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1. 发明申请

WO2011073400A3 CAPROLACTAM RECOVERY WITH MEMBRANE TREATMENT 审中-公开
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
申请人： DSM IP ASSETS B.V. , AVRAMESCU, Maria Elena , TINGE, Johan Thomas
发明人： AVRAMESCU, Maria Elena , TINGE, Johan Thomas
IPC分类号： C07D201/16
摘要： 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.

2. 发明申请

WO2009080621A1 CYCLOHEXANONE PRODUCTION PROCESS WITH MODIFIED POST-DISTILLATION 审中-公开
标题翻译：具有改性后蒸馏的环辛砜生产工艺
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
申请人： DSM IP ASSETS B.V. , HORSELS, Marleen , PARTON, Rudy Francois Maria Jozef , TINGE, Johan Thomas
发明人： HORSELS, Marleen , PARTON, Rudy Francois Maria Jozef , TINGE, Johan Thomas
IPC分类号： C07C45/82 , C07C49/403 , B01J10/00 , C07C29/48 , C07C45/00 , C07C45/29 , C07C51/00 , C07C55/14 , C07C35/08 , C08F232/00
CPC分类号： C07C29/50 , C07C45/006 , C07C45/82 , C07C51/00 , C07C2601/14 , C07C49/403 , C07C55/14 , C07C35/08
摘要： 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.
摘要翻译：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。

3. 发明申请

WO2012143331A1 CATALYZED HYDROXYLAMINE PREPARATION 审中-公开
标题翻译：催化羟基胺制备
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
申请人： DSM IP ASSETS B.V. , GROOTHAERT, Marijke Hilde Leen , TINGE, Johan Thomas , GUIT, Rudolf Philippus Maria
发明人： GROOTHAERT, Marijke Hilde Leen , TINGE, Johan Thomas
IPC分类号： C01B21/14
CPC分类号： C07C249/08 , C01B21/1418 , C07C2601/14 , C07C2601/20 , C07D201/04 , C07D211/76 , C07D227/087 , C07C251/44
摘要： 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.
摘要翻译：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。

4. 发明申请

WO2010069870A1 CATALYSED CYCLOHEXANE OXIDATION 审中-公开
标题翻译：催化环己烷氧化
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
申请人： DSM IP Assets B.V. , DAGUENET, Corinne , PARTON, Rudy Francois Maria Jozef , TINGE, Johan Thomas
发明人： DAGUENET, Corinne , PARTON, Rudy Francois Maria Jozef , TINGE, Johan Thomas
IPC分类号： C07C45/33 , C07C49/403 , C07C29/50 , C07C35/08
CPC分类号： C07C29/50 , C07C45/33 , C07C2601/14 , C07C35/08 , C07C49/403
摘要： 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.
摘要翻译：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。

5. 发明申请

WO2009080620A1 CYCLOHEXANONE PRODUCTION PROCESS WITH MULTIPLE POST-DISTILLATION 审中-公开
标题翻译：具有多次后蒸馏的环辛砜生产工艺
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
申请人： DSM IP Assets B.V. , DORTMONT, VAN, Godefridus Maria , HORSELS, Marleen , PARTON, Rudy Francois Maria Jozef , TINGE, Johan Thomas
发明人： DORTMONT, VAN, Godefridus Maria , HORSELS, Marleen , PARTON, Rudy Francois Maria Jozef , TINGE, Johan Thomas
IPC分类号： C07C45/82 , C07C29/48 , C07C45/00 , C07C45/29 , C07C51/00 , B01J10/00 , C08F232/00 , C07C49/403 , C07C55/14 , C07C35/08
CPC分类号： C07C29/50 , C07C45/006 , C07C45/82 , C07C51/00 , C07C2601/14 , C07C49/403 , C07C55/14 , C07C35/08
摘要： 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.
摘要翻译：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。

6. 发明申请

WO2012143332A1 CATALYZED HYDROXYLAMINE PREPARATION 审中-公开
标题翻译：催化羟基胺的制备
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
申请人： DSM IP Assets B.V. , GROOTHAERT, Marijke Hilde Leen , TINGE, Johan Thomas , GUIT, Rudolf Philippus Maria
发明人： GROOTHAERT, Marijke Hilde Leen , TINGE, Johan Thomas , GUIT, Rudolf Philippus Maria
IPC分类号： C01B21/14
CPC分类号： C01B21/1418 , B01J21/08 , B01J23/44 , B01J23/54
摘要： 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.
摘要翻译：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。

7. 发明申请

WO2012143330A1 METHOD FOR PREPARING HYDROXYLAMINE 审中-公开
标题翻译：制备羟基胺的方法
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
申请人： DSM IP Assets B.V. , GROOTHAERT, Marijke Hilde Leen , TINGE, Johan Thomas , GUIT, Rudolph Philippus Maria
发明人： GROOTHAERT, Marijke Hilde Leen , TINGE, Johan Thomas , GUIT, Rudolph Philippus Maria
IPC分类号： C01B21/14
CPC分类号： C01B21/1418 , B01J21/08 , B01J23/44 , B01J23/54
摘要： 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.
摘要翻译：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。

8. 发明申请

WO2011073233A1 CATALYSED PHENOL HYDROGENATION 审中-公开
标题翻译：催化酚氢化
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
申请人： DSM IP Assets B.V. , PARTON, Rudy Francois Maria Jozef , TINGE, Johan Thomas , HOEKSEMA, Bert
发明人： PARTON, Rudy Francois Maria Jozef , TINGE, Johan Thomas , HOEKSEMA, Bert
IPC分类号： C07C45/00 , C07C29/20 , C07C49/403 , C07C35/08
CPC分类号： C07C29/20 , C07C45/006 , C07C2601/14 , C07C35/08 , C07C49/403
摘要： 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.
摘要翻译：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。

9. 发明申请

WO2015010885A1 CONTINUOUS PROCESS FOR RECOVERY OF CAPROLACTAM AND CRYSTALLINE AMMONIUM SULFATE 审中-公开
标题翻译：蓖麻油和硫酸亚铁的回收连续工艺
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
申请人： DSM IP ASSETS B.V.
发明人： CUIPER, Anna Dite , KNAAP, VAN DER, Theodorus Albertus , TINGE, Johan Thomas
IPC分类号： C07D223/10 , C07D201/04
CPC分类号： C07D223/10 , C07D201/04
摘要： 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.
摘要翻译：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。

10. 发明申请

WO2014044593A1 PROCESS FOR PREPARING CRYSTALLINE AMMONIUM SULFATE PRODUCT 审中-公开
标题翻译：制备硫酸亚铁铵产品的方法
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
申请人： DSM IP ASSETS B.V.
发明人： TINGE, Johan Thomas , EKKELENKAMP, Geert , VONK, Pieter
IPC分类号： C01C1/248 , B01D9/00 , C05C3/00
CPC分类号： C01C1/248 , B01D9/0031 , B01D9/0036 , B01D9/0063 , C01C1/24 , C05C3/005
摘要： 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.
摘要翻译：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。

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