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1. 发明授权

US06333411B1 Method for production of hydroxylammonium phosphate in the synthesis of caprolactam 失效
标题翻译：己内酰胺合成中磷酸羟铵的生产方法
公开(公告)号：US06333411B1
公开(公告)日：2001-12-25
申请号：US09221211
申请日：1998-12-24
申请人： Diego Fernandez Echegaray , Antonio Augusto M. Velloso , Matthew Lincoln Wagner
发明人： Diego Fernandez Echegaray , Antonio Augusto M. Velloso , Matthew Lincoln Wagner
IPC分类号： C07D20104
CPC分类号： C07D201/06 , C07D201/10
摘要： A method for production of caprolactam. The method involves: (a) reacting air with ammonia gas in an ammonia conversion zone to produce nitric oxide; (b) oxidizing at least a portion of the nitric oxide to nitrogen dioxide to produce an NOx-rich process gas stream; (c) reactively absorbing the NOx-rich gas stream with phosphoric acid containing solution in an absorption zone to form nitrate ions; (d) contacting the nitrate ions with air in a degassing zone to produce a nitrate-rich aqueous process stream; (e) reducing the nitrate-rich aqueous stream with hydrogen in the presence of phosphoric acid to produce hydroxylammonium phosphate; (f) oximating the hydroxylammonium phosphate with cyclohexanone to produce cyclohexanone oxime; and (g) converting the cyclohexanone oxime to caprolactam. According to the invention, supplemental oxygen is added downstream of the ammonia conversion zone to increase the quantity and rate of formation of nitrogen dioxide in the NOx-rich process gas stream.
摘要翻译：一种生产己内酰胺的方法。该方法包括：（a）在氨转化区中使空气与氨气反应以产生一氧化氮;（b）将至少一部分一氧化氮氧化成二氧化氮以产生富含NO x的工艺气流;（c）在吸收区中用含磷酸溶液反应性吸收富含NO x的气流，形成硝酸根离子;（d）使硝酸根离子与脱气区的空气接触，产生富含硝酸盐的含水工艺流;（e）富含硝酸盐的含水流在磷酸存在下用氢气生成磷酸羟铵;（f）用环己酮肟化磷酸羟铵以制备环己酮肟; 并且（g）将环己酮肟转化为己内酰胺。根据本发明，在氨转化区的下游添加补充氧以增加富氮过程气流中二氧化氮的形成量和速率。

2. 发明授权

US06469163B1 Method for production of hydroxylamine sulfate in the conventional process for the synthesis of caprolactam 有权
标题翻译：用于合成己内酰胺的常规方法生产硫酸羟胺的方法
公开(公告)号：US06469163B1
公开(公告)日：2002-10-22
申请号：US09221209
申请日：1998-12-24
申请人： Diego Fernandez Echegaray , Antonio Augusto M. Velloso , Matthew Lincoln Wagner
发明人： Diego Fernandez Echegaray , Antonio Augusto M. Velloso , Matthew Lincoln Wagner
IPC分类号： C07D20104
CPC分类号： C07D201/06 , C07D201/10
摘要： An improvement in the conventional process for the production of caprolactam. The process involves: (a) reacting air with ammonia gas in an ammonia conversion zone to produce nitric oxide; (b) oxidizing a portion of the nitric oxide to nitrogen dioxide to produce an NOx-rich process gas stream; (c) reacting the NOx-rich stream with ammonium carbonate in a nitriting zone to produce ammonium nitrite; (d) reducing the ammonium nitrite to hydroxylamine diammonium sulfate; (e) hydrolyzing the hydroxylamine diammonium sulfate to hydroxylamine sulfate; (f) oximating the hydroxylamine sulfate with cyclohexanone to produce cyclohexanone oxime; and (g) converting the cyclohexanone oxime to caprolactam. The process is improved by adding supplemental oxygen downstream of the ammonia conversion zone to increase the quantity and rate of formation of nitrogen dioxide in the NOx-rich process gas stream.
摘要翻译：制备己内酰胺的常规方法的改进。该方法包括：（a）在氨转化区中使空气与氨气反应以产生一氧化氮;（b）将一部分氧化氮氧化成二氧化氮以产生富含NO x的工艺气流;（c）使在氮化区中用碳酸铵生成富含NO x的物流以产生亚硝酸铵;（d）将亚硝酸铵还原为羟胺二硫酸铵;（e）将羟胺二硫酸铵水解成硫酸羟胺;（f）用环己酮将硫酸羟胺酸化生产环己酮肟; 并且（g）将环己酮肟转化为己内酰胺。通过在氨转化区下游加入补充氧以提高富氮过程气流中二氧化氮形成的数量和速率，从而提高了工艺。

3. 发明授权

US6165435A Method and production of nitric acid 失效
标题翻译：方法和生产硝酸
公开(公告)号：US6165435A
公开(公告)日：2000-12-26
申请号：US220818
申请日：1998-12-24
申请人： Diego Fernandez Echegaray , Antonio Augusto M. Velloso , Matthew Lincoln Wagner
发明人： Diego Fernandez Echegaray , Antonio Augusto M. Velloso , Matthew Lincoln Wagner
IPC分类号： C01B21/38 , C01B21/26 , C01B21/40
CPC分类号： C01B21/262 , C01B21/40
摘要： A process is described for producing nitric acid involving oxidizing ammonia gas to form dinitrogen tetroxide gas, reacting the dinitrogen tetroxide with water in an absorption zone to form aqueous nitric acid and nitric oxide gas, removing a nitric acid/nitric oxide stream from the absorption zone and feeding the stream into a nitric acid bleaching zone, removing impurities from the nitric acid in the bleaching zone to form nitric acid product and adding supplemental oxygen gas to one or more of the reaction streams to increase nitric acid production and or strength. The improvement involves injecting the supplemental oxygen into a nitric acid-containing process stream to form a gas bubble/liquid mixture in the stream, the mixture forming a fine dispersion of gas bubbles having diameters of less than about 0.1 mm. According to the invention, increased interfacial surface is created between the gas bubbles and the liquid mixture to facilitate removal of impurities from the liquid phase and shifting of the reaction.
摘要翻译：描述了用于生产涉及氧化氨气以形成四氧化二氮气体的硝酸的方法，在吸收区中使四氧化二氮与水反应以形成硝酸和一氧化氮水溶液，从吸收区除去硝酸/一氧化氮流并将料流输送到硝酸漂白区中，从漂白区中的硝酸中除去杂质，形成硝酸产物，并向一个或多个反应流中加入补充的氧气，以增加硝酸的产生和/或强度。改进之处在于将补充氧气注入含硝酸的工艺流中以在流中形成气泡/液体混合物，混合物形成具有小于约0.1mm直径的气泡的精细分散体。根据本发明，在气泡和液体混合物之间产生增加的界面表面，以便于从液相中除去杂质并使反应移动。

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