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1.发明授权Phillips catalyst and its use for preparing ethylene homopolymers and copolymers 失效菲利普斯催化剂及其用于制备乙烯均聚物和共聚物的用途
公开(公告)号：US5324697A
公开(公告)日：1994-06-28
申请号：US904924
申请日：1992-06-26
申请人： Hans-Joachim Mueller , Rainer Konrad , Guenther Schweier , Siegfried Weber , Roland Saive , Peter Koelle
发明人： Hans-Joachim Mueller , Rainer Konrad , Guenther Schweier , Siegfried Weber , Roland Saive , Peter Koelle
CPC分类号： C08F10/02
摘要： A novel Phillips catalyst for the homopolymerization of ethylene and the copolymerization of ethylene with .alpha.-olefins contains as catalytically active components a specific chromium catalyst on an aluminum phosphate support and cocatalysts of the formula I to IV, ##STR1## where M is lithium, sodium and potassium,M.sup.1 is magnesium and zinc,M.sup.2 is boron and aluminum,R is C.sub.1 -C.sub.10 -alkyl and C.sub.6 -C.sub.20 -aryl,R.sup.1 is R and C.sub.1 -C.sub.10 -alkoxy and C.sub.6 -C.sub.20 -aryloxy,X is chlorine, bromine and iodine,n is 0, 1 and 2The chromium catalyst on an aluminum phosphate support can be obtained by applying chromium compounds to a finely divided aluminum phosphate with a P:A1 molar ratio near to or equal to 1 and a pore volume of >1 cm.sup.3 /g and activating the resulting intermediate at elevated temperatures in an oxidizing atmosphere. The novel Phillips catalyst has an exceptionally long duration of activity and its productivity can be increased further by adding hydrogen.
摘要翻译： 用于乙烯均聚和乙烯与α-烯烃共聚的新型菲利普斯催化剂在磷酸铝载体上含有特定的铬催化剂和式I至IV的助催化剂，MR（I）M1R2（II）M2R3的催化活性组分 -n1Xn（III）MM2RR31（IV）其中M是锂，钠和钾，M1是镁和锌，M2是硼和铝，R是C1-C10-烷基和C6-C20-芳基，R1是R和C1- C10烷氧基和C6-C20芳氧基，X是氯，溴和碘，n是0,1和2。磷酸铝载体上的铬催化剂可以通过将铬化合物施加到具有P： A1摩尔比接近或等于1，孔体积> 1cm 3 / g，并在氧化气氛中在高温下活化所得中间体。 新型菲利普斯催化剂具有非常长的活性持续时间，并且通过加入氢可以进一步提高其生产率。
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公开(公告)号：US5321189A
公开(公告)日：1994-06-14
申请号：US22343
申请日：1993-02-25
申请人： Hans-Joachim Mueller , Bernd L. Marczinke , Juergen Kerth , Rainer Konrad , Guenther Schweier , Max Strohmeyer , Bernhard Rieger
发明人： Hans-Joachim Mueller , Bernd L. Marczinke , Juergen Kerth , Rainer Konrad , Guenther Schweier , Max Strohmeyer , Bernhard Rieger
IPC分类号： B01J31/14 , B01J31/22 , C07B61/00 , C07C2/34 , C07C11/02 , C07C11/107 , C08F4/60 , C08F4/642 , C08F4/659 , C08F4/6592 , C08F10/00 , C08F10/06 , C07C2/24
CPC分类号： C07C2/34 , C07C2531/14 , C07C2531/22 , Y02P20/52 , Y10S526/943
摘要： A process for propene oligomerization catalyzed by transition metal complexes in liquid phase to give propene oligomers with a high content of terminal double bonds, comprises oligomerizing propene in the presence of a catalyst of the formula ICp.sub.2 MX.sub.2 Iwhere Cp is an unsubstituted cyclopentadienyl unit and/or a mono-C.sub.1 -C.sub.4 -alkylcyclopentadienyl unit, M is zirconium or hafnium and the ligands X are each hydride and/or halide and/or methyl, and in the presence of an aluminoxane cocatalyst, and where the ratio of the amounts of the catalyst I and the aluminoxane cocatalyst is such that the M/Al atomic ratio is from 1:250 to 1:1000, employing a temperature of from 50.degree. to 110.degree. C. and a pressure of from 30 to 100 bar.
摘要翻译： 在液相中由过渡金属络合物催化丙烯低聚的方法得到具有高含量末端双键的丙烯低聚物的方法包括在式I Cp2MX2I催化剂存在下使丙烯低聚，其中Cp是未取代的环戊二烯基单元和/ 或单C 1 -C 4烷基环戊二烯基单元，M是锆或铪，并且配体X各自为氢化物和/或卤化物和/或甲基，并且在铝氧烷助催化剂的存在下，并且其中 催化剂I和铝氧烷助催化剂使得M / Al原子比为1:250至1:1000，使用温度为50至110℃，压力为30至100巴。
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公开(公告)号：US06197901B1
公开(公告)日：2001-03-06
申请号：US08935664
申请日：1997-09-23
IPC分类号： C08F408
CPC分类号： C08F10/00 , C08F4/63912 , C08F4/63916 , Y10S526/943 , C08F4/63925
摘要： Polyalk-1-enes are prepared by polymerization of alk-1-enes with the aid of the compound bis(cyclopentadienyl)-chromium(II) in which the cyclopentadienyl rings may carry inert organic radicals, said compound being adsorbed on an inorganic oxide carrier, by a process in which the polymerization is carried out in the presence of an organometallic compound of a metal of main groups I to III or of a metal hydride, in particular of n-butyl-lithium.
摘要翻译： 聚炔-1-烯通过在其中环戊二烯基环可以携带惰性有机基团的化合物双（环戊二烯基） - 铬（II）的聚合反应制备烷-1-烯，所述化合物被吸附在无机氧化物载体上 通过在主要I〜III族金属或金属氢化物，特别是正丁基锂的金属的有机金属化合物的存在下进行聚合的方法。
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4.发明授权
公开(公告)号：US4727124A
公开(公告)日：1988-02-23
申请号：US047116
申请日：1987-05-08
IPC分类号： C08F2/06 , C08F4/02 , C08F4/22 , C08F4/24 , C08F4/62 , C08F4/64 , C08F10/00 , C08F10/02 , C08F2/24
CPC分类号： C08F10/00 , C08F2410/01
摘要： Ethane polymers are prepared by Phillips catalysis using (1) a supported catalyst which is laden with chromium, phosphorus and titanium and (2) a cocatalyst, (1) being obtained by a procedure in which (1.1) a catalyst intermediate laden with chromium, phosphorus and titanium is prepared from a silicate carrier, a selected chromium compound, a selected phosphorus compound and a selected titanium compound, and (1.2) the catalyst intermediate is then heated in an oxygen-containing gas stream. In the process, the supported catalyst (1) used is one which is obtained (using specific methods and substances in each case) by a procedure in which (1.1) in a first stage (1.1.1), a suspension is first prepared from (1.1.1.1) a finely divided silicate carrier and (1.1.1.2) an inert organic solvent, (1.1.2) a suspension is then prepared from (1.1.2.1) a finely divided chromium trioxide and (1.1.2.2) an inert organic solvent, (1.1.3) thereafter (1.1.3.1) the suspension resulting from (1.1.2) is combined with (1.1.3.2) a phosphate or phosphite, (1.1.4) then (1.1.4.1) the suspension obtained from (1.1.1) is combined with (1.1.4.2) the reaction product obtained in (1.1.3), (1.1.5) thereafter (1.1.5.1) the suspension formed in (1.1.4) is combined with (1.1.5.2) a titanate, (1.1.6) finally the suspension obtained in (1.1.5) is evaporated to dryness and then (1.2) in a second stage, (1.2.1) the intermediate obtained in (1.1) is first treated with a nitrogen stream, (1.2.2) an intermediate obtained in (1.2.1) is then heated in an oxygen-containing gas stream and finally (1.2.3) the intermediate obtained in (1.2.2) is treated with a nitrogen stream, and a lithiumalkyl is used as (2).
摘要翻译： 通过使用（1）载有铬，磷和钛的载体催化剂和（2）助催化剂的菲尼普斯催化剂制备乙烷聚合物，（1）通过以下程序获得，其中（1.1）载有铬的催化剂中间体， 磷和钛由硅酸盐载体，选择的铬化合物，选择的磷化合物和选择的钛化合物制备，然后在含氧气流中加热催化剂中间体。 在该方法中，使用的负载催化剂（1）是通过第一阶段（1.1.1）中的（1.1）的步骤获得的（使用具体方法和每种情况下的物质），悬浮液首先由 （1.1.1.1）细碎的硅酸盐载体和（1.1.1.2）惰性有机溶剂，（1.1.2）悬浮液然后由（1.1.2.1）细碎的三氧化铬和（1.1.2.2）惰性的 有机溶剂（1.1.3）（1.1.3.1）将得自（1.1.2）的悬浮液与（1.1.3.2）磷酸酯或亚磷酸酯（1.1.4）然后（1.1.4.1）合并得到的悬浮液 （1.1.1）与（1.1.4）中得到的反应产物（1.1.3），（1.1.5）（1.1.5.1）中合并（1.1.4），将（1.1.4）中形成的悬浮液与（1.1 0.5.2）钛酸盐（1.1.6）最后，将（1.1.5）中得到的悬浮液在第二阶段蒸发至干，然后（1.2）（1.2.1），首先处理（1.1）中获得的中间体 用氮气流（1.2.2）中间体 然后在含氧气流中加热（1.2.1），最后（1.2.3）用氮气流处理（1.2.2）中得到的中间体，使用烷基锂作为（2）。
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5.发明授权
公开(公告)号：US4728703A
公开(公告)日：1988-03-01
申请号：US28651
申请日：1987-03-20
CPC分类号： C08F10/02 , C08F2410/01
摘要： Ethene polymers are prepared by Phillips catalysis using (1) a supported catalyst which is loaded with chromium and titanium and (2) a co-catalyst, (1) having been obtained by preparing (1.1) a chromium- and titanium-loaded catalyst intermediate from (1.1.a) a silicate carrier material, (1.1.b) a selected chromium compound and (1.1.c) a selected titanium compound and then (1.2) heating said catalyst intermediate in an oxygen-containing gas stream, the (1) used having been obtained by, in general terms, (1.1) preparing in the first stage (1.1.1) a suspension from (1.1.1.1) a finely divided silicate carrier material and (1.1.1.2) a liquid alkane, (1.1.2) then (1.1.2.1) combining the suspension resulting from (1.1.1.) with (1.1.2.2.) a finely divided chromium trioxide, (1.1.3) thereupon (1.1.3.1) combining the suspension obtained from (1.1.2) with (1.1.3.2) an alkanol, (1.1.4) thereafter (1.1.4.1) combining the suspension formed in (1.1.3) with (1.1.4.2) a titanium compound of the formula Ti(OR).sub.4, where R is alkyl, aryl or cycloalkyl, and (1.1.5) finally evaporating the suspension obtained in (1.1.4) to dryness, and then (1.2) in the second stage first (1.2.1) treating the catalyst intermediate obtained in the first state (1.1) with a nitrogen stream, thereupon (1.2.2) heating the intermediate obtained in (1.2.1) in an oxygen-containing gas stream, and finally (1.2.3) treating the intermediate obtained in (1.2.2) with a nitrogen stream; and as (2) with an alkyllithium.
摘要翻译： 通过菲利普斯催化法，使用（1）载有铬和钛的载体催化剂和（2）助催化剂制备乙烯聚合物，（1）通过制备（1.1）载有铬和钛的催化剂中间体 从（1.1.a）硅酸盐载体材料，（1.1b）选择的铬化合物和（1.1.c）所选择的钛化合物，然后（1.2）在含氧气流中加热所述催化剂中间体，（1 ）（1.1）在第一阶段（1.1.1）中制备了（1.1.1.1）细分硅酸盐载体材料和（1.1.1.2）液体烷烃（1.1 （1.1.2.1）将由（1.1.1。）得到的悬浮液与（1.1.2.2。）细碎的三氧化铬（1.1.3）（1.1.3.1）组合，得到的悬浮液 1.1.2）与（1.1.3.2）链烷醇（1.1.4）（1.1.4.1）将（1.1.3）中形成的悬浮液与（1.1.4.2）结合形成式 Ti（OR）4，其中R是烷基，芳基或环烷基，和（1.1.5）最终将（1.1.4）中得到的悬浮液蒸发至干，然后在第二阶段（1.2.1）中蒸发（1.2） 用氮气流处理在第一状态（1.1）中获得的催化剂中间体，随后（1.2.2）在含氧气流中加热（1.2.1）中获得的中间体，最后（1.2.3）处理 （1.2.2）中获得的中间体与氮气流; 和（2）与烷基锂反应。
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6.发明授权
公开(公告)号：US4814308A
公开(公告)日：1989-03-21
申请号：US110872
申请日：1987-10-21
申请人： Rainer Konrad , Guido Funk , Juergen Schmidt-Thuemmes , Rudolf Mueller-Mall , Guenther Schweier
发明人： Rainer Konrad , Guido Funk , Juergen Schmidt-Thuemmes , Rudolf Mueller-Mall , Guenther Schweier
CPC分类号： C08F10/02
摘要： Ethene polymerization by Phillips catalysis is carried out using (1) a supported catalyst, which is laden with chromium, phosphorus and aluminum, and (2) a cocatalyst, (1) being obtained by a method in which (1.1) a catalyst intermediate laden with chromium, phosphorus and aluminum is prepared from a silicate carrier, a selected chromium compound, a selected phosphorus compound and a selected aluminum compound, and then (1.2) the catalyst intermediate is heated in an oxygen-containing gas stream. In this process, the component (1) used is one which is obtained by a method in which, in each case in a specific manner, (1.1) in a first stage, (1.1.1) first a suspension is prepared from (1.1.1.1) a finely divided silicate carrier and (1.1.1.2) an inert organic solvent, (1.1.2) then, (1.1.2.1) in an inert organic solvent, (1.1.2.2) an organic chromium compound is combined with (1.1.2.3) an aluminum trialkyl, (1.1.3) then (1.1.3.1) the suspension resulting from (1.1.1) is combined with (1.1.3.2) a phosphoric acid or phosphite and (1.1.3.3) the product obtained from (1.1.2), (1.1.4) finally, the suspension obtained in (1.1.3) is evaporated to dryness, and then (1.2) in a second stage, first (1.2.1) the intermediate obtained from (1.1) is treated with a stream of nitrogen, then (1.2.2) the intermediate obtained from (1.2.1) is heated in an oxygen-containing gas stream, and finally (1.2.3) the intermediate obtained from (1.2.2) is treated with a stream of nitrogen, and both a lithiumalkyl and a boronalkyl are used as (2).
摘要翻译： 通过菲利普斯催化进行的乙烯聚合使用（1）负载催化剂，其载有铬，磷和铝，和（2）助催化剂，（1）通过以下方法获得：（1）将载体催化剂中间体 由硅酸盐载体，选择的铬化合物，选择的磷化合物和选择的铝化合物制备铬，磷和铝，然后（1.2）在含氧气流中加热催化剂中间体。 在该方法中，所使用的组分（1）是通过在每种情况下以具体方式（1.1）在第一阶段（1.1.1）中首先从（1.1）制备悬浮液的方法获得的组分 .1.1）精细分散的硅酸盐载体和（1.1.1.2）惰性有机溶剂（1.1.2）然后，（1.1.2.1）在惰性有机溶剂（1.1.2.2）中将有机铬化合物与（ 1.1.2.3）三烷基铝（1.1.3）然后（1.1.3.1）将由（1.1.1）得到的悬浮液与（1.1.3.2）磷酸或亚磷酸酯和（1.1.3.3）得到的产物 从（1.1.2），（1.1.4）最终得到的（1.1.3）中得到的悬浮液蒸发至干，然后在第二阶段（1.2）中，首先（1.2.1）从（1.1 ）用氮气流处理，然后（1.2.2）从（1.2.1）获得的中间体在含氧气流中加热，最后（1.2.3）从（1.2.2）得到的中间体 用氮气流和二氧化钛处理 和硼烷基用作（2）。
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7.发明授权Preparation of homopolymers and copolymers of ethene using a chromium trioxide catalyst 失效使用三氧化铬催化剂制备乙烯的均聚物和共聚物
公开(公告)号：US4845176A
公开(公告)日：1989-07-04
申请号：US105542
申请日：1987-10-08
CPC分类号： C08F10/02 , Y10S526/908 , Y10S526/909
摘要： Ethene homopolymers and ethene copolymers with minor amounts of higher .alpha.-monoolefins are prepared by polymerization of the monomer or monomers using a chromium trioxide catalyst which is obtained by a method in which (1) a finely divided, porous, silicate carrier is laden with (2) chromium trioxide or a chromium compound which is converted to chromium trioxide under the conditions of stage (3), and then (3) the intermediate resulting from stage (2) is heated in an oxygen-containing gas stream. In this process, a cocatalyst which consists of a lithiumalkyl used in addition to the chromium trioxide catalyst.
摘要翻译： 通过使用三氧化铬催化剂聚合单体或单体来制备具有少量较高级α-单烯烃的乙烯均聚物和乙烯共聚物，该三氧化铬催化剂通过以下方法获得，其中（1）细分多孔硅酸盐载体载有（ 2）三氧化铬或在阶段（3）的条件下转化为三氧化铬的铬化合物，然后（3）将由步骤（2）得到的中间体在含氧气体流中加热。 在该方法中，除了三氧化铬催化剂之外，还使用由使用的烷基锂组成的助催化剂。
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公开(公告)号：US4385162A
公开(公告)日：1983-05-24
申请号：US256129
申请日：1981-04-21
CPC分类号： C08F10/00 , Y10S526/906
摘要： A process for the preparation of homopolymers and copolymers of .alpha.-monoolefins by means of a Ziegler-Natta catalyst system comprising (1) a titanium-III component, which is prepared by subjecting (1.1) a titanium trichloride/aluminum trichloride compound (a) and (1.2) an ester (b) to a certain type of milling treatment in which (A) a vibratory ball mill providing a relatively high milling acceleration is used, (B) the mill is first charged with the titanium-containing compound (a) and, if appropriate, is run for a certain period, thereafter (C) the ester (b) is added at a certain rate while milling the charge, thereupon (D) the charge is kept at +15.degree. C. or above for a certain period, while continuing the milling, hereupon (E), if appropriate, the product obtained from (D) is milled further for a certain period at +5.degree. C. or below, then (F), if appropriate, but advantageously so, the product obtained from (D) or (E) is kept at +20.degree. C. or above for a certain period, without milling, and thereafter (G), if appropriate, the product obtained from (F) is milled further for a certain period at +5.degree. C. or below, (2) an aluminum-alkyl component containing a chlorine bonded to the aluminum, and (3), if appropriate, a phenolic compound of a certain category, in which process a titanium-III component (1) is employed, in the preparation of which additionally .sup.- (H) a suspension is prepared from (H.sub.1) the product obtained according to (D), (E), (F) or (G), (H.sub.2) a liquid hydrocarbon (c) and (H.sub.3) an oxygen-containing compound (d), consisting of (d.sub.1) an ether of a certain category and/or (d.sub.2) an ester of a certain category, thereafter (I) the suspension obtained according to (H) is kept at an elevated temperature for a certain period, with vigorous agitation, and is then cooled, hereupon (J), if appropriate, the solid is isolated from the suspension obtained according to (I), and, if desired, is washed with a liquid hydrocarbon and dried, the novel titanium-III component (1) being the solid, in suspended form, obtained according to (I) or the solid, in isolated form, obtained according to (J). Using this Ziegler-Natta catalyst system, polymers with relatively high stereo-regularity and advantageous morphological properties can be obtained in relatively high yield.
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9.发明授权Catalyst for the polymerization of ethylene, its preparation and the use of the resulting ethylene polymers for the production of films exhibiting little blocking 失效用于乙烯聚合的催化剂，其制备和使用所得的乙烯聚合物用于生产几乎没有阻塞的膜
公开(公告)号：US4970184A
公开(公告)日：1990-11-13
申请号：US346899
申请日：1989-05-03
IPC分类号： C08F4/658 , C08F2/34 , C08F4/58 , C08F4/60 , C08F4/64 , C08F4/649 , C08F10/00 , C08F10/02 , C08F210/02
CPC分类号： C08F210/02
摘要： A catalyst for the copolymerization of ethylene by the gas-phase fluidized-bed method is prepared by a process in which a titanium-containing and magnesium-containing active component, reacted with an alcohol as a complexing agent, is applied to a finely divided silica from homogeneous solution, in the presence of a polysiloxane, by evaporating the solvent, and the resulting homogeneous catalyst intermediate is then preactivated by treatment with the alkylaluminum compound and the Lewis base in an inert hydrocarbon solution, and the copolymers prepared using the above catalyst are employed for the production of films exhibiting little blocking.
摘要翻译： 通过气相流化床法共聚乙烯的催化剂通过以下方法制备：使含钛和镁的活性组分与醇作为络合剂反应的方法被加到细分二氧化硅 从均匀溶液中，在聚硅氧烷的存在下，通过蒸发溶剂，然后通过用惰性烃溶液中的烷基铝化合物和路易斯碱处理预先活化所得均匀的催化剂中间体，并且使用上述催化剂制备的共聚物是 用于生产几乎没有阻塞的薄膜。
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公开(公告)号：US4900798A
公开(公告)日：1990-02-13
申请号：US97068
申请日：1987-09-16
CPC分类号： C08F10/02 , Y10S526/901 , Y10S526/903 , Y10S526/904
摘要： Finely divided ethane polymers are prepared using a Ziegler catalyst system consisting of (1) a titanium-containing catalyst component which has been obtained by (1.1) precipitation in an organic liquid comprising (1.1.1) a solution of titanium tetrachloride in a hydrocarbon, (1.1.2) a solution of a certain organoaluminum compound in a hydrocarbon and (1.1.3) an alpha-monoalkene, and (2) an aluminum-containing catalyst component. In this process, the component (1) used is a component where (1.1) precipitation has been carried out at relatively low temperatures in an organic liquid which has a relatively high viscosity at the precipitation temperature and conists of (1) a liquid hydrocarbon an (b) small amounts of a polymer of an alpha-monoalkene dissolved therein, with the provisos that (i) specific amounts of the organic liquid, of the organoaluminum compound and of the alpha-monoalkene are used per g mol of the titanium tetrachloride used in total, and (ii) per molar unit of the titanium tetrachloride used in total, specific amounts per minute are precipitated and specific amounts per minute of the alpha-monoalkene are introduced, and (1.2) the substance precipitated according to (1.1) has been reacted with a lithiumalkyl.
摘要翻译： 使用齐格勒催化剂体系制备精细分散的乙烷聚合物，该齐格勒催化剂体系由（1）通过（1.1）在有机液体中沉淀得到的含钛催化剂组分，所述有机液体包含（1.1.1）四氢化钛在烃中的溶液， （1.1.2）某些有机铝化合物在烃中的溶液和（1.1.3）α-单链烯烃，和（2）含铝催化剂组分。 在该方法中，使用的组分（1）是在相对低的温度下在沉淀温度下具有较高粘度的有机液体中进行沉淀的组分，（1）液体烃 （b）少量其中溶解有α-单链烯烃的聚合物，条件是（i）有机铝化合物和α-单链烯烃的特定量的有机铝化合物与每摩尔所用的四氯化钛相比使用 和（ii）每摩尔单位使用的四氯化钛，每分钟的特定量被沉淀，并且每分钟的特定量的α-单链烯烃被引入，（1.2）根据（1.1）沉淀的物质具有 与烷基锂反应。
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