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公开(公告)号：US4859733A
公开(公告)日：1989-08-22
申请号：US228061
申请日：1988-08-04
摘要： A method is disclosed for the reduction of the extractability of trialkanolamines from polyolefins containing such compounds e.g. as a result of the use of trialkanolamines as catalyst deactivators in processes for the polymerization of olefins. Zinc oxide and/or zeolite molecular sieves are incorporated into the polyolefin, either during the process for the manufacture of the polyolefin or subsequent to such manufacture. Zinc oxide may be used in amount of 0.01-4 parts by weight and zeolite molecular sieves in amounts of 0.05-1 parts by weight, per 100 parts of polyolefin. The resultant compositions may be more acceptable for use in the fabrication of articles intended for the packaging of e.g. foodstuffs.
摘要翻译： 公开了一种降低由含有这种化合物的聚烯烃提取三烷醇胺的方法。 作为在烯烃聚合方法中使用三烷醇胺作为催化剂失活剂的结果。 氧化锌和/或沸石分子筛在聚烯烃的制造过程中或者在制造之后都被引入到聚烯烃中。 氧化锌的用量为0.01-4重量份，沸石分子筛的用量为每100份聚烯烃0.05-1重量份。 所得组合物可以更可接受用于制造用于例如包装的制品。 食品
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2.发明授权Reduction of isomerization in solution process for polymerization of alpha-olefins 失效在α-烯烃聚合反应的溶液中减少异构化
公开(公告)号：US4701504A
公开(公告)日：1987-10-20
申请号：US824354
申请日：1986-01-23
CPC分类号： C08F10/00
摘要： A solution polymerization process for the preparation of high molecular weight polymers of alpha-olefins selected from the group consisting of homopolymers of ethylene and copolymers of ethylene and C.sub.4 -C.sub.12 alpha-olefins is disclosed. The process comprises feeding monomer(s), coordination catalyst and inert hydrocarbon solvent to a reactor, polymerizing the monomers at a temperature of up to 320.degree. C. and a pressure of less than 25 MPa, and deactivating the catalyst in the solution so obtained. The catalyst is deactivated by sequentially admixing therewith a minor amount of a nitrogenous base, especially an aqueous solution of such a base, followed by a solution of a salt of an alkaline earth metal or zinc and an aliphatic monocarboxylic acid dissolved in hydrocarbon solvent. The ratio of water:nitrogenous base should not be greater than 5. The hydrocarbon solvent and other volatile matter are then separated from the resultant solution and a composition comprising said high molecular weight polymer is recovered. The amount of nitrogenous base plus any water is not more than 2.5 moles per mole of halogen plus alkyl radicals in the coordination catalyst.
摘要翻译： 公开了用于制备选自乙烯均聚物和乙烯与C 4 -C 12α-烯烃共聚物的α-烯烃的高分子量聚合物的溶液聚合方法。 该方法包括将单体，配位催化剂和惰性烃溶剂进料到反应器中，在高达320℃的温度和小于25MPa的压力下使单体聚合，并使所得溶液中的催化剂失活 。 通过依次混合少量的含氮碱，特别是这种碱的水溶液，然后将碱土金属或锌的盐和溶解在烃溶剂中的脂族一元羧酸的溶液顺序混合，使催化剂失活。 水：含氮碱的比例不应大于5.然后从所得溶液中分离烃溶剂和其它挥发物，并回收包含所述高分子量聚合物的组合物。 在配位催化剂中，氮碱加上任何水的量不超过2.5摩尔每摩尔卤素加烷基。
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3.发明授权Isopropanolamines as catalyst deactivators in solution process for polymerization of alpha-olefins 失效异丙醇胺作为α-烯烃聚合溶液法中的催化剂失活剂
公开(公告)号：US4803259A
公开(公告)日：1989-02-07
申请号：US41248
申请日：1987-04-22
IPC分类号： C08F2/06 , C08F2/04 , C08F4/60 , C08F4/62 , C08F4/76 , C08F6/02 , C08F6/06 , C08F10/00 , C08F10/02 , C08F6/10
CPC分类号： C08F6/02
摘要： A solution polymerization process for the preparation of high molecular weight polymers of alpha-olefins is disclosed. In the process, the coordination catalyst is deactivated using a solution of at least one trialkanolamine deactivating agent of the formula N(ROH)(R'OH).sub.2 where R is isopropyl and R' is alkyl of 2-4 carbon atoms, especially ethyl or isopropyl. The process is capable of producing polyers of improved color.
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4.发明授权
公开(公告)号：US4430488A
公开(公告)日：1984-02-07
申请号：US443060
申请日：1982-11-19
申请人： Vaclav G. Zboril
发明人： Vaclav G. Zboril
IPC分类号： C08F2/00 , C08F2/04 , C08F2/06 , C08F6/00 , C08F6/02 , C08F6/06 , C08F10/00 , C08F10/02 , C08F2/42
CPC分类号： C08F6/02
摘要： The present invention relates to a solution polymerization process for the preparation of high molecular weight polymers of .alpha.-olefins selected from the group consisting of homopolymers of ethylene and copolymers of ethylene and C.sub.3 -C.sub.12 .alpha.-olefins. The process comprises feeding monomer, coordination catalyst containing vanadium and inert hydrocarbon solvent to a reactor, polymerizing the monomer at a temperature in the range of 105.degree.-320.degree. C. and a pressure of less than 25 MPa and deactivating the catalyst in the solution so obtained by admixing therewith a solution of a salt of an alkaline earth metal or zinc and an aliphatic monocarboxylic acid dissolved in hydrocarbon solvent. The hydrocarbon solvent is then separated from the resultant solution and a composition comprising high molecular weight polymer is recovered. Any catalyst residues remain with the polymer. A particular salt is the salt of a C.sub.8 aliphatic acid, especially calcium 2-ethyl hexanoate.
摘要翻译： 本发明涉及一种用于制备选自乙烯均聚物和乙烯与C 3 -C 12α-烯烃共聚物的α-烯烃的高分子量聚合物的溶液聚合方法。 该方法包括将单体，含有钒和惰性烃溶剂的配位催化剂加入到反应器中，在105℃-320℃的温度和小于25MPa的压力下使单体聚合，并使溶液中的催化剂失活 如此通过将溶解在烃溶剂中的碱土金属或锌的盐和脂族一元羧酸的溶液混合而获得。 然后将烃溶剂与所得溶液分离，并回收包含高分子量聚合物的组合物。 任何催化剂残留在聚合物上。 特定的盐是C8脂族酸的盐，特别是2-乙基己酸钙。
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公开(公告)号：US5589555A
公开(公告)日：1996-12-31
申请号：US499646
申请日：1995-07-07
申请人： Vaclav G. Zboril , Stephen J. Brown
发明人： Vaclav G. Zboril , Stephen J. Brown
IPC分类号： C08F10/00 , C08F10/02 , C08F110/02 , C08F4/654
CPC分类号： C08F10/00 , C08F10/02 , C08F110/02
摘要： A solution process for the preparation of high molecular weight polymers of alpha-olefins selected from the group consisting of homopolymers of ethylene and copolymers of ethylene and C.sub.3 -C.sub.12 higher alpha-olefins is disclosed. Ethylene and/or mixtures of ethylene and C.sub.3 -C.sub.12 higher alpha-olefins are polymerized under non-isothermal conditions in a tubular reactor or in a system of reactors which operate under different conditions, in the presence of a catalytic amount of a titanium-containing coordination catalyst in an inert solvent at a temperature in excess of 105.degree. C. The improvement is characterized in that:(a) the catalyst is activated with a solution of a mixture of aluminum alkyl and alkoxy aluminum alkyl in inert solvent; and(b) the process is controlled by adjusting the ratio of aluminum alkyl to alkoxy aluminum alkyl in the mixture of (a). The aluminum alkyl is of the formula AlR.sub.n X.sub.3-n and the alkoxy aluminum alkyl is of the formula AlR'.sub.m OR".sub.3-m, in which each of R, R' and R" is alkyl or aryl of 1-20 carbon atoms, X is halogen, n is 2-3 and m is 0-3.
摘要翻译： 公开了一种用于制备选自乙烯均聚物和乙烯和C3-C12高级α-烯烃共聚物的α-烯烃的高分子量聚合物的溶液方法。 乙烯和/或乙烯和C 3 -C 12较高级α-烯烃的混合物在非等温条件下在管式反应器或在不同条件下操作的反应器系统中，在催化量的含钛 配位催化剂在惰性溶剂中的温度超过105℃。改进的特征在于：（a）催化剂用烷基铝和烷氧基铝的混合物在惰性溶剂中的混合物的活化; 和（b）通过调节（a）的混合物中烷基铝与烷氧基烷基铝的比例来控制该方法。 烷基铝为式AlRnX3-n，烷氧基烷基为式AlR'mOR'3-m，其中R，R'和R“各自为1-20个碳原子的烷基或芳基 ，X为卤素，n为2-3，m为0-3。
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6.发明授权Reduction of isomerization in solution process for polymerization of alpha-olefins 失效在α-烯烃聚合反应的溶液中减少异构化
公开(公告)号：US4777229A
公开(公告)日：1988-10-11
申请号：US95689
申请日：1987-09-14
IPC分类号： C08F2/06 , C08F2/42 , C08F10/00 , C08F210/16 , C08F10/02
CPC分类号： C08F2/06 , C08F10/00 , C08F210/16
摘要： A solution polymerization process for the preparation of high molecular weight polymers selected from the group consisting of homopolymers of ethylene and copolymers of ethylene and butene-1 is disclosed. The process comprises feeding monomer(s), coordination catalyst and inert hydrocarbon solvent to a reactor, polymerizing the monomers at a temperature of up to 320.degree. C. and a pressure of less than 25 MPa, and deactivating the catalyst in the solution so obtained. The catalyst is deactivated by sequentially admixing therewith a minor amount of dimethyl carbonate followed by a solution of a salt of an alkaline earth metal or zinc and an aliphatic monocarboxylic acid dissolved in hydrocarbon solvent. The hydrocarbon solvent and other volatile matter are then separated from the resultant solution and a composition comprising the high molecular weight polymer is recovered. The amount of dimethyl carbonate is not more than 2.5 moles, per mole of halogen plus alkyl radicals in the coordination catalyst.
摘要翻译： 公开了用于制备选自乙烯均聚物和乙烯和丁烯-1的共聚物的高分子量聚合物的溶液聚合方法。 该方法包括将单体，配位催化剂和惰性烃溶剂进料到反应器中，在高达320℃的温度和小于25MPa的压力下使单体聚合，并使所得溶液中的催化剂失活 。 通过依次与少量的碳酸二甲酯混合，然后将碱土金属或锌的盐和溶解在烃溶剂中的脂肪族单羧酸的溶液依次混合，使催化剂失活。 然后将烃溶剂和其它挥发性物质与所得溶液分离，并回收包含高分子量聚合物的组合物。 在配位催化剂中，每摩尔卤素加上烷基，碳酸二甲酯的量不超过2.5摩尔。
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公开(公告)号：US4769428A
公开(公告)日：1988-09-06
申请号：US919807
申请日：1986-10-16
申请人： Vaclav G. Zboril , Rolf Mulhaupt
发明人： Vaclav G. Zboril , Rolf Mulhaupt
摘要： A solution process, and a catalyst therefor, for the preparation of high molecular weight polymers of alph-olefins viz. homopolymers of ethylene and copolymers of ethylene and C.sub.3 -C.sub.12 alpha-olefins, is disclosed. The process is operated under solution polymerization conditions at 105.degree.-320.degree.. The catalyst is obtained from titanium tetrahalides, vanadium oxytrihalides and organoaluminum compounds, in which an admixture of catalyst components is heat-treated at 150.degree.-320.degree. C., and activated with an aluminoxane. The catalyst has good activity and the polymer obtained has improved color.
摘要翻译： 用于制备α-烯烃的高分子量聚合物的溶液方法及其催化剂， 公开了乙烯的均聚物和乙烯和C 3 -C 12α-烯烃的共聚物。 该方法在105°-320°的溶液聚合条件下进行。 催化剂由四卤化钛，三氧化三钒和有机铝化合物得到，其中催化剂组分的混合物在150-320℃下热处理，并用铝氧烷活化。 催化剂具有良好的活性，所得聚合物的颜色改善。
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公开(公告)号：US5342499A
公开(公告)日：1994-08-30
申请号：US53623
申请日：1993-03-25
申请人： Vaclav G. Zboril
发明人： Vaclav G. Zboril
IPC分类号： G01N27/416 , G01N27/26
CPC分类号： G01N27/4166
摘要： A method and apparatus for the monitoring and control of concentration of an ion in a solution at an elevated temperature of at least 100.degree. C. are disclosed. The method comprises the steps of contacting a first electrode with a flowing first solution containing said ion at the elevated temperature, and contacting a second electrode with a second flowing solution containing said ion at the elevated temperature. The rate of flow of the second solution is substantially lower than the rate of flow of the first solution. The first and second solutions are then contacted or admixed. The electrodes must be capable of detecting the ion at the elevated temperature and have the same response characteristics to changes in concentration of the ion at the elevated temperature. The concentration of the ion in the second solution is measured at a temperature lower than the elevated temperature under conditions permitting accurate measurement of the concentration of the ion, and the concentration of the ion in the first solution is monitored and controlled by adjusting the concentration of the ion in at least one of the first and second solutions. The method is particularly adapted for the monitoring and control of salt solutions used in the manufacture of polyamides, using palladium hydride electrodes.
摘要翻译： 公开了一种在至少100℃的升高的温度下监测和控制溶液中的离子浓度的方法和装置。 该方法包括以下步骤：在升高的温度下使第一电极与含有所述离子的流动的第一溶液接触，并且在升高的温度下将第二电极与含有所述离子的第二流动溶液接触。 第二溶液的流速基本上低于第一溶液的流速。 然后将第一和第二溶液接触或混合。 电极必须能够在升高的温度下检测离子，并且具有与高温下离子浓度变化相同的响应特性。 在允许精确测量离子浓度的条件下，在低于升高温度的温度下测量第二溶液中的离子浓度，并且通过调节第一溶液的浓度来监测和控制第一溶液中的离子浓度 在第一和第二溶液中的至少一个中的离子。 该方法特别适用于使用钯氢化物电极监测和控制用于制造聚酰胺的盐溶液。
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公开(公告)号：US5492876A
公开(公告)日：1996-02-20
申请号：US190750
申请日：1994-02-01
CPC分类号： C08F10/00
摘要： A solution process, and a catalyst therefor, for the preparation of high molecular weight polymers of alpha-olefins viz. homopolymers of ethylene and copolymers of ethylene and C.sub.3 -C.sub.12 alpha-olefins, is disclosed. The process is operated under solution polymerization conditions at 105.degree.-320.degree. C. The catalyst is obtained from titanium tetrahalides, vanadium oxytrihalides and organoaluminum compounds, in which an admixture of catalyst components is heat-treated at 180.degree.-250.degree. C. and subsequently cooled to a temperature of less than 150.degree. C. Additional vanadium oxytrihalide is then added. The resultant catalyst solution is activated with an aluminum compound. The catalyst has good activity, showing superior activity to catalysts in which additional vanadium oxytrihalide is not added or added at temperatures above 150.degree. C.
摘要翻译： 用于制备α-烯烃的高分子量聚合物的溶液方法及其催化剂， 公开了乙烯的均聚物和乙烯和C 3 -C 12α-烯烃的共聚物。 该方法在105℃-320℃的溶液聚合条件下进行。催化剂由四卤化钛，三氧化三钒和有机铝化合物得到，其中催化剂组分的混合物在180-250℃下热处理， 随后冷却至小于150℃的温度。然后加入另外的三氧化二铁。 所得催化剂溶液用铝化合物活化。 该催化剂具有良好的活性，对催化剂具有优异的活性，其中在高于150℃的温度下不加入或加入额外的三氧化二钒
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公开(公告)号：US5213668A
公开(公告)日：1993-05-25
申请号：US829845
申请日：1992-01-31
申请人： Vaclav G. Zboril
发明人： Vaclav G. Zboril
IPC分类号： G01N27/416
CPC分类号： G01N27/4166
摘要： A method and apparatus for the monitoring and control of concentration of an ion in a solution at an elevated temperature of at least 100.degree. C. are disclosed. The method comprises the steps of contacting a first electrode with a flowing first solution containing said ion at the elevated temperature, and contacting a second electrode with a second flowing solution containing said ion at the elevated temperature. The rate of flow of the second solution is substantially lower than the rate of flow of the first solution. The first and second solutions are then contacted or admixed. The electrodes must be capable of detecting the ion at the elevated temperature and have the same response characteristics to changes in concentration of the ion at the elevated temperature. The concentration of the ion in the second solution is measured at a temperature lower than the elevated temperature under conditions permitting accurate measurement of the concentration of the ion, and the concentration of the ion in the first solution is monitored and controlled by adjusting the concentration of the ion in at least one of the first and second solutions. The method is particularly adapted for the monitoring and control of salt solutions used in the manufacture of polyamides, using palladium hydride electrodes.
摘要翻译： 公开了一种在至少100℃的升高的温度下监测和控制溶液中的离子浓度的方法和装置。 该方法包括以下步骤：在升高的温度下使第一电极与含有所述离子的流动的第一溶液接触，并且在升高的温度下使第二电极与含有所述离子的第二流动溶液接触。 第二溶液的流速基本上低于第一溶液的流速。 然后将第一和第二溶液接触或混合。 电极必须能够在升高的温度下检测离子，并且具有与高温下离子浓度变化相同的响应特性。 在允许精确测量离子浓度的条件下，在低于升高温度的温度下测量第二溶液中的离子浓度，并且通过调节第一溶液的浓度来监测和控制第一溶液中的离子浓度 在第一和第二溶液中的至少一个中的离子。 该方法特别适用于使用钯氢化物电极监测和控制用于制造聚酰胺的盐溶液。
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