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1.发明授权Transition-metal catalyst component for a Ziegler catalyst system, and the use of said system 失效用于ZIEGLER催化剂体系的过渡金属催化剂组分和使用系统
公开(公告)号：US5143881A
公开(公告)日：1992-09-01
申请号：US667118
申请日：1991-03-11
CPC分类号： C08F10/00
摘要： A transition-metal catalyst component for a Ziegler catalyst system, obtainable by1) mixing, in a solvent, an inorganic, oxidic carrier with1.1) a vanadium trihalide alcohol complex of the formula VY.sub.3.nZ--OH, whereY is chlorine or bromine,n is from 1 to 6, andZ is a monovalent, saturated, aliphatic, aromatic or araliphatic hydrocarbon radical having not more than 10 carbon atoms, and1.2) a titanium halide or a titanium trihalide/aluminum trihalide complex, where the halogen can be chlorine and/or bromine, or a titanium trihalide complex of the formula TiY.sub.3.nZ--OH or mixtures thereof, whereY is chlorine or bromine,n is from 1 to 6, andZ is a monovalent, saturated, aliphatic, aromatic or araliphatic hydrocarbon radical having not more than 10 carbon atoms, and1.3) a compound of the formula BX.sub.n Y.sub.m R.sub.p or SiX.sub.n Y.sub.m R.sub.q or mixtures thereof, whereX is OR,Y is chlorine, bromine or hydrogen, andR is a C.sub.1 - to C.sub.18 -hydrocarbon radical, with the proviso that n>0 and n+m+p=3 or n+m+q=4,2) removing the solvent by evaporation,3) mixing the solid-phase intermediate from step 2) with3.1) an organoaluminum catalyst component of the formula AlR.sub.m X.sub.3-m, whereR is a C.sub.1 - to C.sub.18 -hydrocarbon radical,m is from 1 to 3, andX is OR, chlorine, bromine or hydrogen, and3.2) an organic carboxylate or an organosilicon compound or a mixture thereof in an organic solvent, and4) if desired, isolating the solid-phase intermediate by filtration, washing and drying,and the use thereof for the homopolymerization or copolymerization of ethene are described.
摘要翻译： 用于齐格勒催化剂体系的过渡金属催化剂组分，其可通过以下步骤获得：1）在溶剂中将无机氧化物载体与1.1）式VY3.nZ-OH的三卤化钒醇络合物混合，其中Y是氯或溴 ，n为1-6，Z为不大于10个碳原子的一价饱和脂族芳族或芳脂族烃基，和1.2）卤化钛或三卤化钛/三卤化铝配合物，其中卤素可以 是氯和/或溴，或式TiY3.nZ-OH的三卤化钛配合物或其混合物，其中Y为氯或溴，n为1至6，Z为单价，饱和，脂族，芳族或 具有不超过10个碳原子的芳脂族烃基，和1.3）式BXnYmRp或SiXnYmRq的化合物或其混合物，其中X为OR，Y为氯，溴或氢，R为C1-至C18-烃基 ，条件是n> 0和n + m + p = 3或n + m + q = 4,2） 通过蒸发除去溶剂，3）将来自步骤2）的固相中间体与3.1）式AlRmX3-m的有机铝催化剂组分混合，其中R是C 1 -C 18烃基，m为1至3 ，和X为OR，氯，溴或氢，以及3.2）有机溶剂中的有机羧酸盐或有机硅化合物或其混合物，以及4）如果需要，通过过滤，洗涤和干燥分离固相中间体， 并描述了其用于乙烯的均聚或共聚的用途。
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2.发明授权
公开(公告)号：US5455216A
公开(公告)日：1995-10-03
申请号：US124047
申请日：1993-09-21
申请人： Hans-Joachim Mueller , Godofredo Follmer , Rainer Konrad , Roland Saive , Martin Lux , Hans-Helmut Goertz , Guido Funk
发明人： Hans-Joachim Mueller , Godofredo Follmer , Rainer Konrad , Roland Saive , Martin Lux , Hans-Helmut Goertz , Guido Funk
CPC分类号： C08F10/00
摘要： A process for the preparation of a supported catalyst for the polymerization of .alpha.-olefins, in which(1) a silicon dioxide-containing support gel is prepared by(1.1) introducing a sodium water glass or potassium water glass solution into a swirling stream of an aqueous mineral acid longitudinally and tangentially to the stream, spraying the resultant silica hydrosol in drop form into a gaseous medium and allowing it to solidify to form a hydrogel, and freeing the resultant hydrogel from salts by washing without prior ageing,(1.2) drying the hydrogel resulting from (1.1) to form the support gel,(2) the support gel (1) is charged with chromium trioxide or a chromium compound which can be converted into chromium trioxide under the conditions of process step (3), giving a chromium-containing support gel, and(3) the chromium-containing support gel (2) is heated at from 400.degree. to 1100.degree. C. for from 10 to 1000 minutes in an anhydrous gas stream containing oxygen in a concentration of greater than 10% by volume,comprises drying the hydrogel resulting from step (1.1) in step (1.2) within a time of not more than 60 seconds in a shaping, high-speed dryer at an inlet temperature of from 80.degree. to 400.degree. C.
摘要翻译： 一种制备用于α-烯烃聚合的负载催化剂的方法，其中（1）含二氧化硅的载体凝胶通过（1.1）将钠水玻璃或钾水玻璃溶液引入旋流 将水性无机酸纵向和切向于料流，将所得的二氧化硅水溶胶以液滴形式喷雾到气态介质中并使其固化形成水凝胶，并通过在没有预先熟化的情况下洗涤将所得水凝胶从盐中释放，（1.2）干燥 由（1.1）产生的形成支持凝胶的水凝胶，（2）载体凝胶（1）中加入三氧化铬或铬化合物，其可以在工艺步骤（3）的条件下转化为三氧化铬，得到 含铬载体凝胶，（3）含铬载体凝胶（2）在含有浓度浓度的氧的无水气流中在400〜1100℃下加热10〜1000分钟 大于10体积％包括在入口温度为80°至400°的成形高速干燥器中在不超过60秒的时间内将步骤（1.2）中由步骤（1.1）得到的水凝胶干燥 DEG C.
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3.发明授权
公开(公告)号：US5625013A
公开(公告)日：1997-04-29
申请号：US422937
申请日：1995-05-24
申请人： Hans-Joachim Mueller , Godofredo Follmer , Rainer Konrad , Roland Saive , Martin Lux , Hans-Helmut Goertz , Guido Funk
发明人： Hans-Joachim Mueller , Godofredo Follmer , Rainer Konrad , Roland Saive , Martin Lux , Hans-Helmut Goertz , Guido Funk
CPC分类号： C08F10/00
摘要： A process for the preparation of a supported catalyst for the polymerization of .alpha.-olefins, in which(1) a silicon dioxide-containing support gel is prepared by(1.1) introducing a sodium water glass or potassium water glass solution into a swirling stream of an aqueous mineral acid longitudinally and tangentially to the stream, spraying the resultant silica hydrosol in drop form into a gaseous medium and allowing it to solidify to form a hydrogel, and freeing the resultant hydrogel from salts by washing without prior ageing,(1.2) drying the hydrogel resulting from (1.1) to form the support gel,(2) the support gel (1) is charged with chromium trioxide or a chromium compound which can be converted into chromium trioxide under the conditions of process step (3), giving a chromium-containing support gel, and(3) the chromium-containing support gel (2) is heated at from 400.degree. to 1100.degree. C. for from 10 to 1000 minutes in an anhydrous gas stream containing oxygen in a concentration of greater than 10% by volume,comprises drying the hydrogel resulting from step (1.1) in step (1.2) within a time of not more than 60 seconds in a shaping, high-speed dryer at an inlet temperature of from 80.degree. to 400.degree. C.
摘要翻译： 一种制备用于α-烯烃聚合的负载催化剂的方法，其中（1）含二氧化硅的载体凝胶通过（1.1）将钠水玻璃或钾水玻璃溶液引入旋流 将水性无机酸纵向和切向于料流，将所得的二氧化硅水溶胶以液滴形式喷雾到气态介质中并使其固化形成水凝胶，并通过在没有预先熟化的情况下洗涤将所得水凝胶从盐中释放，（1.2）干燥 由（1.1）产生的形成支持凝胶的水凝胶，（2）载体凝胶（1）中加入三氧化铬或铬化合物，其可以在工艺步骤（3）的条件下转化为三氧化铬，得到 含铬载体凝胶，（3）含铬载体凝胶（2）在含有浓度浓度的氧的无水气流中在400〜1100℃下加热10〜1000分钟 大于10体积％包括在入口温度为80°至400°的成形高速干燥器中在不超过60秒的时间内将步骤（1.2）中由步骤（1.1）得到的水凝胶干燥 DEG C.
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4.发明授权Process for the preparation of a supported catalyst for the polymerization of .alpha.-olefins 失效制备用于α-烯烃聚合的负载型催化剂的方法
公开(公告)号：US5310712A
公开(公告)日：1994-05-10
申请号：US953629
申请日：1992-09-30
申请人： Guido Funk , Rainer Hemmerich , Hans Gropper , Erich Kolk , Godofredo Follmer
发明人： Guido Funk , Rainer Hemmerich , Hans Gropper , Erich Kolk , Godofredo Follmer
CPC分类号： C08F10/00
摘要： In a novel process for the preparation of a supported catalyst for the polymerization of .alpha.-olefins, a carrier gel (1) is first prepared by a method in which a sodium or potassium waterglass solution is introduced into a stream of an aqueous mineral acid which is subjected to angular momentum and may contain aluminum ions, longitudinally and tangentially to the stream, the resulting silica hydrosol sprayed in the form of drops into a gaseous medium and allowed to solidify into a hydrogel, and the resulting hydrogel is freed from salts by washing without prior aging and, if necessary, freed from some of the water by extraction with alcohols and/or ketones and is then dried. This gives the carrier gel (1), which is milled and is fractionated according to particle size. In a second process step, the carrier gel (1) is laden with chromium trioxide or with a chromium compound which can be converted into chromium trioxide, after which the resulting chromium-containing carrier gel (2) is heated at from 400.degree. to 1100.degree. C. for from 10 to 1,000 minutes in an anhydrous gas stream containing oxygen in a concentration of more than 10% by volume. In the novel process, it is essential that the drying of the hydrogel be carried out with formation of the carrier gel (1) in a fast dryer in the course of not more than 300 seconds at an inlet temperature of from 200.degree. to 600.degree. C. The supported catalyst prepared in this manner gives homo- and copolymers of ethylene having excellent low temperature impact strength.
摘要翻译： 在制备用于α-烯烃聚合的负载催化剂的新方法中，首先通过一种方法制备载体凝胶（1），其中将钠或钾水玻璃溶液引入无机酸水溶液的流中， 经受角动量并且可以包含与流纵向和切向的铝离子，所得到的二氧化硅水溶胶以液滴的形式喷入气态介质中并使其固化成水凝胶，并且通过洗涤将所得水凝胶除去盐 没有预先老化，如果需要，通过用醇和/或酮萃取除去一些水，然后干燥。 这得到载体凝胶（1），其被研磨并根据粒度进行分级。 在第二工艺步骤中，载体凝胶（1）装载有三氧化铬或可以转化成三氧化铬的铬化合物，之后将所得含铬载体凝胶（2）在400℃加热至1100℃ 在含有浓度超过10体积％的氧气的无水气流中10分钟至1000分钟。 在新颖的方法中，必须在200〜600℃的入口温度下，在不超过300秒的快速干燥器中形成载体凝胶（1），进行水凝胶的干燥。 C.以这种方式制备的负载催化剂得到具有优异的低温冲击强度的乙烯均聚物和共聚物。
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