公开(公告)号：WO2013083512A1

公开(公告)日：2013-06-13

申请号：PCT/EP2012/074210

申请日：2012-12-03

Applicant: DSM IP ASSETS B.V.

Inventor： TINGE, Johan Thomas ,  VERSCHUREN, Iris ,  DAGUENET, Corinne

IPC: B01J10/00 ,  C07C29/132 ,  C07C31/135 ,  C07C45/33 ,  C07C45/53 ,  C07C49/403

CPC classification number: C07C29/132 ,  C07C45/33 ,  C07C45/53 ,  C07C49/403 ,  C07C31/1355

Abstract: A continuous process for the preparation of a mixture of cyclohexanone and cyclohexanol, said process comprising: a) oxidizing, in an oxidation section, cyclohexane in the presence of an oxygen-containing gas, without a transition metal-containing catalyst to form an oxidized reaction mixture; b) cooling, in a cooling section, the oxidized reaction mixture from a temperature T 1 to a temperature T 3 ; c) decomposing, in a decomposition section, the oxidized reaction mixture to form a decomposed reaction mixture, which decomposed reaction mixture has a temperature T 4 ; and d) removing cyclohexane from the decomposed reaction mixture; characterized in that step b) comprises i) cooling the oxidized reaction mixture from a temperature T 1 to a temperature T 2 by means of an in-process heat exchanger configured to heat the decomposed reaction mixture obtained in step c) from a temperature T 4 to a temperature T 5 ; and ii) cooling the oxidized reaction mixture from a temperature T 2 to a temperature T 3 by means of a cooling unit; and apparatus for carrying out the same.

Abstract translation: 一种用于制备环己酮和环己醇的混合物的连续方法，所述方法包括：a）在氧化段中，在含氧气体的存在下，不含过渡金属的催化剂氧化环己烷，形成氧化反应 混合物; b）在冷却段中将氧化反应混合物从温度T1冷却至温度T3; c）在分解部分中分解氧化反应混合物以形成分解反应混合物，其分解反应混合物具有温度T4; 和d）从分解的反应混合物中除去环己烷; 其特征在于步骤b）包括：i）通过在步骤c）中获得的分解的反应混合物中的温度T 1至温度T 2的温度T 1将氧化反应混合物从温度T1冷却至温度T2 T5; 和ii）借助于冷却单元将氧化的反应混合物从温度T2冷却至温度T3; 以及用于执行该装置的装置。

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：WO2011073233A1

公开(公告)日：2011-06-23

申请号：PCT/EP2010/069707

申请日：2010-12-15

Applicant: DSM IP Assets B.V. ,  PARTON, Rudy Francois Maria Jozef ,  TINGE, Johan Thomas ,  HOEKSEMA, Bert

Inventor： PARTON, Rudy Francois Maria Jozef ,  TINGE, Johan Thomas ,  HOEKSEMA, Bert

IPC: C07C45/00 ,  C07C29/20 ,  C07C49/403 ,  C07C35/08

CPC classification number: C07C29/20 ,  C07C45/006 ,  C07C2601/14 ,  C07C35/08 ,  C07C49/403

Abstract: The invention relates to a method for hydrogenating an aromatic compound. The invention in particular relates to a method for preparing cyclohexanone, cyclohexanol or a mixture thereof in a continuous way by catalytically hydrogenating phenol fed into a reactor comprising a supported hydrogenation catalyst, comprising a dopant selected from the group of alkali metal hydroxides, alkaline earth metal hydroxides, alkaline earth metal oxides, carbonates of alkali metals and carbonates of alkaline earth metals, and in which process during the hydrogenation of phenol continuously or intermittently water is fed into the reactor, the weight to weight ratio of water fed into the reactor to phenol fed into the reactor on average being 0.1 or less.

Abstract translation: 本发明涉及一种使芳族化合物氢化的方法。 本发明特别涉及通过催化氢化进料到包含负载氢化催化剂的反应器的反应器中以连续方式制备环己酮，环己醇或其混合物的方法，该方法包括选自碱金属氢氧化物，碱土金属 氢氧化物，碱土金属氧化物，碱金属的碳酸盐和碱土金属的碳酸盐，并且其中在苯酚氢化期间连续或间歇地将水加入的过程进料到反应器中，将反应器中的水的重量比与苯酚 平均送入反应器的是0.1以下。

公开(公告)号：WO2014102106A1

公开(公告)日：2014-07-03

申请号：PCT/EP2013/077057

申请日：2013-12-18

Applicant: DSM IP ASSETS B.V.

Inventor： TINGE, Johan Thomas ,  OLZHEIM, Daniël Julius Maria

IPC: C07C249/08 ,  C07C249/14

CPC classification number: C07C249/08 ,  C07C249/14 ,  C07C251/44

Abstract: A continuous process for preparing cyclohexanone oxime comprising steps including passing an extracted aqueous phase comprising organic solvent directly from the extraction zone to a water stripping zone; evaporating at least 5 % by weight of the water present in the extracted aqueous phase; passing the water vapour containing stream into a heat exchanger and transferring energy from the water vapour containing stream to an in-process liquid, thereby heating the in-process liquid and condensing at least part of water vapour containing stream.

Abstract translation: 一种用于制备环己酮肟的连续方法，包括以下步骤：将包含有机溶剂的萃取水相直接从萃取区提取到水汽提区; 蒸发提取的水相中存在的水的至少5重量％; 将含水蒸气流送入热交换器并将能量从含水蒸汽流中传送到工艺液体，从而加热过程中的液体并冷凝至少部分含水蒸汽的流。

公开(公告)号：WO2014086676A1

公开(公告)日：2014-06-12

申请号：PCT/EP2013/075087

申请日：2013-11-29

Applicant: DSM IP ASSETS B.V.

Inventor： TINGE, Johan Thomas ,  EKKELENKAMP, Geert ,  DEBEIJ, Johannes Elisabeth Pierre ,  GEERTMAN, Robert ,  YSACKER VAN, Peter

IPC: C01C1/248 ,  B01D9/00 ,  C05C3/00

CPC classification number: C01C1/24 ,  B01D9/0031 ,  B01D9/0036 ,  B01D9/004 ,  B01D9/0059 ,  B01D9/0063 ,  B01D2009/0086 ,  C01C1/248 ,  C05C3/00 ,  C05C3/005

Abstract: The present invention provides a continuous process for producing ammonium sulfate crystals, wherein said process comprises: i)feeding to a series of crystallization sections, which crystallization sections are heat integrated in series, a solution of ammonium sulfate; ii)crystallizing ammonium sulfate crystals from said solution of ammonium sulfate; iii)purging a fraction of the solution of ammonium sulfate from each of said crystallization sections;and iv)discharging ammonium sulfate crystals from each crystallization section, characterized in that: a fraction of said solution of ammonium sulfate is purged from at least one crystallization section to at least one other crystallization section; and an apparatus suitable for producing ammonium sulfate crystals.

Abstract translation: 本发明提供了一种生产硫酸铵晶体的连续方法，其中所述方法包括：i）将一系列结晶部分送入一系列结晶部分，该结晶部分串联加热一体化，形成硫酸铵溶液; ii）从所述硫酸铵溶液中结晶出硫酸铵晶体; iii）从每个所述结晶部分清洗一部分硫酸铵溶液;和iv）从每个结晶部分排出硫酸铵晶体，其特征在于：将所述硫酸铵溶液的一部分从至少一个结晶部分 至少另一个结晶部分; 和适用于生产硫酸铵晶体的装置。

公开(公告)号：WO2014040858A1

公开(公告)日：2014-03-20

申请号：PCT/EP2013/067788

申请日：2013-08-28

Applicant: DSM IP ASSETS B.V.

Inventor： EKKELENKAMP, Geert ,  TINGE, Johan Thomas ,  VONK, Pieter

IPC: C01C1/248 ,  B01D9/00 ,  C05C3/00

CPC classification number: B01D9/0018 ,  B01D9/0031 ,  B01D9/0036 ,  B01D2009/0086 ,  C01C1/24 ,  C01C1/248 ,  C01P2004/60 ,  C05C3/00

Abstract: A continuous process for producing crystalline ammonium sulfate, said process comprising a start-up operation followed by a steady-state operation, wherein the start-up operation comprises: i) in a crystallizer, evaporating solvent from an approximately saturated ammonium sulfate solution; ii) replacing evaporated solvent with further approximately saturated ammonium sulfate solution; iii) introducing to the crystallizer seed crystals of ammonium sulfate; iv) continuing to evaporate solvent, until a desired degree of supersaturation is reached; and v) recovering crystalline ammonium sulfate from ammonium sulfate solution in a recovery unit, and the steady-state operation comprises: vi) continuously feeding approximately saturated ammonium sulfate solution into the crystallizer and continuously withdrawing ammonium sulfate crystals from the crystallizer, such that the total combined volume of ammonium sulfate solution and ammonium sulfate crystals within the crystallizer remains constant; and vii) recovering crystalline ammonium sulfate from ammonium sulfate solution in a recovery unit, characterized in that the degree of supersaturation in the crystallizer during the start-up operation is maintained between 1.2% and the point at which primary nucleation occurs; and apparatus suitable for carrying out the process.

Abstract translation: 一种用于生产结晶硫酸铵的连续方法，所述方法包括启动操作，随后是稳态操作，其中启动操作包括：i）在结晶器中，从大约饱和的硫酸铵溶液蒸发溶剂; ii）用进一步的大约饱和的硫酸铵溶液代替蒸发的溶剂; iii）将结晶器引入硫酸铵晶种; iv）继续蒸发溶剂，直到达到所需的过饱和度; 和v）在回收单元中从硫酸铵溶液中回收结晶硫酸铵，并且稳态操作包括：vi）将大约饱和的硫酸铵溶液连续地进料到结晶器中并连续地从结晶器中取出硫酸铵晶体，使得总计 结晶器中硫酸铵溶液和硫酸铵晶体的组合体积保持不变; 和vii）在回收单元中从硫酸铵溶液中回收结晶硫酸铵，其特征在于，启动操作期间结晶器中的过饱和度保持在1.2％和初始成核出现点之间; 以及适于执行该过程的装置。

公开(公告)号：WO2013083513A1

公开(公告)日：2013-06-13

申请号：PCT/EP2012/074216

申请日：2012-12-03

Applicant: DSM IP ASSETS B.V.

Inventor： TINGE, Johan Thomas ,  DAGUENET, Corinne ,  VERSCHUREN, Iris

IPC: C07C29/132 ,  C07C45/33 ,  C07C45/53 ,  C07C31/135 ,  C07C49/403 ,  B01J10/00

CPC classification number: C07C29/132 ,  C07C45/33 ,  C07C45/53 ,  C07C49/403 ,  C07C31/1355

Abstract: A continuous process for the preparation of a mixture of cyclohexanone and cyclohexanol, said process comprising: a) oxidizing cyclohexane, in an oxidation section, without a transition metal- containing catalyst, in the presence of an oxygen-containing gas to form an oxidized reaction mixture; b) cooling the oxidized reaction mixture, in a cooling section, c) decomposing the oxidized reaction mixture, in a decomposition section, at a temperature below 130 °C in the presence of a transition metal-containing catalyst and an aqueous caustic solution, to form a decomposed reaction mixture; and d) recovering cyclohexane, in a recovery section, from the decomposed reaction mixture; characterized in that b) comprises i) evaporating cyclohexane in one or more fractionation columns operated at a pressure lower than the pressure of the oxidation section, without external heat input, and returning a portion of the cyclohexane so evaporated to the oxidation section; and ii) cooling the reaction mixture in one or more indirect heat exchangers; and apparatus for carrying out the same.

Abstract translation: 一种用于制备环己酮和环己醇的混合物的连续方法，所述方法包括：a）在含氧气体的存在下，在氧化段中氧化环己烷，不含过渡金属的催化剂，以形成氧化反应 混合物; b）在冷却段中冷却氧化的反应混合物，c）在分解部分中，在含过渡金属的催化剂和苛性碱水溶液存在下，在低于130℃的温度下分解氧化的反应混合物， 形成分解的反应混合物; 和d）在回收段中从分解的反应混合物中回收环己烷; 其特征在于b）包括：i）在低于氧化段压力的压力下运行的一个或多个分馏塔中蒸发环己烷，无需外部热量输入，并使一部分环己烷蒸发至氧化段; 和ii）在一个或多个间接热交换器中冷却反应混合物; 以及用于执行该装置的装置。

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：WO2010069870A1

公开(公告)日：2010-06-24

申请号：PCT/EP2009/066919

申请日：2009-12-11

Applicant: DSM IP Assets B.V. ,  DAGUENET, Corinne ,  PARTON, Rudy Francois Maria Jozef ,  TINGE, Johan Thomas

Inventor： DAGUENET, Corinne ,  PARTON, Rudy Francois Maria Jozef ,  TINGE, Johan Thomas

IPC: C07C45/33 ,  C07C49/403 ,  C07C29/50 ,  C07C35/08

CPC classification number: C07C29/50 ,  C07C45/33 ,  C07C2601/14 ,  C07C35/08 ,  C07C49/403

Abstract: The invention is directed to a method for preparing a mixture comprising cyclohexanol and cyclohexanone. In accordance with the invention a mixture comprising cyclohexanol and cyclohexanone is prepared in a molar cyclohexanone/cyclohexanol ratio of at least 1.2 at a cyclohexane conversion of below 5 mol%. The method comprises oxidising cyclohexane in a liquid phase, said oxidising being catalysed by a cobalt compound and a chromium compound, wherein the atomic cobalt to chromium ratio is in the range of 0.05-0.8, wherein the sum of the concentrations of cobalt and chromium is 0.05-0.9 ppm by weight based on the total weight of the reaction mixture, and wherein the cobalt compound and chromium compound are dissolved in the liquid phase.

Abstract translation: 本发明涉及制备包含环己醇和环己酮的混合物的方法。 根据本发明，在环己烷转化率低于5mol％的环己酮/环己醇摩尔比为至少1.2的情况下制备包含环己醇和环己酮的混合物。 该方法包括在液相中氧化环己烷，所述氧化由钴化合物和铬化合物催化，其中原子钴与铬的比例在0.05-0.8的范围内，其中钴和铬的浓度之和为 基于反应混合物的总重量为0.05-0.9重量ppm，其中钴化合物和铬化合物溶解在液相中。