公开(公告)号：US09168519B2

公开(公告)日：2015-10-27

申请号：US13275518

申请日：2011-10-18

Applicant: Alexander E. Kuperman ,  Theodorus Maesen ,  Dennis Dykstra

Inventor： Alexander E. Kuperman ,  Theodorus Maesen ,  Dennis Dykstra

IPC: B01J37/20 ,  B01J37/34 ,  B01J23/85 ,  B01J23/888 ,  B01J37/03 ,  B01J27/051 ,  B01J37/04 ,  B01J37/08

CPC classification number: B01J37/342 ,  B01J23/85 ,  B01J23/8885 ,  B01J27/0515 ,  B01J37/03 ,  B01J37/036 ,  B01J37/04 ,  B01J37/08 ,  B01J37/20 ,  B01J37/34

Abstract: In a process for forming a bulk hydroprocessing catalyst by sulfiding a catalyst precursor made in a co-precipitation reaction, up to 60% of the metal precursor feeds do not react to form catalyst precursor and end up in the supernatant as metal residuals. In the present disclosure, the metals can be recovered in a chemical precipitation step, wherein the supernatant is mixed with at least one of an acid, a sulfide-containing compound, a base, and combinations thereof to precipitate at least 50% of metal ions in at least one of the metal residuals, wherein the precipitation is carried out at a pre-select pH. The precipitate is isolated and recovered, yielding an effluent stream. The precipitate and/or the effluent stream can be further treated to form at least a metal precursor feed which can be used in the co-precipitation reaction. The process generates an effluent to waste treatment containing less than 50 ppm metals.

Abstract translation: 在通过硫化在共沉淀反应中制备的催化剂前体形成本体加氢处理催化剂的方法中，多达60％的金属前体进料不反应形成催化剂前体，最后作为金属残余物结合在上清液中。 在本公开中，可以在化学沉淀步骤中回收金属，其中将上清液与酸，含硫化物的化合物，碱及其组合中的至少一种混合以沉淀至少50％的金属离子 在至少一个金属残留物中，其中沉淀是在预先选择的pH下进行的。 分离并回收沉淀物，产生流出物流。 可以将沉淀物和/或流出物流进一步处理以形成可用于共沉淀反应的至少一种金属前体进料。 该过程产生含有少于50ppm金属的废水处理废水。

公开(公告)号：US08658558B2

公开(公告)日：2014-02-25

申请号：US13275482

申请日：2011-10-18

Applicant: Theodorus Maesen ,  Alexander E. Kuperman ,  Dennis Dykstra

Inventor： Theodorus Maesen ,  Alexander E. Kuperman ,  Dennis Dykstra

IPC: B01J27/051

CPC classification number: B01J37/036 ,  B01J23/85 ,  B01J23/8885 ,  B01J37/34

Abstract: In a process for forming a bulk hydroprocessing catalyst by sulfiding a catalyst precursor made in a co-precipitation reaction, up to 60% of the metal precursor feeds do not react to form catalyst precursor and end up in the supernatant. In the present disclosure, the metals can be recovered in an electro-coagulation reactor, wherein portion of the metal residuals in the supernatant reacts with the electrodes to form a slurry containing insoluble metal compounds. The insoluble metal compounds are isolated and recovered, forming an effluent stream. The insoluble metal compounds and/or the effluent stream can be further treated to form at least a metal precursor feed which can be used in the co-precipitation reaction.

Abstract translation: 在通过硫化在共沉淀反应中制备的催化剂前体形成本体加氢处理催化剂的方法中，多达60％的金属前体进料不反应形成催化剂前体并最终在上清液中。 在本公开中，金属可以在电凝反应器中回收，其中上清液中的金属残余物的一部分与电极反应形成含有不溶性金属化合物的浆料。 分离和回收不溶性金属化合物，形成流出物流。 可以进一步处理不溶性金属化合物和/或流出物流以形成可用于共沉淀反应的至少一种金属前体进料。

公开(公告)号：US08575062B2

公开(公告)日：2013-11-05

申请号：US13275597

申请日：2011-10-18

Applicant: Alexander E. Kuperman ,  Theodorus Maesen ,  Dennis Dykstra

Inventor： Alexander E. Kuperman ,  Theodorus Maesen ,  Dennis Dykstra

IPC: B01J23/00

CPC classification number: B01J37/03 ,  B01J23/002 ,  B01J23/8885 ,  B01J37/009 ,  B01J37/036 ,  B01J37/20 ,  B01J37/341 ,  B01J37/348 ,  C10G45/08 ,  C10G47/04 ,  C10G49/04 ,  C10G2300/1033 ,  B01J2523/00 ,  B01J2523/68 ,  B01J2523/69 ,  B01J2523/847 ,  B01J2523/845

Abstract: In a process for forming a bulk hydroprocessing catalyst by sulfiding a catalyst precursor in a co-precipitation reaction, up to 60% of the metal precursor feeds do not react to form catalyst precursor and stay in the supernatant. In one embodiment, at least a precipitant is added to the product mixture at a molar ratio of precipitant to metal residuals in the supernatant ranging from 1.5:1 to 20:1 to precipitate at least 50 mole % of metal ions in the residuals forming additional catalyst precursor. The remaining metal residuals can be recovered via any of chemical precipitation, ion exchange, electro-coagulation, and combinations thereof to generate an effluent stream containing less than 50 mole % of at least one of the metal residuals. In one embodiment, at least one of the metal residuals is recovered and recycled for use as a metal precursor feed in the co-precipitation reaction.

Abstract translation: 在通过在共沉淀反应中硫化催化剂前体形成本体加氢处理催化剂的方法中，多达60％的金属前体进料不反应形成催化剂前体并停留在上清液中。 在一个实施方案中，至少一种沉淀剂以1.5:1至20:1的上清液中的沉淀剂与金属残留物的摩尔比加入到产物混合物中，以沉淀残留物中至少50摩尔％的金属离子，形成额外的 催化剂前体。 剩余的金属残余物可以通过化学沉淀，离子交换，电凝和其组合中的任何一种回收，以产生含有小于50摩尔％的至少一种金属残余物的流出物流。 在一个实施方案中，至少一种金属残余物被回收并再循环用作共沉淀反应中的金属前体进料。

公开(公告)号：US08383543B2

公开(公告)日：2013-02-26

申请号：US12770388

申请日：2010-04-29

Applicant: Theodorus Maesen ,  Alexander E. Kuperman ,  Dennis Dykstra

Inventor： Theodorus Maesen ,  Alexander E. Kuperman ,  Dennis Dykstra

IPC: B01J31/00 ,  B01J27/045 ,  B01J27/047 ,  B01J27/14 ,  B01J27/24

CPC classification number: B01J31/04 ,  B01J23/002 ,  B01J23/24 ,  B01J23/652 ,  B01J23/85 ,  B01J23/8885 ,  B01J31/0201 ,  B01J31/2226 ,  B01J35/002 ,  B01J35/0026 ,  B01J35/1014 ,  B01J35/1019 ,  B01J35/1042 ,  B01J35/1061 ,  B01J35/1066 ,  B01J37/0009 ,  B01J37/031 ,  B01J37/20 ,  B01J2523/00 ,  B01J2531/64 ,  B01J2531/66 ,  B01J2531/847 ,  C10G45/04 ,  B01J2523/68 ,  B01J2523/69 ,  B01J2523/847

Abstract: The invention relates to a bulk multi-metallic catalyst for hydrotreating heavy oil feeds and to a method for preparing the catalyst. The bulk multi-metallic catalyst is prepared by sulfiding a catalyst precursor having a poorly crystalline structure with disordered stacking layers, with a type IV adsorption-desorption isotherms of nitrogen with a hysteresis starting point value of about 0.35, for a sulfided catalyst that will facilitate the reactant's and product's diffusion in catalytic applications. In another embodiment, the precursor is characterized as having a type H3 hysteresis loop. In a third embodiment, the hysteresis loop is characterized as having a well developed plateau above P/Po of about 0.55. The mesapores of the precursor can be adjustable or tunable.

Abstract translation: 本发明涉及用于加氢处理重油进料的本体多金属催化剂及其制备方法。 本体多金属催化剂是通过硫化具有无序堆叠层的结晶结构不良的催化剂前体，具有约0.35的磁滞起始点值的氮的IV型吸附 - 解吸等温线来制备的，所述硫化催化剂将促进 反应物和产品在催化应用中的扩散。 在另一个实施方案中，前体的特征在于具有H3型磁滞回线。 在第三实施例中，磁滞回线的特征在于具有高于P / Po的良好发展的平台约为0.55。 前体的介孔可以是可调节的或可调节的。

公开(公告)号：US20120122658A1

公开(公告)日：2012-05-17

申请号：US13275459

申请日：2011-10-18

Applicant: Alexander E. Kuperman ,  Theodorus Maesen ,  Dennis Dykstra

Inventor： Alexander E. Kuperman ,  Theodorus Maesen ,  Dennis Dykstra

IPC: B01J37/30 ,  B01J27/051

CPC classification number: B01J37/03 ,  B01J23/002 ,  B01J23/8885 ,  B01J37/009 ,  B01J37/036 ,  B01J37/20 ,  B01J37/341 ,  B01J37/348 ,  B01J2523/00 ,  C10G45/08 ,  C10G47/04 ,  C10G49/04 ,  C10G2300/1033 ,  B01J2523/68 ,  B01J2523/69 ,  B01J2523/847

Abstract: In a process for forming a bulk hydroprocessing catalyst by sulfiding a catalyst precursor made in a co-precipitation reaction, up to 60% of metal ions in at least one of the metal precursor feeds do not react to form catalyst precursor and end up in the supernatant as metal residuals. In the present disclosure, the metals can be recovered via ion-exchange, wherein an exchange resin is provided for a portion of the metal ions in the supernatant to be exchanged and bound onto the resin. The previously resin-bound metals can be subsequently recovered, or the effluent stream for the exchange resin column can also be recovered, forming at least a metal precursor feed which can be used in the co-precipitation reaction.

Abstract translation: 在通过硫化在共沉淀反应中制备的催化剂前体形成本体加氢处理催化剂的方法中，至少一种金属前体进料中至多60％的金属离子不反应形成催化剂前体，最终在 上清液作为金属残留物。 在本公开中，可以通过离子交换回收金属，其中为要交换并结合到树脂上的上清液中的一部分金属离子提供交换树脂。 可以随后回收先前的树脂结合的金属，或者还可以回收用于交换树脂柱的流出物流，形成至少可以用于共沉淀反应的金属前体进料。

公开(公告)号：US20120122656A1

公开(公告)日：2012-05-17

申请号：US13275597

申请日：2011-10-18

Applicant: Alexander E. Kuperman ,  Theodorus Maesen ,  Dennis Dykstra

Inventor： Alexander E. Kuperman ,  Theodorus Maesen ,  Dennis Dykstra

IPC: B01J27/047 ,  B01J37/20 ,  B01J27/051 ,  B01J37/03 ,  B01J37/34 ,  B01J37/30

CPC classification number: B01J37/03 ,  B01J23/002 ,  B01J23/8885 ,  B01J37/009 ,  B01J37/036 ,  B01J37/20 ,  B01J37/341 ,  B01J37/348 ,  C10G45/08 ,  C10G47/04 ,  C10G49/04 ,  C10G2300/1033 ,  B01J2523/00 ,  B01J2523/68 ,  B01J2523/69 ,  B01J2523/847 ,  B01J2523/845

Abstract: In a process for forming a bulk hydroprocessing catalyst by sulfiding a catalyst precursor in a co-precipitation reaction, up to 60% of the metal precursor feeds do not react to form catalyst precursor and stay in the supernatant. In one embodiment, at least a precipitant is added to the product mixture at a molar ratio of precipitant to metal residuals in the supernatant ranging from 1.5:1 to 20:1 to precipitate at least 50 mole % of metal ions in the residuals forming additional catalyst precursor. The remaining metal residuals can be recovered via any of chemical precipitation, ion exchange, electro-coagulation, and combinations thereof to generate an effluent stream containing less than 50 mole % of at least one of the metal residuals. In one embodiment, at least one of the metal residuals is recovered and recycled for use as a metal precursor feed in the co-precipitation reaction.

Abstract translation: 在通过在共沉淀反应中硫化催化剂前体形成本体加氢处理催化剂的方法中，多达60％的金属前体进料不反应形成催化剂前体并停留在上清液中。 在一个实施方案中，至少一种沉淀剂以1.5:1至20:1的上清液中的沉淀剂与金属残留物的摩尔比加入到产物混合物中，以沉淀残留物中至少50摩尔％的金属离子，形成额外的 催化剂前体。 剩余的金属残余物可以通过化学沉淀，离子交换，电凝和其组合中的任何一种回收，以产生含有小于50摩尔％的至少一种金属残余物的流出物流。 在一个实施方案中，至少一种金属残余物被回收并再循环用作共沉淀反应中的金属前体进料。

公开(公告)号：US20120122653A1

公开(公告)日：2012-05-17

申请号：US13275482

申请日：2011-10-18

Applicant: Theodorus Maesen ,  Alexander E. Kuperman ,  Dennis Dykstra

Inventor： Theodorus Maesen ,  Alexander E. Kuperman ,  Dennis Dykstra

IPC: B01J37/34 ,  B01J27/051

CPC classification number: B01J37/036 ,  B01J23/85 ,  B01J23/8885 ,  B01J37/34

Abstract: In a process for forming a bulk hydroprocessing catalyst by sulfiding a catalyst precursor made in a co-precipitation reaction, up to 60% of the metal precursor feeds do not react to form catalyst precursor and end up in the supernatant. In the present disclosure, the metals can be recovered in an electro-coagulation reactor, wherein portion of the metal residuals in the supernatant reacts with the electrodes to form a slurry containing insoluble metal compounds. The insoluble metal compounds are isolated and recovered, forming an effluent stream. The insoluble metal compounds and/or the effluent stream can be further treated to form at least a metal precursor feed which can be used in the co-precipitation reaction.

Abstract translation: 在通过硫化在共沉淀反应中制备的催化剂前体形成本体加氢处理催化剂的方法中，多达60％的金属前体进料不反应形成催化剂前体并最终在上清液中。 在本公开中，金属可以在电凝反应器中回收，其中上清液中的金属残余物的一部分与电极反应形成含有不溶性金属化合物的浆料。 分离和回收不溶性金属化合物，形成流出物流。 可以进一步处理不溶性金属化合物和/或流出物流以形成可用于共沉淀反应的至少一种金属前体进料。

公开(公告)号：US20120122659A1

公开(公告)日：2012-05-17

申请号：US13275628

申请日：2011-10-18

Applicant: Alexander E. Kuperman ,  Theodorus Maesen ,  Dennis Dykstra ,  Ping Wang ,  Soy Uckung

Inventor： Alexander E. Kuperman ,  Theodorus Maesen ,  Dennis Dykstra ,  Ping Wang ,  Soy Uckung

IPC: B01J37/30 ,  B01J27/051

CPC classification number: B01J37/031 ,  B01J23/24 ,  B01J23/85 ,  B01J23/8885 ,  B01J37/20 ,  C10G1/08 ,  C10G1/10 ,  C10G49/02 ,  C10G49/04 ,  C10G2300/70

Abstract: In a process for forming a bulk hydroprocessing catalyst by sulfiding a catalyst precursor made in a co-precipitation reaction, up to 60% of the metal precursor feeds end up in the supernatant. The metals can be recovered via any of chemical precipitation, ion exchange, electro-coagulation, and combinations thereof to generate an effluent stream containing less than 50 mole % of metal ions in at least one of the metal residuals, and for at least one of the metal residuals recovered as a metal precursor feed for use in the co-precipitation reaction. In one embodiment, the resin functions as an anion exchange resin with an acidic supernatant to recover Group VIB metal residuals, and a cation exchange resin with a basic supernatant to recover Promoter metal residuals. An effluent stream from the process to waste treatment contains less than 50 ppm metals.

Abstract translation: 在通过硫化在共沉淀反应中制备的催化剂前体形成本体加氢处理催化剂的方法中，高达60％的金属前体进料最终在上清液中。 可以通过化学沉淀，离子交换，电凝和其组合中的任何一种来回收金属，以在至少一个金属残余物中产生含有少于50摩尔％金属离子的流出物流，并且对于至少一种 作为用于共沉淀反应的金属前体原料回收金属残留物。 在一个实施方案中，树脂起到具有酸性上清液的阴离子交换树脂的作用，以回收VIB族金属残余物，以及具有碱性上清液的阳离子交换树脂以回收助催化剂金属残留物。 从过程到废物处理的流出物流含有少于50ppm的金属。

公开(公告)号：US20120122655A1

公开(公告)日：2012-05-17

申请号：US13275557

申请日：2011-10-18

Applicant: Alexander E. Kuperman ,  Theodorus Maesen ,  Dennis Dykstra

Inventor： Alexander E. Kuperman ,  Theodorus Maesen ,  Dennis Dykstra

IPC: B01J37/34 ,  B01J27/051 ,  B01J37/20 ,  B01J27/049 ,  B01J37/03 ,  B01J37/30 ,  B01J27/047

CPC classification number: B01J37/03 ,  B01J23/002 ,  B01J23/8885 ,  B01J37/009 ,  B01J37/036 ,  B01J37/20 ,  B01J37/341 ,  B01J37/348 ,  B01J2523/00 ,  C10G45/08 ,  C10G47/04 ,  C10G49/04 ,  C10G2300/1033 ,  B01J2523/68 ,  B01J2523/69 ,  B01J2523/847

Abstract: In a process for forming a bulk hydroprocessing catalyst by sulfiding a catalyst precursor made in a co-precipitation reaction, up to 60% of the metal precursor feeds do not react to form catalyst precursor and end up in the supernatant. In the present disclosure, the metals can be recovered via any of chemical precipitation, ion exchange, electro-coagulation, and combinations thereof to generate an effluent stream containing less than 50 mole % of metal ions in at least one of the metal residuals, and for at least one of the metal residuals is recovered as a metal precursor feed, which can be recycled for use in the co-precipitation reaction. An effluent stream from the process to waste treatment contains less than 50 ppm metal ions.

Abstract translation: 在通过硫化在共沉淀反应中制备的催化剂前体形成本体加氢处理催化剂的方法中，多达60％的金属前体进料不反应形成催化剂前体并最终在上清液中。 在本公开中，可以通过化学沉淀，离子交换，电凝和其组合中的任何一种来回收金属，以在至少一个金属残余物中产生含有少于50摩尔％的金属离子的流出物流，以及 对于至少一种金属残余物作为金属前体原料回收，其可以再循环用于共沉淀反应。 从过程到废物处理的流出物流含有少于50ppm的金属离子。

公开(公告)号：US07964524B2

公开(公告)日：2011-06-21

申请号：US12432719

申请日：2009-04-29

Applicant: Alexander E. Kuperman ,  Theodorus Maesen ,  Dennis Dykstra

Inventor： Alexander E. Kuperman ,  Theodorus Maesen ,  Dennis Dykstra

IPC: B01J27/04 ,  B01J27/045 ,  B01J27/047 ,  B01J27/051 ,  B01J27/049 ,  B01J31/00

CPC classification number: B01J37/031 ,  B01J23/24 ,  B01J23/85 ,  B01J23/8885 ,  B01J37/0009 ,  B01J37/0018 ,  B01J37/20 ,  C10G45/04 ,  C10G47/02

Abstract: A catalyst and a process for making a catalyst from a precursor composition containing rework materials are disclosed. The catalyst is made by sulfiding a catalyst precursor containing 5-95 wt. % rework material. The catalyst precursor employing rework materials can be a hydroxide or oxide material. Rework can be materials generated in the forming or shaping of the catalyst precursor, or formed upon the breakage or handling of the shaped catalyst precursor. Rework can also be in the form of catalyst precursor feed material to the shaping process, e.g., extrusion process, or catalyst precursor material generated as reject or scrap in the shaping process. In some embodiment, rework may be of the consistency of shapeable dough. In another embodiment, rework is in the form of small pieces or particles, e.g., fines, powder.

Abstract translation: 公开了一种催化剂和由含有返修材料的前体组合物制备催化剂的方法。 催化剂是通过硫化含有5-95wt。 ％返修材料。 使用返工材料的催化剂前体可以是氢氧化物或氧化物材料。 返工可以是在催化剂前体的形成或成形中产生的材料，或者在成形催化剂前体的断裂或处理时形成的材料。 返工还可以是成型过程中的催化剂前体进料的形式，例如在成型过程中作为废料或废料生产的挤出方法或催化剂前体材料。 在一些实施例中，返工可以是可成形面团的一致性。 在另一个实施例中，返工是小块或颗粒的形式，例如细粉，粉末。