公开(公告)号：WO2009080620A1

公开(公告)日：2009-07-02

申请号：PCT/EP2008/067632

申请日：2008-12-16

Applicant: DSM IP Assets B.V. ,  DORTMONT, VAN, Godefridus Maria ,  HORSELS, Marleen ,  PARTON, Rudy Francois Maria Jozef ,  TINGE, Johan Thomas

Inventor： DORTMONT, VAN, Godefridus Maria ,  HORSELS, Marleen ,  PARTON, Rudy Francois Maria Jozef ,  TINGE, Johan Thomas

IPC: C07C45/82 ,  C07C29/48 ,  C07C45/00 ,  C07C45/29 ,  C07C51/00 ,  B01J10/00 ,  C08F232/00 ,  C07C49/403 ,  C07C55/14 ,  C07C35/08

CPC classification number: C07C29/50 ,  C07C45/006 ,  C07C45/82 ,  C07C51/00 ,  C07C2601/14 ,  C07C49/403 ,  C07C55/14 ,  C07C35/08

Abstract: The present invention relates to a method for continuously preparing cyclohexanone from phenol making use of a catalyst comprising at least one catalytically active metal selected from platinum and palladium comprising hydrogenating phenol to form a product stream comprising cyclohexanone and unreacted phenol; separating at least part of the product stream, or at least part of the product stream from which one or more components having a lower boiling point than cyclohexanone have been removed, into a first fraction comprising cyclohexanone and a second fraction comprising phenol and cyclohexanol, using distillation; separating the second fraction into a third fraction, rich in cyclohexanol, and a fourth fraction, rich in phenol, using distillation; - subjecting at least part of the fourth fraction to a further distillation step, thereby forming a fifth fraction and a sixth fraction, wherein the fifth fraction is enriched in phenol compared to the sixth fraction, and wherein the sixth fraction comprises side-products having a higher boiling point than phenol, and phenol; and which method is characterized in the additional step of continuously or intermittently separating at least part of the sixth fraction to yet a further distillation step, thereby forming a seventh fraction and an eight fraction, wherein the seventh fraction is enriched in phenol compared to the eight fraction, and wherein the eight fraction comprises side-products having a higher boiling point than phenol.

Abstract translation: 本发明涉及使用包含至少一种选自铂和钯的催化活性金属的催化剂从苯酚连续制备环己酮的方法，所述催化活性金属包括氢化苯酚以形成包含环己酮和未反应苯酚的产物流; 将至少部分产物流或至少部分产物流从其中除去一个或多个沸点低于环己酮的组分的产物流转化成包含环己酮的第一馏分和包含苯酚和环己醇的第二馏分，使用 蒸馏; 将第二馏分分离成富含环己醇的第三馏分和富含苯酚的第四馏分，使用蒸馏; 将至少部分第四馏分进行进一步的蒸馏步骤，从而形成第五馏分和第六馏分，其中与第六馏分相比，第五馏分富含苯酚，其中第六馏分包含具有 沸点高于苯酚，苯酚; 并且该方法的特征在于连续或间歇地将至少部分第六馏分分离成另外的蒸馏步骤，从而形成第七馏分和八馏分的附加步骤，其中第七馏分富含苯酚，与八 馏分，其中八馏分包含沸点高于苯酚的副产物。

公开(公告)号：EP2897903A1

公开(公告)日：2015-07-29

申请号：EP13762810.3

申请日：2013-09-12

Applicant: DSM IP Assets B.V.

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

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

CPC classification number: C01C1/248 ,  B01D9/0031 ,  B01D9/0036 ,  B01D9/0063 ,  C01C1/24 ,  C05C3/005

Abstract: The invention relates to a process for preparing a crystalline ammonium sulfate product, which process comprises: a) subjecting in a crystallizer a feed solution of ammonium sulfate to crystallization to form a first slurry of ammonium sulfate crystals; b) subjecting the first slurry of ammonium sulfate crystals to a first size classification to yield a first coarse ammonium sulfate crystal fraction and a first fine ammonium sulfate crystal fraction; c) recycling at least part of the first fine ammonium sulfate crystal fraction to the feed solution of ammonium sulfate; and d) recovering a crystalline ammonium sulfate product from the first coarse ammonium sulfate crystal fraction, characterized in that: e) a second size classification is carried out on a second slurry of ammonium sulfate crystals to yield a second coarse ammonium sulfate crystal fraction and a second fine ammonium sulfate crystal fraction.

Abstract translation: 本发明涉及一种制备结晶硫酸铵产物的方法，该方法包括：a）在结晶器中使硫酸铵的进料溶液结晶以形成硫酸铵晶体的第一浆料; b）使硫酸铵晶体的第一浆料进行第一粒度分级以产生第一粗硫酸铵晶体级分和第一细小硫酸铵晶体级分; c）将至少部分第一细小硫酸铵结晶部分再循环到硫酸铵的进料溶液中; 和d）从所述第一粗硫酸铵晶体级分回收结晶硫酸铵产物，其特征在于：e）在硫酸铵晶体的第二浆料上进行二次分级，得到第二粗硫酸铵晶体级分和 第二细小的硫酸铵结晶部分。

公开(公告)号：EP2513050A2

公开(公告)日：2012-10-24

申请号：EP10795353.1

申请日：2010-12-17

Applicant: DSM IP Assets B.V.

Inventor： AVRAMESCU, Maria Elena ,  TINGE, Johan Thomas

IPC: C07D201/16

CPC classification number: C07D223/10 ,  C07D201/16

Abstract: The invention relates to a process for treating an aqueous solution containing ε-caprolactam, ammonium sulphate and one or more other impurities, comprising one or more organic impurities from a caprolactam production process and optionally other salts than ammonium sulphate, by means of a membrane process, thereby obtaining a retentate and a permeate, in which process the membrane used is selected from the group of polyether sulphone membranes, sulphonated polyether sulphone membranes, polyester membranes, polysulphone membranes, aromatic polyamide membranes, polyvinyl alcohol membranes, polypiperazine membranes, cellulose acetate membranes, titanium oxide membranes, zirconium oxide membranes and aluminium oxide membranes, having a molecular weight cut off in the range of 100-1000 g/mol; and wherein more than 60 wt.% of the caprolactam in the aqueous solution is passed through a membrane to the permeate side, to obtain a purified caprolactam containing permeate stream, and wherein at least 50 wt.% of the organic impurities are retained in the retentate solution.

Abstract translation: 本发明涉及一种处理含ε-己内酰胺，硫酸铵和一种或多种其它杂质的水溶液的方法，所述水溶液包含来自己内酰胺生产工艺的一种或多种有机杂质和任选的非硫酸铵以外的其它盐，借助膜工艺 从而获得渗余物和渗透物，其中使用的膜选自聚醚砜膜，磺化聚醚砜膜，聚酯膜，聚砜膜，芳族聚酰胺膜，聚乙烯醇膜，聚哌嗪膜，醋酸纤维素膜 ，氧化钛膜，氧化锆膜和氧化铝膜，其分子量在100-1000g / mol的范围内截断; 并且其中超过60重量％的所述水溶液中的己内酰胺通过膜到达渗透侧，以获得纯化的含有己内酰胺的渗透物流，并且其中至少50重量％的有机杂质保留在 滞留物解决方案。

公开(公告)号：EP2234952A1

公开(公告)日：2010-10-06

申请号：EP08864701.1

申请日：2008-12-16

Applicant: DSM IP Assets B.V.

Inventor： HORSELS, Marleen ,  PARTON, Rudy Francois Maria Jozef ,  TINGE, Johan Thomas

IPC: C07C45/82 ,  C07C49/403 ,  B01J10/00 ,  C07C29/48 ,  C07C45/00 ,  C07C45/29 ,  C07C51/00 ,  C07C55/14 ,  C07C35/08 ,  C08F232/00

CPC classification number: C07C29/50 ,  C07C45/006 ,  C07C45/82 ,  C07C51/00 ,  C07C2601/14 ,  C07C49/403 ,  C07C55/14 ,  C07C35/08

Abstract: The present invention relates to a method for continuously preparing cyclohexanone from phenol making use of a catalyst comprising at least one catalytically active metal selected from platinum and palladium comprising a) hydrogenating phenol to form a product stream comprising cyclohexanone and unreacted phenol; b) separating at least part of the product stream, or at least part of the product stream from which one or more components having a lower boiling point than cyclohexanone have been removed, into a first fraction comprising cyclohexanone and a second fraction comprising phenol and cyclohexanol, using distillation; c) separating the second fraction into a third fraction, rich in cyclohexanol, and a fourth fraction, rich in phenol and, using distillation; d) subjecting at least part of the fourth fraction to a further distillation step, thereby forming a fifth fraction and a sixth fraction, wherein the fifth fraction is enriched in phenol compared to the sixth fraction, and wherein the sixth fraction comprises side-products having a higher boiling point than phenol, and phenol, wherein step d) is carried out in a vacuum distillation column equipped with trays in the lower part of the column, and wherein in the upper part of the column, i.e. in the part above the feed inlet, packing material is present instead of trays in at least part of said upper part, which packing material has a comparable or improved separating efficiency, and provides a reduction of the pressure drop by at least 30%, preferably more than 50%, as compared to the case with trays in the upper part, under otherwise similar distillation conditions.

Abstract translation: 从苯酚连续制备环己酮的方法使用具有至少一种选自铂和钯的催化活性金属的催化剂。 该方法包括与后续馏分相比富集蒸馏馏分中的苯酚，其中后续馏分包括苯酚和沸点高于苯酚的副产物。 蒸馏在塔底部装有塔板的真空蒸馏塔中进行。 在塔的上部，即在进料入口上方的部分，在其至少一部分中存在填料材料代替塔盘。 包装材料具有相当或改进的分离效率，并且与其他类似的蒸馏条件下的上部塔板的情况相比，压降降低至少30％，优选大于50％。

公开(公告)号：EP2231577A1

公开(公告)日：2010-09-29

申请号：EP08863517.2

申请日：2008-12-16

Applicant: DSM IP Assets B.V.

Inventor： DORTMONT, VAN, Godefridus Maria ,  HORSELS, Marleen ,  PARTON, Rudy Francois Maria Jozef ,  TINGE, Johan Thomas

IPC: C07C45/82 ,  C07C29/48 ,  C07C45/00 ,  C07C45/29 ,  C07C51/00 ,  B01J10/00 ,  C08F232/00 ,  C07C49/403 ,  C07C55/14 ,  C07C35/08

CPC classification number: C07C29/50 ,  C07C45/006 ,  C07C45/82 ,  C07C51/00 ,  C07C2601/14 ,  C07C49/403 ,  C07C55/14 ,  C07C35/08

Abstract: The present invention relates to a method for continuously preparing cyclohexanone from phenol making use of a catalyst comprising at least one catalytically active metal selected from platinum and palladium comprising hydrogenating phenol to form a product stream comprising cyclohexanone and unreacted phenol; separating at least part of the product stream, or at least part of the product stream from which one or more components having a lower boiling point than cyclohexanone have been removed, into a first fraction comprising cyclohexanone and a second fraction comprising phenol and cyclohexanol, using distillation; separating the second fraction into a third fraction, rich in cyclohexanol, and a fourth fraction, rich in phenol, using distillation; - subjecting at least part of the fourth fraction to a further distillation step, thereby forming a fifth fraction and a sixth fraction, wherein the fifth fraction is enriched in phenol compared to the sixth fraction, and wherein the sixth fraction comprises side-products having a higher boiling point than phenol, and phenol; and which method is characterized in the additional step of continuously or intermittently separating at least part of the sixth fraction to yet a further distillation step, thereby forming a seventh fraction and an eight fraction, wherein the seventh fraction is enriched in phenol compared to the eight fraction, and wherein the eight fraction comprises side-products having a higher boiling point than phenol.

Abstract translation: 本发明涉及一种使用包含至少一种选自铂和钯的催化活性金属的催化剂从苯酚连续制备环己酮的方法，其包括氢化苯酚以形成包含环己酮和未反应苯酚的产物流; 将至少部分产物流或至少部分产物流从其中除去一个或多个沸点低于环己酮的组分的产物流转化成包含环己酮的第一馏分和包含苯酚和环己醇的第二馏分，使用 蒸馏; 将第二级分分离成富含环己醇的第三级分，和使用蒸馏富含苯酚的第四级分; - 将第四部分的至少一部分喷射至另一蒸馏步骤，从而形成第五馏分和第六馏分，其中与第六馏分相比，第五馏分富含苯酚，其中第六馏分包含具有 沸点高于苯酚，苯酚; 并且该方法的特征在于将第六馏分的至少一部分连续或间歇地分离成另外的蒸馏步骤的另外步骤，从而形成第七馏分和八馏分，其中第七馏分富含苯酚，与八 馏分，其中八馏分包含沸点高于苯酚的副产物。

公开(公告)号：EP2513025A1

公开(公告)日：2012-10-24

申请号：EP10793225.3

申请日：2010-12-15

Applicant: DSM IP Assets B.V.

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，将反应器中加入反应器的水的重量比与苯酚 进料至反应器平均为0.1或更小。

公开(公告)号：EP2928828A1

公开(公告)日：2015-10-14

申请号：EP13799026.3

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.

公开(公告)号：EP2895426A1

公开(公告)日：2015-07-22

申请号：EP13758793.7

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 crystal-line 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 proximately 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: 一种用于生产结晶线硫酸铵的连续方法，所述方法包括启动操作，然后进行稳态操作，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）用进一步的近似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）连续将约饱和的硫酸铵溶液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总体积保持恒定; 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，在启动操作期间结晶器中的过饱和度保持在1.2％和发生初始成核的点之间; 以及适于执行该过程的装置。

公开(公告)号：EP2231577B1

公开(公告)日：2012-02-08

申请号：EP08863517.2

申请日：2008-12-16

Applicant: DSM IP Assets B.V.

Inventor： DORTMONT, VAN, Godefridus Maria ,  HORSELS, Marleen ,  PARTON, Rudy Francois Maria Jozef ,  TINGE, Johan Thomas

IPC: C07C45/82 ,  C07C29/48 ,  C07C45/00 ,  C07C45/29 ,  C07C51/00 ,  B01J10/00 ,  C08F232/00 ,  C07C49/403 ,  C07C55/14 ,  C07C35/08

CPC classification number: C07C29/50 ,  C07C45/006 ,  C07C45/82 ,  C07C51/00 ,  C07C2601/14 ,  C07C49/403 ,  C07C55/14 ,  C07C35/08

Abstract: The present invention relates to a method for continuously preparing cyclohexanone from phenol making use of a catalyst comprising at least one catalytically active metal selected from platinum and palladium comprising hydrogenating phenol to form a product stream comprising cyclohexanone and unreacted phenol; separating at least part of the product stream, or at least part of the product stream from which one or more components having a lower boiling point than cyclohexanone have been removed, into a first fraction comprising cyclohexanone and a second fraction comprising phenol and cyclohexanol, using distillation; separating the second fraction into a third fraction, rich in cyclohexanol, and a fourth fraction, rich in phenol, using distillation; - subjecting at least part of the fourth fraction to a further distillation step, thereby forming a fifth fraction and a sixth fraction, wherein the fifth fraction is enriched in phenol compared to the sixth fraction, and wherein the sixth fraction comprises side-products having a higher boiling point than phenol, and phenol; and which method is characterized in the additional step of continuously or intermittently separating at least part of the sixth fraction to yet a further distillation step, thereby forming a seventh fraction and an eight fraction, wherein the seventh fraction is enriched in phenol compared to the eight fraction, and wherein the eight fraction comprises side-products having a higher boiling point than phenol.