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1. 发明授权

US08581002B2 Process for working up diacetone acrylamide solutions for the preparation of pure diacetone acrylamide 有权
标题翻译：加工双丙酮丙烯酰胺溶液用于制备纯双丙酮丙烯酰胺的方法
公开(公告)号：US08581002B2
公开(公告)日：2013-11-12
申请号：US12597960
申请日：2008-05-08
申请人： Sascha Braune , Bernhard Holub , Christoph Huber
发明人： Sascha Braune , Bernhard Holub , Christoph Huber
IPC分类号： C07C231/06
CPC分类号： C07C231/24 , C07C231/06 , C07C231/22 , C07C233/31
摘要： Improved process for working up diacetone acrylamide solutions, obtained by reaction of acetone or diacetone alcohol with acrylonitrile and sulfuric acid and subsequent dilution and neutralization, in which a) the organic phase obtained subsequent to the neutralization, which comprises the crude diacetone acrylamide, is hydrolyzed by addition of an aqueous alkaline solution in order to remove acrylamide, then b) after phase separation has been carried out, the organic phase, which comprises the crude diacetone acrylamide, is neutralized by addition of an acid, and c) in succession, low-boiling-point byproducts are removed by distillation in the presence of one or more polymerization inhibitors, then t-butylacrylamide is removed by distillation and, finally, the diacetone acrylamide is isolated by product distillation, and d) the diacetone acrylamide thus obtained is converted into its final form.
摘要翻译：通过丙酮或双丙酮醇与丙烯腈和硫酸反应得到的丙酮丙烯酰胺溶液的改进方法，随后的稀释和中和，其中a）包含粗双丙酮丙烯酰胺的中和后获得的有机相被水解通过加入碱性水溶液以除去丙烯酰胺，然后b）进行相分离后，通过加入酸中和含有粗双丙酮丙烯酰胺的有机相，c）连续地低 - 沸点副产物在一种或多种聚合抑制剂存在下通过蒸馏除去，然后通过蒸馏除去叔丁基丙烯酰胺，最后通过产物蒸馏分离双丙酮丙烯酰胺，并且d）将由此获得的双丙酮丙烯酰胺转化进入其最终形式。

2. 发明申请

US20050131246A1 Method for producing 2,2-dichloro or dibromo-phenyl alkyl acetates 审中-公开
标题翻译： 2,2-二氯或二溴 - 苯基烷基乙酸酯的制备方法
公开(公告)号：US20050131246A1
公开(公告)日：2005-06-16
申请号：US10507305
申请日：2003-03-10
申请人： Sylvia Krich , Bernhard Holub
发明人： Sylvia Krich , Bernhard Holub
IPC分类号： C07C67/22 , C07C69/76
CPC分类号： C07C67/22 , C07C69/65
摘要： The invention relates to an improved method for producing 2,2-dichloro or dibromo-phenyl alkyl acetates of formula (1), in which X represents Cl or Br, n represents a whole number from 1 to 5, R represents hydrogen, C1-C8 alkyl, aryl, heteroaryl, C1-C8 alkoxy, aryloxy or halogen and R1 represents C1-C8 alkyl. According to said method, a 2,2-dichloro- or dibromo-phenylacetonitrile of formula (II) is reacted in 0.8 to 2 mol water per mol nitrile of formula (II), 1 to 8 mol alcohol of formula R1OH (III) per mol nitrile of formula (II) and in the presence of 1 to 3 mol HCl or HBr per mol nitrile of formula (II), optionally in the presence of a solvent that is inert in the reaction conditions, to form the corresponding 2,2-dichloro- or dibromo-phenyl alkyl acetates of formula (I), whereby the reaction temperature in the first phase lies between 30 and 60° C. and in the second phase between 60 and 100° C. Once the reaction has taken place, the reaction mixture is cooled to between 20 and 40° C., diluted with water and the 2,2-dichloro- or dibromo-phenyl alkyl acetate of formula (I) is isolated.
摘要翻译：本发明涉及一种制备式（1）的2,2-二氯或二溴 - 苯基烷基乙酸酯的改进方法，其中X表示Cl或Br，n表示1至5的整数，R表示氢， C 1 -C 8烷基，芳基，杂芳基，C 1 -C 8烷氧基，芳氧基或卤素，R 1表示 C 1 -C 8烷基。根据所述方法，式（II）的2,2-二氯或二溴 - 苯基乙腈在0.8-2摩尔水/摩尔的式（II）腈，1至8摩尔的式R 1 OH（III）的醇/ 式（II）的咪唑腈和在1至3mol HCl或HBr / mol式（II）腈存在下，任选地在反应条件下为惰性的溶剂存在下，形成相应的2,2 （I）的二氯或二溴 - 苯基烷基乙酸酯，其中第一相中的反应温度为30至60℃，第二相为60至100℃。一旦发生反应，将反应混合物冷却至20-40℃，用水稀释，分离式（I）的2,2-二氯或二溴 - 苯基烷基乙酸酯。

3. 发明申请

US20100217042A1 PROCESS FOR WORKING UP DIACETONE ACRYLAMIDE SOLUTIONS FOR THE PREPARATION OF PURE DIACETONE ACRYLAMIDE 有权
标题翻译：用于制备纯二胺丙烯酰胺的二胺酮丙烯酰胺溶液的方法
公开(公告)号：US20100217042A1
公开(公告)日：2010-08-26
申请号：US12597960
申请日：2008-05-08
申请人： Sascha Braune , Bernhard Holub , Christoph Huber
发明人： Sascha Braune , Bernhard Holub , Christoph Huber
IPC分类号： C07C231/06
CPC分类号： C07C231/24 , C07C231/06 , C07C231/22 , C07C233/31
摘要： Improved process for working up diacetone acrylamide solutions, obtained by reaction of acetone or diacetone alcohol with acrylonitrile and sulfuric acid and subsequent dilution and neutralization, in which a) the organic phase obtained subsequent to the neutralization, which comprises the crude diacetone acrylamide, is hydrolyzed by addition of an aqueous alkaline solution in order to remove acrylamide, then b) after phase separation has been carried out, the organic phase, which comprises the crude diacetone acrylamide, is neutralized by addition of an acid, and c) in succession, low-boiling-point byproducts are removed by distillation in the presence of one or more polymerization inhibitors, then t-butylacrylamide is removed by distillation and, finally, the diacetone acrylamide is isolated by product distillation, and d) the diacetone acrylamide thus obtained is converted into its final form
摘要翻译：通过丙酮或双丙酮醇与丙烯腈和硫酸反应得到的丙酮丙烯酰胺溶液的改进方法，随后的稀释和中和，其中a）包含粗双丙酮丙烯酰胺的中和后获得的有机相被水解通过加入碱性水溶液以除去丙烯酰胺，然后b）进行相分离后，通过加入酸中和含有粗双丙酮丙烯酰胺的有机相，c）连续地低 - 沸点副产物在一种或多种聚合抑制剂存在下通过蒸馏除去，然后通过蒸馏除去叔丁基丙烯酰胺，最后通过产物蒸馏分离双丙酮丙烯酰胺，并且d）将由此获得的双丙酮丙烯酰胺转化进入其最终形式

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