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1. 发明授权

US6080889A Production of tertiary amine oxides 失效
标题翻译：生产叔胺氧化物
公开(公告)号：US6080889A
公开(公告)日：2000-06-27
申请号：US53444
申请日：1998-04-01
申请人： Rebecca S. Cochran , Andrea P. Wight , Douglas H. Krzystowczyk , Dustin H. Thomas
发明人： Rebecca S. Cochran , Andrea P. Wight , Douglas H. Krzystowczyk , Dustin H. Thomas
IPC分类号： C07C291/04 , C07C291/00
CPC分类号： C07C291/04
摘要： Exothermic oxidation of tertiary amine with aqueous hydrogen peroxide in an aqueous reaction medium formed or being formed from tertiary amine, aqueous hydrogen peroxide, carbon dioxide, and optionally chelating agent and/or additional water, is initiated at about 15 to about 25.degree. C., and while agitating the reaction mixture, the temperature is allowed to rise adiabatically to a temperature in the range of about 50 to about 100.degree. C. In this way, it is possible to produce tertiary amine oxides with very low levels, if any, of nitrosamine impurity, without addition of metal and/or phosphorus-containing components recommended in the prior art. Even though a substantial portion of the reaction is performed at temperatures in the range of about 50-100.degree. C., nitrosamine content, if any, in the resultant tertiary amine oxide product can be well below 30 ppb. Use of such relatively exothermically achieved high temperatures in turn results in faster reaction rates and enables use of shorter reaction periods.
摘要翻译：在叔胺，过氧化氢水溶液，二氧化碳和任选的螯合剂和/或另外的水中形成或形成的水性反应介质中的叔胺与过氧化氢水溶液的放热氧化在约15至约25℃下开始并且在搅拌反应混合物的同时，将温度绝热升温至约50至约100℃的温度。以这种方式，可以生产具有非常低水平（如果有的话）的叔胺氧化物，的亚硝胺杂质，而不添加现有技术中推荐的金属和/或含磷成分。即使大部分反应在约50-100℃的温度下进行，所得叔胺氧化物产物中的亚硝胺含量（如果有的话）也可以低于30ppb。这种相对放热实现的高温的使用反过来导致更快的反应速率并且能够使用更短的反应时间。

2. 发明授权

US6037497A Process for producing amine oxides 失效
标题翻译：氧化胺生产工艺
公开(公告)号：US6037497A
公开(公告)日：2000-03-14
申请号：US162956
申请日：1998-09-29
申请人： Dustin H. Thomas , Douglas H. Krzystowczyk , Luc G. Six
发明人： Dustin H. Thomas , Douglas H. Krzystowczyk , Luc G. Six
IPC分类号： C07C291/04 , C07C292/02
CPC分类号： C07C291/04
摘要： A process is described in which tertiary amine is oxidized with hydrogen peroxide in the presence of carbon dioxide until the reaction mass contains (i) about 0.5 to about 6.5%, and preferably about 1 to about 2.5%, of unreacted free amine, (ii) carbon dioxide, and (iii) unreacted hydrogen peroxide. At this point individual portions of the reaction mass are dispensed into a plurality of shipping containers, or alternatively, the reaction mass is transferred to a cooling vessel, cooled therein, and then dispensed into a plurality of shipping containers. Thereafter the reaction is allowed to slowly continue to completion at ambient temperature in the shipping containers with venting of off-gases, as required. The process makes it possible to produce amine oxides with increased plant throughput without need for additional plant reaction equipment such as glass-lined reactors, and the consequent substantial additional capital investment. Also the process enables production of amine oxides having, if any, very low levels of nitrosoamine impurities without increasing reactor residence time and without need for such additional plant reaction equipment and associated additional capital outlay.
摘要翻译：描述了一种方法，其中叔胺在二氧化碳存在下用过氧化氢氧化，直到反应物料包含（i）约0.5至约6.5％，优选约1至约2.5％的未反应游离胺，（ii ）二氧化碳，和（iii）未反应的过氧化氢。此时，将反应物质的各个部分分配到多个运输容器中，或者，将反应物质转移到冷却容器中，在其中冷却，然后分配到多个运输容器中。此后，根据需要，允许反应在环境温度下在运输容器中缓慢地继续完成，排放废气。该方法使得可以生产具有增加的植物产量的氧化胺，而不需要额外的植物反应设备，例如玻璃衬里的反应器，并且因此大量额外的资本投资。此外，该方法还能够生产具有非常低水平的亚硝基杂质的氧化胺，而不增加反应器停留时间，并且不需要这种额外的植物反应设备和相关的附加资本支出。

3. 发明授权

US5593619A Granulated flame retardant products 失效
标题翻译：颗粒状阻燃产品
公开(公告)号：US5593619A
公开(公告)日：1997-01-14
申请号：US406225
申请日：1995-03-16
申请人： Scott A. Bottelberghe , Dustin H. Thomas , Terry M. Shurtleff , Roland G. Poertner
发明人： Scott A. Bottelberghe , Dustin H. Thomas , Terry M. Shurtleff , Roland G. Poertner
IPC分类号： C09K21/08 , C09K21/14
CPC分类号： C09K21/08
摘要： This invention relates to compositions containing improved granulated hexabromocyclododecane flame retardant products, flame retardant formulations containing products, and to a process for forming the improved granulated flame retardant products, wherein the granulated product is characterized as having a friability loss of less than about 8 percent.
摘要翻译：本发明涉及包含改进的颗粒状六溴环十二烷阻燃产品，含阻燃剂的产品的组合物，以及形成改进的粒状阻燃产品的方法，其中造粒产品的脆性损失小于约8％。

4. 发明授权

US07999118B2 Process for producing N-halogenated hydantoins 有权
标题翻译：生产N-卤代乙内酰脲的方法
公开(公告)号：US07999118B2
公开(公告)日：2011-08-16
申请号：US11251640
申请日：2005-10-17
申请人： Hassan Y. Elnagar , Bruce C. Peters , Edgar E. Spielman, Jr. , Dustin H. Thomas
发明人： Hassan Y. Elnagar , Bruce C. Peters , Edgar E. Spielman, Jr. , Dustin H. Thomas
IPC分类号： C07D233/74 , C07D233/82
CPC分类号： A01N43/50 , C07D233/82 , Y10T428/2982
摘要： This invention provides a process for the N-halogenation of at least one 5-hydrocarbyl hydantoin and/or at least one 5,5-dihydrocarbyl hydantoin. The process comprises concurrently feeding into a reaction zone (i) water, inorganic base, and 5,5-dimethylhydantoin, these being fed separately and/or in any combination(s), (ii) a separate feed of a brominating agent, and (iii) a separate feed of a chlorinating agent, in proportions such that during all or substantially all of the time the concurrent feeding is occurring halogenation of the 5-hydrocarbyl hydantoin and/or 5,5-dihydrocarbyl hydantoin occurs and resultant halogenated product precipitates in the liquid phase of an aqueous reaction mixture, and in which the pH of the liquid phase is continuously or substantially continuously maintained in the range of about 2.0 to about 8.0 during all or substantially all of the time the concurrent feeding is occurring. Also provided by this invention is a composition of matter which is a halogenated 5-hydrocarbyl hydantoin or a halogenated 5,5-dihydrocarbyl hydantoin, which is a mixture of the 1,3-dibromo-, 1,3-dichloro-, and/or N,N′-bromochloro-species of the halogenated hydantoin.
摘要翻译：本发明提供了至少一种5-烃基乙内酰脲和/或至少一种5,5-二烃基乙内酰脲N-卤化的方法。该方法同时进料到反应区（i）水，无机碱和5,5-二甲基乙内酰脲，这些分别单独和/或以任何组合进料，（ii）单独的溴化剂进料和（iii）氯化剂的单独进料，其比例使得在所有或基本上所有时间内同时进料发生5-烃基乙内酰脲和/或5,5-二烃基乙内酰脲的卤化，得到的卤代产物沉淀在水性反应混合物的液相中，并且其中液相的pH在所有或基本上所有的同时进料期间连续地或基本上连续地保持在约2.0至约8.0的范围内。本发明还提供了一种物质组合物，其是卤代5-烃基乙内酰脲或卤代的5,5-二烃基乙内酰脲，其是1,3-二溴 - ，1,3-二氯 - 和/ 或卤代乙内酰脲的N，N'-溴氯物质。

5. 发明授权

US4593129A Polyphosphazene process 失效
标题翻译：聚磷腈工艺
公开(公告)号：US4593129A
公开(公告)日：1986-06-03
申请号：US601505
申请日：1984-04-18
申请人： R. Woodrow Wilson, Jr. , Dustin H. Thomas
发明人： R. Woodrow Wilson, Jr. , Dustin H. Thomas
IPC分类号： C07C27/00 , C07C29/70 , C07C31/34 , C07C37/66 , C07C39/235 , C07C67/00 , C07F9/06 , C07F9/6581 , C08G79/02 , C07C2/56
CPC分类号： C07C29/70 , C07C37/66 , C07F9/067 , C07F9/65812 , C08G79/02
摘要： A process for making an alkali metal alkoxide (e.g. sodium alkoxide) of a halogen-substituted alcohol (e.g. fluorine-substituted alcohols) by dispersing an alkali metal (e.g. sodium) in a cycloalkane (e.g. cyclohexane) containing a phenol (e.g. o-allylphenol) and adding the resultant dispersion to an ether (e.g. THF) solution of a halogen-substituted alcohol. The resultant alkali metal haloalkoxide solution contains phenoxides and can be reacted with a phosphonitrilic chloride polymer to introduce haloalkoxide and phenoxide substituents.
摘要翻译：通过将碱金属（例如钠）分散在含有苯酚的环烷烃（例如环己烷）中来制备卤素取代的醇（例如氟取代的醇）的碱金属醇盐（例如烷氧基化钠）的方法（例如邻 - 烯丙基苯酚），并将所得分散体加入到卤素取代的醇的醚（例如THF）溶液中。得到的碱金属卤代醇溶液含有苯氧化物，并且可与磷酰氯化聚合物反应以引入卤代醇和苯酚取代基。

6. 发明授权

US06809205B1 Process for producing N-halogenated organic compounds 失效
标题翻译：制备N-卤代有机化合物的方法
公开(公告)号：US06809205B1
公开(公告)日：2004-10-26
申请号：US09484844
申请日：2000-01-18
申请人： Hassan Y. Elnagar , Bruce C. Peters , Edgar E. Spielman, Jr. , Dustin H. Thomas
发明人： Hassan Y. Elnagar , Bruce C. Peters , Edgar E. Spielman, Jr. , Dustin H. Thomas
IPC分类号： C07D23374
CPC分类号： C07D233/82
摘要： The process enables highly effective N-halogenation of a compound having one or more halogenatable amido or imido functional groups in the molecule. The process involves, for example, concurrently feeding into a reactor (i) water, inorganic base, and the compound to be N-halogenated, e.g., a hydantoin, and a feed of (ii) a brominating agent and/or a chlorinating agent. The proportions of these feeds are such that the pH is kept within the range of ca. 5.5-8.5 (preferably 6.5-8.5, and most preferably 6.8-7.2) and one or more of the amido or imido nitrogen atoms is substituted by a bromine or chlorine atom. A feature of the process is that it can be conducted at elevated temperatures as high as about 90° C. without appreciable thermal decomposition of reactants or product. The resultant product continuously precipitates in high yield and purity. Moreover, products can be produced that are very pale yellow to almost pure white in appearance. Further, the process has been found capable of producing 1,3-dibromo-5,5-dimethylhydantoin with far larger particle sizes than previously produced on a commercial basis.
摘要翻译：该方法能够在分子中具有一个或多个可卤化酰氨基或亚氨基官能团的化合物的高效N-卤化。该方法包括例如同时进料到反应器（i）水，无机碱和待卤化的化合物，例如乙内酰脲，和（ii）溴化剂和/或氯化剂的进料。这些进料的比例使得pH保持在约 5.5-8.5（优选6.5-8.5，最优选6.8-7.2），一个或多个酰胺基或亚氨基氮原子被溴或氯原子取代。该方法的特征在于它可以在高达约90℃的高温下进行，而没有明显的反应物或产物的热分解。所得产物以高产率和纯度连续沉淀。此外，可以生产非常浅黄色至几乎纯白色的产品。此外，已经发现该方法能够生产出比以前在商业上生产的粒度大得多的1,3-二溴-5,5-二甲基乙内酰脲。

7. 发明授权

US6166255A Production of tertiary amine oxides 失效
标题翻译：生产叔胺氧化物
公开(公告)号：US6166255A
公开(公告)日：2000-12-26
申请号：US150820
申请日：1998-09-11
申请人： Rebecca S. Cochran , Andrea P. Wight , Douglas H. Krzystowczyk , Dustin H. Thomas
发明人： Rebecca S. Cochran , Andrea P. Wight , Douglas H. Krzystowczyk , Dustin H. Thomas
IPC分类号： C07C291/04 , C07C209/68
CPC分类号： C07C291/04
摘要： Exothermic oxidation of tertiary amine with aqueous hydrogen peroxide in an aqueous reaction medium formed or being formed from tertiary amine, aqueous hydrogen peroxide, carbon dioxide, and optionally chelating agent and/or additional water, is initiated at about 15 to about 25.degree. C., and while agitating the reaction mixture, the temperature is allowed to rise adiabatically to a temperature in the range of about 50 to about 100.degree. C. In this way, it is possible to produce tertiary amine oxides with very low levels, if any, of nitrosamine impurity, without addition of metal and/or phosphorus-containing components recommended in the prior art. Even though a substantial portion of the reaction is performed at temperatures in the range of about 50-100.degree. C., nitrosamine content, if any, in the resultant tertiary amine oxide product can be well below 30 ppb, and the free amine content, if any, can be well below 0.3 wt %. Use of such relatively exothermically achieved high temperatures in turn results in faster reaction rates and enables use of shorter reaction periods.
摘要翻译：在叔胺，过氧化氢水溶液，二氧化碳和任选的螯合剂和/或另外的水中形成或形成的水性反应介质中的叔胺与过氧化氢水溶液的放热氧化在约15至约25℃下开始并且在搅拌反应混合物的同时，将温度绝热升温至约50至约100℃的温度。以这种方式，可以生产具有非常低水平（如果有的话）的叔胺氧化物，的亚硝胺杂质，而不添加现有技术中推荐的金属和/或含磷成分。尽管大部分反应在约50-100℃的温度下进行，但所得叔胺氧化物产物中的亚硝胺含量（如果有的话）可以远低于30ppb，游离胺含量，如果有的话，可以很好地低于0.3wt％。这种相对放热实现的高温的使用反过来导致更快的反应速率并且能够使用更短的反应时间。

8. 发明授权

US06508954B1 1,3-dibromo-5,5-dimethylhydantoin of enhanced properties 有权
标题翻译：增强性能的1,3-二溴-5,5-二甲基乙内酰脲
公开(公告)号：US06508954B1
公开(公告)日：2003-01-21
申请号：US09484687
申请日：2000-01-18
申请人： Hassan Y. Elnagar , Jonathan N. Howarth , Bruce C. Peters , Edgar E. Spielman, Jr. , Dustin H. Thomas
发明人： Hassan Y. Elnagar , Jonathan N. Howarth , Bruce C. Peters , Edgar E. Spielman, Jr. , Dustin H. Thomas
IPC分类号： C02F512
CPC分类号： C07D233/82 , A01N59/00 , Y10S514/951 , A01N25/34 , A01N25/12 , A01N2300/00
摘要： Among the enhanced properties of the 1,3-dibromo-5,5-dimethylhydantoins described are their larger average particle sizes, their compactibility even though devoid of a binder, their excellent free-flowing and low-dust properties, and their more appealing aesthetic qualities, as compared to previously known 1,3-dibromo-5,5-dimethylhydantoins. These novel 1,3-dibromo-5,5-dimethylhydantoins can be produced, for example, by concurrently feeding (i) an aqueous solution or slurry formed from an inorganic base and 5,5-dimethylhydantoin, and (ii) a brominating agent, in proportions such that each nitrogen atom is substituted by a bromine atom, thereby forming product which precipitates in an aqueous reaction mixture. The pH of the reaction mixture is maintained in the range of about 5.5 to about 8.5.
摘要翻译：所描述的1,3-二溴-5,5-二甲基乙内酰脲的增强性能是它们更大的平均粒度，即使没有粘合剂，它们的优异的自由流动性和低灰尘性质，以及它们更具吸引力的美学质量，与以前已知的1,3-二溴-5,5-二甲基乙内酰脲相比。这些新型的1,3-二溴-5,5-二甲基乙内酰脲可以例如通过同时进料（i）由无机碱和5,5-二甲基乙内酰脲形成的水溶液或浆料，和（ii）溴化剂以比例使得每个氮原子被溴原子取代，从而形成在水性反应混合物中沉淀的产物。反应混合物的pH保持在约5.5至约8.5的范围内。

9. 发明授权

US06281176B1 Process for producing betaine/amine oxide mixtures 失效
标题翻译：生产甜菜碱/氧化胺混合物的方法
公开(公告)号：US06281176B1
公开(公告)日：2001-08-28
申请号：US09454983
申请日：1999-12-03
申请人： Rebecca S. Cochran , Patrick C. Hu , Michael S. McCaig , Edmund F. Perkins, Jr. , Joe D. Sauer , Dustin H. Thomas
发明人： Rebecca S. Cochran , Patrick C. Hu , Michael S. McCaig , Edmund F. Perkins, Jr. , Joe D. Sauer , Dustin H. Thomas
IPC分类号： A61K7075
CPC分类号： C07C227/08 , C07C229/12
摘要： This invention provides a process for producing a betaine/amine oxide mixture. This process comprises reacting, in a liquid medium, an alkali metal &ohgr;-halocarboxylate with a first tertiary amine of the formula Ra2RbN, wherein each Ra group is a hydrocarbyl group which independently has from 1 to about 4 carbon atoms, and wherein the Rb group is a hydrocarbyl group which has from about 8 to about 24 carbon atoms, to produce a betaine product solution. To the betaine product solution is added a second tertiary amine of the formula Ra2RbN, wherein each Ra group is a hydrocarbyl group which independently has from 1 to about 4 carbon atoms, and wherein the Rb group is a hydrocarbyl group which has from about 8 to about 24 carbon atoms, to produce an amine/betaine mixture. The first and second tertiary amines can be separate portions of the same amine. Preferably, however, the first and second tertiary amines differ from each other. In a carbon dioxide atmosphere, the amine/betaine mixture is mixed with hydrogen peroxide to yield a betaine/amine oxide mixture.
摘要翻译：本发明提供了一种生产甜菜碱/氧化胺混合物的方法。该方法包括在液体介质中使碱金属ω-卤代羧酸盐与式Ra2RbN的第一叔胺反应，其中每个R a基团是独立地具有1至约4个碳原子的烃基，其中R b基团是具有约8至约24个碳原子的烃基，以产生甜菜碱产物溶液。向甜菜碱产物溶液中加入式Ra2RbN的第二叔胺，其中每个R a基团是独立地具有1至约4个碳原子的烃基，并且其中R b基团是烃基，其具有约8至约24个碳原子，以产生胺/甜菜碱混合物。第一和第二叔胺可以是相同胺的分开部分。然而，优选第一和第二叔胺彼此不同。在二氧化碳气氛中，将胺/甜菜碱混合物与过氧化氢混合以产生甜菜碱/氧化胺混合物。

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