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公开(公告)号：US08071688B2
公开(公告)日：2011-12-06
申请号：US12636250
申请日：2009-12-11
IPC分类号： C08F12/08
摘要： Concurrently fed into a reaction zone held at about 10° C. or less are brominating agent, aluminum halide catalyst, and a solution of anionic styrenic polymer having a GPC Mn about 2000-30,000. The components are in at least two separate feed streams. The feeds are proportioned to maintain (a) the amount of aluminum halide being fed at about 0.8 mole percent or less based on the amount of aromatic monomeric units in the polymer being fed, and (b) amounts of brominating agent and unbrominated polymer in the reaction zone that produce a final washed and dried polymer product containing about 60-71 wt % bromine. The catalyst is deactivated, bromide ions and catalyst residues are washed away from the reaction mixture, and the brominated anionic styrenic polymer is recovered and dried. The dried polymer has a volatile bromobenzene content of about 600 ppm (wt/wt) or less as well as other beneficial properties.
摘要翻译： 同时加入保持在约10℃或更低的反应区域的是溴化剂，卤化铝催化剂和具有大约2000-30,000的GPC Mn的阴离子苯乙烯聚合物溶液。 这些组件至少有两个单独的进料流。 进料成比例以维持（a）基于所加入的聚合物中芳族单体单元的量，以约0.8摩尔％或更少的量加入卤化铝的量，和（b）溴化剂和未溴化聚合物的量 反应区，其产生含有约60-71重量％溴的最终洗涤和干燥的聚合物产物。 催化剂失活，溴化物离子和催化剂残余物从反应混合物中洗去，回收溴化阴离子苯乙烯聚合物并干燥。 干燥的聚合物具有约600ppm（wt / wt）或更低的挥发性溴苯含量以及其它有益特性。
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公开(公告)号：US07638583B2
公开(公告)日：2009-12-29
申请号：US11612991
申请日：2006-12-19
IPC分类号： C08F12/08
摘要： Concurrently fed into a reaction zone held at about 10° C. or less are brominating agent, aluminum halide catalyst, and a solution of anionic styrenic polymer having a GPC Mn about 2000-30,000. The components are in at least two separate feed streams. The feeds are proportioned to maintain (a) the amount of aluminum halide being fed at about 0.8 mole percent or less based on the amount of aromatic monomeric units in the polymer being fed, and (b) amounts of brominating agent and unbrominated polymer in the reaction zone that produce a final washed and dried polymer product containing about 60-71 wt % bromine. The catalyst is deactivated, bromide ions and catalyst residues are washed away from the reaction mixture, and the brominated anionic styrenic polymer is recovered and dried. The dried polymer has a volatile bromobenzene content of about 600 ppm (wt/wt) or less as well as other beneficial properties.
摘要翻译： 同时加入保持在约10℃或更低的反应区域的是溴化剂，卤化铝催化剂和具有大约2000-30,000的GPC Mn的阴离子苯乙烯聚合物溶液。 这些组件至少有两个单独的进料流。 进料成比例以维持（a）以所加入的聚合物中的芳族单体单元的量为基准，以约0.8摩尔％或更少的量加入卤化铝的量，和（b）溴化剂和未溴化聚合物的量 反应区，其产生含有约60-71重量％溴的最终洗涤和干燥的聚合物产物。 催化剂失活，溴化物离子和催化剂残余物从反应混合物中洗去，回收溴化阴离子苯乙烯聚合物并干燥。 干燥的聚合物具有约600ppm（wt / wt）或更低的挥发性溴苯含量以及其它有益特性。
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公开(公告)号：US07632893B2
公开(公告)日：2009-12-15
申请号：US11453542
申请日：2006-06-14
IPC分类号： C08F12/08
摘要： Preparing brominated styrenic polymer by maintaining a mixture formed from (i) brominating agent, (ii) a solvent solution of styrenic polymer, and (iii) aluminum halide catalyst, at −20 to +20° C., and terminating bromination in 20 minutes or less. New brominated anionic styrenic polymers have better melt flow and/or lower initial ΔE values than the best previously-known brominated anionic styrenic polymers. Other features of such new polymers include high thermal stabilities at 320° C. and/or very low initial color values. Brominated styrenic polymers, especially brominated anionic styrenic polymers, are useful as flame retardants for thermoplastic polymers.
摘要翻译： 通过保持由（i）溴化剂，（ii）苯乙烯聚合物的溶剂溶液和（iii）卤化铝催化剂）在-20至+ 20℃形成的混合物，并在20分钟内终止溴化，制备溴化苯乙烯聚合物 或更少。 新的溴化阴离子苯乙烯聚合物具有比先前已知的溴代阴离子苯乙烯聚合物更好的熔体流动和/或较低的初始DeltaE值。 这种新聚合物的其它特征包括在320℃下的高热稳定性和/或非常低的初始颜色值。 溴化苯乙烯聚合物，特别是溴化阴离子苯乙烯聚合物，可用作热塑性聚合物的阻燃剂。
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公开(公告)号：US5760262A
公开(公告)日：1998-06-02
申请号：US877227
申请日：1997-06-17
申请人： Troy E. DeSoto , Ronny W. Lin , John F. Balhoff
发明人： Troy E. DeSoto , Ronny W. Lin , John F. Balhoff
CPC分类号： C07F17/00
摘要： The reaction between a hafnium tetrahalide-diamine adduct and a metallated bis(cyclopentadienyl-moiety containing) ligand, offers great promise as a way of producing racemic hafnocenes, but involves a number of complications. Tetrahydrofuran, a commonly-used solvent/diluent for such reactions, when present in substantial portions in the liquid reaction medium containing the reactants and/or reaction product(s) has been found to cause a substantial reduction in yields of chiral hafnocenes. Apparently the presence of a substantial amount of THF causes or at least results in the formation of increased amounts of the undesirable meso isomer, tends to cause or result in tar formation, and results in a product having poor filterability. Thus large amounts of THF if fed to the reactor with the reactant(s) are purged to a suitably low level, replaced by a liquid aromatic hydrocarbon, and then the reaction mixture is heated to a higher reaction temperature. Large amounts of liquid paraffins and free diamine in the reaction mixture during reaction also contribute to tar formation and reduction in yields of chiral hafnocene. Thus the presence of such materials in the reaction mixture is kept to a minimum. These process modifications make it possible to increase yields of the chiral hafnocene, to reduce formation of the meso isomer, and to sharply reduce the amount of tar formation in the synthesis of chiral hafnocenes from diamine adducts of hafnium tetrahalide and metallated bis(cyclopentadienyl-moiety containing) ligands. Moreover, the hafnocene reaction product so formed has significantly improved filterability characteristics.
摘要翻译： 四卤化铪 - 二胺加合物与金属化的双（环戊二烯基部分）配体之间的反应作为生产外消旋体的方法提供了巨大的希望，但是涉及许多并发症。 已经发现四氢呋喃是用于这种反应的常用溶剂/稀释剂，当存在于含有反应物和/或反应产物的液体反应介质中时，实质上部分地引起手性茂金属的产率的显着降低。 显然，大量THF的存在导致或至少导致不期望的内消旋异构体的增加量的形成，倾向于引起或导致焦油形成，并导致具有差的过滤性的产品。 因此，如果用反应物加入到反应器中，则将大量的THF吹扫至适当的低水平，用液态芳烃代替，然后将反应混合物加热至更高的反应温度。 反应过程中反应混合物中大量的液体石蜡和游离二胺也有助于焦油的形成和手性茂金属的产率的降低。 因此，将反应混合物中这种物质的存在保持最小。 这些方法修饰使得可以增加手性茂金属的产率，减少内消旋异构体的形成，并且在四卤化铪和金属化双（环戊二烯基部分）的二胺加合物合成手性茂金属时急剧减少焦油的产生量 含有）配体。 此外，如此形成的铪矿反应产物具有显着改善的过滤性能。
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公开(公告)号：US20130012663A1
公开(公告)日：2013-01-10
申请号：US13619256
申请日：2012-09-14
申请人： Charles H. Kolich , John F. Balhoff , Douglas W. Luther , Robert C. Herndon, JR. , Ronny W. Linn , Bruce C. Peters , Arthur G. Mack , David A. Lee
发明人： Charles H. Kolich , John F. Balhoff , Douglas W. Luther , Robert C. Herndon, JR. , Ronny W. Linn , Bruce C. Peters , Arthur G. Mack , David A. Lee
IPC分类号： C08F132/04
CPC分类号： C08F6/02 , B29C47/0004 , B29C47/0011 , B29C47/30 , B29C47/38 , B29C47/765 , B29C47/92 , B29C2947/92514 , B29C2947/92704 , C08F6/001 , C08F8/20 , Y10T428/2982 , C08L25/18 , C08F12/08
摘要： Brominated styrenic polymer is recovered from solution in a vaporizable solvent by converting the solution in a devolatilization extruder into a brominated styrenic polymer melt or flow and a separate vapor phase comprised predominately of vaporizable solvent, recovering the melt or flow from the devolatilization extruder, and allowing or causing the melt or flow to solidify. The solidified brominated styrenic polymer can be subdivided into a powder or pelletized form. Pellets so made have improved hardness and/or crush strength properties along with reduced formation of fines. Brominated anionic styrenic polymer is preferably used in the process.
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公开(公告)号：US20100081762A1
公开(公告)日：2010-04-01
申请号：US12631333
申请日：2009-12-04
IPC分类号： C08L25/06 , C08F112/08
摘要： Preparing brominated styrenic polymer by maintaining a mixture formed from (i) brominating agent, (ii) a solvent solution of styrenic polymer, and (iii) aluminum halide catalyst, at −20 to +20° C., and terminating bromination in 20 minutes or less. New brominated anionic styrenic polymers have better melt flow and/or lower initial ΔE values than the best previously-known brominated anionic styrenic polymers. Other features of such new polymers include high thermal stabilities at 320° C. and/or very low initial color values. Brominated styrenic polymers, especially brominated anionic styrenic polymers, are useful as flame retardants for thermoplastic polymers.
摘要翻译： 通过保持由（i）溴化剂，（ii）苯乙烯聚合物的溶剂溶液和（iii）卤化铝催化剂）在-20至+ 20℃形成的混合物，并在20分钟内终止溴化，制备溴化苯乙烯聚合物 或更少。 新的溴化阴离子苯乙烯聚合物具有比最先前已知的溴代阴离子苯乙烯聚合物更好的熔体流动和/或较低的初始＆Dgr; E值。 这种新聚合物的其它特征包括在320℃下的高热稳定性和/或非常低的初始颜色值。 溴化苯乙烯聚合物，特别是溴化阴离子苯乙烯聚合物，可用作热塑性聚合物的阻燃剂。
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公开(公告)号：US20100016530A1
公开(公告)日：2010-01-21
申请号：US12374138
申请日：2007-07-25
申请人： Ronny W. Lin , John F. Balhoff
发明人： Ronny W. Lin , John F. Balhoff
IPC分类号： C08F4/46 , C08F112/08
摘要： This invention provides a process which comprises heating a lithium-containing mixture to one or more temperatures of at least about 90° C. and at one or more pressures sufficient to maintain substantially the entire mixture in the liquid phase. The lithium-containing mixture which comprises water, lithium ions, at least one liquid saturated hydrocarbon, and at least one styrenic polymer formed by anionic polymerization. The amount of water is at least about 10 wt % relative to the weight of the styrenic polymer, and the styrenic polymer has a weight average molecular weight of at least about 1000.
摘要翻译： 本发明提供了一种方法，其包括将含锂混合物加热至至少约90℃的一个或多个温度和足以将基本上整个混合物保持在液相中的一个或多个压力。 包含水，锂离子，至少一种液体饱和烃和至少一种通过阴离子聚合形成的苯乙烯类聚合物的含锂混合物。 水的量相对于苯乙烯类聚合物的重量为至少约10重量％，苯乙烯聚合物的重均分子量为至少约1000。
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8.发明申请Terminating Bromination of Styrenic Polymer in a Bromination Reaction Mixture 审中-公开在溴化反应混合物中终止苯乙烯聚合物的溴化公开(公告)号：US20090264599A1
公开(公告)日：2009-10-22
申请号：US12375549
申请日：2007-08-22
申请人： John F. Balhoff , Charles H. Kolich
发明人： John F. Balhoff , Charles H. Kolich
IPC分类号： C08F8/20
摘要： A brominated styrenic polymer reaction mixture containing at least (i) brominated styrenic polymer, (ii) bromination reaction solvent, (iii) hydrogen bromide, and (iv) Lewis acid bromination catalyst, and an aqueous medium in an amount sufficient to deactivate the Lewis acid catalyst but insufficient to form a separate continuous liquid phase in the resultant mixture are mixed together to terminate bromination. The advantages of using such small amounts of aqueous medium, as well as various follow on procedures are described.
摘要翻译： 含有至少（i）溴化苯乙烯类聚合物，（ⅱ）溴化反应溶剂，（ⅲ）溴化氢和（ⅳ）路易斯酸溴化催化剂的溴化苯乙烯类聚合物反应混合物和含量足以使路易斯酸失活的水性介质 酸催化剂但不足以在所得混合物中形成单独的连续液相混合在一起以终止溴化。 描述了使用这种少量水性介质的优点以及各种方法。
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公开(公告)号：US07446153B2
公开(公告)日：2008-11-04
申请号：US11612705
申请日：2006-12-19
IPC分类号： C08F8/18
摘要： Bromination of styrenic polymer is carried out in a closed reaction system to retain HX coproduct (where HX is HBr or HCl, or both) in the bromination reaction mixture at superatmospheric pressure. Preferably, the reaction mixture which includes the brominated styrenic polymer and substantially all of the HX coproduct formed is discharged into an aqueous quenching medium. By operating in this manner, the reaction is terminated and the brominated styrenic polymer of desired bromine content and substantially all HX coproduct are captured in the same operation, process equipment costs are reduced, and processing of the reaction mixture is facilitated.
摘要翻译： 苯乙烯聚合物的溴化在闭合反应体系中进行，以在超大气压下在溴化反应混合物中保留HX副产物（其中HX为HBr或HCl或两者）。 优选地，将包含溴化苯乙烯聚合物和基本上所有形成的HX副产物的反应混合物排出到含水淬火介质中。 以这种方式操作，终止反应，并且在相同的操作中捕获所需溴含量和基本上所有HX副产物的溴化苯乙烯聚合物，降低了工艺设备成本，并且促进了反应混合物的加工。
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公开(公告)号：US5789631A
公开(公告)日：1998-08-04
申请号：US756104
申请日：1996-11-25
申请人： John F. Balhoff , Ronny W. Lin
发明人： John F. Balhoff , Ronny W. Lin
CPC分类号： C07C25/13 , C07C17/208
摘要： An anhydrous mixture containing a liquid phase and a solids phase formed from components comprising finely-divided sodium fluoride, hexabromobenzene, and a phosphonium catalyst, and optionally a liquid aprotic solvent/diluent, is heated at a temperature and for a time at which sodium bromide and at least one hexahalobenzene containing at least two fluorine atoms are produced. Preferably, the sodium fluoride is activated by one or more of procedures specified herein.
摘要翻译： 将包含细分的氟化钠，六溴苯和鏻催化剂的组分以及任选的液体非质子溶剂/稀释剂的组分的液相和固体相的无水混合物在溴化钠的温度和时间内加热 并且产生至少一种含有至少两个氟原子的六卤代苯。 优选地，氟化钠由本文规定的一种或多种方法活化。
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