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31. 发明授权

US07429549B2 Process for improved coupling of rubbery polymers 失效
标题翻译：改进橡胶状聚合物偶联的方法
公开(公告)号：US07429549B2
公开(公告)日：2008-09-30
申请号：US10966192
申请日：2004-10-15
申请人： Adel Farhan Halasa , Wen-Liang Hsu
发明人： Adel Farhan Halasa , Wen-Liang Hsu
IPC分类号： B01J31/00
CPC分类号： C08F297/04 , C08F297/044
摘要： Rubbery polymers made by anionic polymerization can be coupled with tin halides or silicon halides to improve the characteristics of the rubber for use in some applications, such as fire treads. In cases where the rubbery polymer was synthesized utilizing a polar modifier it is difficult to attain a high level of coupling. This invention is based upon the unexpected finding that coupling efficiency can be significantly improved by conducting the coupling reaction in the presence of a lithium salt of a saturated aliphatic alcohol, such as lithium t-amylate. This invention discloses a process for coupling a living rubbery polymer that comprises reacting the living rubbery polymer with coupling agent selected from the group consisting of tin halides and silicon halides in the presence of a lithium salt of a saturated aliphatic alcohol. The lithium salt of the saturated aliphatic alcohol can be added immediately prior to the coupling reaction or it can be present throughout the polymerization and coupling process. Lithium t-amylate reacts with water to form t-amyl alcohol during steam stripping. Since t-amyl alcohol forms an azeotrope with hexane, it co-distills with hexane and can contaminate recycle feed streams. This problem of recycle stream contamination can be solved by using metal salts of cyclic alcohols that do not co-distill with hexane or form compounds during steam stripping which co-distill with hexane. Thus, the use of metal salts of cyclic alcohols is preferred for this reason and because they are considered to be environmentally safe.
摘要翻译：通过阴离子聚合制备的橡胶聚合物可与锡卤化物或卤化硅偶联，以改善用于某些应用中的橡胶的特性，例如防火踏面。在使用极性改性剂合成橡胶状聚合物的情况下，难以获得高水平的偶联。本发明基于意想不到的发现，通过在饱和脂肪醇的锂盐如叔戊醇锂的存在下进行偶联反应可以显着改善偶联效率。本发明公开了一种使活性橡胶状聚合物偶合的方法，其包括在饱和脂肪醇的锂盐存在下使活性橡胶状聚合物与选自锡卤化物和卤化硅的偶联剂反应。饱和脂肪醇的锂盐可以在偶联反应之前立即加入，或者可以在整个聚合和偶联过程中存在。在蒸汽汽提期间，叔戊醇钠与水反应形成叔戊醇。由于叔戊醇与己烷形成共沸物，因此与己烷共蒸馏，可能污染再循环进料流。循环流污染的这个问题可以通过使用在与汽油共蒸馏的汽提过程中不与己烷共蒸馏或形成化合物的环醇的金属盐来解决。因此，由于这个原因，优选使用环状醇的金属盐，并且因为它们被认为是环境安全的。

32. 发明申请

US20070293610A1 Silica reinforced rubber composition containing an ionic compound and article having a component thereof 失效
标题翻译：含有离子性化合物的硅橡胶组合物及其成分的制品
公开(公告)号：US20070293610A1
公开(公告)日：2007-12-20
申请号：US11455608
申请日：2006-06-19
申请人： Adel Farhan Halasa , Wen-Liang Hsu , Aaron Scott Puhala
发明人： Adel Farhan Halasa , Wen-Liang Hsu , Aaron Scott Puhala
IPC分类号： C08K5/52
CPC分类号： B60C1/0016 , B60C1/0025 , B60C11/0058 , B60C19/08 , C08K5/19 , C08K5/3445 , C08K5/50 , C08K2201/001 , C08L21/00
摘要： This invention relates to a silica reinforced rubber composition containing an ionic compound and article having a component thereof. The invention particularly relates to an article such as a rubber tire having a component of such rubber composition. Said ionic compound is composed of a combination of an organic cation moiety and an organic or inorganic anion moiety. Said ionic compound is desirably an ionically conductive ionic compound. The invention particularly relates to improvement of one or more physical properties of a rubber composition by an inclusion of such ionic compound and/or providing a path of least electrical resistance for a electrically resistive component of an article such as a tire by an inclusion in the rubber composition of said component of an ionically conductive ionic compound composed of a combination of an organic cation moiety and an organic or inorganic anion moiety.
摘要翻译：本发明涉及一种含有离子化合物的二氧化硅增强橡胶组合物及其组分。本发明特别涉及具有这种橡胶组合物成分的橡胶轮胎的制品。所述离子化合物由有机阳离子部分和有机或无机阴离子部分的组合构成。所述离子化合物理想地是离子导电的离子化合物。本发明特别涉及通过包含这种离子化合物来改善橡胶组合物的一种或多种物理性能和/或通过包含在轮胎中的方式为诸如轮胎的制品的电阻部件提供最小电阻的路径由有机阳离子部分和有机或无机阴离子部分的组合构成的离子导电离子化合物的所述组分的橡胶组合物。

33. 发明授权

US07087549B2 Calcium-based catalyst system 失效
标题翻译：钙基催化剂体系
公开(公告)号：US07087549B2
公开(公告)日：2006-08-08
申请号：US11106813
申请日：2005-04-15
申请人： Adel Farhan Halasa , Wen-Liang Hsu , John Robert Zuppo, III
发明人： Adel Farhan Halasa , Wen-Liang Hsu , John Robert Zuppo, III
IPC分类号： B01J31/00
CPC分类号： C08F136/08 , C08F236/10 , C08F4/54
摘要： This invention reveals a catalyst system for use in isothermal polymerizations which consists essentially of (a) an organolithium compound, (b) a calcium alkoxide and (c) a lithium alkoxide. The subject invention further discloses a process for synthesizing a random styrene-butadiene rubber having a low vinyl content by a process which comprises copolymerizing styrene and 1,3-butadiene under isothermal conditions in an organic solvent in the presence of a catalyst system which consists essentially of (a) an organolithium compound, (b) a calcium alkoxide and (c) a lithium alkoxide. An amine can also be added to the catalyst system to increase the molecular weight (Mooney viscosity) of the rubber.
摘要翻译：本发明揭示了用于等温聚合的催化剂体系，其基本上由（a）有机锂化合物，（b）醇盐和（c）醇锂组成。本发明还公开了一种合成具有低乙烯基含量的无规苯乙烯 - 丁二烯橡胶的方法，该方法包括在等温条件下在有机溶剂中在催化剂体系存在下共聚苯乙烯和1,3-丁二烯的方法，所述催化剂体系基本上组成（a）有机锂化合物，（b）烷氧基钙和（c）醇锂。还可以向催化剂体系中加入胺以提高橡胶的分子量（门尼粘度）。

34. 发明授权

US07041761B2 Functionalized monomers for synthesis of rubbery polymers 失效
标题翻译：用于合成橡胶状聚合物的官能化单体
公开(公告)号：US07041761B2
公开(公告)日：2006-05-09
申请号：US10894562
申请日：2004-07-20
申请人： Adel Farhan Halasa , Wen-Liang Hsu
发明人： Adel Farhan Halasa , Wen-Liang Hsu
IPC分类号： C08F236/14 , C08F2/06
CPC分类号： C08C19/44 , C08F236/10 , C08F236/14 , Y10T152/10495
摘要： The present invention relates to a process for synthesizing a rubbery polymer that comprises copolymerizing at least one conjugated diolefin monomer and at least one functionalized monomer in an organic solvent at a temperature which is within the range of 0° C. to about 150° C., wherein the polymerization is initiated with an anionic initiator, wherein the polymerization is conducted in the absence of conventional polar modifiers, and wherein the functionalized monomer is of the structural formula: wherein the R′ groups in repeat units and in different repeat units can be the same or different and represent hydrogen atoms or alkyl groups containing from 1 to about 4 carbon atoms, wherein x represents an integer from 1 to about 10, and wherein the R groups in repeat units and in different repeat units can be the same or different and represent alkyl groups containing from 1 to about 10 carbon atoms or alkoxy groups containing from 1 to about 10 carbon atoms.
摘要翻译：本发明涉及一种合成橡胶状聚合物的方法，该方法包括在0℃至约150℃的温度范围内使至少一种共轭二烯烃单体与至少一种官能化单体在有机溶剂中共聚。其中所述聚合由阴离子引发剂引发，其中所述聚合在不存在常规极性改性剂的情况下进行，并且其中所述官能化单体具有以下结构式：其中重复单元和不同重复单元中的R'基团可以是相同或不同，表示含有1至约4个碳原子的氢原子或烷基，其中x表示1至约10的整数，并且其中重复单元和不同重复单元的R基团可以相同或不同并且表示含有1至约10个碳原子的烷基或含有1至约10个碳原子的烷氧基。

35. 发明授权

US07022783B2 Group III-B metal catalyst system 有权
标题翻译： III-B族金属催化剂体系
公开(公告)号：US07022783B2
公开(公告)日：2006-04-04
申请号：US10765485
申请日：2004-01-27
申请人： Wen-Liang Hsu , Adel Farhan Halasa , Chad Aaron Jasiunas
发明人： Wen-Liang Hsu , Adel Farhan Halasa , Chad Aaron Jasiunas
IPC分类号： C08F4/52 , C08F236/06 , C08F236/08
CPC分类号： C08F36/04 , C08F136/06 , C08F136/08 , C08F4/58 , C08F4/545 , C08F236/06 , C08F236/08
摘要： The subject invention relates to a technique for synthesizing rubbery non-tapered, random, copolymers of 1,3-butadiene and isoprene. These rubbery copolymers exhibit an excellent combination of properties for utilization in tire sidewall rubber compounds for truck tires. By utilizing these isoprene-butadiene rubbers in tire sidewalls, tires having improved cut growth resistance can be built without sacrificing rolling resistance. Such rubbers can also be employed in tire tread compounds to improve tread wear characteristics and decrease rolling resistance without sacrificing traction characteristics. This invention more specifically discloses a process for the synthesis of isoprene-butadiene rubber which comprises copolymerizing isoprene monomer and 1,3-butadiene monomer in an organic solvent in the presence of a Group III-B metal containing catalyst system that is made by the sequential steps of (I) reacting an organometalic compound that contains a metal from Group III-B of the Periodic System with an organoaluminum compound at a temperature which is within the range of 50° C. to 100° C. to produce an aluminum modified Group III-B metal containing catalyst component, and (II) mixing the aluminum modified Group III-B metal containing catalyst component with a halogen containing compound, wherein the catalyst system is void of compounds selected from the group consisting of aliphatic alcohols, cycloaliphatic alcohols, aliphatic thiols, cycloaliphatic thiols, trialkyl silanols, and triaryl silanols.
摘要翻译：本发明涉及一种用于合成1,3-丁二烯和异戊二烯橡胶状非渐变，无规共聚物的技术。这些橡胶状共聚物表现出用于卡车轮胎的轮胎胎侧橡胶化合物中的优异的性能组合。通过在轮胎侧壁中使用这些异戊二烯 - 丁二烯橡胶，可以在不牺牲滚动阻力的情况下构建具有改善的耐切割生长性的轮胎。这种橡胶也可以用在轮胎胎面胶料中以改善胎面磨损特性并降低滚动阻力而不牺牲牵引特性。本发明更具体地公开了一种用于合成异戊二烯 - 丁二烯橡胶的方法，该方法包括在含有III-B族金属的催化剂体系存在下，将异戊二烯单体和1,3-丁二烯单体在有机溶剂中共聚，步骤（I）使含有周期性体系的III-B族金属的有机金属化合物与有机铝化合物在50℃至100℃的温度范围内反应，生成铝改性基团含有III-B族金属的催化剂组分，和（II）将含有铝的改性的含III-B族金属的催化剂组分与含卤素化合物混合，其中催化剂体系没有选自脂族醇，脂环族醇，脂族硫醇，脂环族硫醇，三烷基硅烷醇和三芳基硅烷醇。

36. 发明授权

US06869685B2 Adhesion between rubber components 失效
标题翻译：橡胶部件之间的粘合力
公开(公告)号：US06869685B2
公开(公告)日：2005-03-22
申请号：US10630274
申请日：2003-07-30
申请人： Bruce Raymond Hahn , Adel Farhan Halasa , Wen-Liang Hsu
发明人： Bruce Raymond Hahn , Adel Farhan Halasa , Wen-Liang Hsu
IPC分类号： C08J5/12 , C08L21/00 , C09J5/06 , C09J121/00 , B32B25/04
CPC分类号： C08J5/124 , C08J2321/00 , C08L2666/08 , C09J121/00 , Y10T428/31826
摘要： The process of this invention can be utilized to improve the adhesion between rubber components. It is generally most useful for improving the adhesion between two different pre-cured rubber components or for improving the adhesion between a pre-cured rubber component and an uncured (green) rubber component. However, the technique of this invention can also be employed to improve the adhesion between two uncured rubber components. The technique of this invention is based upon the unexpected discovery that low molecular weight trans-1,4-polybutadiene containing rubber compounds can be used to improve the adhesion between rubber components. This invention more specifically reveals a technique for improving the adhesion between a first rubber component and a second rubber component in a process for manufacturing a cured rubber article, said technique comprising the steps of: (1) positioning a layer of an adhesion-promoting rubber composition which is comprised of a low molecular weight trans-1,4-polybutadiene rubber between the first rubber component and the second rubber component, (2) bringing the first rubber component into contact with one side of the layer of adhesion-promoting rubber composition and bringing the second rubber composition into contact with the other side of the layer of adhesion-promoting rubber composition and (3) curing the first rubber composition, the second rubber composition and the adhesion-promoting rubber composition together under conditions of heat and pressure to produce the cured rubber article.
摘要翻译：本发明的方法可用于改善橡胶组分之间的粘合性。通常最有用的是改善两种不同的预固化橡胶组分之间的粘附性或改善预固化橡胶组分和未固化的（绿色）橡胶组分之间的粘合性。然而，本发明的技术也可用于改善两种未固化橡胶组分之间的粘合性。本发明的技术基于意想不到的发现，即低分子量的反式-1,4-聚丁二烯的橡胶化合物可用于改善橡胶组分之间的粘合性。本发明更具体地揭示了在固化橡胶制品的制造方法中提高第一橡胶组分和第二橡胶组分之间的粘合力的技术，所述技术包括以下步骤：（1）将粘合促进橡胶层在第一橡胶组分和第二橡胶组分之间由低分子量反式1,4-聚丁二烯橡胶组成的组合物，（2）使第一橡胶组分与粘合促进橡胶组合物层的一侧接触并使第二橡胶组合物与粘合促进橡胶组合物的另一侧接触，以及（3）在热和压力条件下将第一橡胶组合物，第二橡胶组合物和粘合促进橡胶组合物固化在一起，生产固化橡胶制品。

37. 发明授权

US06686504B2 Synthesis of soluble functionalized lithium initiators 失效
标题翻译：可溶性官能化锂引发剂的合成
公开(公告)号：US06686504B2
公开(公告)日：2004-02-03
申请号：US09944664
申请日：2001-08-31
申请人： Adel Farhan Halasa , Wen-Liang Hsu
发明人： Adel Farhan Halasa , Wen-Liang Hsu
IPC分类号： G09B1102
CPC分类号： B60C1/0016 , C07F1/005 , C07F1/02 , C08C19/44 , C08F36/04 , C08F4/488
摘要： This invention discloses a process for making dilithium initiators in high purity. This process can be conducted in the absence of amines which is desirable since amines can act as modifiers for anionic polymerizations. The dilithium compounds made are highly desirable because they are soluble in aromatic solvents. The present invention more specifically discloses a process for synthesizing a dilithium initiator which comprises reacting diisopropenylbenzene with a tertiary alkyl lithium compound in an aromatic solvent at a temperature which is within the range of about 0° C. to about 100° C. The present invention further discloses a process for synthesizing m-di-(1-lithio-1-methyl-3,3-dimethylbutyl)benzene which comprises reacting diisopropenylbenzene with tertiary-butyllithium in an aromatic solvent at a temperature which is within the range of about 0° C. to about 100° C. The present invention also discloses a process for synthesizing a functionalized lithium initiator which comprises reacting a dilithium initiator with a alkylaminoaryl compound of the structural formula: wherein R, R′, and R″ can be the same or different, wherein R is selected from the group consisting of hydrogen atoms, alkyl groups, aryl groups, alkaryl groups, and amino aryl groups, and wherein R′ and R″ represent alkyl groups.
摘要翻译：本发明公开了一种制备高纯度二锂引发剂的方法。该方法可以在不存在胺的情况下进行，因为胺可以用作阴离子聚合的改性剂。所制备的二锂化合物是非常需要的，因为它们可溶于芳族溶剂。本发明更具体地公开了一种合成二锂引发剂的方法，其包括在芳族溶剂中在约0℃至约100℃的温度范围内使二异丙烯基苯与叔烷基锂化合物反应。本发明进一步公开了一种合成间二 - （1-锂 - 1-甲基-3,3-二甲基丁基）苯的方法，该方法包括使二异丙烯基苯与叔丁基锂在芳族溶剂中在约0℃的范围内本发明还公开了一种合成官能化锂引发剂的方法，该方法包括使二锂引发剂与以下结构式的烷基氨基芳基化合物反应：其中R，R'和R“可以相同或不同的，其中R选自氢原子，烷基，芳基，烷芳基和氨基芳基，并且其中R'和R“表示烷基 l组。

38. 发明授权

US06583244B1 Synthesis of rubber having a low vinyl content 失效
标题翻译：低乙烯基含量的橡胶的合成
公开(公告)号：US06583244B1
公开(公告)日：2003-06-24
申请号：US09999854
申请日：2001-10-31
申请人： Chad Aaron Jasiunas , John Robert Zuppo, III , Adel Farhan Halasa , Wen-Liang Hsu
发明人： Chad Aaron Jasiunas , John Robert Zuppo, III , Adel Farhan Halasa , Wen-Liang Hsu
IPC分类号： C08F446
CPC分类号： C08F4/48 , C08C19/44 , C08F36/04
摘要： Metal salts of cyclic alcohols can be used as modifiers in lithium initiated solution polymerizations of diene monomers into rubbery polymers having a low vinyl content. For instance, such initiator systems can be used in the copolymerization of styrene and isoprene to produce low vinyl styrene-isoprene rubber having a random distribution of repeat units that are derived from styrene. It is important for such polymerizations to be conducted in the absence of polar modifiers, such as Lewis bases. The subject invention more specifically discloses an initiator system which is comprised of (a) a lithium initiator and (b) a metal salt of a cyclic alcohol, wherein said initiator system is void of polar modifiers. The present invention also discloses a process for preparing a rubbery polymer having a low vinyl content which comprises: polymerizing at least one diene monomer with a lithium initiator at a temperature which is within the range of about 5° C. to about 100° C. in the presence of a metal salt of a cyclic alcohol, wherein the molar ratio of the metal salt of the cyclic alcohol to the lithium initiator is within the range of about 0.05:1 to about 10:1, and wherein the process is conducted in the absence of polar modifiers.
摘要翻译：环醇的金属盐可以用作二烯单体的锂引发溶液聚合成具有低乙烯基含量的橡胶状聚合物中的改性剂。例如，这种引发剂体系可以用于苯乙烯和异戊二烯的共聚合以制备具有衍生自苯乙烯的重复单元的随机分布的低乙烯基苯乙烯 - 异戊二烯橡胶。在没有极性改性剂如路易斯碱的情况下进行这种聚合是重要的。本发明更具体地公开了一种引发剂体系，其包括（a）锂引发剂和（b）环状醇的金属盐，其中所述引发剂体系没有极性改性剂。本发明还公开了一种制备低乙烯基含量的橡胶状聚合物的方法，该方法包括：在约5℃至约100℃范围内的温度下，用锂引发剂聚合至少一种二烯单体。在环醇的金属盐的存在下，其中环醇与锂引发剂的金属盐的摩尔比在约0.05:1至约10:1的范围内，并且其中所述方法在没有极性改性剂。

39. 发明授权

US06558805B2 Functionalized rubbery polymer containing polysiloxane 失效
标题翻译：含有聚硅氧烷的官能化橡胶状聚合物
公开(公告)号：US06558805B2
公开(公告)日：2003-05-06
申请号：US09970110
申请日：2001-10-03
申请人： Abderrahim Khadir , Adel Farhan Halasa , Wen-Liang Hsu
发明人： Abderrahim Khadir , Adel Farhan Halasa , Wen-Liang Hsu
IPC分类号： B32B904
CPC分类号： C08G77/442 , Y10T152/10495 , Y10T428/31663
摘要： The present invention relates to an anionic polymerization technique for synthesizing functionalized rubbery polymers containing polysiloxane that have excellent characteristics for utilization in (a) tire tread compounds that are highly loaded with silica, (b) shiny tire side-wall compounds, and (c) tire building bladders having improved mold release characteristics. The rubbery polymers of this invention can optionally be coupled with tin halides or silicon halides to further improve the characteristics of the rubber for use in tire tread compounds. The present invention more specifically discloses a process for synthesizing a rubbery polymer that comprises (1) polymerizing at least one conjugated diolefin monomer to produce a living rubbery polymer, wherein said polymerization is optionally carried out in the presence of a polar modifier, wherein said polymerization is an anionic polymerization that is initiated with an alkylsilyloxy protected functional lithium initiator having a structural formula selected from the group consisting: wherein X represents a group IVa element selected from the group consisting of carbon, silicon, germanium, and tin, wherein Y represents phosphorous or nitrogen, wherein R represents alkyl groups that can be the same or different, wherein the alkyl groups contain from 1 to about 8 carbon atoms, and wherein A represents an alkylene group containing from 1 to about 8 carbon atoms; (2) adding a hexaalkylcyclotrisiloxane monomer to the living rubbery polymer; (3) allowing the hexaalkylcyclotrisiloxane monomer to polymerize to produce a living polysiloxane containing rubber; and optionally, (4) reacting the living polysiloxane containing rubber with a coupling agent selected from the group consisting of tin halides and silicon halides to produce a coupled polysiloxane containing rubber.
摘要翻译：本发明涉及一种用于合成含有聚硅氧烷的官能化橡胶聚合物的阴离子聚合技术，其具有优异的（a）高度负载二氧化硅的轮胎胎面胶料，（b）有光泽的轮胎侧壁化合物，（c）具有改善脱模特性的轮胎成型气囊。本发明的橡胶状聚合物可以任选与锡卤化物或卤化硅偶联，以进一步改善用于轮胎胎面胶料的橡胶的特性。本发明更具体地公开了一种合成橡胶状聚合物的方法，其包括（1）聚合至少一种共轭二烯单体以制备活性橡胶状聚合物，其中所述聚合反应任选在极性改性剂存在下进行，其中所述聚合是由具有选自以下的结构式的烷基甲硅烷氧基保护的官能锂引发剂引发的阴离子聚合：其中X表示选自碳，硅，锗和锡的IVa族元素，其中Y表示磷或氮，其中R表示可以相同或不同的烷基，其中烷基含有1至约8个碳原子，并且其中A表示含有1至约8个碳原子的亚烷基; （2）向活性橡胶状聚合物中加入六烷基环三硅氧烷单体; （3）使六烷基环三硅氧烷单体聚合以制备含有活性聚硅氧烷的橡胶; 和（4）使含有活性聚硅氧烷的橡胶与选自卤化锡和卤化硅的偶合剂反应，生成含有橡胶的偶联聚硅氧烷。

40. 发明授权

US06518214B2 Synthesis of functionalized lithium initiator 失效
标题翻译：官能化锂引发剂的合成
公开(公告)号：US06518214B2
公开(公告)日：2003-02-11
申请号：US09865326
申请日：2001-05-25
申请人： Adel Farhan Halasa , Wen-Liang Hsu
发明人： Adel Farhan Halasa , Wen-Liang Hsu
IPC分类号： B01J3100
CPC分类号： C07F1/02 , C07F7/0803 , C07F7/2208 , C07F9/5068 , C08F4/48
摘要： This invention discloses a process for making dilithium initiators in high purity. This process can be conducted in the absence of amines which is desirable since amines can act as modifiers for anionic polymerizations. The dilithium compounds made are highly desirable because they are soluble in aromatic solvents. The present invention more specifically discloses a process for synthesizing a dilithium initiator which comprises reacting disopropenylbenzene with a tertiary alkyl lithium compound in an aromatic solvent at a temperature which is within the range of about 0° C. to about 100° C. The present invention further discloses a process for synthesizing m-di-(1-methyl-3,3-dimethylbutyllithio)benzene which comprises reacting diisopropenylbenzene with tertiary-butyllithium in an aromatic solvent at a temperature which is within the range of about 0° C. to about 100° C. The present invention also discloses a process for synthesizing a functionalized lithium initiator which comprises the steps of (1) reacting diisopropenylbenzene with a tertiary alkyl lithium compound in an aromatic solvent at a temperature which is within the range of about 0° C. to about 100° C. to produce a dilithium initiator; and (2) reacting the dilithium initiator with a halide compound selected from the group consisting of (a) tin halides, (b) silicon halides, (c) amine halides, and (d) phosphorus halides of the structural formula: wherein X represents a halogen atom, and wherein R1, R2, and R3 represent alkyl groups, aryl groups, and/or alkoxy groups containing from 1 to about 10 carbon atoms.
摘要翻译：本发明公开了一种制备高纯度二锂引发剂的方法。该方法可以在不存在胺的情况下进行，因为胺可以用作阴离子聚合的改性剂。所制备的二锂化合物是非常需要的，因为它们可溶于芳族溶剂。本发明更具体地公开了一种合成二锂引发剂的方法，其包括在芳族溶剂中在约0℃至约100℃的温度范围内使二丙烯基苯与叔烷基锂化合物反应。本发明进一步公开了一种合成间二 - （1-甲基-3,3-二甲基丁基二硫基）苯的方法，该方法包括使二异丙烯基苯与叔丁基锂在芳族溶剂中在约0℃至约本发明还公开了一种合成官能化锂引发剂的方法，该方法包括以下步骤：（1）使二异丙烯基苯与叔烷基锂化合物在芳族溶剂中在约0℃的范围内至约100℃以产生二锂引发剂; 和（2）使二锂引发剂与选自（a）卤化锡，（b）卤化硅，（c）胺卤化物和（d）以下结构式的卤化磷的卤化物反应：其中X表示卤素原子，并且其中R 1，R 2和R 3表示含有1至约10个碳原子的烷基，芳基和/或烷氧基。

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