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1. 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。

2. 发明授权

US06207795B1 Removal of hydrogenation catalyst from polymer solutions by treatment with ammonia and carbon dioxide 有权
标题翻译：通过用氨和二氧化碳处理从聚合物溶液中除去氢化催化剂
公开(公告)号：US06207795B1
公开(公告)日：2001-03-27
申请号：US09371303
申请日：1999-08-10
申请人： John David Wilkey
发明人： John David Wilkey
IPC分类号： C08G600
CPC分类号： C08F6/02
摘要： This invention is a process comprising the steps of contacting a Group VIII metal hydrogenation catalyst residue-containing polymer solution with an aqueous solution of ammonia and carbon dioxide, separating the residue from the solution, and recovering a polymer solution preferably comprising less than 15 ppm by weight based on polymer, of the Group VIII metal. The concentration of the ammonia in the aqueous solution is from 2 to 7% by weight, preferably 3 to 6% by weight. The concentration of the carbon dioxide in the solution is from 1 to 7% by weight, preferably 2 to 6% by weight.
摘要翻译：本发明是一种方法，包括使含有Ⅷ族金属氢化催化剂残余物的聚合物溶液与氨和二氧化碳水溶液接触的步骤，将残余物与溶液分离，并回收优选包含小于15ppm的聚合物溶液基于聚合物的第VIII族金属的重量。水溶液中氨的浓度为2〜7重量％，优选为3〜6重量％。溶液中二氧化碳的浓度为1〜7重量％，优选为2〜6重量％。

3. 发明授权

US06187873B1 Increased throughput in the manufacture of block copolymers by reduction in polymer cement viscosity through the addition of polar solvents 失效
标题翻译：通过添加极性溶剂降低聚合物粘合剂粘度，增加了嵌段共聚物制造中的生产量
公开(公告)号：US06187873B1
公开(公告)日：2001-02-13
申请号：US09130248
申请日：1998-08-06
申请人： Dale Lee Handlin, Jr. , David Ralph Stewart , John David Wilkey
发明人： Dale Lee Handlin, Jr. , David Ralph Stewart , John David Wilkey
IPC分类号： C08F804
CPC分类号： C08F6/02
摘要： This invention is an improvement upon the current process for the production of block copolymers, especially hydrogenated block copolymers, of conjugated dienes and/or vinyl aromatic hydrocarbons which comprises anionically polymerizing the monomers in an inert hydrocarbon solvent in the presence of an alkali metal initiator whereby a polymer cement is produced and then contacting the cement with hydrogen under hydrogenation conditions in the presence of a hydrogenation catalyst. This invention and the improvement to the foregoing process comprises reducing the viscosity of the polymer cement by adding to it, preferably prior to hydrogenation (if the polymer is to be hydrogenated), from 2 to 50 % wt of a polar compound. The polar compound must be a poorer solvent for the block copolymer than is the inert hydrocarbon solvent. Preferred polar compounds include diethyl ether, tetrahydrofuran, diethoxyethane, monoglyme, diglyme, diethoxypropane, dioxane ortho-dimethoxybenzene, and the like.
摘要翻译：本发明是对现有的制备共轭二烯和/或乙烯基芳族烃的嵌段共聚物，特别是氢化嵌段共聚物的方法的改进，其包括在惰性烃溶剂中在碱金属引发剂的存在下将单体阴离子聚合，生产聚合物水泥，然后在氢化催化剂存在下，在氢化条件下使水泥与氢气接触。本发明和对上述方法的改进包括通过加入聚合物粘合剂，优选在氢化之前（如果聚合物被氢化），从2-50％wt的极性化合物降低聚合物粘合剂的粘度。与惰性烃溶剂相比，极性化合物必须是较差的嵌段共聚物溶剂。优选的极性化合物包括乙醚，四氢呋喃，二乙氧基乙烷，单甘醇二甲醚，二甘醇二甲醚，二乙氧基丙烷，二恶烷邻二甲氧基苯等。

4. 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。

5. 发明授权

US5847072A Removal of lithium from polymer cements 失效
标题翻译：从聚合物水泥中去除锂
公开(公告)号：US5847072A
公开(公告)日：1998-12-08
申请号：US652261
申请日：1996-05-23
申请人： Zaida Diaz , John David Wilkey
发明人： Zaida Diaz , John David Wilkey
IPC分类号： C04B41/60 , B01J39/04 , C08C2/04 , C08F6/00 , C08F6/02 , C08F6/08 , C08F6/24
CPC分类号： B01J39/043 , C08C2/04 , C08F6/02
摘要： The selectivity of ion exchange processes for the removal of lithium from acids is improved when weak acids such as citric and acetic, are used in the wash step. An added improvement is realized by a two stage process of contacting the acid solution first with an ion exchange resin functional to remove the nickel and aluminum compounds from the acid solution; and then contacting the acid solution with an ion exchange resin which is more selective to remove the alkali metal compound from the acid solution.
摘要翻译：在洗涤步骤中使用弱酸（如柠檬酸和乙酸）时，离子交换方法从酸中除去锂的选择性得到改善。通过使酸溶液首先与用于从酸溶液中除去镍和铝化合物的离子交换树脂接触的两阶段方法实现了另外的改进; 然后使酸溶液与离子交换树脂接触，该离子交换树脂从酸溶液中除去碱金属化合物更具选择性。

6. 依法登记的发明

USH1703H Removal of lithium from polymer cements 失效
标题翻译：从聚合物水泥中去除锂
公开(公告)号：USH1703H
公开(公告)日：1998-01-06
申请号：US652191
申请日：1996-05-23
申请人： John David Wilkey , Zaida Diaz , Dale Lee Handlin, Jr.
发明人： John David Wilkey , Zaida Diaz , Dale Lee Handlin, Jr.
IPC分类号： C08C2/04 , C08F6/02 , C08F297/02 , C08F8/00
CPC分类号： C08C2/04 , C08F6/02 , C08F297/02
摘要： A process for preparing a polymer cement which is relatively free of alkali metal salt by preparing the polymer cement with a polymerization terminating agent which is an acid which leaves alkali metal salt in the cement which is readily removable by centrifugation.
摘要翻译：一种制备聚合物胶浆的方法，该聚合物胶浆通过用聚合终止剂制备聚合物胶泥，该聚合终止剂是在水泥中留下碱金属盐的酸，该酸可以通过离心而容易地除去。

7. 发明授权

US6153727A Extraction of metal residues from polymer cements 失效
标题翻译：从聚合物水泥中提取金属残留物
公开(公告)号：US6153727A
公开(公告)日：2000-11-28
申请号：US135725
申请日：1998-08-18
申请人： John David Wilkey , Zaida Diaz
发明人： John David Wilkey , Zaida Diaz
IPC分类号： C08F6/02 , C08F6/00
CPC分类号： C08F6/02
摘要： There is provided a method of removing metal residues from a polymer cement, the method comprising polymerizing a monomer with a metal-based polymerization initiator to give a polymer cement having metal polymerization initiator residue; adding an organic-soluble acid having a pKa no greater than about 4.5 to the polymer cement, thereby forming an acid containing organic phase; mixing the organic phase with an aqueous phase containing a mineral acid; and recovering the polymer cement substantially free of metal residue.
摘要翻译：提供了从聚合物水泥中除去金属残留物的方法，该方法包括用金属基聚合引发剂使单体聚合，得到具有金属聚合引发剂残基的聚合物粘合剂; 向聚合物胶浆中加入pKa不大于约4.5的有机溶解酸，从而形成含酸的有机相; 将有机相与含有无机酸的水相混合; 并回收基本上不含金属残渣的聚合物胶浆。

8. 发明授权

US5767207A Removal of lithium from polymer cements 失效
标题翻译：从聚合物水泥中去除锂
公开(公告)号：US5767207A
公开(公告)日：1998-06-16
申请号：US652084
申请日：1996-05-23
申请人： John David Wilkey , Zaida Diaz
发明人： John David Wilkey , Zaida Diaz
IPC分类号： C08C2/04 , C08F6/02 , C08F297/02
CPC分类号： C08C2/04 , C08F297/02 , C08F6/02
摘要： A process for preparing a polymer cement which is relatively free of alkali metal salt by preparing the polymer cement with a polymerization terminating agent which is a diketone which leaves alkali metal salt in the cement which is readily removable by centrifugation.
摘要翻译：一种制备聚合物胶浆的方法，该聚合物胶浆通过制备具有聚合终止剂的聚合物粘合剂来制备聚合物粘合剂，所述聚合终止剂是在水泥中留下碱金属盐的二酮，其可通过离心容易地除去。

9. 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。

10. 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

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