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公开(公告)号：US4110523A
公开(公告)日：1978-08-29
申请号：US762856
申请日：1977-01-27
申请人： Guenther Schweier , Erich Kolk , Heinz Mueller-Tamm , Hans Frielingsdorf , Robert Bachl , Wolfgang Gruber
发明人： Guenther Schweier , Erich Kolk , Heinz Mueller-Tamm , Hans Frielingsdorf , Robert Bachl , Wolfgang Gruber
CPC分类号： C08F10/00
摘要： A process for the manufacture of homopolymers and copolymers of .alpha.-monoolefins of 2 to 6 carbon atoms by polymerizing the monomer or monomers by means of a Ziegler catalyst system comprising (1) a catalyst component containing titanium and (2) a particular compound of the metals aluminum, magnesium or zinc, the atomic ratio of titanium from catalyst component (1) to metal from catalyst component (2) being from 1:0.1 to 1:500, wherein the titanium-containing catalyst component (1) employed is the solid-phase product (IV) obtained by bringing into contact (1.1) a finely divided, porous, inorganic oxidic material (I) which has the formula SiO.sub.2 . aAl.sub.2 O.sub.3 --, where a is a number from 0 to 2, and (1.2) a solution (II) formed on bringing together (IIa) 100 parts by weight of an alcohol of the general formula Z--OH, where Z is a saturated hydrocarbon radical of 1 to 8 carbon atoms, (IIb) from 0.01 to 6 parts by weight (calculated as titanium) of a titanium trihalide and (IIc) from 0.01 to 4 parts by weight (calculated as magnesium) of a magnesium compound which is soluble in the alcohol (IIa), so as to form a dispersion (III), with the proviso that the weight ratio of inorganic oxidic material (I) to titanium in the titanium trihalide (IIb) is from 1:0.01 to 1:0.2 and the weight ratio of inorganic oxidic material (I) to magnesium in the magnesium compound (IIc) is from 1:0.01 to 1:0.25, and evaporating the dispersion (III) until it has a dry consistency, thus forming the solid-phase product (IV). The new process is particularly advantageous for the manufacture of homopolymers and copolymers having, for example, particularly advantageous morphological properties.
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公开(公告)号：US4175170A
公开(公告)日：1979-11-20
申请号：US720777
申请日：1976-09-07
申请人： Guenther Schweier , Robert Bachl , Heinz Mueller-Tamm , Hans Frielingsdorf , Wolfgang Gruber , Erich Kolk
发明人： Guenther Schweier , Robert Bachl , Heinz Mueller-Tamm , Hans Frielingsdorf , Wolfgang Gruber , Erich Kolk
CPC分类号： C08F10/00
摘要： Manufacture of polymers of .alpha.-monoolefins by polymerization with a Ziegler catalyst system comprising (1) a catalyst component containing titanium and/or vanadium and (2) a particular compound of the metals aluminum, magnesium or zinc. The characteristic feature of the process according to the invention is that the catalyst component (1) containing titanium and/or vanadium is the solid-phase product (VII) contained by first (1.1) bringing a finely divided porous inorganic oxidic material (I), which has the formula Al.sub.2 O.sub.3 or SiO.sub.2.aAl.sub.2 O.sub.3, where a is a number from 0 to 2, into contact with an aluminum compound (II) dissolved in an organic solvent, to form a solid-phase product (III), then (1.2) bringing the solid-phase product (III) obtained in stage (1.1) into contact with a magnesium compound (IV), dissolved in an organic solvent, to form a solid-phase product (V), and finally (1.3) bringing the solid-phase product (V) obtained in stage (1.2) into contact with a compound (VI) of the transition metals titanium and/or vanadium to form a solid-phase product (VII). This process functions better than comparable conventional processes.
摘要翻译： 通过用齐格勒催化剂体系聚合制备α-单烯烃的聚合物，其包含（1）含有钛和/或钒的催化剂组分和（2）金属铝，镁或锌的特定化合物。 根据本发明的方法的特征在于，含有钛和/或钒的催化剂组分（1）是首先（1.1）所含的固体相产物（VII），使细碎的多孔无机氧化物质（I） ，其中a为0至2的数为Al 2 O 3或SiO 2·aAl 2 O 3，与溶于有机溶剂的铝化合物（II）接触，形成固相产物（III），然后（1.2 ）使得在阶段（1.1）中获得的固相产物（III）与溶解在有机溶剂中的镁化合物（IV）接触形成固相产物（V），最后（1.3） 在阶段（1.2）中获得的固相产物（V）与过渡金属钛和/或钒的化合物（VI）接触以形成固相产物（VII）。 该过程比可比较的常规方法更好。
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公开(公告)号：US4113933A
公开(公告)日：1978-09-12
申请号：US762858
申请日：1977-01-27
申请人： Gunther Schweier , Erich Kolk , Heinz Mueller-Tamm , Hans Frielingsdorf , Robert Bachl , Wolfgang Gruber
发明人： Gunther Schweier , Erich Kolk , Heinz Mueller-Tamm , Hans Frielingsdorf , Robert Bachl , Wolfgang Gruber
CPC分类号： C08F10/00
摘要： A process for the manufacture of homopolymers and copolymers of .alpha.-monoolefins of 2 to 6 carbon atoms by polymerizing the monomer or monomers by means of a Ziegler catalyst system comprising (1) a catalyst component containing titanium and (2) a particular compound of aluminum, magnesium or zinc, the atomic ratio of titanium from catalyst component (1) to metal (Me) from catalyst component (2) being from 1 : 0.1 to 1 : 500, wherein the titanium-containing catalyst component (1) employed is the solid-phase product (VI) obtained by (1.1) first bringing into contact (1.1.1) a particular finely divided, porous, inorganic oxidic material (I) and (1.1.2) a particular aluminum compound (II) dissolved in an organic solvent, to form a solid-phase product (III) and (1.2) then bringing into contact (1.2.1) the solid-phase product (III) obtained from stage (1.1) and (1.2.2) a solution (IV) which is obtained on bringing together (IVa) 100 parts by weight of a particular alcohol, (IVb) from 0.01 to 6 parts by weight (calculated as titanium) of a titanium trihalide and (IVc) from 0.01 to 4 parts by weight (calculated as magnesium) of a magnesium compound which is soluble in the alcohol (IVa), to form a dispersion (V), and evaporating the dispersion (V) until it has a dry consistency, thus forming the solid-phase product (VI). The new process is particularly advantageous for the manufacture of homopolymers and copolymers having, for example, particularly advantageous morphological properties.
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公开(公告)号：US4042770A
公开(公告)日：1977-08-16
申请号：US631642
申请日：1975-11-13
摘要： This invention relates to a process for the manufacture of olefin polymers by polymerization of monoolefins with the aid of a silicic xerogel/chromium trioxide catalyst obtained by (1) synthesizing a particulate silicic xerogel, (2) doping this xerogel with chromium trioxide or a chromium compound which converts to chromium trioxide under conditions of stage (3) and (3) maintaining the resulting product at an elevated temperature in a water-free oxygen-containing stream of gas. The characteristic feature of the process of the invention is that the silicic xerogel/chromium trioxide catalyst used is one obtained by (1) synthesizing the silicic xerogel in the first stage as follows: (1.1) taking an aqueous solution of a sodium silicate, (1.2) substituting substantially all of the sodium ions contained in said solution by hydrogen ions by means of an ion exchanger, (1.3) introducing a water-soluble aluminum salt into the resulting aqueous silicic acid solution, (1.4) adjusting the pH of the solution obtained in stage (1.3) to from 0.1 to 3.5, if necessary, (1.5) adjusting the solution obtained in (1.3) or (1.4) to a pH of from 4 to 12 by means of a nitrogen-base compound, (1.6) extracting the product forming the solid phase in stage (1.5) (silicic hydrogel) by means of an alkanol and/or alkanone until the organic liquid absorbs no more water and, finally, (1.7) drying the dehydrated gel saturated with organic liquid resulting from stage (1.6) (xerogel formation). This process makes it possible to obtain polymers having a satisfactory particle size distribution and a favorable melt index.
摘要翻译： 本发明涉及一种通过使用（1）合成硅氧烷干凝胶得到的硅胶干凝胶/三氧化铬催化剂，通过单烯烃的聚合制备烯烃聚合物的方法，（2）将这种干凝胶与三氧化铬或铬 在阶段（3）和（3）的条件下转化成三氧化铬的化合物在无水的含氧气流中保持所得产物在升高的温度。 本发明方法的特征在于，使用的硅干燥剂/三氧化铬催化剂是通过（1）在第一阶段合成硅干凝胶得到的催化剂如下：（1.1）取硅酸钠水溶液（ 1.2）通过离子交换器用氢离子基本上全部取代所述溶液中所含的所有钠离子，（1.3）将水溶性铝盐引入所得水性硅酸溶液中，（1.4）调节溶液的pH （1.3）中得到的化合物为0.1至3.5，如果需要，（1.5）通过氮碱化合物将（1.3）或（1.4）中获得的溶液调节至4至12的pH，（1.6） 通过链烷醇和/或烷酮萃取在阶段（1.5）（硅水凝胶）中形成固相的产物，直到有机液体吸收不再多的水，最后（1.7）干燥由有机液体饱和的脱水凝胶 阶段（1.6）（干凝胶形成）。 该方法可以获得具有令人满意的粒度分布和良好熔融指数的聚合物。
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公开(公告)号：US4169925A
公开(公告)日：1979-10-02
申请号：US901196
申请日：1978-04-28
CPC分类号： C08F10/00
摘要： A process for the manufacture of olefin polymers by polymerizing .alpha.-monoolefins at relatively low temperatures and relatively low olefin pressures by means of a catalyst obtained from a silicate carrier (component a), an aluminum compound (component b) and a chromium compound (component c). The catalyst is obtained by (1) in a first stage, initially (1.1) charging a particular silicate carrier (component a) with (1.2) a mixture of (1.2.1) an aluminum salt or a mixture of an aluminum salt with up to 80 mole%, based on the salt mixture, of a nickel-II salt (component b) and (1.2.2) a chromium compound (component c), this compound being chromium trioxide or a compound which is converted to chromium trioxide under the conditions of stage (2), by treatment with a solution of the mixture (1.2), and (2), in a second stage then maintaining the product, obtained from stage (1), for a certain time at a high temperature in an anhydrous oxygen-containing gas stream. The process may be used to produce polymers having a relatively broad molecular weight distribution.
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公开(公告)号：US4007321A
公开(公告)日：1977-02-08
申请号：US551494
申请日：1975-02-20
申请人： Norbert Scholz , Georg Friedrich Vock , Kurt Erdmann , Guenther John , Hans Frielingsdorf , Wolfgang Gruber , Heinz Mueller-Tamm
发明人： Norbert Scholz , Georg Friedrich Vock , Kurt Erdmann , Guenther John , Hans Frielingsdorf , Wolfgang Gruber , Heinz Mueller-Tamm
IPC分类号： C08F2/00 , B01J3/04 , B01J8/00 , B01J19/18 , C08F2/04 , C08F6/00 , C08F6/06 , C08F10/00 , C08F110/00 , C08F110/02 , C08F2/14 , C08F6/24
CPC分类号： B01J19/1837 , B01J3/044 , B01J8/0055 , B01J8/007 , C08F110/00 , C08F10/00 , C08F110/02
摘要： Particulate olefin polymers are prepared by catalytic polymerization of monoolefins in an auxiliary liquid containing the monomers to be polymerized in dissolved form and the particulate polymer product in suspended form. The reaction mixture is recycled in a loop to which the starting materials are fed and from which the particulate polymer formed is removed. The essential features are (a) that a side stream is branched off from the loop, (b) that the side stream is caused to pass through a separating zone in which particulate olefin polymer is separated by centrifugal acceleration at temperatures and pressures in the same range as present in the loop and (c) that the separated particulate olefin polymer is discharged through flashing means.
摘要翻译： 颗粒状烯烃聚合物是通过单链烯烃在含有待溶解形式聚合的单体的辅助液体和悬浮形式的颗粒状聚合物产物进行催化聚合来制备的。 将反应混合物循环在起始原料进料的循环中，从中除去形成的颗粒聚合物。 基本特征是（a）侧流从环分支，（b）使侧流通过分离区，其中通过离心加速在相同温度和压力下分离出颗粒烯烃聚合物 存在于循环中的范围，（c）分离的颗粒状烯烃聚合物通过闪蒸装置排出。
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公开(公告)号：US4092468A
公开(公告)日：1978-05-30
申请号：US761259
申请日：1977-01-21
CPC分类号： C08F10/00
摘要： A process for the manufacture of olefin polymers by polymerizing .alpha.-monoolefins of 2 to 8 carbon atoms by means of a catalyst which is obtained from a silicon-containing material (component a), an organo-metallic compound containing alkyl groups (component b) and a chromium compound (component c), wherein the catalyst employed is obtained by (1) first bringing into contact (1.1) an alkogel (component a) of the empirical formula SiO.sub.2 .multidot. m Al.sub.2 O.sub.3 .multidot. n ROH, where m is a number from 0 to 2, n is a number such that the content of ROH in the alkogel is from 1 to 85 per cent by weight and R is alkyl of 3 to 8 carbon atoms, and (1.2) an aluminum compound containing certain alkyl groups (component b), with intimate mixing, to form a solid-phase reaction product, (2) then bringing into contact (2.1) the solid-phase reaction product obtained from stage (1) and (2.2) a solution of a particular chromium compound (component c), with intimate mixing and evaporation of the solvent, and (3) finally heating the product, obtained from stage (2), in an anhydrous stream of gas containing oxygen, with the proviso that the product obtained from stage (1) or from stage (2) is dried and comminuted before it is used further in the next stage. This process makes it possible to influence the essential properties of the polymers in relatively diverse ways, in the desired direction, by relatively slight modifications of the catalyst.
摘要翻译： 通过由含硅材料（组分a），含有烷基的有机金属化合物（组分b）获得的催化剂聚合2-8个碳原子的α-单烯烃制备烯烃聚合物的方法， 和铬化合物（成分c），其中所用的催化剂通过以下步骤获得：（1）首先使经验式SiO x x Al 2 O 3 xn ROH的烷烃（组分a）接触（1.1），其中m是从0到 2中，n是使烷烃中的ROH含量为1〜85重量％，R为3〜8个碳原子的烷基，（1.2）含有某些烷基的铝化合物（成分b） ，紧密混合，形成固相反应产物，（2）然后使从（1）和（2.2）阶段获得的固相反应产物与特定的铬化合物（组分c ），溶剂充分混合和蒸发，（3）最终他 将从阶段（2）获得的产物在含氧气体的无水流中搅拌，条件是从阶段（1）或阶段（2）获得的产物干燥并粉碎，然后再在下一个 阶段。 该方法可以通过催化剂的相对轻微的改变，以相对多种方式在所需方向上影响聚合物的基本性能。
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公开(公告)号：US4110522A
公开(公告)日：1978-08-29
申请号：US761258
申请日：1977-01-21
CPC分类号： C08F10/00
摘要： A process for the manufacture of olefin polymers by polymerizing .alpha.-monoolefins of 2 to 8 carbon atoms by means of a catalyst which is obtained from a silicate carrier (component a), an organo-metallic compound containing alkoxide groups (component b) and a chromium compound (component c), wherein the catalyst employed is obtained by (1) first charging (1.1) a finely divided porous xerogel (component a) of the formula SiO.sub.2 . m Al.sub.2 O.sub.3, where m is a number from 0 to 2, with (1.2) a particular aluminum compound containing alkoxide groups (component b), (2) then charging (2.1) the product obtained from stage (1) with (2.2) a particular chromium compound (component c) by treatment with a solution of the chromium compound, with intimate mixing and evaporation of the solvent and (3) finally heating the product, obtained from stage (2), in an anhydrous stream of gas containing oxygen. This process makes it possible to influence the essential properties of the polymers in relatively diverse ways, in the desired direction, by relatively slight modifications of the catalyst.
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公开(公告)号：US4037042A
公开(公告)日：1977-07-19
申请号：US720249
申请日：1976-09-02
CPC分类号： C08F10/00
摘要： A process for the manufacture of olefin polymers by polymerization of .alpha.-monoolefins by means of a silicic acid xerogel/chromium trioxide catalyst, which is obtained by a method wherein (1) a finely divided silicic acid xerogel is first manufactured by (1.1) employing a silicic acid hydrogel of relatively high solids content, (1.2) extracting at least 60% of the water contained in the hydrogel from the latter by means of a particular organic liquid, (1.3) drying the gel thus obtained until there is no further loss in weight (xerogel formation) and (1.4) reducing the xerogel thus obtained to particles of diameter from 20 to 2,000 .mu.m,2. this xerogel is then charged with the desired amount of chromium from a solution of chromium trioxide or a solution of a chromium compound which under the conditions of stage (3) is converted to chromium trioxide, with evaporation of the solvent, and3. finally the product thus obtained is heated in an anhydrous stream of gas containing oxygen. The process according to the invention is charaterized in that a catalyst is employed which is manufactured under such conditions that in stage (1) the starting material is a silicic acid hydrogel (1.1) which is substantially spherical, has a particle diameter of from 1 to 8 mm and is obtained byA. introducing a solution of sodium waterglass or potassium waterglass both longitudinally and tangentially into a vortical stream of an aqueous inorganic acid,B. spraying droplets of the resulting silicic acid hydrosol into a gaseous medium,C. allowing the sprayed hydrosol to solidify to a hydrogel in the gaseous medium andD. freeing the resulting substantially spherical hydrogel from salts by washing, without prior aging. The catalyst gives polymers having good processability.
摘要翻译： 一种通过使用硅酸干凝胶/三氧化铬催化剂聚合α-单烯烃制备烯烃聚合物的方法，其通过以下方法获得：其中（1）细分硅酸干凝胶首先由（1.1）采用 具有相对较高固体含量的硅酸水凝胶，（1.2）借助于特定的有机液体从后者中提取水凝胶中至少60％的水，（1.3）干燥所获得的凝胶，直至不再有损失 重量（干凝胶形成）和（1.4）将由此获得的干凝胶还原至直径为20至2,000μm的颗粒。2.该XEROGEL随着三氯化铬溶液或A溶液中所需的铬量而充满 在三级条件下（3）的铬化合物转化为三氧化二铬，溶剂的蒸发，以及3.最终获得的产物在含有氧气的气体的不稳定流中被加热。 根据本发明的方法的特征在于，使用在这样的条件下制造的催化剂：在步骤（1）中，起始材料是基本上为球形的硅酸水凝胶（1.1），其粒径为1至 8毫米，通过A.将钠水玻璃或钾水玻璃的溶液纵向和切向地引入无机酸水溶液的涡旋流中，将所得硅酸水溶胶的液滴喷射到气体介质中，C.允许 喷雾的水溶胶固化成气态介质中的水凝胶，并且通过洗涤将所得到的基本上球形的水凝胶从盐中释放，而无需预先熟化。 该催化剂产生具有良好加工性能的聚合物。
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公开(公告)号：US4048414A
公开(公告)日：1977-09-13
申请号：US657863
申请日：1976-02-13
CPC分类号： C08F10/00
摘要： A process for the manufacture of olefin polymers by polymerization of monoolefins using a silicic xerogel/chromium trioxide catalyst obtained by (1) synthesizing a particulate silicic xerogel, (2) doping said xerogel with chromium trioxide or a chromium compound capable of converting to chromium trioxide under the conditions of stage (3) and (3) heating the resulting product in a gas stream containing oxygen. The silicic xerogel/chromium trioxide catalyst used is one which has been obtained by (1) synthesizing the silicic xerogel in the first stage by (1.1) starting with a silicic hydrogel having a relatively high solids content, (1.2) extracting water from said hydrogel by means of an alkanol and/or alkanone until the organic liquid absorbs no further water, (1.3) extracting the organic liquid used in stage (1.2) from the resulting dehydrated gel saturated with said organic liquid by means of a hydrocarbon or oxohydrocarbon until said hydrocarbon or oxohydrocarbon absorbs no further organic liquid from stage (1.2), and (1.4) drying the resulting dehydrated gel saturated with hydrocarbon or oxohydrocarbon (xerogel formation), and (2) doping said xerogel in the second stage with the desired amount of chromium from a solution of chromium trioxide in an alkanone or solution of a chromium compound capable of converting to chromium trioxide under the conditions of stage (3) in an alkanol or alkanone with evaporation of the solvent.
摘要翻译： 一种通过使用（1）合成硅氧烷干燥剂获得的硅干燥剂/三氧化铬催化剂聚合单烯烃的方法，（2）用三氧化铬或能够转化成三氧化铬的铬化合物掺杂干燥剂 在阶段（3）和（3）的条件下，将所得产物加热到含氧的气流中。 所使用的硅干凝胶/三氧化铬催化剂是通过（1）通过（1.1）由具有相对高的固体含量的硅水凝胶合成硅酸凝胶得到的，（1.2）从所述水凝胶中提取水 通过烷醇和/或烷酮直到有机液体不再吸收其他水，（1.3）从所得到的用烃或氧代烃饱和的有机液体的脱水凝胶中提取阶段（1.2）中使用的有机液体，直到所述 碳氢化合物或氧代烃不会从阶段（1.2）吸收进一步的有机液体，和（1.4）干燥所得到的用烃或氧代烃饱和的脱水凝胶（干凝胶形成），和（2）在第二阶段用所需量的铬掺杂所述干凝胶 在三烷基铬溶液中，在烷烃或烷烃或碱的阶段（3）的条件下，可以在烷酮或能够转化成三氧化铬的铬化合物的溶液中， 无溶剂蒸发。
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