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1. 发明授权

US06455651B1 Uniform initiation of anionic polymerization using organo-substituted alkali metal initiators 有权
标题翻译：使用有机取代的碱金属引发剂均匀引发阴离子聚合
公开(公告)号：US06455651B1
公开(公告)日：2002-09-24
申请号：US09525137
申请日：2000-03-14
申请人： Carl Lesley Willis , Daniel Earl Goodwin
发明人： Carl Lesley Willis , Daniel Earl Goodwin
IPC分类号： C08F448
CPC分类号： C08F297/048 , C08F12/04 , C08F297/04 , C08F4/46
摘要： The present invention is an improvement in a method of anionically polymerizing monomers by contacting them with an anionic polymerization initiator which is an organo-substituted alkali metal compound in the presence of low amounts of an accelerator/promoter and/or a highly active microstructure modifier. The improvement comprises adding from 0.1 to 1.0 equivalents of a metal alkyl compound per equivalent of alkali metal initiator wherein alkyl groups of the metal alkyl compound are chosen so that they will not exchange with the organo substituents of the alkali metal compound. The preferred initiator for use herein is the sec-butyl lithium adduct of diisopropenyl benzene and the preferred metal alkyl is triethyl aluminum.
摘要翻译：本发明是通过在少量加速剂/促进剂和/或高活性显微组织调节剂的存在下使它们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单体阴离子聚合的方法的改进。该改进包括每当量的碱金属引发剂加入0.1至1.0当量的金属烷基化合物，其中金属烷基化合物的烷基被选择为不与碱金属化合物的有机取代基交换。用于本文的优选引发剂是二异丙烯基苯的仲丁基锂加合物，优选的金属烷基是三乙基铝。

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

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。

4. 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。

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