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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：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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