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21. 发明授权

US6140434A Synthesis of high vinyl rubber 有权
标题翻译：高乙烯基橡胶的合成
公开(公告)号：US6140434A
公开(公告)日：2000-10-31
申请号：US227367
申请日：1999-01-08
申请人： Adel Farhan Halasa , Wen-Liang Hsu
发明人： Adel Farhan Halasa , Wen-Liang Hsu
IPC分类号： C08F2/38 , C08F4/46 , C08F4/48 , C08F36/04 , C08F136/04
CPC分类号： C08F36/04
摘要： Metal salts of saturated aliphatic alcohols can be used as modifiers in lithium initiated solution polymerizations of diene monomers into rubbery polymers. Sodium t-amylate is a preferred modifiers because of its exceptional solubility in non-polar aliphatic hydrocarbon solvents that are employed as the medium for such solution polymerizations. However, using sodium t-amylate as the polymerization modifier in commercial operations where recycle is required can lead to certain problems. These problems arise due to the fact that sodium t-amylate reacts with water to form t-amyl alcohol during steam stripping in the polymer finishing step. Since t-amyl alcohol forms an azeotrope with hexane, it co-distills with hexane and thus contaminates the feed stream. The present invention solves the problem of recycle stream contamination. This invention is based upon the discovery of highly effective modifiers that do not co-distill with hexane or-form-compounds during steam stripping which co-distill with hexane. The modifiers of this invention are metal salts of cyclic alcohols. Since the boiling points of these metal salts of cyclic alcohols are very high, they do not co-distill with hexane and contaminate recycle streams. Additionally, metal salts of cyclic alcohols are considered to be environmentally safe. The, subject invention more specifically discloses an initiator system which is comprised of (a) a lithium initiator, (b) a metal salt of a cyclic alcohol, and (c) a polar modifier.
摘要翻译：饱和脂族醇的金属盐可用作二烯单体进入橡胶状聚合物的锂引发溶液聚合中的改性剂。由于在用于这种溶液聚合的介质的非极性脂族烃溶剂中具有优异的溶解度，因此，叔戊醇钠是优选的改性剂。然而，在需要再循环的商业操作中使用叔戊醇钠作为聚合改性剂可能导致某些问题。这些问题是由于在聚合物整理步骤中的蒸汽汽提期间，叔戊醇钠与水反应形成叔戊醇的事实。由于叔戊醇与己烷形成共沸物，因此与己烷共蒸馏，从而污染进料流。本发明解决了循环流污染的问题。本发明基于在蒸汽汽提过程中与己烷共沸蒸馏而不与己烷或形式化合物共蒸馏的高效改性剂的发现。本发明的改性剂是环醇的金属盐。由于这些环状醇的金属盐的沸点非常高，因此它们不与己烷共蒸馏并污染再循环物流。此外，环醇的金属盐被认为是环境安全的。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，（b）环状醇的金属盐和（c）极性改性剂。

22. 发明授权

US5994448A High performance tire tread rubber composition 失效
标题翻译：高性能轮胎胎面胶组成
公开(公告)号：US5994448A
公开(公告)日：1999-11-30
申请号：US133503
申请日：1998-08-12
申请人： Edward John Blok , Paul Harry Sandstrom , Wen-Liang Hsu , Adel Farhan Halasa
发明人： Edward John Blok , Paul Harry Sandstrom , Wen-Liang Hsu , Adel Farhan Halasa
IPC分类号： B60C1/00 , C08C19/44 , C08L9/00 , C08K3/00
CPC分类号： C08C19/44 , B60C1/0016 , C08L9/00 , C08K3/36 , C08L7/00 , C08L9/06
摘要： This invention relates to a tire tread compound that can be used in manufacturing tires having outstanding traction characteristics without compromising treadwear and rolling resistance. The tire tread compounds of this invention are made utilizing an isoprene-butadiene rubber having a high glass transition temperature and having SnR.sub.3 end groups, wherein R represents an alkyl group, such as a tertiary-butyl group. These isoprene-butadiene rubbers are made by reacting an isoprene-butadiene rubber having a glass transition temperature which is within the range of about -50.degree. C. to about 0.degree. C. with a tin compound of the formula SnR.sub.3 X, wherein R represents an alkyl group and wherein X represents a halogen. This invention more specifically discloses a tire tread rubber composition which is comprised of (1) about 60 phr to about 95 phr of an isoprene-butadiene rubber having a glass transition temperature which is within the range of about -50.degree. C. to about 0.degree. C. and having --SnR.sub.3 end groups, (2) about 5 phr to about 30 phr of natural rubber and (3) up to about 25 phr of a rubbery polymer having a low glass transition temperature which is within the range of about -85.degree. C. to about -55.degree. C., with the proviso that the total amount of the natural rubber and the rubbery polymer having a low glass transition temperature does not exceed about 40 phr. The rubbery polymer having a low glass transition temperature will typically be high cis-1,4-polybutadiene, isoprene-butadiene rubber, styrene-butadiene rubber or styrene-isoprene-butadiene rubber.
摘要翻译：本发明涉及一种轮胎胎面胶，其可用于制造具有优异牵引特性的轮胎，而不损害胎面和滚动阻力。本发明的轮胎胎面胶料采用高玻璃化转变温度的异戊二烯 - 丁二烯橡胶制成，并具有SnR 3端基，其中R表示烷基，如叔丁基。这些异戊二烯 - 丁二烯橡胶通过使玻璃化转变温度在约-50℃至约0℃范围内的异戊二烯 - 丁二烯橡胶与式SnR 3 X的锡化合物反应制备，其中R表示烷基，其中X表示卤素。本发明更具体地公开了一种轮胎胎面橡胶组合物，其包含（1）约60phr至约95phr的玻璃化转变温度在约-50℃至约0的范围内的异戊二烯 - 丁二烯橡胶具有-SnR 3端基，（2）约5phr至约30phr的天然橡胶和（3）至多约25phr的玻璃化转变温度低于约 - 约25phr的橡胶状聚合物， 85℃至约-55℃，条件是具有低玻璃化转变温度的天然橡胶和橡胶状聚合物的总量不超过约40phr。具有低玻璃化转变温度的橡胶状聚合物通常是高顺式-1,4-聚丁二烯，异戊二烯 - 丁二烯橡胶，苯乙烯 - 丁二烯橡胶或苯乙烯 - 异戊二烯 - 丁二烯橡胶。

23. 发明授权

US5981639A Stabilization of tin-coupled polymers 失效
标题翻译：锡偶合聚合物的稳定化
公开(公告)号：US5981639A
公开(公告)日：1999-11-09
申请号：US58572
申请日：1998-04-10
申请人： Wen-Liang Hsu , Adel Farhan Halasa
发明人： Wen-Liang Hsu , Adel Farhan Halasa
IPC分类号： C08C19/44 , C08K5/04 , C08K5/17 , C08K5/34 , C08K5/35 , C08K5/09
CPC分类号： C08C19/44 , C08K5/17 , C08K5/34
摘要： The process of this invention can be utilized to stabilize tin-coupled rubbery polymers. This process involves adding a chelating diamine or a sodium alkoxide to the rubbery polymer after the tin coupling has been carried out. This invention more specifically discloses a process for improving the stability of a tin-coupled rubbery polymer which comprises adding a sodium alkoxide to the tin-coupled rubbery polymer subsequent to the time at which the tin-coupled rubbery polymer is coupled. Sodium alkoxide is a representative example of a sodium alkoxide that can be used to stabilize the tin-coupled rubbery polymer.
摘要翻译：本发明的方法可用于稳定锡偶联的橡胶状聚合物。该方法包括在进行锡偶合之后向橡胶状聚合物中加入螯合二胺或醇钠。本发明更具体地公开了一种改进锡偶合橡胶状聚合物的稳定性的方法，该方法包括在锡偶合的橡胶状聚合物偶合的时间之后向锡偶联的橡胶状聚合物中加入醇钠。烷氧基钠是可用于稳定锡偶联橡胶状聚合物的烷醇钠的代表性实例。

24. 发明授权

US5859133A Tire tread compound 失效
标题翻译：轮胎胎面复合物
公开(公告)号：US5859133A
公开(公告)日：1999-01-12
申请号：US617234
申请日：1996-03-18
申请人： David John Zanzig , Adel Farhan Halasa , Wen-Liang Hsu , Paul Harry Sandstrom , Laurie Elizabeth Austin
发明人： David John Zanzig , Adel Farhan Halasa , Wen-Liang Hsu , Paul Harry Sandstrom , Laurie Elizabeth Austin
IPC分类号： B60C1/00 , C08L9/00 , C08L21/00 , C08L53/00 , C08L53/02 , C08F236/08 , C08F236/06
CPC分类号： C08L21/00 , B60C1/0016 , C08F297/04 , C08L53/00 , C08L9/00 , C08L9/06
摘要： The subject invention discloses a pneumatic tire having an outer circumferential tread wherein said tread is a sulfur-cured rubber composition comprised of (a) an isoprene-butadiene diblock rubber, said isoprene-butadiene diblock rubber being comprised of a butadiene block and an isoprene-butadiene block, wherein said butadiene block has a number average molecular weight which is within the range of about 25,000 to about 350,000, wherein said isoprene-butadiene block has a number average molecular weight which is within the range of about 25,000 to about 350,000, wherein said isoprene-butadiene diblock rubber has essentially one glass transition temperature which is within the range of about -100.degree. C. to about -70.degree. C., wherein said isoprene-butadiene diblock polymer has a Mooney ML-4 viscosity at 100.degree. C. which is within the range of about 50 to about 140, and wherein the repeat units derived from isoprene and 1,3-butadiene in the isoprene-butadiene block are in essentially random order; and (b) a second rubber selected from the group consisting of high vinyl polybutadiene rubber, styrene-isoprene-butadiene rubber, solution styrene-butadiene rubber and emulsion styrene-butadiene rubber.
摘要翻译：本发明公开了一种具有外周胎面的充气轮胎，其中所述胎面是由（a）异戊二烯 - 丁二烯二嵌段橡胶组成的硫固化橡胶组合物，所述异戊二烯 - 丁二烯二嵌段橡胶由丁二烯嵌段和异戊二烯 - 丁二烯嵌段，其中所述丁二烯嵌段的数均分子量在约25,000至约350,000的范围内，其中所述异戊二烯 - 丁二烯嵌段的数均分子量在约25,000至约350,000的范围内，其中所述异戊二烯 - 丁二烯二嵌段橡胶具有在约-100℃至约-70℃范围内的基本上一个玻璃化转变温度，其中所述异戊二烯 - 丁二烯二嵌段聚合物在100℃下具有门尼ML-4粘度，其在约50至约140的范围内，并且其中衍生自异戊二烯和1,3-丁二烯的异戊二烯 - 丁二烯嵌段中的重复单元基本上为兰德呃订单和（b）选自高乙烯基聚丁二烯橡胶，苯乙烯 - 异戊二烯 - 丁二烯橡胶，溶剂苯乙烯 - 丁二烯橡胶和乳液丁苯橡胶的第二橡胶。

25. 发明授权

US5798408A Tire tread of coupled SIBR 失效
标题翻译：耦合SIBR轮胎胎面
公开(公告)号：US5798408A
公开(公告)日：1998-08-25
申请号：US811629
申请日：1997-03-05
申请人： David John Zanzig , Wen-Liang Hsu , Adel Farhan Halasa , Barry Allen Matrana
发明人： David John Zanzig , Wen-Liang Hsu , Adel Farhan Halasa , Barry Allen Matrana
IPC分类号： B60C1/00 , C08F236/10 , C08L9/00 , C08L53/00
CPC分类号： C08F236/10 , B60C1/0016 , C08L9/00 , C08K3/36 , C08L7/00 , C08L9/06 , Y10S156/91 , Y10T152/10495
摘要： This invention relates to a tire having a tread composed of quantitatively silica reinforced rubber composition, with a minor amount, if any, of carbon black where the tread elastomers are primarily composed of coupled styrene/isoprene/butadiene terpolymer with tin or silicon in combination with selected diene-based elastomers.
摘要翻译：本发明涉及一种具有由定量二氧化硅增强橡胶组合物构成的胎面的轮胎，其中少量（如果有的话）为炭黑，其中胎面弹性体主要由与锡或硅组合的苯乙烯/异戊二烯/丁二烯三元共聚物组合，选择的二烯基弹性体。

26. 发明授权

US5739182A Stabilization of tin-coupled polymers 失效
标题翻译：锡偶合聚合物的稳定化
公开(公告)号：US5739182A
公开(公告)日：1998-04-14
申请号：US791929
申请日：1997-01-31
申请人： Wen-Liang Hsu , Adel Farhan Halasa
发明人： Wen-Liang Hsu , Adel Farhan Halasa
IPC分类号： C08C19/44 , C08K5/04 , C08K5/17 , C08K5/34 , C08K5/35 , C08K5/3495
CPC分类号： C08K5/17 , C08C19/44 , C08K5/34
摘要： The process of this invention can be utilized to stabilize tin-coupled rubbery polymers. This process involves adding a chelating diamine to the rubbery polymer after the tin coupling has been carried out. This invention more specifically discloses a process for improving the stability of a tin-coupled rubbery polymer which comprises adding a tertiary chelating amine to the tin-coupled rubbery polymer subsequent to the time at which the tin-coupled rubbery polymer is coupled. The tertiary chelating amine will preferably be a tertiary chelating alkyl 1,2-ethylene diamine, such as N,N,N',N'-tetramethylethylenediamine.
摘要翻译：本发明的方法可用于稳定锡偶联的橡胶状聚合物。该方法包括在进行锡偶合之后将螯合二胺加入到橡胶状聚合物中。本发明更具体地公开了一种改进锡 - 偶联橡胶状聚合物稳定性的方法，该方法包括在锡 - 偶联的橡胶状聚合物偶合的时间之后向锡偶合的橡胶状聚合物中加入叔螯合胺。叔螯合胺优选为叔螯合烷基1,2-乙二胺，例如N，N，N'，N'-四甲基乙二胺。

27. 发明授权

US5679751A Solution polymerization process for synthesis of styrene-butadiene or styrene-isoprene rubber 失效
标题翻译：用于合成苯乙烯 - 丁二烯或苯乙烯 - 异戊二烯橡胶的溶液聚合方法
公开(公告)号：US5679751A
公开(公告)日：1997-10-21
申请号：US599542
申请日：1996-02-12
申请人： Adel Farhan Halasa , Laurie Elizabeth Austin , Wen-Liang Hsu , Bill Bud Gross
发明人： Adel Farhan Halasa , Laurie Elizabeth Austin , Wen-Liang Hsu , Bill Bud Gross
IPC分类号： B60C1/00 , C08F4/46 , C08F4/48 , C08F236/10
CPC分类号： B60C1/0016 , C08F236/10
摘要： The subject invention relates to a technique for synthesizing rubbery copolymers of styrene and butadiene and/or isoprene. These rubbers exhibit an excellent combination of properties for utilization in high performance tire tread rubber compounds. The subject invention specifically discloses a process for preparing a styrene-butadiene rubber (SBR) which comprises: copolymerizing from about 30 weight percent to about 55 weight percent styrene and from about 45 weight percent to about 70 weight percent 1,3-butadiene in an alkane solvent, such as hexane, at a temperature which is within the range of about -10.degree. C. to about 150.degree. C. in the presence of (a) an alkali metal alkoxide, and (b) an organolithium compound, wherein the molar ratio of the alkali metal alkoxide to the organolithium compound is within the range of about 0.01:1 to about 1:1. The subject invention further discloses a process for preparing a rubbery copolymer of styrene and isoprene having an excellent combination of properties for use in making tire treads by a solution polymerization process which comprises: copolymerizing from about 30 weight percent to about 55 weight percent styrene and from about 45 weight percent to about 70 weight percent isoprene in an alkane solvent at a temperature which is within the range of about -10.degree. C. to about 150.degree. C. in the presence of (a) an alkali metal alkoxide, and (b) an organolithium compound, wherein the molar ratio of the alkali metal alkoxide to the organolithium compound is within the range of about 0.01:1 to about 1:1.
摘要翻译：本发明涉及一种合成苯乙烯和丁二烯和/或异戊二烯橡胶共聚物的技术。这些橡胶在高性能轮胎胎面橡胶化合物中表现出优异的性能组合。本发明具体公开了一种制备苯乙烯 - 丁二烯橡胶（SBR）的方法，其包括：以约30重量％至约55重量％的苯乙烯和约45重量％至约70重量％的1,3-丁二烯的共聚合烷烃溶剂如己烷，在（a）碱金属醇盐存在下，在约-10℃至约150℃的温度范围内，和（b）有机锂化合物，其中，碱金属醇盐与有机锂化合物的摩尔比在约0.01:1至约1:1的范围内。本发明进一步公开了一种制备苯乙烯和异戊二烯的橡胶共聚物的方法，其具有通过溶液聚合方法制备轮胎胎面的优异的性能组合，其包括：共聚约30重量％至约55重量％的苯乙烯和在（a）碱金属醇盐存在下，在约-10℃至约150℃的温度下，在烷烃溶剂中约45重量％至约70重量％的异戊二烯，和（b ）有机锂化合物，其中碱金属醇盐与有机锂化合物的摩尔比在约0.01:1至约1:1的范围内。

28. 发明授权

US5677402A Process for preparing 3,4-polyisoprene rubber 失效
标题翻译：制备3,4-聚异戊二烯橡胶的方法
公开(公告)号：US5677402A
公开(公告)日：1997-10-14
申请号：US685762
申请日：1996-07-24
申请人： Adel Farhan Halasa , Wen-Liang Hsu
发明人： Adel Farhan Halasa , Wen-Liang Hsu
IPC分类号： C08F4/48 , C08F136/06 , C08F136/08
CPC分类号： C08F136/08 , C08F136/06
摘要： This invention reveals an initiator system which is comprised of (a) a lithium initiator, (b) a sodium alkoxide and (c) a polar modifier; wherein the molar ratio of the sodium alkoxide to the lithium initiator is within the range of about 0.05:1 to about 3:1; and wherein the molar ratio of the polar modifier to the lithium initiator is within the range of about 0.25:1 to about 5:1. The subject invention also discloses a process for preparing 3,4-polyisoprene rubber which comprises polymerizing isoprene monomer with a lithium initiator at a temperature which is within the range of about 30.degree. C. to about 100.degree. C. in the presence of a sodium alkoxide and a polar modifier, wherein the molar ratio of the sodium alkoxide to the lithium initiator is within the range of about 0.05:1 to about 3:1; and wherein the molar ratio of the polar modifier to the lithium initiator is within the range of about 0.25:1 to about 5:1.
摘要翻译：本发明揭示了一种引发剂体系，其包括（a）锂引发剂，（b）醇钠和（c）极性改性剂; 其中所述醇钠与所述锂引发剂的摩尔比在约0.05:1至约3:1的范围内; 并且其中极性改性剂与锂引发剂的摩尔比在约0.25:1至约5:1的范围内。本发明还公开了一种制备3,4-聚异戊二烯橡胶的方法，该方法包括在钠存在下，在约30℃至约100℃的温度范围内用锂引发剂聚合异戊二烯单体醇盐和极性改性剂，其中烷氧基钠与锂引发剂的摩尔比在约0.05:1至约3:1的范围内; 并且其中极性改性剂与锂引发剂的摩尔比在约0.25:1至约5:1的范围内。

29. 发明授权

US5654384A Process for preparing high vinyl polbutadiene rubber 失效
标题翻译：制备高乙烯基聚丁二烯橡胶的方法
公开(公告)号：US5654384A
公开(公告)日：1997-08-05
申请号：US622272
申请日：1996-03-27
申请人： Adel Farhan Halasa , Wen-Liang Hsu , David John Zanzig , Paul Harry Sandstrom , Steven Kristofer Henning , Danielle Lucas
发明人： Adel Farhan Halasa , Wen-Liang Hsu , David John Zanzig , Paul Harry Sandstrom , Steven Kristofer Henning , Danielle Lucas
IPC分类号： B60C1/00 , C08F2/38 , C08F2/44 , C08F4/48 , C08F36/00 , C08F36/04 , C08F36/06 , C08F136/06 , C08L9/00 , C08L21/00
CPC分类号： C08F36/04 , C08F136/06 , C08L9/00 , C08K5/06 , C08K5/17 , Y10S152/905
摘要： This invention reveals a process for preparing high vinyl polybutadiene rubber which comprises polymerizing 1,3-butadiene monomer with a lithium initiator at a temperature which is within the range of about 5.degree. C. to about 100.degree. in the presence of a sodium alkoxide and a polar modifier, wherein the molar ratio of the sodium alkoxide to the polar modifier is within the range of about 0.1:1 to about 10:1; and wherein the molar ratio of the sodium alkoxide to the lithium initiator is within the range of about 0.05:1 to about 10:1.
摘要翻译：本发明揭示了一种制备高乙烯基聚丁二烯橡胶的方法，其包括在醇钠存在下，在约5℃至约100℃的温度范围内使锂引发剂聚合1,3-丁二烯单体，以及极性改性剂，其中烷氧基钠与极性改性剂的摩尔比在约0.1:1至约10:1的范围内; 并且其中所述醇钠与所述锂引发剂的摩尔比在约0.05:1至约10:1的范围内。

30. 发明申请

US20100288407A1 DENDRIMERS OF RUBBERY POLYMERS 失效
标题翻译：橡胶聚合物胶粘剂
公开(公告)号：US20100288407A1
公开(公告)日：2010-11-18
申请号：US12845171
申请日：2010-07-28
申请人： Adel Farhan Halasa , Wen-Liang Hsu , Chad Aaron Jasiunas
发明人： Adel Farhan Halasa , Wen-Liang Hsu , Chad Aaron Jasiunas
IPC分类号： B60C11/00 , C08F8/18
CPC分类号： C08C19/44 , B60C1/0016 , C08G83/003 , C08L15/00 , C08L101/005 , Y10T152/10 , Y10T152/10495
摘要： This invention discloses a process for synthesizing a dendrimer of a rubbery polymer comprising: (a) reacting a lithium terminated rubbery polymer with a halogenated tin containing compound to produce a polymer which is terminated with halogenated tin moieties, wherein the halogenated tin containing compound is of the structural formula: wherein X represents a halogen atom, wherein Z1 groups can be the same or different and are selected from alkyl groups containing from 1 to 8 carbon atoms, wherein x represents an integer from 1 to 20, wherein the molar ratio of the lithium terminated rubbery polymer to halogen atoms in the halogenated tin containing compound is within the range of 2:n to (n−1):n, wherein n represents the number of halogen atoms that are bonded directly to tin atoms in the halogenated tin containing compound; (b) reacting the polymer which is terminated with halogenated tin moieties with a molar excess of a tertiary alcohol to produce a polymer which is terminated with hydroxy tin moieties; and (c) allowing the polymer which is terminated with the hydroxy tin moieties to couple under conditions sufficient to produce a dendrimer of the rubbery polymer.
摘要翻译：本发明公开了一种用于合成橡胶状聚合物树枝状聚合物的方法，包括：（a）使锂封端的橡胶状聚合物与含卤化锡的化合物反应以制备用卤化锡部分封端的聚合物，其中含卤化锡的化合物为结构式：其中X表示卤素原子，其中Z1基团可以相同或不同，并且选自含有1至8个碳原子的烷基，其中x表示1至20的整数，其中，含卤化锡化合物中的锂封端橡胶状聚合物与卤素原子在2：n至（n-1）：n的范围内，其中n表示与含锡卤化锡中的锡原子直接键合的卤素原子数复合; （b）使用卤化锡部分封端的聚合物与摩尔过量的叔醇反应，以产生用羟基锡部分封端的聚合物; 和（c）允许用羟基锡部分封端的聚合物在足以产生橡胶状聚合物的树枝状聚合物的条件下偶联。

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