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1. 发明授权

US06462143B1 Gel-free process for making functionalized anionically polymerized polymers 失效
标题翻译：制备官能化阴离子聚合聚合物的无凝胶工艺
公开(公告)号：US06462143B1
公开(公告)日：2002-10-08
申请号：US09234335
申请日：1999-01-20
申请人： Carl Lesley Willis , Daniel Earl Goodwin , Robert Charles Bening , Dale Lee Handlin, Jr. , John David Wilkey
发明人： Carl Lesley Willis , Daniel Earl Goodwin , Robert Charles Bening , Dale Lee Handlin, Jr. , John David Wilkey
IPC分类号： C08F842
CPC分类号： C08F8/42
摘要： This invention relates to a gel-free process for making functionalized polymers. When multi-alkali metal initiators are used to make these polymers anionically, the process comprises anionically polymerizing at least one monomer with a multi-alkali metal initiator in a hydrocarbon solvent, capping the polymer by adding to the polymer a capping agent that reacts with the ends of the polymer chains such that strongly associating chain ends are formed wherein a strongly associating gel is formed, and, finally, adding a trialkyl aluminum compound to the gel. The important characteristic of the capping agent herein is that it will cap the living polymer and will add a functional group to the polymer chain end which will be strongly associating in the hydrocarbon solvent. In a second embodiment, the present invention relates to a process for making such polymers which comprises anionically polymerizing them as described and adding to the polymer a trialkyl aluminum compound before the alkali metal reacts with the capping agent-functionalized chain ends. Finally, the polymer is capped by adding the above-described capping agent. In the first embodiment, a gel is formed and then removed. In the second embodiment, the gel never is formed because of the presence of the trialkyl aluminum compound.
摘要翻译：本发明涉及无凝胶的制备官能化聚合物的方法。当使用多碱金属引发剂阴离子制造这些聚合物时，该方法包括在烃溶剂中将至少一种单体与多碱金属引发剂进行阴离子聚合，通过向聚合物中加成封端剂，该封端剂与聚合物链的末端，使得形成强缔合链末端，其中形成强缔合性凝胶，最后在凝胶中加入三烷基铝化合物。本发明的封端剂的重要特征在于它将覆盖活性聚合物，并且将在烃溶剂中与聚合物链末端加成官能团，该聚合物链末端将强烈缔合。在第二个实施方案中，本发明涉及一种制备这样的聚合物的方法，其包括如上所述对其进行阴离子聚合，并在碱金属与封端剂官能化的链末端反应之前向聚合物中加入三烷基铝化合物。最后，通过加入上述封端剂封闭聚合物。在第一实施方案中，形成凝胶然后除去。在第二实施方案中，由于存在三烷基铝化合物，所以不会形成凝胶。

2. 发明授权

US06242537B1 Gel-free process for making hydrogenated functionalized anionically polymerized polymers 有权
标题翻译：制备氢化官能化阴离子聚合聚合物的无凝胶工艺
公开(公告)号：US06242537B1
公开(公告)日：2001-06-05
申请号：US09260239
申请日：1999-03-02
申请人： Robert Charles Bening , Carl Lesley Willis , Charles Roy Donaho , Daniel Earl Goodwin , Zaida Diaz , John David Wilkey
发明人： Robert Charles Bening , Carl Lesley Willis , Charles Roy Donaho , Daniel Earl Goodwin , Zaida Diaz , John David Wilkey
IPC分类号： C08F804
CPC分类号： C08C19/44 , C08C19/42 , C08F8/00 , C08F12/00
摘要： This invention relates to a gel-free process for making hydrogenated functionalized polymers that mitigates the problem of ionic gel. When multi-alkali metal initiators are used to make these polymers anionically, the process comprises anionically polymerizing at least one monomer with a multi-alkali metal initiator, usually a lithium alkyl, in a hydrocarbon solvent, capping the polymer by adding to the polymer a capping agent that reacts with the ends of the polymer chains such that strongly associating chain ends are formed wherein a strongly associating polymer gel is formed, adding a trialkyl aluminum compound to the polymer gel, whereby the gel dissipates, optionally terminating the polymerization by addition of an alcohol, washing the polymer with aqueous acid, preferably aqueous mineral acid, most preferably phosphoric acid, wherein there is at least one mole of phosphoric acid per mole of alkali metal and at least three moles of phosphoric acid per mole of aluminum, and hydrogenating the polymer with a hydrogenation catalyst. In a second embodiment, the present invention relates to a process for making such polymers which comprises anionically polymerizing them as described and adding a trialkyl aluminum compound prior to the addition of the functionalizing agent and washing the product prior to hydrogenation as described above. In the first embodiment, a gel is formed and then removed. In the second embodiment, the gel never is formed because of the presence of the trialkyl aluminum compound.
摘要翻译：本发明涉及一种用于制备氢化官能化聚合物的无凝胶方法，其减轻了离子凝胶的问题。当使用多碱金属引发剂阴离子制造这些聚合物时，该方法包括在烃溶剂中将至少一种单体与多碱金属引发剂（通常为烷基锂）进行阴离子聚合，通过向聚合物加入聚合物形成与聚合物链的端部反应的封端剂，从而形成强缔合的链端，其中形成强缔合的聚合物凝胶，将三烷基铝化合物加入到聚合物凝胶中，由此凝胶消散，任选地通过加入聚合物终止聚合醇，用酸水溶液洗涤聚合物，优选无机酸水溶液，最优选磷酸，其中每摩尔铝存在至少1摩尔磷酸/摩尔碱金属和至少3摩尔磷酸/摩尔氢化该聚合物与氢化催化剂。在第二个实施方案中，本发明涉及一种制备这种聚合物的方法，其包括如上所述阴离子聚合它们，并且在加入官能化试剂之前加入三烷基铝化合物并在如上所述的氢化之前洗涤产物。在第一实施方案中，形成凝胶然后除去。在第二实施方案中，由于存在三烷基铝化合物，所以不会形成凝胶。

3. 发明授权

US06492466B2 Increased throughput in the manufacture of anionic polymers by reduction in polymer cement viscosity through the addition of metal alkyls 有权
标题翻译：通过加入金属烷基酯降低聚合物水泥粘度，增加了阴离子聚合物制造中的生产量
公开(公告)号：US06492466B2
公开(公告)日：2002-12-10
申请号：US10106737
申请日：2002-03-26
申请人： Carl Lesley Willis , Robert Charles Bening , Peter Taylor Murany , Steven Jon Weddle , Dale Lee Handlin, Jr.
发明人： Carl Lesley Willis , Robert Charles Bening , Peter Taylor Murany , Steven Jon Weddle , Dale Lee Handlin, Jr.
IPC分类号： C08F27900
CPC分类号： C08F297/042 , C08F4/46 , C08F4/50 , C08F4/52 , C08F12/08 , C08F36/04 , C08F297/04 , C08F4/48
摘要： The present invention is an improvement upon the known method of anionically polymerizing monomers by contacting the monomers with an anionic polymerization initiator which is an organo-substituted alkali metal compound. The improvement comprises decreasing the viscosity of the polymer cement by adding at least 0.01 equivalent of a metal alkyl compound per equivalent of alkali metal initiator if the metal alkyl is added before or at the beginning of polymerization. If the metal alkyl is added during the polymerization or after but before the living polymer is terminated, then at least 0.01 equivalent of the metal alkyl compound per equivalent of living polymer chain ends is should be used. The alkyl groups of the metal alkyl are chosen such that they do not exchange with the organo substituents of the alkali metal, which can be the living polymer chain ends or the organo substituents of the initiator. To avoid this undesired exchange reaction, the alkyl groups of the metal alkyl compound are selected to be more basic and/or less bulky or both than the organo substituents of the alkali metal compound.
摘要翻译：本发明是通过使单体与作为有机取代的碱金属化合物的阴离子聚合引发剂接触而使已知的阴离子聚合单体的方法的改进。改进之处在于，如果在聚合开始之前或开始时加入金属烷基，则每当量的碱金属引发剂加入至少0.01当量的金属烷基化合物来降低聚合物粘合剂的粘度。如果在聚合期间或在活性聚合物终止之前加入金属烷基，则应使用每当量活性聚合物链末端至少0.01当量的金属烷基化合物。选择金属烷基的烷基使得它们不与碱金属的有机取代基交换，碱金属可以是活性聚合物链末端或引发剂的有机取代基。为了避免这种不希望的交换反应，金属烷基化合物的烷基被选择为比碱金属化合物的有机取代基更碱性和/或更小体积或两者。

4. 发明授权

US06492469B2 Increased throughput in the manufacture of anionic polymers by reduction in polymers by reduction in polymer cement viscosity through the addition of metal alkyls 有权
标题翻译：通过通过添加金属烷基酯降低聚合物粘合剂粘度来降低聚合物，从而提高阴离子聚合物的制造量
公开(公告)号：US06492469B2
公开(公告)日：2002-12-10
申请号：US10106265
申请日：2002-03-26
申请人： Carl Lesley Willis , Robert Charles Bening , Peter Taylor Murany , Steven Jon Weddle , Dale Lee Handlin, Jr.
发明人： Carl Lesley Willis , Robert Charles Bening , Peter Taylor Murany , Steven Jon Weddle , Dale Lee Handlin, Jr.
IPC分类号： C08F842
CPC分类号： C08F297/042 , C08F4/46 , C08F4/50 , C08F4/52 , C08F12/08 , C08F36/04 , C08F297/04 , C08F4/48
摘要： The present invention is an improvement upon the known method of anionically polymerizing monomers by contacting the monomers with an anionic polymerization initiator which is an organo-substituted alkali metal compound. The improvement comprises decreasing the viscosity of the polymer cement by adding at least 0.01 equivalent of a metal alkyl compound per equivalent of alkali metal initiator if the metal alkyl is added before or at the beginning of polymerization. If the metal alkyl is added during the polymerization or after but before the living polymer is terminated, then at least 0.01 equivalent of the metal alkyl compound per equivalent of living polymer chain ends is should be used. The alkyl groups of the metal alkyl are chosen such that they do not exchange with the organo substituents of the alkali metal, which can be the living polymer chain ends or the organo substituents of the initiator. To avoid this undesired exchange reaction, the alkyl groups of the metal alkyl compound are selected to be more basic and/or less bulky or both than the organo substituents of the alkali metal compound.
摘要翻译：本发明是通过使单体与作为有机取代的碱金属化合物的阴离子聚合引发剂接触而使已知的阴离子聚合单体的方法的改进。改进之处在于，如果在聚合开始之前或开始时加入金属烷基，则每当量的碱金属引发剂加入至少0.01当量的金属烷基化合物来降低聚合物粘合剂的粘度。如果在聚合期间或在活性聚合物终止之前加入金属烷基，则应使用每当量活性聚合物链末端至少0.01当量的金属烷基化合物。选择金属烷基的烷基使得它们不与碱金属的有机取代基交换，碱金属可以是活性聚合物链末端或引发剂的有机取代基。为了避免这种不希望的交换反应，金属烷基化合物的烷基被选择为比碱金属化合物的有机取代基更碱性和/或更小体积或两者。

5. 发明授权

US06391981B1 Increased throughput in the manufacture of anionic polymers by reduction in polymer cement viscosity through the addition of metal alkyls 有权
公开(公告)号：US06391981B1
公开(公告)日：2002-05-21
申请号：US09537500
申请日：2000-03-29
申请人： Carl Lesley Willis , Robert Charles Bening , Peter Taylor Murany , Steven Jon Weddle , Dale Lee Handlin, Jr.
发明人： Carl Lesley Willis , Robert Charles Bening , Peter Taylor Murany , Steven Jon Weddle , Dale Lee Handlin, Jr.
IPC分类号： C08F842
CPC分类号： C08F297/042 , C08F4/46 , C08F4/50 , C08F4/52 , C08F12/08 , C08F36/04 , C08F297/04 , C08F4/48
摘要： The present invention is an improvement upon the known method of anionically polymerizing monomers by contacting the monomers with an anionic polymerization initiator which is an organo-substituted alkali metal compound. The improvement comprises decreasing the viscosity of the polymer cement by adding at least 0.01 equivalent of a metal alkyl compound per equivalent of alkali metal initiator if the metal alkyl is added before or at the beginning of polymerization. If the metal alkyl is added during the polymerization or after but before the living polymer is terminated, then at least 0.01 equivalent of the metal alkyl compound per equivalent of living polymer chain ends is should be used. The alkyl groups of the metal alkyl are chosen such that they do not exchange with the organo substituents of the alkali metal, which can be the living polymer chain ends or the organo substituents of the initiator. To avoid this undesired exchange reaction, the alkyl groups of the metal alkyl compound are selected to be more basic and/or less bulky or both than the organo substituents of the alkali metal compound.

6. 发明授权

US6103846A Process for making anionic polymeric di-and polyfunctional polymers using protected functional initiators 有权
标题翻译：使用保护的官能引发剂制备阴离子聚合二 - 和多官能聚合物的方法
公开(公告)号：US6103846A
公开(公告)日：2000-08-15
申请号：US305491
申请日：1999-05-05
申请人： Carl Lesley Willis , Robert Charles Bening , Michael Wayne Potter , Grant Wesley Haddix , David Karl Schisla , Thomas Carl Semple , Daniel Earl Goodwin
发明人： Carl Lesley Willis , Robert Charles Bening , Michael Wayne Potter , Grant Wesley Haddix , David Karl Schisla , Thomas Carl Semple , Daniel Earl Goodwin
IPC分类号： C08F2/00 , C08F4/46 , C08F4/58 , C08F4/72 , C08F36/04 , C08F36/06
CPC分类号： C08F4/72 , C08F36/04 , C08F4/58
摘要： The preparation of di- or polyfunctional polymers by anionic polymerization using functionalized initiators having the structure R.sup.1 R.sup.2 R.sup.3 Si--A--B, wherein each R is methyl and A is a hydrocarbon bridging group containing from 1 to 25 carbon atoms, and B is an alkali metal, is improved when polymerization occurs in the presence of a polymerization termination inhibitor which is a metal alkyl which has been added at a concentration to afford a molar ratio of the termination inhibitor to living polymer chain ends of about 0.1:1 to about 10:1.
摘要翻译：通过使用具有结构R1R2R3Si-AB的官能化引发剂通过阴离子聚合制备二官能或多官能聚合物，其中每个R是甲基，A是含有1至25个碳原子的烃桥联基团，B是碱金属，其被改进当在聚合终止抑制剂存在下进行聚合时，该聚合终止抑制剂是以浓度提供终止抑制剂与活性聚合物链末端的摩尔比为约0.1:1至约10:1的金属烷基。

7. 发明授权

US06242538B1 Process for making hydrogenated gel-free functionalized anionically polymerized polymers 有权
标题翻译：制备无凝胶的官能化阴离子聚合聚合物的方法
公开(公告)号：US06242538B1
公开(公告)日：2001-06-05
申请号：US09304915
申请日：1999-05-04
申请人： Robert Charles Bening , Carl Lesley Willis , John David Wilkey , Zaida Diaz
发明人： Robert Charles Bening , Carl Lesley Willis , John David Wilkey , Zaida Diaz
IPC分类号： C08F804
CPC分类号： C08F8/04
摘要： This invention relates to a process for making gel-free functionalized polymers. When multi-lithium initiators are used to make these polymers anionically, the process comprises anionically polymerizing at least one monomer with a multi-lithium initiator in a hydrocarbon solvent, functionalizing the polymer by adding to the polymer a capping agent that reacts with the ends of the polymer chains such that strongly-associating chain ends are formed wherein a polymer gel is formed, adding a trialkyl aluminum compound to the polymer gel, whereby the gel dissipates, adding a sufficient amount of a proton source to provide at least 1 mole of protons per mole of lithium ions and at least 2 moles of protons per mole of aluminum wherein the proton source is an organic acid with a pKa of 11 or less or a mixture of the organic acid and an alkanol, provided that sufficient organic acid is added to provide at least 0.4 moles of protons per mole of lithium ions, hydrogenating the polymer with a hydrogenation catalyst, and optionally washing the polymer with aqueous mineral acid in sufficient.
摘要翻译：本发明涉及一种制备不含凝胶的官能化聚合物的方法。当使用多锂引发剂阴离子制造这些聚合物时，该方法包括在烃溶剂中使多个锂引发剂的至少一种单体阴离子聚合，通过向聚合物中添加与端基反应的封端剂官能化聚合物聚合物链使得形成强缔合的链端，其中形成聚合物凝胶，将三烷基铝化合物加入到聚合物凝胶中，由此凝胶消散，加入足够量的质子源以提供至少1摩尔的质子每摩尔锂离子和至少2摩尔质子/摩尔铝，其中质子源是pKa为11或更低的有机酸或有机酸和链烷醇的混合物，条件是将足够的有机酸加入到每摩尔锂离子提供至少0.4摩尔质子，用氢化催化剂氢化聚合物，并任选地用无机酸水溶液洗涤聚合物足够了

8. 发明授权

US06218478B1 Deprotection of polymers prepared with silyloxy protected functional initiators by reaction with hydride reducing agents 有权
标题翻译：通过与氢化物还原剂反应，用甲硅烷氧基保护的官能引发剂制备的聚合物脱保护
公开(公告)号：US06218478B1
公开(公告)日：2001-04-17
申请号：US09379843
申请日：1999-08-24
申请人： Robert Charles Bening , Carl Lesley Willis
发明人： Robert Charles Bening , Carl Lesley Willis
IPC分类号： C08C1902
CPC分类号： C08C19/44
摘要： The present invention provides a process for making functionalized polymers comprising the steps of (a) initiating polymerization of an unsaturated monomer with a lithium initiator having the structure R1R2R3Si—O—A—Li wherein A is a branched or straight chain bridging group having at least two carbon atoms, R1,R2, and R3 are alkyl, alkoxy, aryl, or alkaryl groups having from 1 to 10 carbon atoms, thus producing a functionalized polymer which has a protecting silyl group at one end thereof; and (b) contacting the protected polymer with aqueous acid to remove residual lithium, and (c) contacting the protected polymer with from 1 to 10 equivalents of an organic or inorganic hydride; and (d) contacting the resulting solution with aqueous acid, and (e) recovering a linear or branched deprotected polymer having one or more terminal functional groups.
摘要翻译：本发明提供了制备官能化聚合物的方法，其包括以下步骤：（a）引发不饱和单体与具有结构R1R2R3Si-OA-Li的锂引发剂的聚合，其中A是具有至少两个碳的支链或直链桥连基团原子，R 1，R 2和R 3是具有1至10个碳原子的烷基，烷氧基，芳基或烷芳基，从而制备其一端具有保护甲硅烷基的官能化聚合物; 和（b）使受保护的聚合物与酸水溶液接触以除去残留的锂，和（c）使被保护的聚合物与1至10当量的有机或无机氢化物接触; 和（d）使所得溶液与酸水溶液接触，和（e）回收具有一个或多个末端官能团的直链或支链脱保护的聚合物。

9. 发明授权

US6075097A Process for producing conjugated diene diols using carbon dioxide 失效
标题翻译：使用二氧化碳制备共轭二烯二醇的方法
公开(公告)号：US6075097A
公开(公告)日：2000-06-13
申请号：US80999
申请日：1998-05-19
申请人： Robert Charles Bening , John David Wilkey
发明人： Robert Charles Bening , John David Wilkey
IPC分类号： C08F8/00 , C08C19/02 , C08C19/44 , C08F6/08 , C08F8/04 , C08F297/02 , C08F36/00 , C08F36/06 , C08F293/00
CPC分类号： C08C19/44 , C08C19/02 , C08F297/02
摘要： A process for making hydrogenated polymers is presenting. Polymerization is initiated with a lithium initiator and one or more unsaturated monomers are polymerized to a polymer cement. The polymerization process is terminated and dry carbon dioxide is introduced to the polymer cement to make a CO.sub.2 -treated polymer cement. The CO.sub.2 -treated polymer cement is hydrogenated in the presence of a Ni/Al catalyst.
摘要翻译：提出了一种制备氢化聚合物的方法。用锂引发剂引发聚合，并将一种或多种不饱和单体聚合成聚合物粘合剂。终止聚合过程，并将干二氧化碳引入聚合物粘合剂中以制备经二氧化碳处理的聚合物粘合剂。在Ni / Al催化剂存在下，将二氧化碳处理的聚合物水泥氢化。

10. 发明授权

US5681895A Coupling of anionic polymers with trialkoxysilanes having silicon-hydrogen bonds 失效
标题翻译：阴离子聚合物与具有硅 - 氢键的三烷氧基硅烷的偶联
公开(公告)号：US5681895A
公开(公告)日：1997-10-28
申请号：US705032
申请日：1996-08-29
申请人： Robert Charles Bening , Ronald James Hoxmeier
发明人： Robert Charles Bening , Ronald James Hoxmeier
IPC分类号： C08C19/42 , C08C19/44 , C08F4/48 , C08F4/72 , C08F8/42 , C08F12/08 , C08F36/04
CPC分类号： C08C19/44
摘要： A high yield of three armed radial anionic polymers is produced by the process of coupling metal terminated anionic polymers with a trialkoxysilane having a silicon-hydrogen bond, preferably trimethoxysilane. The metal terminated anionic polymer is preferably produced by initiating polymerization with a protected functional initiator which is readily converted to terminal hydroxyl groups or derivatives thereof for use in adhesives, sealants, and coatings.
摘要翻译：通过将金属封端的阴离子聚合物与具有硅 - 氢键的三烷氧基硅烷，优选三甲氧基硅烷偶联的方法制备出三臂式放射状阴离子聚合物的高产率。金属封端的阴离子聚合物优选通过用易于转化为末端羟基的保护的官能引发剂或其衍生物引发聚合来制备，以用于粘合剂，密封剂和涂料。

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