公开(公告)号：WO2015010885A1

公开(公告)日：2015-01-29

申请号：PCT/EP2014/064517

申请日：2014-07-08

Applicant: DSM IP ASSETS B.V.

Inventor： CUIPER, Anna Dite ,  KNAAP, VAN DER, Theodorus Albertus ,  TINGE, Johan Thomas

IPC: C07D223/10 ,  C07D201/04

CPC classification number: C07D223/10 ,  C07D201/04

Abstract: Present application discloses an industrial scale continuous process for recovery of caprolactam and crystalline ammonium sulfate. By controlling the weight ratio of the amount of aqueous ammonium sulfate solution being recycled to the amount of Beckmann rearrangement mixture charged into the neutralization section within the range of more than 0.001 and less than 1, the productivity of the crystalline ammonium sulfate is increased, however neither the color of the crystalline ammonium sulfate nor the quality of the produced pure caprolactam is unduly influenced.

Abstract translation: 本申请公开了用于回收己内酰胺和结晶硫酸铵的工业规模的连续方法。 通过将循环的硫酸铵水溶液的量的重量控制在大于0.001且小于1的范围内装入中和部分的贝克曼重排混合物的量，结晶硫酸铵的生产率增加 结晶硫酸铵的颜色和生产的纯己内酰胺的质量都不会受到不适当的影响。

公开(公告)号：WO2014044593A1

公开(公告)日：2014-03-27

申请号：PCT/EP2013/068920

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尺寸分级，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：WO2016075047A1

公开(公告)日：2016-05-19

申请号：PCT/EP2015/075951

申请日：2015-11-06

Applicant: CAP III B.V. ,  DSM IP ASSETS B.V.

Inventor： TINGE, Johan Thomas ,  DAGUENET, Corinne ,  VERSCHUREN, Iris ,  MARTENS, Wilhelmus Rudolf Maria ,  BRANDS, Roeland Wilhelmus Theodorus Maria ,  KORTE, DE, Robert Jan

IPC: C07C29/20 ,  C07C29/80 ,  C07C45/00 ,  C07C45/82 ,  C07C49/403 ,  C07C35/08

CPC classification number: C07C29/20 ,  C07C29/80 ,  C07C45/002 ,  C07C45/006 ,  C07C45/82 ,  C07C2601/14 ,  C07C49/403 ,  C07C35/08

Abstract: An industrial scale continuous process for the production and recovery of cyclohexanone from phenol and hydrogen, said process comprising: hydrogenating phenol in a phenol hydrogenation reactor; separating cyclohexanone from a hydrogenated product stream in a separation and purification section [II] comprising at least 4 distillation sections; wherein at least some of the reaction heat produced in the phenol hydrogenation reaction section [I] is applied for the production of steam; and wherein the molar ratio of cyclohexanone to phenol that is charged to said phenol hydrogenation reactor is from 0.02 to 0.10; and/or wherein the molar ratio of cyclohexanol to phenol that is charged to said phenol hydrogenation reactor is from 0.001 to 0.10.

Abstract translation: 一种用于从苯酚和氢气生产和回收环己酮的工业规模的连续方法，所述方法包括：在苯酚氢化反应器中氢化苯酚; 在包含至少4个蒸馏段的分离和纯化部分[II]中将氢化产物流中的环己酮分离; 其中在苯酚氢化反应段[I]中产生的反应热中的至少一部分被用于生产蒸汽; 并且其中装入所述苯酚氢化反应器中的环己酮与苯酚的摩尔比为0.02至0.10; 和/或其中装入所述苯酚氢化反应器中的环己醇与苯酚的摩尔比为0.001至0.10。

公开(公告)号：WO2015010928A1

公开(公告)日：2015-01-29

申请号：PCT/EP2014/064937

申请日：2014-07-11

Applicant: DSM IP ASSETS B.V.

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

IPC: C07C45/33 ,  C07C45/53 ,  C07C45/80

CPC classification number: C07C29/50 ,  C07C29/132 ,  C07C35/08

Abstract: A continuous process for the production of purified cyclohexanone which comprises at least the following steps: oxidation of cyclohexane; decomposition of cyclohexyl hydroperoxide; separation of an organic phase and aqueous phase; removal of cyclohexane from the organic phase; removal of alkali metal salts by washing with water; distillation and recovery of cyclohexanonewherein any residue obtained after washing contains less than 10 ppm alkali metal salts.

Abstract translation: 用于生产纯化的环己酮的连续方法，其包括至少以下步骤：环己烷的氧化; 环己基氢过氧化物的分解; 分离有机相和水相; 从有机相中除去环己烷; 通过用水洗涤去除碱金属盐; 在洗涤后获得的任何残留物中，环己酮水合物的蒸馏和回收均含有少于10ppm的碱金属盐。

公开(公告)号：WO2011073400A3

公开(公告)日：2011-06-23

申请号：PCT/EP2010/070097

申请日：2010-12-17

Applicant: DSM IP ASSETS B.V. ,  AVRAMESCU, Maria Elena ,  TINGE, Johan Thomas

Inventor： AVRAMESCU, Maria Elena ,  TINGE, Johan Thomas

IPC: 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.

公开(公告)号：WO2014206869A1

公开(公告)日：2014-12-31

申请号：PCT/EP2014/062987

申请日：2014-06-20

Applicant: DSM IP ASSETS B.V.

Inventor： TINGE, Johan Thomas ,  EKKELENKAMP, Geert ,  GEERTMAN, Robert

IPC: C01C1/24 ,  C01C1/248 ,  B01D9/00 ,  C07D201/16 ,  C07C249/14

CPC classification number: C01C1/24 ,  B01D9/0022 ,  B01D9/0031 ,  B01D9/004 ,  B01D9/0063 ,  B01D2009/0086 ,  C01C1/248 ,  C07C249/08 ,  C07C2601/14 ,  C07D201/04 ,  C07D201/16 ,  C07C251/44

Abstract: The present invention provides a continuous process for producing ammonium sulfate crystals, wherein said process comprises: (a) feeding to a first group of crystallization sections, which crystallization sections are heat integrated in series, a first aqueous ammonium sulfate solution that contains one or more impurities; (b) feeding to a second group of crystallization sections, which crystallization sections are heat integrated in series, a second aqueous ammonium sulfate solution that contains one or more impurities; (c) crystallizing ammonium sulfate crystals in each crystallization section respectively from each of said solutions of ammonium sulfate that contain one or more impurities; (d) purging a fraction of the ammonium sulfate solution that contains one or more impurities from each of said crystallization sections; and (e) discharging ammonium sulfate crystals from each crystallization section, characterized in that: (i) both the first group of crystallization sections and the second group of crystallization sections are together heat integrated in one series of crystallization sections; wherein the first group of crystallization sections operates at higher temperature than the second group of crystallization sections; and (ii) the composition of the first aqueous ammonium sulfate solution that contains one or more impurities is different to the composition of the second aqueous ammonium sulfate solution that contains one or more impurities. Further provided is apparatus suitable for producing ammonium sulfate crystal.

Abstract translation: 本发明提供了一种用于生产硫酸铵晶体的连续方法，其中所述方法包括：（a）将第一组结晶部分进料到该第一组结晶部分，该结晶部分串联加热一体化，含有一种或多种的第一硫酸铵水溶液 杂质; （b）将第二组结晶部分进料到该第二组结晶部分，该结晶部分串联加热一体化，含有一种或多种杂质的第二硫酸铵溶液; （c）分别从含有一种或多种杂质的所述硫酸铵溶液中分别在每个结晶段中结晶硫酸铵晶体; （d）从每个所述结晶部分清洗含有一种或多种杂质的硫酸铵溶液的一部分; 和（e）从每个结晶部分排出硫酸铵晶体，其特征在于：（i）第一组结晶部分和第二组结晶部分一起热集成在一系列结晶部分中; 其中所述第一组结晶段在比所述第二组结晶段更高的温度下操作; 和（ii）含有一种或多种杂质的第一硫酸铵水溶液的组成与含有一种或多种杂质的第二硫酸铵水溶液的组成不同。 还提供了适用于生产硫酸铵晶体的装置。

公开(公告)号：WO2014206862A1

公开(公告)日：2014-12-31

申请号：PCT/EP2014/062969

申请日：2014-06-19

Applicant: DSM IP ASSETS B.V.

Inventor： ROOS, Peter ,  RIESTHUIS, Theodorus Friederich Maria ,  TINGE, Johan Thomas ,  LUIJK VAN, Cornelis Marinus

IPC: C01C1/24 ,  C07D201/16

CPC classification number: C01C1/24 ,  C07D201/16

Abstract: The present invention provides a continuous process for the production of ammonium sulfate in combination with caprolactam, said process comprising, a) neutralizing with ammonia a mixture comprising caprolactam and sulfuric acid to form an aqueous ammonium sulfate phase and an aqueous crude caprolactam phase; b) separating the aqueous ammonium sulfate phase from the aqueous crude caprolactam phase; c) extracting into an organic solvent caprolactam present in the aqueous ammonium sulfate phase to form a caprolactam-containing organic phase and a purified aqueous ammonium sulfate phase; d) stripping organic solvent from the purified aqueous ammonium sulfate phase; and e) withdrawing organic solvent-containing gas produced in, or subsequent to, any one of steps c) and d), characterized in that f) organic solvent is recovered from said organic solvent-containing gas.

Abstract translation: 本发明提供了与己内酰胺组合生产硫酸铵的连续方法，所述方法包括：a）用氨中和含己内酰胺和硫酸的混合物以形成硫酸铵水相和含水的己内酰胺相; b）从含水的己内酰胺相中分离出硫酸铵水相; c）提取存在于硫酸铵水溶液相中的有机溶剂己内酰胺以形成含己内酰胺的有机相和纯化的硫酸铵水相; d）从纯化的硫酸铵水相中汽提有机溶剂; 和e）取出在步骤c）和d）中的任何一个中或之后产生的含有机溶剂的气体，其特征在于f）从所述含有机溶剂的气体中回收有机溶剂。

公开(公告)号：WO2013098174A1

公开(公告)日：2013-07-04

申请号：PCT/EP2012/076289

申请日：2012-12-20

Applicant: DSM IP ASSETS B.V.

Inventor： TINGE, Johan Thomas ,  GUIT, Rudolf Philippus Maria ,  RIESTHUIS, Theodorus Friederich Maria

IPC: C01B21/14 ,  B01J19/02

CPC classification number: C01B21/1418 ,  B01J19/02 ,  B01J2219/0286

Abstract: A method for preparing hydroxylammonium in a reaction zone in a continuous process, comprising optionally directly introducing nitric acid comprising

Abstract translation: 一种在连续方法中在反应区中制备羟基铵的方法，包括任选地将包含<0.1ppm Mo的硝酸直接引入反应区; 其中引入的硝酸被输送，储存，转移到容器和包含钢的管道中; 其中反应在容器和连接管的壁包括钢的容器中进行; 其中所述钢包含0至0.08重量％的C和0至0.03重量％的Mo。

公开(公告)号：WO2009080621A1

公开(公告)日：2009-07-02

申请号：PCT/EP2008/067635

申请日：2008-12-16

Applicant: DSM IP ASSETS B.V. ,  HORSELS, Marleen ,  PARTON, Rudy Francois Maria Jozef ,  TINGE, Johan Thomas

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: 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，其包括：a）氢化苯酚以形成包含环己酮和未反应苯酚的产物流; b）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; c）将第二级分分离成富含环己醇的第三馏分和富含苯酚的第四级分，并使用蒸馏; d）使至少部分第四馏分进一步蒸馏步骤，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 比苯酚高的沸点和苯酚，其中步骤d）在柱的下部配备有塔板的真空蒸馏塔中进行，并且其中在塔的上部，即在进料的上方的部分 入口，包装材料代替所述上部的至少一部分中的托盘，该填充材料具有相当或改进的分离效率，并且将压降降低至少30％，优选大于50％，如 与上部托盘的情况相比，在相似的蒸馏条件下。

公开(公告)号：WO2013164371A1

公开(公告)日：2013-11-07

申请号：PCT/EP2013/059067

申请日：2013-05-01

Applicant: DSM IP ASSETS B.V.

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

IPC: C07C249/14

CPC classification number: C07C249/14

Abstract: A continuous process for purifying organic product solution comprising oxime dissolved in an organic medium comprising: (1) discharging the organic product solution from a oxime synthesis section [I] to a liquid-liquid mixing section [III]; (2) mixing the organic product solution with a water and/ or an aqueous solution and discharging the resulting mixture to liquid-liquidseparator [IV]; (3) separating organic top layer from aqueous bottom layer in liquid-liquidseparator [IV] and recovering oxime from the organic top layer in an oxime recovery section; (4) feeding the aqueous bottom layer of liquid-liquidseparator [IV] to the oxime synthesis section [I], optionally a fraction of which being fed back into the liquid- liquid mixing section [III].

Abstract translation: 一种用于纯化含有溶解于有机介质中的肟的有机产物溶液的连续方法，包括：（1）将有机产物溶液从肟合成段[I]排出至液 - 液混合段[III]; （2）将有机产物溶液与水和/或水溶液混合并将所得混合物排出至液体分离器[IV]; （3）在液液分离器[IV]中分离有机顶层与水底层，并在肟回收段中从有机顶层回收肟; （4）将液液分离器[IV]的底部底层进料到肟合成部分[I]，任选地其一部分被反馈到液 - 液混合部分[III]中。