公开(公告)号：WO2012143331A1

公开(公告)日：2012-10-26

申请号：PCT/EP2012/056924

申请日：2012-04-16

Applicant: DSM IP ASSETS B.V. ,  GROOTHAERT, Marijke Hilde Leen ,  TINGE, Johan Thomas ,  GUIT, Rudolf Philippus Maria

Inventor： GROOTHAERT, Marijke Hilde Leen ,  TINGE, Johan Thomas

IPC: C01B21/14

CPC classification number: C07C249/08 ,  C01B21/1418 ,  C07C2601/14 ,  C07C2601/20 ,  C07D201/04 ,  C07D211/76 ,  C07D227/087 ,  C07C251/44

Abstract: Method for preparing hydroxylamine in a continuous process, comprising hydrogenating nitrate in a reaction zone comprising a liquid phase, a gas phase and a heterogeneous hydrogenation catalyst, in which reaction zone hydroxylamine and nitrous oxide (N20) are formed, characterized in that the nitrous oxide concentration in the gas phase, is monitored and is maintained within a predetermined range by means of controlled addition of a promoter for the heterogeneous hydrogenation catalyst and/or controlled addition of further amounts of heterogeneous hydrogenation catalyst to the reaction zone; a method for preparing an oxime and a method of preparing a lactam comprising said method for preparing hydroxylamine.

Abstract translation: 在连续方法中制备羟胺的方法，包括在包含液相，气相和异相氢化催化剂的反应区中使硝酸盐氢化，其中反应区羟胺和一氧化二氮（N 2 O 2）形成，其特征在于一氧化二氮 通过控制加入非均相氢化催化剂的促进剂和/或将另外量的非均相氢化催化剂加入到反应区中来监测气体中的浓度并保持在预定范围内。 制备肟的方法和制备内酰胺的方法，包括所述的制备羟胺的方法。

公开(公告)号：WO2009080240A2

公开(公告)日：2009-07-02

申请号：PCT/EP2008/010687

申请日：2008-12-16

Applicant: DSM IP ASSETS B.V. ,  TJIOE, Tjay, Tjien ,  GROOTHAERT, Marijke, Hilde, Leen ,  VAN DER SPOEL, Jan

Inventor： TJIOE, Tjay, Tjien ,  GROOTHAERT, Marijke, Hilde, Leen ,  VAN DER SPOEL, Jan

IPC: C07D251/62 ,  B01J8/02

CPC classification number: C07D251/62

Abstract: The invention relates to process for the preparation of melamine comprising at least the following steps: a. feeding ammonia and hydrogen cyanide, either separately or combined, to a first reactor that contains a catalyst that comprises at least one element selected from group 11 of the Periodic Table of the Elements and which reactor is maintained at a pressure of at least 0.2 MPa and a temperature of 300-500 °C, at a space velocity lying between 10 2 and 10 6 ml/(g.hr), whereby a gaseous mixture (a) is formed comprising at least melamine, b. optionally purifying mixture (a), producing a melamine containing mixture (b), c. separating at least a part of the formed melamine, thereby forming a mixture (c) and separated melamine.

Abstract translation: 本发明涉及制备三聚氰胺的方法，其至少包括以下步骤：a。 将氨和氰化氢分别或组合地供给至第一反应器，该第一反应器包含催化剂，该催化剂包含至少一种选自元素周期表第11族的元素并且该反应器保持在至少0.2MPa的压力下， 温度为300-500℃，空间速度介于10 2和10 6 ml /（g·hr）之间，由此得到气态混合物（a） 形成至少包含三聚氰胺，b。 任选地纯化混合物（a），产生含三聚氰胺的混合物（b），c。 分离至少一部分形成的三聚氰胺，从而形成混合物（c）并分离出三聚氰胺。

公开(公告)号：WO2009080240A3

公开(公告)日：2009-09-11

申请号：PCT/EP2008010687

申请日：2008-12-16

Applicant: DSM IP ASSETS BV ,  TJIOE TJAY TJIEN ,  GROOTHAERT MARIJKE HILDE LEEN ,  VAN DER SPOEL JAN

Inventor： TJIOE TJAY TJIEN ,  GROOTHAERT MARIJKE HILDE LEEN ,  VAN DER SPOEL JAN

IPC: C07D251/62 ,  B01J8/02

CPC classification number: C07D251/62

Abstract: The invention relates to process for the preparation of melamine comprising at least the following steps: a. feeding ammonia and hydrogen cyanide, either separately or combined, to a first reactor that contains a catalyst that comprises at least one element selected from group 11 of the Periodic Table of the Elements and which reactor is maintained at a pressure of at least 0.2 MPa and a temperature of 300-500 °C, at a space velocity lying between 102 and 106 ml/(g.hr), whereby a gaseous mixture (a) is formed comprising at least melamine, b. optionally purifying mixture (a), producing a melamine containing mixture (b), c. separating at least a part of the formed melamine, thereby forming a mixture (c) and separated melamine.

Abstract translation: 本发明涉及三聚氰胺的制备方法，该方法至少包括以下步骤：a。 将氨和氰化氢单独或组合供给到含有包含至少一种选自元素周期表第11族的元素的催化剂的第一反应器，并且该反应器保持在至少0.2MPa的压力和 温度为300-500℃，空间速度为102至106ml /（g·hr），由此形成至少包含三聚氰胺的气态混合物（a），b。 任选地，纯化混合物（a），产生含三聚氰胺的混合物（b），c。 分离形成的三聚氰胺的至少一部分，从而形成混合物（c）和分离的三聚氰胺。

公开(公告)号：WO2009080241A2

公开(公告)日：2009-07-02

申请号：PCT/EP2008010688

申请日：2008-12-16

Applicant: DSM IP ASSETS BV ,  TJIOE TJAY TJIEN ,  GROOTHAERT MARIJKE HILDE LEEN ,  FELLAY CELINE

Inventor： TJIOE TJAY TJIEN ,  GROOTHAERT MARIJKE HILDE LEEN ,  FELLAY CELINE

IPC: C07D251/62 ,  B01J8/02

CPC classification number: C07D251/62

Abstract: The present invention relates to a process for the preparation of melamine, which process comprises at least the following steps: i) feeding methane and ammonia to a pre- reactor which pre- reactor is maintained at a temperature between 700 and 1500 °C whereby a gaseous mixture (i) is formed comprising at least hydrogen cyanide, ii) optionally, purifying mixture (i) thereby forming a mixture (ii) that contains at least gaseous hydrogen cyanide, a. feeding hydrogen cyanide from mixture (i) or (ii) and ammonia, either separately or combined, to a reactor that contains a catalyst and which reactor is maintained at a temperature of 300-500°C, at a space velocity lying between 102 and 106 ml/(g.hr), whereby a gaseous mixture (a) is formed comprising at least melamine, b. optionally, purifying mixture (a) producing a melamine containing mixture (b), c. separating at least a part of the formed melamine thereby forming a mixture (c) and separated melamine.

Abstract translation: 本发明涉及一种制备三聚氰胺的方法，该方法包括至少以下步骤：i）将甲烷和氨进料到预反应器中，将预反应器保持在700和1500℃之间，由此得到 形成气态混合物（i），其至少包含氰化氢，ii）任选地，纯化混合物（i），从而形成至少含有氰化氢气体的混合物（ii）。 将来自混合物（i）或（ii）的氰化氢和单独或组合的氨加入到含有催化剂的反应器中，并将该反应器保持在温度为300-500℃，空间速度为102至 106ml /（g.hr），由此形成至少包含三聚氰胺的气体混合物（a），b。 任选地，纯化混合物（a）产生含三聚氰胺的混合物（b），c。 分离形成的三聚氰胺的至少一部分，从而形成混合物（c）并分离出三聚氰胺。

公开(公告)号：WO2008000390A1

公开(公告)日：2008-01-03

申请号：PCT/EP2007/005497

申请日：2007-06-22

Applicant: DSM IP ASSETS B.V. ,  PETERS, Alexander, Volker ,  ANDERSON, Bruce, Gordon ,  PESTMAN, Robert ,  GROOTHAERT, Marijke, Hilde, Leen ,  TJIOE, Tjay, Tjien ,  KANAPARTHI, Ramesh

Inventor： PETERS, Alexander, Volker ,  ANDERSON, Bruce, Gordon ,  PESTMAN, Robert ,  GROOTHAERT, Marijke, Hilde, Leen ,  TJIOE, Tjay, Tjien ,  KANAPARTHI, Ramesh

IPC: C01C3/02 ,  B01J23/46

CPC classification number: B01J23/58 ,  B01J21/10 ,  B01J23/462 ,  B01J37/086 ,  C01C3/008 ,  C01C3/0208 ,  C01C3/0216 ,  C01C3/0229 ,  C01C3/14 ,  C07C209/00 ,  C07C273/00 ,  C07D239/50

Abstract: Process for the preparation of a nitrogen-containing Compound, comprising the Steps of: a) bringing N 2 , optionally NH 3 and optionally a recycle stream together with a carbon- and hydrogen-containing Compound or a carbon-containing Compound and H2 to form a reaction mixture, whereby the ammonia in the reaction mixture, if present, originates for at least 30 wt.% from the recycle stream; b) bringing the reaction mixture in contact with a catalyst at a temperature lying between 200°C and 800°C and at a space velocity lying between 10 2 and 10 6 ml/(g.h), said catalyst containing a metal M1 on a support, M1 being chosen from the group consisting of metals in group 3, 4, 5, 6, 7, 8, 9, 10, 11 and 12 of the IUPAC Periodic Table of Elements or mixtures thereof, whereby the nitrogen- containing Compound is formed; c) optionally separating, subsequent to step b), a portion of between 1 and 99 vol.% off from the reaction mixture, said portion being the recycle stream.

Abstract translation: 制备含氮化合物的方法，包括以下步骤：a）将N 2，任选的NH 3和任选的再循环流与碳 - 和/ 含氢化合物或含碳化合物和H 2形成反应混合物，由此反应混合物中的氨（如果存在）起源于至少30重量％的循环流; b）使反应混合物在200℃至800℃之间的温度下和在10℃至10℃之间的空间速度下与催化剂接触。 /（gh），所述催化剂在载体上含有金属M1，M1选自IUPAC周期表第3,4,5,6,7,8,9,10,11和12族中的金属 的元素或其混合物，由此形成含氮化合物; c）任选地在步骤b）之后分离从反应混合物中的1至99体积％的部分，所述部分是再循环流。

公开(公告)号：WO2012143332A1

公开(公告)日：2012-10-26

申请号：PCT/EP2012/056925

申请日：2012-04-16

Applicant: DSM IP Assets B.V. ,  GROOTHAERT, Marijke Hilde Leen ,  TINGE, Johan Thomas ,  GUIT, Rudolf Philippus Maria

Inventor： GROOTHAERT, Marijke Hilde Leen ,  TINGE, Johan Thomas ,  GUIT, Rudolf Philippus Maria

IPC: C01B21/14

CPC classification number: C01B21/1418 ,  B01J21/08 ,  B01J23/44 ,  B01J23/54

Abstract: Method for preparing hydroxylamine in a continuous process, comprising hydrogenating nitrate in a reaction zone comprising a liquid phase, a gas phase and a heterogeneous hydrogenation catalyst, in which reaction zone hydroxylamine and nitrous oxide (N20) are formed, characterized in that the nitrous oxide concentration in the gas phase, is monitored and is maintained within a pre¬ determined range by means of controlled addition of a promoter for the heterogeneous hydrogenation catalyst and/or controlled addition of further amounts of heterogeneous hydrogenation catalyst to the reaction zone until the total amount of catalyst present reaches a pre-determined upper limit; and then (i) withdrawing a fraction of the heterogeneous hydrogenation catalyst from the reaction zone; and (ii) adding one or more further doses of heterogeneous hydrogenation catalyst until the total amount of catalyst present is at most at said pre-determined upper limit; and (iii) optionally repeating steps (i) and (ii); a method for producing an oxime and a method for producing a lactam comprising said process for producing hydroxylamine.

Abstract translation: 在连续方法中制备羟胺的方法，包括在包含液相，气相和异相氢化催化剂的反应区中使硝酸盐氢化，其中反应区羟胺和一氧化二氮（N 2 O）形成，其特征在于一氧化二氮 监测气相中的浓度，并通过控制加入非均相加氢催化剂的促进剂和/或向反应区域控制加入另外量的非均相氢化催化剂，将其保持在预定范围内，直到总量 的催化剂存在达到预定的上限; 然后（i）从反应区抽出一部分异相氢化催化剂; 和（ii）加入一种或多种另外的非均相氢化催化剂剂量，直到催化剂的总量至多在所述预定的上限值为止; 和（iii）任选地重复步骤（i）和（ii）; 制备肟的方法和制备内酰胺的方法，包括所述羟胺的制备方法。

公开(公告)号：WO2012143330A1

公开(公告)日：2012-10-26

申请号：PCT/EP2012/056923

申请日：2012-04-16

Applicant: DSM IP Assets B.V. ,  GROOTHAERT, Marijke Hilde Leen ,  TINGE, Johan Thomas ,  GUIT, Rudolph Philippus Maria

Inventor： GROOTHAERT, Marijke Hilde Leen ,  TINGE, Johan Thomas ,  GUIT, Rudolph Philippus Maria

IPC: C01B21/14

CPC classification number: C01B21/1418 ,  B01J21/08 ,  B01J23/44 ,  B01J23/54

Abstract: The invention relates to a method for preparing hydroxylamine in a continuous process, comprising feeding nitrate and phosphate in an acidic aqueous liquid into a reaction zone and reducing nitrate with hydrogen thereby forming hydroxylamine, wherein the nitrate concentration in the reaction zone is less than 1.0 mol/kg, as determined in the liquid leaving the reaction zone, wherein the molar ratio of nitrate to phosphate in the reaction zone is 0.5 or less, and wherein the molar ratio of ammonia to nitrate is in the range of from 2.2 to 7; a method for preparing an oxime and a method of preparing a lactam comprising said method for preparing hydroxylamine.

Abstract translation: 本发明涉及一种在连续方法中制备羟胺的方法，包括将酸性含水液体中的硝酸盐和磷酸盐供入反应区，用氢还原硝酸盐，形成羟胺，其中反应区中的硝酸盐浓度小于1.0mol 在离开反应区的液体中测定，其中反应区中硝酸盐与磷酸盐的摩尔比为0.5以下，其中氨与硝酸盐的摩尔比在2.2〜7的范围内; 制备肟的方法和制备含有所述羟胺制备方法的内酰胺的制备方法。

公开(公告)号：WO2009080241A3

公开(公告)日：2009-07-02

申请号：PCT/EP2008/010688

申请日：2008-12-16

Applicant: DSM IP ASSETS B.V. ,  TJIOE, Tjay, Tjien ,  GROOTHAERT, Marijke, Hilde, Leen ,  FELLAY, Céline

Inventor： TJIOE, Tjay, Tjien ,  GROOTHAERT, Marijke, Hilde, Leen ,  FELLAY, Céline

IPC: C07D251/62 ,  B01J8/02

Abstract: The present invention relates to a process for the preparation of melamine, which process comprises at least the following steps: i) feeding methane and ammonia to a pre- reactor which pre- reactor is maintained at a temperature between 700 and 1500 °C whereby a gaseous mixture (i) is formed comprising at least hydrogen cyanide, ii) optionally, purifying mixture (i) thereby forming a mixture (ii) that contains at least gaseous hydrogen cyanide, a. feeding hydrogen cyanide from mixture (i) or (ii) and ammonia, either separately or combined, to a reactor that contains a catalyst and which reactor is maintained at a temperature of 300-500°C, at a space velocity lying between 10 2 and 10 6 ml/(g.hr), whereby a gaseous mixture (a) is formed comprising at least melamine, b. optionally, purifying mixture (a) producing a melamine containing mixture (b), c. separating at least a part of the formed melamine thereby forming a mixture (c) and separated melamine.