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    Bisphenol-A bis(diphenyl phosphate)-based flame retardant
    1.
    发明授权
    Bisphenol-A bis(diphenyl phosphate)-based flame retardant 失效
    双酚A双（二苯基磷酸酯）系阻燃剂

    公开(公告)号：US06319432B1

    公开(公告)日：2001-11-20

    申请号：US09330688

    申请日：1999-06-11

    申请人： William B. Harrod ,  W. Dirk Klobucar

    发明人： William B. Harrod ,  W. Dirk Klobucar

    IPC分类号： C09K2112

    CPC分类号： C08K5/523 ,  C07F9/12

    摘要： Disclosed is a flame retardant comprising bisphenol A bis(diphenyl phosphate) and its dimer, the former having an HPLC determined 78 to 87 area % and an 85 to less than 90 normalized area %, the normalized area % being based on the total HPLC area % of the bisphenol A bis(diphenyl phosphate) and the dimer. The flame retardant also has a low isopropenylphenyl diphenyl phosphate and a low triphenylphosphate content.

    摘要翻译： 公开了一种包含双酚A双（磷酸二苯酯）及其二聚物的阻燃剂，前者具有HPLC测定为78至87面积％和85至小于90标准化面积％，归一化面积％基于总HPLC面积 ％的双酚A双（磷酸二苯酯）和二聚体。 阻燃剂也具有低的异丙烯基苯基二苯基磷酸酯和低的三苯基磷酸盐含量。

    Purification of arylene polyphosphate esters
    2.
    发明授权
    Purification of arylene polyphosphate esters 失效
    亚磷酸多聚磷酸酯的纯化

    公开(公告)号：US06399685B1

    公开(公告)日：2002-06-04

    申请号：US09734053

    申请日：2000-12-11

    申请人： W. Dirk Klobucar ,  William B. Harrod ,  Billie B. Dadgar ,  Joseph D. McLean ,  Gary D. Heidebrecht ,  Hao V. Phan ,  Thomas R. Nicholas ,  Jeffrey L. Broeker

    发明人： W. Dirk Klobucar ,  William B. Harrod ,  Billie B. Dadgar ,  Joseph D. McLean ,  Gary D. Heidebrecht ,  Hao V. Phan ,  Thomas R. Nicholas ,  Jeffrey L. Broeker

    IPC分类号： C08K552

    CPC分类号： C07F9/025 ,  C07F9/12

    摘要： Emulsion formation is minimized or prevented and hydrolytic product degradation is suppressed during purification of impure bisphenol-A bis(diphenylphosphate). This is accomplished by forming a hydrocarbon solution of bisphenol-A bis(diphenylphosphate) plus impurities in a solvent comprising at least one aromatic hydrocarbon and at least one paraffinic hydrocarbon. Optionally, but preferably, this solution is washed with water or an aqueous buffer solution. Next, the hydrocarbon solution is washed one or more times with an aqueous alkaline washing solution that has a specific gravity that differs from the specific gravity of the hydrocarbon solution by at least about 0.05 gram per cubic centimeter. After each washing the mixture settles into a purified organic phase and a separate aqueous phase, and these phases are separated from each other. After completing the one or more alkaline washings and separations, the resultant purified organic phase is washed one or more times with water to remove alkaline components from the hydrocarbon solution, and after each such washing the washed mixture is settled into a less alkaline purified organic phase and a separate aqueous phase. These phases are separated, and preferably the purified product is recovered from the organic phase.

    摘要翻译： 在纯化双酚A双（二苯基磷酸酯）的纯化期间，乳液形成被最小化或防止并且抑制了水解产物降解。 这通过在包含至少一种芳族烃和至少一种链烷烃的溶剂中形成双酚-A双（二苯基磷酸酯）加杂质的烃溶液来实现。 任选地，但优选地，该溶液用水或缓冲液水溶液洗涤。 接下来，将烃溶液用比表面积与烃溶液的比重不同的碱性水溶液洗涤一次或多次至少约0.05克/立方厘米。 每次洗涤后，混合物沉降到纯化的有机相和单独的水相中，并且这些相彼此分离。 在完成一次或多次碱性洗涤和分离之后，将所得纯化的有机相用水洗涤一次或多次以从烃溶液中除去碱性组分，并且在每次这样洗涤后，将洗涤的混合物沉降到较不碱性的纯化的有机相 和单独的水相。 分离这些相，优选从有机相中回收纯化的产物。

    Preparation of olefinic compounds and carboxylic derivatives thereof
    3.
    发明授权
    Preparation of olefinic compounds and carboxylic derivatives thereof 失效
    烯烃化合物及其羧酸衍生物的制备

    公开(公告)号：US6080888A

    公开(公告)日：2000-06-27

    申请号：US780310

    申请日：1997-01-08

    申请人： Tse-Chong Wu ,  Kannappan C. Chockalingham ,  W. Dirk Klobucar ,  Gary D. Focht

    发明人： Tse-Chong Wu ,  Kannappan C. Chockalingham ,  W. Dirk Klobucar ,  Gary D. Focht

    IPC分类号： C07B37/04 ,  C07C2/86 ,  C07C51/14 ,  C07C63/34

    CPC分类号： C07C2/861 ,  C07B37/04 ,  C07C51/14 ,  C07C2531/22 ,  C07C2531/24

    摘要： Arylolefinic compounds are prepared by reacting aryl halide with an olefinic compound in the presence of a polar liquid reaction medium containing (a) secondary or tertiary amine as a hydrogen halide acceptor (b) a catalyst system formed from (i) Pd or Pd(0) compound, and/or Pd(I) salt or Pd(II) salt, and (ii) a tertiary phosphine ligand, and (c) a reaction accelerating amount of water in the range of about 0.5 to about 5 weight percent of the total weight of the reaction mixture. The arylolefinic compounds can be converted to an arylcarboxylic acid by hydrocarboxylation with CO in a reaction medium freed of amine and containing water and a Pd catalyst system as above in which a copper component may be included, and which preferably includes an ether such as THF.

    摘要翻译： 芳基卤化合物通过芳基卤化物与烯属化合物在极性液体反应介质存在下反应来制备，所述极性液体反应介质含有（a）仲胺或叔胺作为卤化氢受体（b）由（i）Pd或Pd ）化合物和/或Pd（I）盐或Pd（II）盐，和（ii）叔膦配体，和（c）反应加速量的水的范围为约0.5至约5重量％ 反应混合物的总重量。 通过在不含胺并含有水的反应介质中使用CO进行加氢羧化，可以将芳基烯烃化合物转化为芳基羧酸，并且可以包括其中可以包含铜组分的Pd催化剂体系，并且其优选包括醚如THF。

    Preparation and recovery of N-hydrocarbylthiophosphoric triamides or N-hydrocarbylphosphoric triamides
    4.
    发明授权
    Preparation and recovery of N-hydrocarbylthiophosphoric triamides or N-hydrocarbylphosphoric triamides 失效
    N-烃基硫代磷酸三酰胺或N-烃基磷酸三酰胺的制备和回收

    公开(公告)号：US5883297A

    公开(公告)日：1999-03-16

    申请号：US58367

    申请日：1998-04-09

    申请人： Gerald M. Sulzer ,  Chi Hung Cheng ,  W. Dirk Klobucar ,  Charles H. Kolich

    发明人： Gerald M. Sulzer ,  Chi Hung Cheng ,  W. Dirk Klobucar ,  Charles H. Kolich

    IPC分类号： C01C1/16 ,  C07F9/02 ,  C07F9/22 ,  C07F9/26

    CPC分类号： C01C1/164 ,  C07F9/025 ,  C07F9/224 ,  C07F9/26

    摘要： A reaction mixture containing N-hydrocarbylthiophosphoric triamide or N-hydrocarbylphosphoric triamide ("Triamide") is formed by reacting ammonia with N-hydrocarbylaminothiophosphoryl dichloride or N-hydrocarbylaminophosphoryl dichloride in a liquid organic medium, in proportions of at least 16 moles of ammonia per mole of such dichloride and that keep in solution the ammonium chloride co-product formed in the reaction. The temperature of the reaction mixture is kept high enough to keep ammonium chloride-ammonia complex from forming a solid phase in the reaction mixture, but low enough to avoid significant reduction in Triamide yield. The reaction mixture is then caused/allowed to separate into an inorganic phase comprising ammonia, ammonium chloride and co-product thiophosphoric triamide or phosphoric triamide, and an organic phase comprising Triamide, liquid organic medium, dissolved ammonia and, usually, phosphorus impurities. These phases are separated from each other. The ammonia is removed from the organic phase to leave a concentrated solution of Triamide in residual liquid organic medium usually also containing phosphorus impurities. The Triamide is separated or recovered from this residual mixture by continuously introducing a stream of the liquid mixture into a wiped film evaporator operating at a temperature of about 60.degree.-140.degree. C., and at a pressure that avoids solids formation on the heating surface of the wiped film evaporator, and continuously collecting the Triamide product. Triamides are urease inhibitors for use with urea-based fertilizers.

    摘要翻译： 通过使氨与N-烃基氨基硫代磷酰基二氯化物或N-烃基氨基磷酰基二氯化物在液体有机介质中反应，按每摩尔至少16摩尔氨的比例形成含有N-烃基硫代磷酰三胺或N-烃基磷酸三酰胺（“三酰胺”）的反应混合物 的这种二氯化物，并保持溶液中形成的氯化铵副产物在反应中。 反应混合物的温度保持足够高以保持氯化铵 - 氨络合物在反应混合物中形成固相，但足够低以避免三酰胺产率的显着降低。 然后使反应混合物分离成包含氨，氯化铵和副产物硫代磷酸三酰胺或磷酸三酰胺的无机相，以及包含三酰胺，液体有机介质，溶解氨和通常为磷杂质的有机相。 这些阶段相互分离。 从有机相中除去氨，留下通常也含有磷杂质的残留液体有机介质中的三酰胺浓缩溶液。 通过将液体混合物流连续地引入到在约60-140℃的温度下操作的擦拭膜蒸发器中并且在避免在加热表面上形成固体的压力下将三酰胺分离或回收 的擦拭膜蒸发器，并连续收集三酰胺产物。 三酰胺是用于尿素肥料的尿素酶抑制剂。

    Anionic polymerization process
    9.
    发明授权
    Anionic polymerization process 有权
    阴离子聚合工艺

    公开(公告)号：US06657028B1

    公开(公告)日：2003-12-02

    申请号：US10211648

    申请日：2002-08-01

    申请人： J. Todd Aplin ,  Charles H. Kolich ,  W. Dirk Klobucar ,  Kimberly A. Maxwell

    发明人： J. Todd Aplin ,  Charles H. Kolich ,  W. Dirk Klobucar ,  Kimberly A. Maxwell

    IPC分类号： C08F448

    CPC分类号： C08F12/04 ,  C08F4/48

    摘要： A batch process for the anionic polymerization of a styrenic monomer is described. The process brings together a liquid saturated hydrocarbon diluent, an ether promoter, an organolithium initiator and a styrenic monomer in such a way so as to maintain the reaction mixture at or below about 55° C. and so that the amount of organolithium initiator employed is in the range of about 1 to about 10 mol %, based upon the total amount of styrenic monomer to be added. Favorable polydispersity and molecular weight polymer characteristics are obtained.

    摘要翻译： 描述了苯乙烯单体的阴离子聚合的间歇方法。 该方法将液体饱和烃稀释剂，醚助催化剂，有机锂引发剂和苯乙烯类单体混合在一起，以使反应混合物保持在或低于约55℃，使得所用有机锂引发剂的用量为 在约1至约10mol％的范围内，基于待加入的苯乙烯类单体的总量。 获得有利的多分散性和分子量聚合物特性。