Abstract:
The invention relates to a process for preparing an essentially spherical support for olefin polymerization catalysts, which comprises the steps: preparation of a hydrogel comprising a cogel of silicon oxide and at least one further metal oxide, if appropriate, washing of the hydrogel until the content of alkali metal ions is less than 0.1% by weight, based on the weight of solids, extraction of the water from the hydrogel until the water content is less than 5% by weight, based on the total content of liquid, and drying of the hydrogel to form a xerogel. According to the invention, the extraction step comprises at least one first extraction with a first organic solvent which is at least partially miscible with water down to a water content of 50% by weight, followed by at least one second extraction with a second organic solvent which is at least partially miscible with water.
Abstract:
The invention relates to a method for producing supported chromium catalysts for the polymerisation of olefins by loading a xerogel support with chromium by adding to the xerogel support a volume of a 0.025 to 15% by weight solution of a chromium compound or a volume of a solution comprising from 0.025 to 7.8% by weight of Cr which is essentially converted into a chromium(VI) compound on heating in a water-free stream of gas under oxidizing conditions at temperatures in the range from 300 to 1100° C. for a period of from 10 to 1000 minutes in a solvent which comprises a maximum of 20% by weight of water, and subsequently evaporating the solvent, where the volume of the chromium salt solution employed is smaller than the pore volume of the xerogel support.
Abstract:
A novel Phillips catalyst for the copolymerization of ethylene with .alpha.-olefins, contains, as a catalytically active component, a finely divided, aluminum silicate-supported, phosphorus-containing chromium catalyst. This can be prepared by applying at least one organic phosphorus(III), (IV) and/or (V) compound and at least one chromium(III) compound which does not react with said phosphorus compounds under the reaction conditions used, in succcession in any order or simultaneously, to a finely divided aluminum silicate hydrogel or xerogel with formation of a catalyst intermediate and activating the catalyst intermediate at elevated temperatures in an oxidizing atmosphere, with the result that the chromium catalyst is formed. The novel Phillips catalyst gives ethylene/.alpha.-olefin copolymers in which the comonomers are more uniformly distributed over the copolymer chains than is the case with ethylene/.alpha.-olefin copolymers which have been prepared with the aid of conventional Phillips catalysts. Moldings which have been produced from the ethylene/.alpha.-olefin copolymers obtained in the novel procedure have a particularly high environmental stress cracking resistance and an excellent creep rupture strength.
Abstract:
The homopolymerization and copolymerization of ethene are carried out using a Ziegler catalyst system consisting of(1) a transition metal catalyst component,(2) an organoaluminum catalyst component and(3) an organohalogen catalyst component.In the homopolymerization or copolymerization, the solid-phase product (VI) used as (1) is the product which has been obtained by a method in which (1.1) first (1.1.1) an inorganic oxidic substance (I) as the carrier and (1.1.2) a solution (II) of (IIa) a certain oxahydrocarbon and (IIb) a vanadium trichloride/alcohol complex and (IIc) a silicon or boron compound are combined with formation of a suspension (III), the latter is evaporated down to form a solid-phase intermediate (IV), and (1.2) then (1.2.1) the intermediate (IV) obtained in (1.1) and (1.2.2) a dissolved organoaluminum compound (V) are combined with the formation of a suspension, the solid-phase product (VI) obtained as the suspended substance being the transition metal catalyst component (1).
Abstract:
Homopolymerization and copolymerization of ethene are carried out using a Ziegler catalyst system consisting of (1) a transition metal catalyst component prepared by a method in which (1.1) first (1.1.1) an inorganic oxide substance (I) as a carrier and (1.1.2) a solution (II) of (IIa) a certain oxahydrocarbon and (IIb) a mixture of (IIb1) a vanadium trichloride/alcohol complex, (IIb2) a titanium trihalide or titanium trihalide/alcohol complex and, if desired, (IIb3) a zirconium tetrahalide, are combined with formation of a suspension (III), the latter is evaporated down to form a solid-phase intermediate (IV), (1.2) then (1.2.1) the solid-phase intermediate (IV) obtained from (1.1), and (1.2.2) a dissolved organoaluminum compound (V), are combined with formation of a suspension, the resulting suspended substance being a solid-phase product (VI), (2) an organoaluminum catalyst component and (3) an organohalogen catalyst component. In this process, the transition metal catalyst component (1) used is one prepared by a method in which (1.3) in addition (1.3.1) the product (VI) obtained from (1.2) is reacted with (1.3.2) oxygen, the resulting solid-phase end product (VII) being the novel transition metal catalyst component (1).
Abstract:
A transition metal catalyst component (1) for Ziegler catalyst systems is prepared by (1.1) first combining (1.1.1) an inorganic oxidic substance (I), as the carrier, with (1.1.2) a solution (II) consisting of (IIa) an organic solvent and (IIb) a transition metal composition to form a suspension (III), evaporating down this suspension to form a solid-phase intermediate (IV) and (1.2) then combining (1.2.1) the solid-phase intermediate (IV) obtained from (1.1) with (1.2.2) a solution of an organoaluminum compound (V) to form a suspension, the resulting suspended solid-phase products (VI) being the transition metal catalyst component (1).The characteristic feature is that the solution (II) employed in stage (1.1) consists of (IIa) a certain oxahydrocarbon and (IIb) a mixture of (IIb1) a vanadium trichloride/alcohol complex, (IIb2) a titanium trihalide and (IIb3) a zirconium tetrahalide.
Abstract:
A process for introducing a catalyst powder based on a titanium compound supported on magnesium halide into a gas-phase olefin polymerization reactor, characterized in that it comprises: (a) storing the catalyst powder under an atmosphere of a liquid C3-C12 alkane; (b) withdrawing from step (a) a measured amount of said catalyst powder by means of a rotary valve; (c) transferring said metered amount of catalyst powder to a catalyst activation section by a continuous pick-up flow of a liquid C3-C12 alkane; (d) contacting the catalyst powder with a liquid phase comprising an organo-aluminum compound and optionally an external donor compound, at a temperature ranging from −20° C. to 60° C.; (e) introducing the activated catalyst powder in one or more gas-phase olefin polymerization reactors, where a gaseous mixture comprising at least one alpha-olefin is subjected to polymerization.
Abstract:
A process for introducing a catalyst powder based on a titanium compound supported on magnesium halide into a gas-phase olefin polymerization reactor, characterized in that it comprises: (a) storing the catalyst powder under an atmosphere of a liquid C3-C12 alkane; (b) withdrawing from step (a) a measured amount of said catalyst powder by means of a rotary valve; (c) transferring said metered amount of catalyst powder to a catalyst activation section by a continuous pick-up flow of a liquid C3-C12 alkane; (d) contacting the catalyst powder with a liquid phase comprising an organo-aluminum compound and optionally an external donor compound, at a temperature ranging from −20° C. to 60° C.; (e) introducing the activated catalyst powder in one or more gas-phase olefin polymerization reactors, where a gaseous mixture comprising at least one alpha-olefin is subjected to polymerization.
Abstract:
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.
Abstract translation: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.