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    Method of selecting operation of a fluid-bed reactor and apparatus for doing so
    1.
    发明授权
    Method of selecting operation of a fluid-bed reactor and apparatus for doing so 失效
    选择流化床反应器的操作方法和这样做的装置

    公开(公告)号：US4226798A

    公开(公告)日：1980-10-07

    申请号：US949170

    申请日：1978-10-06

    申请人： Joseph A. Cowfer ,  Dane E. Jablonski ,  Ronald M. Kovach ,  Angelo J. Magistro

    发明人： Joseph A. Cowfer ,  Dane E. Jablonski ,  Ronald M. Kovach ,  Angelo J. Magistro

    IPC分类号： C07C19/045 ,  B01J8/18 ,  B01J8/24 ,  C07C17/00 ,  C07C17/02 ,  C07C17/156 ,  C07C67/00 ,  G01N11/16 ,  C07C120/14 ,  C07C17/15 ,  C07C45/04 ,  G05D24/00

    CPC分类号： B01J8/1809 ,  C07C17/156 ,  G01N11/162 ,  B01J2208/00575 ,  Y10S423/16 ,  Y10T137/0335 ,  Y10T137/2506 ,  Y10T436/12

    摘要： A method is disclosed for using a pendulum viscometer having damped torsional oscillations, in a laboratory catalytic fluid-bed reactor, to monitor a propensity to stick which is exhibited by certain supported catalysts. A fluid-bed of such catalysts has been found to become suddenly more sticky just before a point at which a change in pressure drop across the fluid-bed can be measured due to a process "upset". At this point ("the inversion point"), the upset is usually irremediable. The method includes correlating data on catalyst stickiness from a laboratory reactor operating at atmospheric pressure, with an expected level of catalyst stickiness in a commercial reactor operating at elevated pressure.A pendulum viscometer and related auxiliary apparatus is disclosed for magnetically and electrically measuring and recording the rate at which the pendulum's torsional oscillations are damped. Frequent measurements are made during normal operation of the fluid-bed to determine its stickiness (as evidenced by the rate at which the pendulum's torsional oscillations are damped) relative to the stickiness at the inversion point. Operation of the fluid-bed under conditions for which measured rates of damping are predeterminedly lower than the rate near the inversion point, assures operation of the fluid-bed reactor at maximum efficiency.

    摘要翻译： 公开了一种在实验室催化流化床反应器中使用具有阻尼扭转振荡的摆式粘度计来监测某些负载型催化剂显示出的粘附倾向的方法。 已经发现，这种催化剂的流化床在刚好在过程“不舒服”之前可以测量流化床上的压降变化的点之前突然变得更粘。 在这一点上（“反转点”），烦恼通常是不可接受的。 该方法包括将来自在大气压下操作的实验室反应器的催化剂粘性的数据与在高压下操作的商业反应器中的催化剂粘性的预期水平相关联。 公开了一种摆式粘度计和相关的辅助设备，用于磁和电测量和记录摆动扭转振荡被阻尼的速率。 在流体床的正常运行期间进行频繁的测量，以确定其相对于反转点处的粘性的粘性（摆锤的扭转振荡被阻尼的速率证明）。 在测量的阻尼比预定低于反转点附近的速率的条件下，流化床的操作确保了流化床反应器的最大效率。

    Copper-catalyzed fluid-bed ethylene oxhydrochlorination process
    2.
    发明授权
    Copper-catalyzed fluid-bed ethylene oxhydrochlorination process 失效
    铜催化流化床乙烯氯化氢过程

    公开(公告)号：US4339620A

    公开(公告)日：1982-07-13

    申请号：US239806

    申请日：1981-03-02

    申请人： Joseph A. Cowfer ,  Jamal S. Eden ,  Angelo J. Magistro

    发明人： Joseph A. Cowfer ,  Jamal S. Eden ,  Angelo J. Magistro

    IPC分类号： B01J23/72 ,  C07C17/156 ,  C07C17/15

    CPC分类号： B01J23/72 ,  C07C17/156

    摘要： There is disclosed a method and composition for improving the fluidization characteristics and alleviating or inhibiting stickiness in a supported cupric chloride catalyst used as fluid bed catalyst in oxyhydrochlorinations reactions. The method involves the in situ preparation of the supported cupric chloride catalyst by addition of bare support on which no cupric chloride is deposited to the supported cupric chloride catalyst in the fluidized bed, or the use in the bed as the initial charge or as addition to the bed as makeup, of a composition which is a mixture of supported cupric chloride catalyst and bare support. In either event, as the oxyhydrochlorination proceeds, a portion of the cupric chloride on the supported catalyst becomes released therefrom and deposited in situ on the bare support, and stickiness of the cupric chloride containing catalyst particles to one another in the fluid bed is alleviated or inhibited.

    摘要翻译： 公开了一种改善流化特性并减轻或抑制用于羟基氢氯化反应中作为流化床催化剂的负载型氯化铜催化剂中的粘性的方法和组合物。 该方法包括通过添加裸式载体来原位制备负载的氯化铜催化剂，其上没有将氯化铜沉积在流化床中的负载的氯化铜催化剂上，或者在床中用作初始电荷或作为添加 作为化妆品的床，作为负载的氯化铜催化剂和裸支撑物的混合物的组合物。 在任一情况下，随着氧化氢氯化的进行，载体催化剂上的一部分氯化铜被释放出来，并在裸露的载体上原位沉积，并且在流化床中彼此含有氯化铜的催化剂颗粒的粘性得到缓解或 抑制。

    Process for finishing vinyl chloride monomer
    3.
    发明授权
    Process for finishing vinyl chloride monomer 失效
    完成氯乙烯单体的方法

    公开(公告)号：US4642400A

    公开(公告)日：1987-02-10

    申请号：US779337

    申请日：1985-09-23

    申请人： Joseph A. Cowfer ,  James E. Best

    发明人： Joseph A. Cowfer ,  James E. Best

    IPC分类号： C07C17/38

    CPC分类号： C07C17/38

    摘要： This process stems from the discovery that the solubility of water in vinyl chloride monomer ("VCM") is so low in a cold aqueous caustic solution at a temperature below 0.degree. C., that the aqueous solution will remove water dissolved in the monomer, and at the same time, will neutralize the HCl associated with the monomer and prevent the formation of acetylene. This discovery makes it possible to dry and neutralize a HCl and water-containing vinyl chloride ("VCl") stream, by intimately contacting the stream with a cold aqueous 2 to 30 wt % caustic soda solution at a temperature below 25.degree. F. and above the freezing point of the caustic solution. In a commercial VCM producing facility, VCl can be "finished" in a "stand-alone" processing facility with greater economy than in a conventional VCM plant, yet avoid the hazards of operating a conventional VCl stripping column and scrubbers packed with solid caustic pellets. The process allows simultaneously drying and neutralizing a VCl stream containing from about 1 part per million (ppm) to about 500 ppm HCl, and from about 10 ppm to about 300 ppm of water by contacting it with a 10% to 25% aqueous cold caustic solution, and separating dry and neutralized VCM monomer containing no more than 100 ppm water.

    摘要翻译： 这个过程源于发现，在低于0℃的温度下，水在氯乙烯单体（“VCM”）中的溶解度如此低，在苛性碱水溶液中，水溶液将除去溶解在单体中的水， 同时中和与单体相关的HCl，防止形成乙炔。 该发现使得可以通过在低于25°F的温度下将流与冷的2-30重量％苛性钠水溶液紧密接触来干燥和中和HCl和含水氯乙烯（“VCl”）流， 高于苛性碱溶液的凝固点。 在商业VCM生产设施中，VCl可以在“独立”处理设备中“处理”，其经济性比常规VCM工厂更​​高，但避免了操作常规VCl汽提塔和填充有固体苛性碱颗粒的洗涤器的危险 。 该方法允许通过使其与10％至25％的冷苛性碱水溶液接触，同时干燥和中和含有约1ppm（ppm）至约500ppm HCl的VCl流和约10ppm至约300ppm的水 分离干燥和中和的含有不超过100ppm水的VCM单体。

    Oxychlorination process
    4.
    发明授权
    Oxychlorination process 失效
    氧氯化过程

    公开(公告)号：US5600043A

    公开(公告)日：1997-02-04

    申请号：US411023

    申请日：1995-03-27

    申请人： Victor J. Johnston ,  Joseph A. Cowfer

    发明人： Victor J. Johnston ,  Joseph A. Cowfer

    IPC分类号： C07C17/156 ,  C07C17/15 ,  C07C17/154

    CPC分类号： C07C17/156

    摘要： The subject invention relates to a process for oxychlorination of ethylene to produce 1,2-dichloroethane. The process comprises contacting a mixture of ethylene, oxygen or oxygen containing gas and hydrogen chloride with a fixed or fluidized catalyst composition in a reaction zone and recovering 1,2-dichloroethane from the effluents of the reaction zone.The invention is embodied in a process for the oxychlorination of ethylene to produce 1,2-dichloroethane by contacting a mixture of ethylene, oxygen containing gas and hydrogen chloride with a catalyst composition in a reaction zone and recovering 1,2-dichloroethane from the effluents of the reaction zone the process comprising introducing ethylene, HCl and oxygen containing gas into said reaction zone in a ratio of 1.8 and 2.2 moles of HCl per mole of ethylene and from 0.5 to 1 mole of oxygen per mole of ethylene, the oxychlorination process taking place at a temperature of from 215.degree. C. to 230.degree. C., ethylene conversion on a weight basis is at 99% or higher and the mixture is contacted with a catalyst including a support which has deposited thereon a combination of metal chloride salts, the combination consisting essentially of from 2 to 8% copper, from 0.2 to 2% potassium and from 0.01 to 0.19% magnesium, all percentages expressed as the metals on a weight percent basis.

    摘要翻译： 本发明涉及乙烯氧氯化生产1,2-二氯乙烷的方法。 该方法包括将乙烯，含氧气或含氧气体和氯化氢的混合物与固定或流化催化剂组合物在反应区中接触并从反应区的流出物回收1,2-二氯乙烷。 本发明体现在通过使乙烯，含氧气体和氯化氢的混合物与催化剂组合物在反应区中接触并从流出物回收1,2-二氯乙烷的乙烯氧氯化生产1,2-二氯乙烷的方法中 的反应区，该方法包括以每摩尔乙烯1.8至2.2摩尔HCl /摩尔乙烯和0.5至1摩尔氧/摩尔乙烯的比例将乙烯，HCl和含氧气体引入所述反应区，所述氧氯化方法 在215℃-230℃的温度下放置，乙烯基于重量的转化率为99％以上，并将混合物与包含沉积有金属氯化物盐的载体的催化剂接触， 该组合基本上由2至8％的铜，0.2至2％的钾和0.01至0.19％的镁组成，所有百分比以重量百分数表示为金属。

    Catalyst and process for the fluid-bed oxychlorination of ethylene to EDC
    6.
    发明授权
    Catalyst and process for the fluid-bed oxychlorination of ethylene to EDC 失效
    催化剂和乙烯流动床氧氯化为EDC的方法

    公开(公告)号：US4849393A

    公开(公告)日：1989-07-18

    申请号：US140272

    申请日：1987-12-31

    申请人： Jamal S. Eden ,  Joseph A. Cowfer

    发明人： Jamal S. Eden ,  Joseph A. Cowfer

    IPC分类号： B01J23/78 ,  B01J27/10 ,  C07C17/156

    CPC分类号： B01J27/10 ,  B01J23/78 ,  C07C17/156

    摘要： A fluidizable catalyst composition is provided containing about 2% to about 8% by weight of copper (about 4% to about 17% by weight of copper salt), from about 1.0% to about 10% by weight of a rare earth metal salt(s), preferably the chloride salt(s), and from about 0.25% to about 2.3% by weight of an alkali metal salt(s), preferably the chloride salt(s), all weight percents based upon the total weight of the catalyst composition. The metals are codeposited on a fluidizable, high surface area alumina support. The weight of the alkali metal employed is not over 2.5% by weight (as the chloride) and the weight ratio of the rare earth metal salt(s) to the alkali metal salt(s) must be at least 1:1. Such catalyst compositions are extremely useful as fluid bed catalysts in the vapor phase oxychlorination reaction of ethylene, oxygen and hydrogen chloride to produce 1,2-dichloroethane (EDC). The use of the catalysts results in improved, high percent ethylene efficiencies and high percent HCl conversions, and avoids operating problems caused by stickiness of the catalyst in the fluid bed. A combination of copper chloride, potassium chloride and one or more of the rare earth chlorides on a fluidizable gamma alumina support, produces an excellent catalyst for a fluid bed ethylene oxychlorination process.

    摘要翻译： 提供了一种可流化催化剂组合物，其含有约2％至约8％重量的铜（约4％至约17％重量的铜盐），约1.0％至约10％重量的稀土金属盐（ s），优选氯化物盐，和约0.25重量％至约2.3重量％的碱金属盐，优选氯化物盐，基于催化剂的总重量，所有重量百分比 组成。 金属共沉积在可流化的高表面积氧化铝载体上。 所用碱金属的重量不超过2.5重量％（作为氯化物），稀土金属盐与碱金属盐的重量比必须至少为1:1。 这种催化剂组合物在乙烯，氧气和氯化氢的气相氧氯化反应中作为流化床催化剂非常有用，以产生1,2-二氯乙烷（EDC）。 催化剂的使用导致乙烯效率提高，乙烯转化率高，HCl转化率高，避免了催化剂在流化床中的粘性引起的操作问题。 在可流化的γ氧化铝载体上，氯化铜，氯化钾和一种或多种稀土氯化物的组合产生用于流化床乙烯氧氯化方法的优异催化剂。

    Catalyst and process for oxychlorination of ethylene to EDC
    7.
    发明授权
    Catalyst and process for oxychlorination of ethylene to EDC 失效
    催化剂和乙烯氧氯化为EDC的方法

    公开(公告)号：US5382726A

    公开(公告)日：1995-01-17

    申请号：US156142

    申请日：1993-11-22

    申请人： George H. Young ,  Joseph A. Cowfer ,  Victor J. Johnston

    发明人： George H. Young ,  Joseph A. Cowfer ,  Victor J. Johnston

    IPC分类号： B01J23/78 ,  B01J23/83 ,  B01J27/138 ,  C07B61/00 ,  C07C17/156 ,  C07C19/045

    CPC分类号： B01J23/83 ,  C07C17/156

    摘要： The subject invention relates to catalyst compositions for oxychlorination of ethylene to produce 1,2-dichloroethane. The catalysts comprise copper chloride, at least one alkali metal, at least one rare earth metal, and at least one Group IIA metal on a high surface area support for fluid bed applications or on a high or low surface area support for fixed bed applications. The catalyst compositions are prepared by depositing the metals on a support. The use of the catalyst compositions of the invention in the oxychlorination of ethylene to EDC results in high percent ethylene efficiency, high EDC product purity and high percent HCl conversion without exhibiting catalyst stickiness. A process for oxychlorination of ethylene to produce 1,2-dichloroethane is also disclosed. The process relies on contacting a mixture of ethylene, oxygen or oxygen containing gas and hydrogen chloride with a fixed or fluidized catalyst composition in a reaction zone and recovering 1,2-dichloroethane from the effluents of the reaction zone.

    摘要翻译： 本发明涉及乙烯氧氯化以产生1,2-二氯乙烷的催化剂组合物。 催化剂包括氯化铜，至少一种碱金属，至少一种稀土金属和高表面积上的至少一种IIA族金属，用于流化床应用或用于固定床应用的高表面或低表面积。 通过将金属沉积在载体上来制备催化剂组合物。 使用本发明的催化剂组合物将乙烯氧氯化成EDC导致乙烯效率高，高EDC产物纯度和高HCl HCl转化率而不显示催化剂粘性。 还公开了乙烯氧氯化生产1,2-二氯乙烷的方法。 该方法依靠将乙烯，含氧气或含氧气体和氯化氢的混合物与固定或流化催化剂组合物在反应区中接触并从反应区的流出物回收1,2-二氯乙烷。

    Catalyst and process for oxychlorination of ethylene to EDC
    8.
    发明授权
    Catalyst and process for oxychlorination of ethylene to EDC 失效
    催化剂和乙烯氧氯化为EDC的方法

    公开(公告)号：US5292703A

    公开(公告)日：1994-03-08

    申请号：US920721

    申请日：1992-07-28

    申请人： George H. Young ,  Joseph A. Cowfer ,  Victor J. Johnston

    发明人： George H. Young ,  Joseph A. Cowfer ,  Victor J. Johnston

    IPC分类号： B01J23/78 ,  B01J23/83 ,  B01J27/138 ,  C07B61/00 ,  C07C17/156 ,  C07C19/045 ,  B01J23/72 ,  B01J23/10

    CPC分类号： B01J23/83 ,  C07C17/156

    摘要： The subject invention relates to catalyst compositions for oxychlorination of ethylene to produce 1,2-dichloroethane. The catalysts comprise copper chloride, at least one alkali metal, at least one rare earth metal, and at least one Group IIA metal on a high surface area support for fluid bed applications or on a high or low surface area support for fixed bed applications. The catalyst compositions are prepared by depositing the metals on a support. The use of the catalyst compositions of the invention in the oxychlorination of ethylene to EDC results in high percent ethylene efficiency, high EDC product purity and high percent HCl conversion without exhibiting catalyst stickiness. A process for oxychlorination of ethylene to produce 1,2-dichloroethane is also disclosed. The process relies on contacting a mixture of ethylene, oxygen or oxygen containing gas and hydrogen chloride with a fixed or fluidized catalyst composition in a reaction zone and recovering 1,2-dichloroethane from the effluents of the reaction zone.

    摘要翻译： 本发明涉及乙烯氧氯化以产生1,2-二氯乙烷的催化剂组合物。 催化剂包括氯化铜，至少一种碱金属，至少一种稀土金属和高表面积上的至少一种IIA族金属，用于流化床应用或用于固定床应用的高表面或低表面积。 通过将金属沉积在载体上来制备催化剂组合物。 使用本发明的催化剂组合物将乙烯氧氯化成EDC导致乙烯效率高，高EDC产物纯度和高HCl HCl转化率而不显示催化剂粘性。 还公开了乙烯氧氯化生产1,2-二氯乙烷的方法。 该方法依靠将乙烯，含氧气或含氧气体和氯化氢的混合物与固定或流化催化剂组合物在反应区中接触并从反应区的流出物回收1,2-二氯乙烷。

    Recovery of ethylene, chlorine and HCl from vented waste gas from direct chlorination reactor
    9.
    发明授权
    Recovery of ethylene, chlorine and HCl from vented waste gas from direct chlorination reactor 失效
    从直接氯化反应器排出的废气中回收乙烯，氯和HCl

    公开(公告)号：US4760207A

    公开(公告)日：1988-07-26

    申请号：US908744

    申请日：1986-09-18

    申请人： Joseph A. Cowfer

    发明人： Joseph A. Cowfer

    IPC分类号： C07C19/045 ,  C01B7/07 ,  C07C17/00 ,  C07C17/02 ,  C07C17/156 ,  C07C17/38 ,  C07C67/00 ,  C07C17/154

    CPC分类号： C07C17/38 ,  C01B7/07 ,  C01B7/0706 ,  C07C17/02

    摘要： In a process for producing 1,2-dichloroethane or ethylene dichloride ("EDC") in a high temperature direct chlorination ("HTDC") reactor in which ethylene is reacted with wet chlorine having a water content more than 100 ppm but no more than 1% by wt of the chlorine, the water leaves the reactor with the EDC product draw-off, either in the vapor overhead (if the HTDC is a boiling reactor), or, as a liquid sidestream (if the HTDC is a non-boiling reactor). In a subsequent step, the EDC draw-off is distilled in a product distillation column in which the water leaves in the overhead which is condensed to remove condensables in a first stage, and vent a non-condensable vent streams. The vent stream is corrosive due to the presence of minor amounts of chlorine, HCl and water, along with oxygen which is injected into the HTDC to improve selectivity of the reaction. The vent gases from the first stage are further cooled to a temperature in the range from about -30.degree. C. to about 0.degree. C. to condense condensables and freeze water without plugging the liquid lines. Plugging is avoided provided the vent stream contains less than 1.5% by wt of water, based on the weight of the vent stream. The essentially moisture-free non-condensables remaining are relatively non-corrosive and may be recycled to an oxychlorination reactor, also for the production of EDC, without unduly sacrificing the vent compressor and other carbon steel equipment in the recycle line.

    摘要翻译： 在高温直接氯化（“HTDC”）反应器中制备1,2-二氯乙烷或二氯乙烷（“EDC”）的方法中，其中乙烯与水含量大于100ppm但不超过 1％（重量）的氯，水在蒸汽塔顶（如果HTDC是沸腾反应器）中离开反应器，EDC产物排出，或作为液体侧流（如果HTDC是非离子表面活性剂） 沸腾反应器）。 在随后的步骤中，在产物蒸馏塔中蒸馏EDC馏出物，其中水在塔顶馏出，其被冷凝以在第一阶段除去可冷凝物，并排出不可冷凝的排放物流。 由于存在少量的氯，HCl和水以及注入HTDC中的氧气以提高反应的选择性，排气流是腐蚀性的。 来自第一阶段的排出气体进一步冷却至约-30℃至约0℃的温度，以冷凝可冷凝物和冷冻水而不堵塞液体管线。 避免堵塞，只要排气流含有小于1.5重量％的水，基于排气流的重量。 剩余的基本上不含湿气的不可冷凝物是相对非腐蚀性的，并且可以再循环到氧氯化反应器中，也用于生产EDC，而不会过度地牺牲再循环管线中的排气压缩机和其它碳钢设备。