6-trisulphonic acid 失效
标题翻译： 1-萘胺-4,6-二磺酸和1-萘胺-2,4,6-三磺酸的制备方法
公开(公告)号：US4338261A
公开(公告)日：1982-07-06
申请号：US247416
申请日：1981-03-25
申请人： Heinz U. Blank , Horst Behre , Hans W. Linden , Werner Mentzel
发明人： Heinz U. Blank , Horst Behre , Hans W. Linden , Werner Mentzel
IPC分类号： C07C309/47 , C07C67/00 , C07C301/00 , C07C303/06 , C07C143/60
CPC分类号： C07C303/06
摘要： Improved process for the preparation of 1-naphthylamine-4,6-disulphonic acid wherein the sulphonation of the 1-naphthylamine-6-sulphonic acid is carried out by adding the oleum at a temperature of 10.degree. to 70.degree. C., either to initially introduce sulphuric acid simultaneously with the 1-naphthylamine-6-sulphonic acid or to 1-naphthylamine-6-sulphonic acid, which is dissolved or suspended in sulphuric acid, and by using such a molar ratio of sulphur trioxide to 1-naphthylamine-6-sulphonic acid that 1.2 to 3 mols of sulphur trioxide are present per mol of 1-naphthylamine-6-sulphonic acid. The sulphonation mixture formed in the preparation can be sulphonated in a second sulphonation stage to 1-naphthylamine-2,4,6-trisulphonic acid.
摘要翻译：制备1-萘胺-4,6-二磺酸的改进方法，其中1-萘胺-6-磺酸的磺化是通过在10℃至70℃的温度下加入发烟硫酸来进行的，最初与1-萘胺-6-磺酸或溶解或悬浮在硫酸中的1-萘胺-6-磺酸同时引入硫酸，并且通过使用三氧化硫与1-萘胺-6-磺酸的摩尔比， 6-磺酸，每摩尔1-萘胺-6-磺酸存在1.2〜3摩尔三氧化硫。在制备中形成的磺化混合物可以在第二个磺化阶段中磺化成1-萘胺-2,4,6-三磺酸。

2. 发明授权

US4407762A Process for the isolation of 1-naphthylamine-4,8-disulphonic acid 失效
标题翻译：分离1-萘胺-4,8-二磺酸的方法
公开(公告)号：US4407762A
公开(公告)日：1983-10-04
申请号：US410746
申请日：1982-08-23
申请人： Heinz U. Blank , Horst Behre , Hans W. Linden , Werner Mentzel
发明人： Heinz U. Blank , Horst Behre , Hans W. Linden , Werner Mentzel
IPC分类号： C07C309/47 , C07C67/00 , C07C301/00 , C07C303/44 , C07C143/60
CPC分类号： C07C303/44
摘要： Process for the isolation of 1-naphthylamine-4,8-disulphonic acid from sulphonation mixtures containing it according to which process the sulphonation mixture is introduced into preheated water in such a manner that, at the start of crystallization, a temperature of at least 100.degree. C. is reached and the 1-naphthylamine-4,8-disulphonic acid is separated from the mother liquor at a temperature not higher than 70.degree. C. The process is applied particularly advantageously for the isolation of 1-naphthylamine-4,8-disulphonic acid from sulphonation mixtures which have been obtained by introducing in turns alkali metal sulphate, 1-naphthylamine-8-sulphonic acid and SO.sub.3 into sulphuric acid which has been introduced initially, a total of 1.5 to 3 mols of SO.sub.3 and 0.6 to 1.5 mols of alkali metal sulphate being employed per mol of 1-naphthylamine-8-sulphonic acid.
摘要翻译：从含有它的磺化混合物中分离出1-萘胺-4,8-二磺酸的方法，根据该方法，将磺化混合物引入预热的水中，使得在结晶开始时，温度至少为100 达到C，并且在不高于70℃的温度下将1-萘胺-4,8-二磺酸与母液分离。该方法特别有利地用于分离1-萘胺-4,8 来自磺化混合物的二磺酸通过将碱金属硫酸盐，1-萘胺-8-磺酸和SO 3引入到最初引入的硫酸中，总共含有1.5至3摩尔的SO 3和0.6至1.5 每摩尔1-萘胺-8-磺酸使用碱金属硫酸盐的摩尔数。

3. 发明授权

US4393234A Process for the preparation of 3-hydroxybenzoic acid 失效
标题翻译： 3-羟基苯甲酸的制备方法
公开(公告)号：US4393234A
公开(公告)日：1983-07-12
申请号：US378922
申请日：1982-05-17
申请人： Heinz U. Blank , Eike Gabel , Ernst Goldschmitt , Werner Mentzel
发明人： Heinz U. Blank , Eike Gabel , Ernst Goldschmitt , Werner Mentzel
IPC分类号： C07C51/367 , C07C65/05 , C07C65/04
CPC分类号： C07C309/00 , C07C51/367
摘要： 3-Hydroxybenzoic acid is obtained by reaction with an alkali metal hydroxide at a temperature of 220.degree. to 450.degree. C. and under a pressure of 1 to 120 bars, from a technical 3-sulphobenzoic acid mixture which contains sulphuric acid and/or sulphur trioxide and which contains at least 75% by weight of 3-sulphobenzoic acid, relative to the total organic constituents present, and not more than 35% by weight of sulphuric acid and/or SO.sub.3, relative to the total mass. For this purpose, this technical 3-sulphobenzoic acid mixture, if desired after dilution with an equal volume of water, is mixed with sufficient 50 to 100% strength by weight alkali metal hydroxide wherein the remaining 50 to 0% by weight consists essentially of water, for 2.5 to 8 mols of alkali metal hydroxide to be present per mol of 3-sulphobenzoic acid, after neutralization of the sulphuric acid and all the sulpho and carboxyl groups. In general, 10 to 45% by weight of water are present in the batch. The reaction mixture is acidified with a mineral acid to a pH value of less than 4, if appropriate after dilution with water, and the 3-hydroxybenzoic acid is isolated at temperatures within the range from -5.degree. C. to +40.degree. C.
摘要翻译：通过在含有硫酸和/或硫的工业3-磺基苯甲酸混合物的温度在220-450℃和1至120巴的压力下与碱金属氢氧化物反应获得3-羟基苯甲酸三氧化硫，相对于存在的总有机成分含有至少75重量％的3-磺基苯甲酸，相对于总质量不超过35重量％的硫酸和/或SO 3。为此目的，如果需要，在等体积水稀释后，将该技术性3-磺基苯甲酸混合物与足量的50至100％重量的碱金属氢氧化物混合，其中剩余的50至0重量％基本上由水对于每摩尔3-磺基苯甲酸存在的2.5至8摩尔碱金属氢氧化物，中和硫酸和所有磺基和羧基后。通常，批料中存在10至45重量％的水。如果在用水稀释后，将反应混合物用无机酸酸化至pH值小于4，并且在-5℃至+ 40℃的温度下分离出3-羟基苯甲酸。

4. 发明授权

US4354038A Process for the preparation of 3-hydroxybenzoic acid 失效
标题翻译： 3-羟基苯甲酸的制备方法
公开(公告)号：US4354038A
公开(公告)日：1982-10-12
申请号：US257676
申请日：1981-04-27
申请人： Ruthard Potthast , Werner Mentzel , Horst-Dieter Kramer
发明人： Ruthard Potthast , Werner Mentzel , Horst-Dieter Kramer
IPC分类号： C07C65/03 , C07C51/00 , C07C51/367 , C07C51/377 , C07C67/00
CPC分类号： C07C51/367
摘要： A process for the preparation of an alkali metal salt of 3-hydroxybenzoic acid and the preparation of 3-hydroxybenzoic acid therefrom is disclosed wherein sulphophthalic acid or a salt thereof is reacted with an alkali metal hydroxide at a temperature in the range of 200.degree. to 300.degree. C. at a pressure of 10 to 30 bars.
摘要翻译：公开了一种制备3-羟基苯甲酸的碱金属盐及其制备方法，其中将磺基邻苯二甲酸或其盐与碱金属氢氧化物反应，温度范围为200- 300℃，压力为10〜30巴。

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