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公开(公告)号：US4193901A
公开(公告)日：1980-03-18
申请号：US19312
申请日：1979-03-12
申请人： Henry S. Makowski , Robert D. Lundberg , Jan Bock
发明人： Henry S. Makowski , Robert D. Lundberg , Jan Bock
CPC分类号： C08C19/20 , C08F8/36 , C08F8/44 , C08F2800/20 , Y10S260/31
摘要： An improved process for the sulfonation of an unsaturated elastomeric polymer to form a sulfonated elastomeric polymer, wherein a cement which contains an elastomeric polymer dissolved in a non-reactive solvent is contacted with a sulfonating agent at between about -100.degree. C. and +100.degree. C. for a period of time sufficient to result in the sulfonation of the elastomeric polymer wherein the improvement includes the use of a sulfonating agent which is formed from mixtures of a sulfur trioxide donor complexed with a Lewis base and a carboxylic acid anhydride ##STR1## or an acyl halide ##STR2## or with both, wherein R is selected from the group consisting of CH.sub.3 --, C.sub.2 H.sub.5 --, C.sub.3 H.sub.7 --, C.sub.4 H.sub.9 --, C.sub.5 H.sub.11, C.sub.6 H.sub.13 and C.sub.6 H.sub.5 and mixtures thereof. The molar ratio of ##STR3## and/or ##STR4## with the SO.sub.3 of the complex is at least 0.5.
摘要翻译： 用于磺化不饱和弹性体聚合物以形成磺化弹性体聚合物的改进方法，其中含有溶解在非反应性溶剂中的弹性体聚合物的水泥在约-100℃和+ 100℃之间与磺化剂接触 在一段时间内足以导致弹性体聚合物的磺化，其中改进包括使用磺化剂，其由与路易斯碱和羧酸酐复合的三氧化硫供体的混合物形成
和/或 与络合物的SO 3的摩尔比为至少0.5。 -
公开(公告)号：US4316828A
公开(公告)日：1982-02-23
申请号：US47753
申请日：1979-06-12
申请人： Henry S. Makowski , Robert D. Lundberg , Jan Bock
发明人： Henry S. Makowski , Robert D. Lundberg , Jan Bock
摘要： An improved process for the manufacture of extended gel free sulfonated elastomeric products includes the formation of a homogeneous mixture of fillers and oils with the acid form of the sulfonated polymer prior to the neutralization of the acid form of the sulfonated polymer with a basic material thereby resulting in a composition having improved physical properties.
摘要翻译： 用于制造延伸的无凝胶磺化弹性体产品的改进方法包括在用磺化聚合物的酸形式与碱性物质中和之前，将磺酸化聚合物的酸形式的填料和油的均匀混合物形成，由此得到 在具有改进的物理性质的组合物中。
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公开(公告)号：US4222914A
公开(公告)日：1980-09-16
申请号：US22951
申请日：1979-03-23
CPC分类号： C08F8/44
摘要： This invention relates to a process for the formation of a neutralized sulfonated polymer having about 10 to about 60 meq. sulfonate groups, wherein the sulfonate groups are neutralized with a zinc counterion. A cement of a polymer having olefinic functional groups and a non-reactive solvent is contacted with a sulfonated agent such as an acyl sulfate. The sulfonated polymer is then neutralized with a solution of zinc acetate dissolved in a solvent system of methanol alone or methanol and water, wherein the volume percent of methanol based on non-reactive solvent is less than about 10. A carboxylic acid can be then added to the cement of the neutralized sulfonated polymer thereby forming a zinc salt of the carboxylic acid in situ, wherein the zinc salt of the carboxylic acid is a preferential plasticizer for the zinc sulfonate groups. The Brookfield viscosity at 0.6 rpm at room temperature of the cement of the zinc neutralized sulfonated polymer is less than about 50,000 cps.
摘要翻译： 本发明涉及形成约10至约60meq的中和磺化聚合物的方法。 磺酸盐基团，其中磺酸盐基团用锌抗衡离子中和。 具有烯属官能团和非反应性溶剂的聚合物的水泥与磺化剂如酰基硫酸盐接触。 然后将磺化聚合物用溶于仅甲醇溶剂体系的乙酸锌溶液或甲醇和水中和，其中基于非反应性溶剂的甲醇的体积百分比小于约10.然后可以加入羧酸 到中和的磺化聚合物的水泥上，由此原位形成羧酸的锌盐，其中羧酸的锌盐是磺酸锌基团的优选增塑剂。 锌中和磺化聚合物的水泥在室温下在0.6rpm下的Brookfield粘度小于约50,000cps。
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公开(公告)号：US4221712A
公开(公告)日：1980-09-09
申请号：US22976
申请日：1979-03-23
申请人： Henry S. Makowski , Jan Bock , Robert D. Lundberg
发明人： Henry S. Makowski , Jan Bock , Robert D. Lundberg
CPC分类号： C08F8/44
摘要： This invention relates to an improved process for the formation of an improved gel-free neutralized sulfonated elastomeric polymer having about 10 to about 50 meq. unneutralized sulfonate groups, wherein the unneutralized sulfonate groups are neutralized with a metal counterion being selected from the group including lithium, sodium, potassium, cesium, barium, calcium, magnesium, zinc, lead, iron (II), copper (II), mercury (II), and nickel. A cement of an elastomeric polymer having olefinic functional groups dissolved in a non-reactive solvent is contacted with a sulfonating agent such as an acyl sulfate thereby sulfonating the elastomeric polymer, and the sulfonation reaction is subsequently quenched by the addition of isopropanol at a concentration level of about 5 to about 30 volume percent based on a volume of the non-reactive solvent. The unneutralized sulfonated elastomeric polymer is then neutralized with a neutralizing agent dissolved in water, the water being at a concentration level of less than about 2.5 volume percent based on the volume of the non-reactive solvent thereby forming a gel-free cement of the neutralized sulfonated elastomeric polymer having a Brookfield viscosity at room temperature of less than about 20,000 cps.
摘要翻译： 本发明涉及形成具有约10至约50meq的改进的无凝胶中和磺化弹性体聚合物的改进方法。 未中和磺酸酯基团，其中所述未中和磺酸酯基团被金属抗衡离子中和，所述金属抗衡离子选自锂，钠，钾，铯，钡，钙，镁，锌，铅，铁（II），铜（II），汞 （II）和镍。 将具有溶解在非反应性溶剂中的烯属官能团的弹性体聚合物的水泥与磺化剂如酰基硫酸酯接触，从而使弹性体聚合物磺化，然后通过加入浓度级别的异丙醇淬灭磺化反应 约5至约30体积％，基于非反应性溶剂的体积。 然后将未中和的磺化弹性体聚合物用溶解在水中的中和剂中和，基于非反应性溶剂的体积，水的浓度水平低于约2.5体积％，从而形成中和的无凝胶的水泥 磺化弹性体聚合物在室温下的Brookfield粘度小于约20,000cps。
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公开(公告)号：US4169820A
公开(公告)日：1979-10-02
申请号：US855757
申请日：1977-11-29
申请人： Jan Bock , Robert D. Lundberg , Henry S. Makowski
发明人： Jan Bock , Robert D. Lundberg , Henry S. Makowski
CPC分类号： C08L23/32
摘要： This invention relates to extrusion and injection moldable type elastomeric compositions having a viscosity at 200.degree. C. at 0.73 sec.sup.-1 of about 8.times.10.sup.4 to about 8.times.10.sup.5 poises. The compositions used for elastomeric articles include 100 parts of a neutralized sulfonated EPDM terpolymer; about 25 to about 150 parts per hundred of a non-polar process oil; about 50 to about 300 parts per hundred of a filler; and a preferential plasticizer at about 0 to about 50 parts per hundred based on 100 parts of the sulfonated elastomeric polymer. The composition may also include a crystalline polyolefinic thermoplastic at less than about 100 parts per hundred by weight.These blend compositions can be readily processed due to their superior rheological properties on conventional plastic fabrication equipment into elastomeric articles having excellent physical properties and desirable rubbery characteristics.
摘要翻译： 本发明涉及在200℃，0.73秒-1时粘度为约8×10 4至约8×10 5泊的挤出和注射成型型弹性体组合物。 用于弹性制品的组合物包括100份中和的磺化EPDM三元共聚物; 每百份非极性加工油约25至约150份; 每百份填料约50至约300份; 和基于100份磺化弹性体聚合物的约0至约50份/ 100的优选增塑剂。 组合物还可以包含小于约100重量份/ 100重量份的结晶聚烯烃热塑性塑料。
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公开(公告)号：US4160751A
公开(公告)日：1979-07-10
申请号：US855765
申请日：1977-11-29
申请人： Jan Bock , Robert D. Lundberg , Henry S. Makowski
发明人： Jan Bock , Robert D. Lundberg , Henry S. Makowski
CPC分类号： C08L23/32 , Y10S260/31
摘要： This invention relates to injection moldable type elastomeric compositions having a viscosity at 200.degree. C. at 0.73 sec.sup.-1 of less than about 8.times.10.sup.4 poises. The compositions used for elastomeric articles include 100 parts of a neutralized sulfonated EPDM terpolymer; about 25 to about 150 parts per hundred of a non-polar process oil; about 25 to about 200 parts per hundred of a filler; and a preferential plasticizer at about less than 50 parts per hundred based on 100 parts of the sulfonated elastomeric polymer. The composition may also include a crystalline polyolefinic thermoplastic at least than about 100 parts per hundred by weight.These blend compositions can be readily processed due to their superior rheological properties on conventional plastic fabrication equipment, especially on low pressure injection molding equipment into elastomeric articles having excellent physical properties and desirable rubbery characteristics.
摘要翻译： 本发明涉及可注射成型的弹性体组合物，其在200℃下的粘度为0.73秒-1小于约8×10 4泊。 用于弹性制品的组合物包括100份中和的磺化EPDM三元共聚物; 每百份非极性加工油约25至约150份; 每百份填料约25至约200份; 和基于100份磺化弹性体聚合物的约百分之50的优选增塑剂。 组合物还可以包括至少约100重量份/ 100重量％的结晶聚烯烃热塑性塑料。
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公开(公告)号：US4208310A
公开(公告)日：1980-06-17
申请号：US19704
申请日：1979-03-12
申请人： Robert D. Lundberg , Jan Bock , Henry S. Makowski
发明人： Robert D. Lundberg , Jan Bock , Henry S. Makowski
CPC分类号： C08L91/06 , C08L23/32 , Y10S260/31
摘要： This invention relates to elastomeric blend compositions of a neutralized sulfonated elastomeric polymer. The compositions include a major portion of a sulfonated elastomeric polymer and a minor proportion of a non-polar wax, wherein the resultant composition has both improved physical and rheological properties.
摘要翻译： 本发明涉及中和磺化弹性体聚合物的弹性共混组合物。 组合物包括磺化弹性体聚合物的主要部分和少部分非极性蜡，其中所得组合物具有改善的物理和流变性质。
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公开(公告)号：US4147677A
公开(公告)日：1979-04-03
申请号：US855764
申请日：1977-11-29
申请人： Robert D. Lundberg , Henry S. Makowski , Jan Bock
发明人： Robert D. Lundberg , Henry S. Makowski , Jan Bock
IPC分类号： C08L23/00 , C08J3/12 , C08K5/09 , C08L7/00 , C08L21/00 , C08L23/26 , C08L23/32 , C08L101/00 , C08L91/00
CPC分类号： C08L23/32 , Y10S260/31
摘要： This invention relates to a process for first preparing a free flowing finely divided powder of a neutralized sulfonated elastomer and subsequently and optionally admixing said formed powder with other agents such as fillers and oils thereby providing free flowing powders capable of being subsequently fabricated into tough elastomeric objects. The neutralized sulfonated elastomeric polymer can be converted into a free flowing finely divided powder which does not agglomerate or cold flow under ambient conditions by a variety of processes, preferably by a grinding process conducted at low temperatures. The formed powder of the neutralized sulfonated elastomeric polymer is blended with at least one chemical additive into a homogeneous mixture, wherein the chemical additive is selected from the group including fillers, polyolefinic thermoplastics, non-polar backbone process oils, lubricants or a metallic oxide and mixtures thereof. The homogeneous mixture is formed into a finished elastomeric article by conventional fabrication.
摘要翻译： {PG，1]本发明涉及一种首先制备中和的磺化弹性体的自由流动细碎粉末的方法，随后任选地将所形成的粉末与其它试剂如填料和油混合，从而提供能够随后制成的自由流动的粉末 变成坚韧的弹性物体。 中和的磺化弹性体聚合物可以转化成自由流动的细分散的粉末，其在环境条件下通过各种方法，优选通过在低温下进行的研磨过程不凝聚或冷流。 所形成的中和的磺化弹性体聚合物的粉末与至少一种化学添加剂混合成均匀的混合物，其中所述化学添加剂选自填料，聚烯烃热塑性塑料，非极性主链工艺油，润滑剂或金属氧化物，以及 其混合物。 均匀混合物通过常规制造形成成品弹性制品。
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9.发明授权Process for the formation of elastomeric blends of a sulfonated elastomeric polymer 失效用于形成磺化弹性体聚合物的弹性共混物的方法
公开(公告)号：US4277381A
公开(公告)日：1981-07-07
申请号：US22977
申请日：1979-03-23
申请人： Jan Bock , Henry S. Makowski , Robert D. Lundberg
发明人： Jan Bock , Henry S. Makowski , Robert D. Lundberg
CPC分类号： C08J3/21 , C08K5/01 , C08L23/32 , C08J2323/32 , Y10S260/31
摘要： This invention relates to a process for the manufacture of a blend composition of a neutralized sulfonated ethylene propylene terpolymer (EPDM) which includes the steps of sulfonating the EPDM dissolved in a solvent to form an unneutralized sulfonated elastomeric polymer. The solution of the unneutralized sulfonated EPDM is quenched with an aliphatic alcohol. The unneutralized sulfonated elastomeric polymer in solution is then neutralized with a neutralizing agent to form the neutralized sulfonated EPDM in solution. A critically selected non-polar backbone process oil is added under agitation to the solution thereby plasticizing the neutralized sulfonated EPDM with the process oil. The neutralized sulfonated EPDM plasticized with the process oil is then recovered from the solution.
摘要翻译： 本发明涉及一种制备中和磺化乙烯丙烯三元共聚物（EPDM）的共混组合物的方法，其包括将溶于溶剂中的EPDM磺化以形成未中和的磺化弹性体聚合物的步骤。 将未中和磺化EPDM的溶液用脂族醇淬灭。 然后将溶液中的未中和的磺化弹性体聚合物用中和剂中和以在溶液中形成中和的磺化EPDM。 在搅拌下向溶液中加入一种非常选择的非极性主链工艺油，由此用工艺油增塑中和的磺化EPDM。 然后从溶液中回收用工艺油增塑的中和磺化EPDM。
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公开(公告)号：US4157432A
公开(公告)日：1979-06-05
申请号：US855692
申请日：1977-11-29
CPC分类号： C08C19/20 , C08F8/36 , C08F8/44 , C08F2800/20 , Y10S260/31
摘要： A bulk sulfonation process for the preparation of sulfonated polymers from hydrocarbon polymers having olefinic unsaturation or aromatic moieties, or both, includes intimately mixing the polymer by mechanical means in the absence of a solvent for the polymers with a sulfonation reagent at a sufficient temperature and time to effect the desired degree of sulfonation. The sulfonated polymer may be recovered as the free sulfonic acid or neutralized ionically with a basic compound. Sulfonated polymers including a substantial proportion of aromatic moieties yield water-soluble or water-dispersible salts, useful as thickening and flocculating agents, when neutralized with ammonia monobasic cations or lower alkyl amines. These materials, however, when sulfonated at a low level, e.g.
摘要翻译： {PG，1用于由具有烯属不饱和键或芳族部分的烃聚合物制备磺化聚合物的本体磺化方法或两者包括通过机械方式在不存在溶剂的情况下将聚合物与磺化试剂在 足够的温度和时间来实现所需的磺化程度。 可以将磺化聚合物作为游离磺酸回收或用碱性化合物离子中和。 包括相当比例的芳族部分的磺化聚合物当用氨一元阳离子或低级烷基胺中和时产生水溶性或水分散性盐，可用作增稠剂和絮凝剂。 然而，这些材料当以低水平磺化时，例如， {21 10摩尔SO {HD 3 {L /摩尔芳族，表现像水不敏感的热塑性塑料。 磺化弹性体聚合物产生热塑性弹性体，其可以挤出，吹塑，注塑，并且当用多价阳离子或多胺中和时可用作通用橡胶。
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