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公开(公告)号：US10369493B2
公开(公告)日：2019-08-06
申请号：US14424639
申请日：2013-08-28
申请人： CAP III B.V.
摘要： 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 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.
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公开(公告)号：US20180290955A1
公开(公告)日：2018-10-11
申请号：US15525448
申请日：2015-11-06
申请人： CAP III B.V.
发明人： Johan Thomas Tinge , Corinne Daguenet , Iris Verschuren , Wilhelmus Rudolf Maria Martens , Roeland Wilhelmus Theodorus Maria Brands , Robert Jan de Korte
CPC分类号： C07C45/006 , C07C29/20 , C07C29/80 , C07C45/002 , C07C45/82 , C07C2601/14 , C07C49/403 , C07C35/08
摘要： 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.
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公开(公告)号：US10130895B2
公开(公告)日：2018-11-20
申请号：US15535795
申请日：2015-12-15
申请人： CAP III B.V.
IPC分类号： B01D3/00 , C07C45/82 , B01D3/12 , B01D3/10 , B01D3/14 , C07C27/28 , C07C35/08 , C07C45/00 , C07C49/403
摘要： A process for the construction of a second chemical plant, which second chemical plant is suitable for the separation of cyclohexanone from a second mixture, which second mixture comprises reaction products from the hydrogenation of phenol. The process comprises providing a first chemical plant, which first chemical plant is suitable for the separation of cyclohexanone from a first mixture, and a second chemical plant comprising a distillation column suitable for distilling overhead cyclohexanone reused from the first chemical plant.
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4.发明授权Process for the production of a mixture comprising cyclohexanone and cyclohexanol from phenol 有权从苯酚生产包含环己酮和环己醇的混合物的方法公开(公告)号：US09388107B2
公开(公告)日：2016-07-12
申请号：US14408614
申请日：2013-06-27
申请人： CAP III B.V.
发明人： Wilhelmus Rudolf Maria Martens , Robert Jan De Korte , Iris Verschuren , Corinne Daguenet , Johan Thomas Tinge , Roeland Wilhelmus Theodorus Maria Brands
IPC分类号： C07C45/00 , C07C29/00 , C07C51/00 , C07C29/20 , C07C35/08 , C07C49/603 , C07D223/10
CPC分类号： C07C45/006 , C07C29/20 , C07C35/08 , C07C49/603 , C07C51/00 , C07C2601/14 , C07D223/10 , C07C49/403
摘要： The present invention provides a process for continuously preparing a mixture of cyclohexanone and cyclohexanol comprising, a) hydrogenating phenol with gaseous hydrogen, in the presence of platinum or palladium, in a hydrogenation reactor, to produce a hydrogenation product stream comprising cyclohexanone, cyclohexanol, phenol and hydrogen; b) cooling the hydrogenation product stream to a temperature such that the fraction of phenol by mass in a first gas phase is lower than the fraction of phenol by mass in a first liquid phase; c) separating the first gas phase from the first liquid phase; d) returning at least part of the first gas phase to the hydrogenation reactor; e) heating the first liquid phase; f) purifying the first liquid phase by distillation; characterized in that heat is transferred from the hydrogenation product stream in step b) to another part of the process by means of in-process heat exchange; a mixture of cyclohexanone and cyclohexanol obtained by the process; and a chemical plant suitable for continuously preparing mixture of cyclohexanone and cyclohexanol according to the process.
摘要翻译： 本发明提供一种连续制备环己酮和环己醇的混合物的方法，其包括：a）在氢化反应器中，在铂或钯存在下，用气态氢气氢化苯酚，生成包含环己酮，环己醇，苯酚 和氢; b）将氢化产物流冷却至使第一气相中的质量分数低于第一液相中苯酚质量分数的温度; c）将第一气相与第一液相分离; d）将至少部分第一气相返回到氢化反应器; e）加热第一液相; f）通过蒸馏纯化第一液相; 其特征在于，通过在工艺中的热交换将热量从步骤b）中的氢化产物流转移到另一部分工艺; 通过该方法获得的环己酮和环己醇的混合物; 以及适用于连续制备环己酮和环己醇的混合物的化学植物。
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公开(公告)号：US10138133B2
公开(公告)日：2018-11-27
申请号：US14649823
申请日：2013-11-29
申请人： CAP III B.V.
发明人： Geert Ekkelenkamp , Johannes Elisabeth Pierre Debeij , Robert Geertman , Peter Van Ysacker , Johan Thomas Tinge
摘要： 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.
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公开(公告)号：US09908785B2
公开(公告)日：2018-03-06
申请号：US14899579
申请日：2014-06-20
申请人： CAP III B.V.
IPC分类号： B01D9/00 , C01C1/24 , C01C1/248 , C07D201/16 , C07D201/04 , C07C249/08
CPC分类号： C01C1/24 , B01D9/0022 , B01D9/0031 , B01D9/004 , B01D9/0063 , B01D2009/0086 , C01C1/248 , C07C249/08 , C07C2601/14 , C07D201/04 , C07D201/16 , C07C251/44
摘要： 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 crystals.
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公开(公告)号：US20170368473A1
公开(公告)日：2017-12-28
申请号：US15535795
申请日：2015-12-15
申请人： CAP III B.V.
IPC分类号： B01D3/14 , C07C45/82 , C07C35/08 , C07C27/28 , C07C49/403 , C07C45/00 , C07C2601/14
CPC分类号： B01D3/009 , B01D3/10 , B01D3/12 , B01D3/143 , C07C27/28 , C07C35/08 , C07C45/006 , C07C45/82 , C07C49/403 , C07C2601/14 , Y02P70/34
摘要： A process for the construction of a second chemical plant, which second chemical plant is suitable for the separation of cyclohexanone from a second mixture, which second mixture comprises reaction products from the hydrogenation of phenol, said process comprising: a) providing a first chemical plant, which first chemical plant is suitable for the separation of cyclohexanone from a first mixture, which first mixture comprises reaction products from the oxidation of cyclohexane, and which first plant comprises: i) a distillation column (C) suitable for distilling overhead cyclohexane; ii) a distillation column suitable for distilling overhead cyclohexanone; iii) a cyclohexane oxidation unit (A) suitable for the oxidation of cyclohexane; and iv) a heat recovery unit (B) suitable for the recovery of heat from off-gas from the cyclohexane oxidation unit suitable for the oxidation of cyclohexane; b) disabling in said first chemical plant, said distillation column (C) suitable for distilling overhead cyclohexane, said cyclohexane oxidation unit (A) and said heat recovery unit (B), wherein the second chemical plant comprises a distillation column (F) suitable for distilling overhead cyclohexanone reused from the first chemical plant, wherein each of the first chemical plant and the second chemical plant comprise a distillation column (E) suitable for distilling overhead components having a lower boiling point than cyclohexanone; a distillation column (G) suitable for distilling overhead a mixture comprising cyclohexanol and cyclohexanone in a wt.:wt. ratio of at least 4:1; and a cyclohexanol dehydrogenation unit (H) suitable for the dehydrogenation of cyclohexanol to cyclohexanone.
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公开(公告)号：US20230054797A1
公开(公告)日：2023-02-23
申请号：US17796631
申请日：2021-02-04
申请人： CAP III B.V.
IPC分类号： C01C1/242 , C07D201/06 , C07D201/16
摘要： The invention provides a process for the production of crystalline ammonium sulfate, wherein the process comprises performing a Beckmann rearrangement reaction, neutralizing the Beckmann rearrangement reaction mixture, separating a first aqueous ammonium sulfate phase and an aqueous ε-caprolactam phase, charging the first ammonium sulfate phase to a first evaporative type crystallization section wherein crystalline ammonium sulfate is obtained, discharging from the first evaporative type crystallization section mother liquor enriched in organic components, extracting the aqueous ε-caprolactam phase to obtain an extracted ε-caprolactam phase and a second aqueous ammonium sulfate phase, discharging the mother liquor that is discharged from the first evaporative type crystallization section and/or the second aqueous ammonium sulfate phase to a second evaporative type crystallization section wherein evaporative type crystallization is performed so that a three-phase system occurs. At least a liquid oily phase is recovered from the three-phase system. The invention further provides a plant suitable to carry out the process of the invention, crystalline ammonium sulfate and a liquid oily phase obtained by the process of the invention.
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公开(公告)号：US10301243B2
公开(公告)日：2019-05-28
申请号：US15525448
申请日：2015-11-06
申请人： CAP III B.V.
发明人： Johan Thomas Tinge , Corinne Daguenet , Iris Verschuren , Wilhelmus Rudolf Maria Martens , Roeland Wilhelmus Theodorus Maria Brands , Robert Jan de Korte
摘要： 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.
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公开(公告)号：US09676633B2
公开(公告)日：2017-06-13
申请号：US14425419
申请日：2013-09-12
申请人： CAP III B.V.
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.
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