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公开(公告)号：US10941103B2
公开(公告)日：2021-03-09
申请号：US16636703
申请日：2018-08-13
Applicant: BASF SE
Inventor： Ortmund Lang , Tim Blaschke , Christian Raith , Michael Schafranka , Claus Hechler
Abstract: A process for continuously preparing a butyl acrylate H2C═CH—C(═O)OR, with R=n-butyl or isobutyl, wherein aqueous 3-hydroxypropionic acid is converted under dehydrating and esterifying conditions in the presence of the corresponding butanol R—OH in a reactor with a rectification column and butyl acrylate formed, unconverted butanol and water used and formed are distilled off overhead as a ternary azeotrope, after separation into a liquid aqueous phase and liquid organic phase each of the aqueous and organic phases is at least partly discharged, and the organic phase comprising the butyl acrylate and the butanol is subjected to distillative separation.
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公开(公告)号：US10906862B2
公开(公告)日：2021-02-02
申请号：US16472018
申请日：2017-12-11
Applicant: BASF SE
Inventor： Ortmund Lang , Bernd Metzen , Claus Hechler
Abstract: A process for isolating pure butyl acrylate from crude butyl acrylate, which is carried out in a dividing wall column having separation-active internals and a vaporizer, and in which: a dividing wall is arranged in a longitudinal direction of the column to form an upper joint column region, a lower joint column region, an inflow section having a side feed point and an offtake section having a side offtake point; a ratio of an amount of liquid at an upper end of the dividing wall going to an enrichment section and a stripping section of the column is set in the range from 1:0.2 to 1:5; and a ratio of an amount of vapor streams at a lower end of the dividing wall going to the stripping section and the enrichment section of the column is set in a range from 1:0.5 to 1:2.0.
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公开(公告)号：US10894223B2
公开(公告)日：2021-01-19
申请号：US16472054
申请日：2017-12-11
Applicant: BASF SE
Inventor： Ortmund Lang , Bernd Metzen , Claus Hechler
Abstract: Process for isolating pure 2-ethylhexyl acrylate or pure 2-propylheptyl acrylate from the corresponding crude alkyl acrylate by distillation, wherein the process is carried out in a dividing wall column (1) which has separation-active internals and vaporizer (7) and in which a dividing wall (8) is arranged in the longitudinal direction of the column to form an upper joint column region (9), a lower joint column region (14), an inflow section (10, 12) having a side feed point (2) and an offtake section (11, 13) having a side offtake point (3), the column has a number of theoretical plates in the range from 10 to 60, where the number of theoretical plates of the dividing wall column (1) relates to the sum of the theoretical plates in the joint upper column region (9), the joint lower column region (14) and the inflow section (10, 12), the side feed point (2) for the corresponding crude alkyl acrylate is arranged at a theoretical plate in the region commencing at least two theoretical plates above the bottommost theoretical plate and ending at least two theoretical plates below the uppermost theoretical plate, the side offtake point (3) for the pure 2-ethylhexyl acrylate or pure 2-propylheptyl acrylate is arranged at a theoretical plate in the region commencing at least two theoretical plates above the bottommost theoretical plate and ending at least two theoretical plates below the uppermost theoretical plate and the dividing wall (8) is arranged in the column in the region commencing at least one theoretical plate above the bottommost theoretical plate and ending at least one theoretical plate below the uppermost theoretical plate, where the ratio of amount of liquid at the upper end of the dividing wall (8) going to the enrichment section (10) and the stripping section (11) of the column is set in the range from 1:0.2 to 1:5.
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4.发明授权Continuous process for preparing (meth)acrylates of C10-alcohol mixtures 有权用于制备C10-醇混合物的（甲基）丙烯酸酯的连续方法公开(公告)号：US09388118B2
公开(公告)日：2016-07-12
申请号：US14038972
申请日：2013-09-27
Applicant: BASF SE
Inventor： Ulrich Jaeger , Volker Schliephake , Ortmund Lang , Jochen Petzoldt , Tobias Johannes Korn , Virginie Bette , Claus Hechler
Abstract: A continuous process for preparing (meth)acrylates of C10-alcohol mixtures by reaction of glacial (meth)acrylic acid with an isomer mixture of C10-alcohols composed of 2-propylheptanol as the main isomer and at least one of the C10-alcohols 2-propyl-4-methylhexanol, 2-propyl-5-methylhexanol, 2-isopropylheptanol, 2-isopropyl-4-methylhexanol, 2-isopropyl-5-methylhexanol and/or 2-propyl-4,4-dimethylpentanol, and the use of a diester of dicarboxylic acids which have been esterified with N-oxyl-containing compounds as polymerization inhibitors in such a process.
Abstract translation: 通过冰（甲基）丙烯酸与由2-丙基庚醇组成的C 10醇作为主要异构体的异构体混合物和至少一种C 10醇2来制备C10-醇混合物的（甲基）丙烯酸酯的连续方法 丙基-4-甲基己醇，2-丙基-5-甲基己醇，2-异丙基庚醇，2-异丙基-4-甲基己醇，2-异丙基-5-甲基己醇和/或2-丙基-4,4-二甲基戊醇， 的二羧酸二酯在这种方法中被N-氧基化合物酯化作为聚合抑制剂。
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Patent Agency Ranking
公开(公告)号：US20160289159A1
公开(公告)日：2016-10-06
申请号：US15086715
申请日：2016-03-31
Applicant: BASF SE
Inventor： Catharina HORSTMANN , Claus Hechler , Gregor Grackiewicz , Bernd Schall
Abstract: A process for continuously preparing the tert-butyl ester of an aliphatic C1-C4 carboxylic acid comprises: a) the reaction of an aliphatic C1-C4 carboxylic acid with isobutene in the presence of an acidic catalyst to give an esterification mixture (G1); b) the partial evaporation of the esterification mixture (G1), giving a liquid first high boiler phase (SPh1) comprising the acidic catalyst, and a first vapor (B1) comprising tert-butyl ester; c) the fractional condensation of the first vapor (B1) by partially condensing the first vapor (B1) at a first pressure and a first temperature and obtaining a first condensate (K1), partially condensing the uncondensed second vapor (B2) at a second pressure and a second temperature and obtaining a second condensate (K2), the first temperature being 0 to 45° C. below the condensation temperature of the tert-butyl ester at the first pressure and the second temperature being 45 to 80° C. below the condensation temperature of the tert-butyl ester at the second pressure, with the proviso that the second temperature is at least 5° C. below the first temperature; and d) the combination of the first condensate (K1) and the second condensate (K2) and the feeding to a combined workup, and recycling of the third vapor (B3) not condensed at the second temperature into step a). The process allows the preparation of the tert-butyl ester of an aliphatic C1-C4 carboxylic acid by reaction of the carboxylic acid with isobutene, with isolation of unconverted isobutene from the esterification mixture in an energetically favorable manner and with an improved degree of removal.
Abstract translation: 一种连续制备脂族C 1 -C 4羧酸叔丁酯的方法包括：a）脂肪族C 1 -C 4羧酸与异丁烯在酸性催化剂存在下的反应，得到酯化混合物（G1）; b）酯化混合物（G1）的部分蒸发，得到包含酸性催化剂的液体第一高沸点相（SPh1）和包含叔丁酯的第一蒸气（B1）; c）通过在第一压力和第一温度下部分地冷凝第一蒸气（B1）并获得第一冷凝物（K1），在第二蒸气（B1）的部分冷凝，在第二蒸气 压力和第二温度，并获得第二冷凝物（K2），第一温度低于叔丁酯在第一压力下的冷凝温度为0至45℃，第二温度为45至80℃以下 在第二压力下叔丁酯的冷凝温度，条件是第二温度低于第一温度至少5℃; 和d）第一冷凝物（K1）和第二冷凝物（K2）的组合以及进料到组合后处理中，并且将在第二温度下未冷凝的第三蒸气（B3）再循环进入步骤a）。 该方法允许通过羧酸与异丁烯的反应制备脂肪族C 1 -C 4羧酸的叔丁基酯，同时以有利的方式从分离的酯化混合物中分离出未转化的异丁烯，并提高了去除程度。
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公开(公告)号：US10730823B2
公开(公告)日：2020-08-04
申请号：US16471993
申请日：2017-12-11
Applicant: BASF SE
Inventor： Ortmund Lang , Bernd Metzen , Claus Hechler
Abstract: A process for isolating pure tert-butyl (meth)acrylate from crude tert-butyl (meth)acrylate by distillation, wherein the process is carried out in a dividing wall column having separation-active internals and a vaporizer and in which a dividing wall is arranged in the longitudinal direction of the column to form an upper joint column region, a lower joint column region, an inflow section having a side feed point, and an offtake section having a side offtake point, where the column has from 20-80 theoretical plates and the ratio of the amount of liquid at the upper end of the dividing wall going to the enrichment section and the stripping section of the column is set in the range from 1:0.2 to 1:5.
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公开(公告)号：US10023520B2
公开(公告)日：2018-07-17
申请号：US15086715
申请日：2016-03-31
Applicant: BASF SE
Inventor： Catharina Horstmann , Claus Hechler , Gregor Grackiewicz , Bernd Schall
Abstract: A process for continuously preparing the tert-butyl ester of an aliphatic C1-C4 carboxylic acid comprises: a) the reaction of an aliphatic C1-C4 carboxylic acid with isobutene in the presence of an acidic catalyst to give an esterification mixture (G1); b) the partial evaporation of the esterification mixture (G1), giving a liquid first high boiler phase (SPh1) comprising the acidic catalyst, and a first vapor (B1) comprising tert-butyl ester; c) the fractional condensation of the first vapor (B1) by partially condensing the first vapor (B1) at a first pressure and a first temperature and obtaining a first condensate (K1), partially condensing the uncondensed second vapor (B2) at a second pressure and a second temperature and obtaining a second condensate (K2), the first temperature being 0 to 45° C. below the condensation temperature of the tert-butyl ester at the first pressure and the second temperature being 45 to 80° C. below the condensation temperature of the tert-butyl ester at the second pressure, with the proviso that the second temperature is at least 5° C. below the first temperature; and d) the combination of the first condensate (K1) and the second condensate (K2) and the feeding to a combined workup, and recycling of the third vapor (B3) not condensed at the second temperature into step a). The process allows the preparation of the tert-butyl ester of an aliphatic C1-C4 carboxylic acid by reaction of the carboxylic acid with isobutene, with isolation of unconverted isobutene from the esterification mixture in an energetically favorable manner and with an improved degree of removal.
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公开(公告)号：US10301252B2
公开(公告)日：2019-05-28
申请号：US16062359
申请日：2016-11-28
Applicant: BASF SE
Inventor： Catharina Horstmann , Claus Hechler , Gregor Grackiewicz , Bernd Schall
Abstract: A process for continuously preparing the tert-butyl ester of an ethylenically unsaturated carboxylic acid, by a) reacting an ethylenically unsaturated carboxylic acid with isobutene in the presence of an acidic catalyst to give an esterification mixture; b) removing the acidic catalyst; c) removing low-boiling components; and d) supplying a tert-butyl ester-comprising liquid to a distillation apparatus and subjecting it to purifying distillation in the distillation apparatus, where d1) in the distillation apparatus the tert-butyl ester-comprising liquid is separated into a tert-butyl ester-comprising gaseous top product and a carboxylic acid-comprising liquid bottom product; d2) the tert-butyl ester-comprising gaseous top product is at least partly condensed and the condensate is recycled partly as reflux to the distillation apparatus; d3) the carboxylic acid-comprising liquid bottom product is recycled at least partly to step a); d4) carboxylic acid-comprising liquid bottom product is drawn off and passed to a heater; a superheated, liquid recycle stream is taken from the heater; and the superheated recycle stream is let down into the distillation apparatus; and d5) at least in the top region of the distillation apparatus, the distillation apparatus walls in contact with the vapor, at least in sub-regions, are heated and/or thermally insulated. In the course of the process, the separation of the tert-butyl ester from unreacted carboxylic acid is carried on with a particularly low level of accompanying polymerization both of the tert-butyl ester and of the carboxylic acid.
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9.再颁专利公开(公告)号：USRE44822E1
公开(公告)日：2014-04-01
申请号：US13682129
申请日：2012-11-20
Applicant: BASF SE
Inventor： Claus Hechler , Wilhelm Ruppel , Wolfgang Gerlinger , Wolfgang Schneider , Klaus Joachim Mueller-Engel
IPC: C07C5/48
CPC classification number: C07C5/48 , C07C45/35 , C07C51/252 , C07C51/43 , C07C11/06 , C07C47/22 , C07C57/04
Abstract: A process for heterogeneously catalyzed partial dehydrogenation of a hydrocarbon, in which a reaction gas mixture input stream comprising the hydrocarbon to be dehydrogenated is conducted through a fixed catalyst bed disposed in a shaft and the reaction gas mixture input stream is obtained in the shaft by metering an input gas II comprising molecular oxygen upstream of the fixed catalyst bed into an input gas stream I which comprises molecular hydrogen and the hydrocarbon to be dehydrogenated and is flowing within the shaft toward the fixed catalyst bed.
Abstract translation: 烃的非均相催化部分脱氢的方法，其中包含待脱氢烃的反应气体混合物输入流通过设置在轴中的固定催化剂床进行，反应气体混合物输入流通过计量获得在轴中 将固定催化剂床上游的分子氧的输入气体II输入到输入气流I中，该输入气流I包括分子氢和要脱氢的烃并且在轴内朝向固定的催化剂床流动。
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