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公开(公告)号：US20150368176A1
公开(公告)日：2015-12-24
申请号：US14763196
申请日：2014-01-24
申请人： DAICEL CORPORATION
发明人： Hiroyuki MIURA , Masahiko SHIMIZU , Takashi UENO
摘要： A process and a production apparatus for producing a high-purity carboxylic acid, from which a metal-containing impurity and/or a carbonyl-group-containing impurity have been highly purified, are provided.The process for producing a carboxylic acid according to the present invention comprises subjecting a carboxylic acid stream containing a metal-containing impurity to a first flash system 1 to give a vaporized fraction, distilling the vaporized fraction by a distillation system 5 to separate into a stream mainly containing a carboxylic acid and a fraction containing a high-volatile impurity (or lower boiling point impurity), and feeding the separated stream mainly containing the carboxylic acid to a second flash system 10 or an adsorption system to form a purified carboxylic acid.
摘要翻译： 提供了高纯度地制备含有金属的杂质和/或含有羰基的杂质的高纯度羧酸的方法和制造装置。 根据本发明的制备羧酸的方法包括将含有含金属的杂质的羧酸料流经受第一闪蒸系统1以得到汽化部分，通过蒸馏系统5蒸馏蒸发的馏分以分离成流 主要含有羧酸和含有高挥发性杂质（或低沸点杂质）的级分，并将主要含有羧酸的分离流供给第二闪蒸系统10或吸附系统以形成纯化的羧酸。
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公开(公告)号：US20230048638A1
公开(公告)日：2023-02-16
申请号：US17789113
申请日：2020-12-23
申请人： DAICEL CORPORATION
摘要： Provided is a method capable of manufacturing high-purity 1,3-butylene glycol having a high potassium permanganate test value, a very low content of low boiling point components, and a high initial boiling point with a high recovery rate.
The method for manufacturing 1,3-butylene is a method for obtaining purified 1,3-butylene glycol from a crude reaction liquid containing 1,3-butylene glycol. In a dehydration column used in a dehydration step, a liquid feed containing 1,3 butylene glycol and water with an acetaldehyde content of 1000 ppm or lower and a crotonaldehyde content of 400 ppm or lower is distilled under a condition of a reflux ratio of higher than 0.3, and a liquid concentrated with a low boiling point component containing water is distilled off from above a feed tray. In a product column used in a product distillation step, a liquid feed containing 1,3-butylene glycol with an acetaldehyde content of 500 ppm or lower and a crotonaldehyde content of 200 ppm or lower is distilled under a condition of a reflux ratio of higher than 0.1.-
公开(公告)号：US20230035233A1
公开(公告)日：2023-02-02
申请号：US17788803
申请日：2020-12-23
申请人： DAICEL CORPORATION
发明人： Masahiko SHIMIZU
摘要： Provided is a method capable of yielding high-purity 1,3-butylene glycol having a very low content of a low boiling point component and a high initial boiling point, with a high recovery ratio. A reaction crude liquid containing 1,3-butylene glycol is subjected to product distillation to yield purified 1,3-butylene glycol, through dehydration including removing water by distillation and performing high boiling point component removal including removing a high boiling point component by distillation. A method for producing 1,3 butylene glycol, the method including: distilling a charged liquid having a water content of 1.2 wt.% or less in a product column for use in the product distillation under a condition of a reflux ratio of greater than 0.1; distilling off a liquid in which a low boiling point component is concentrated from above a charging plate; and extracting 1,3-butylene glycol from below the charging plate.
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公开(公告)号：US20210355063A1
公开(公告)日：2021-11-18
申请号：US16483808
申请日：2018-07-25
申请人： DAICEL CORPORATION
发明人： Masahiko SHIMIZU
摘要： Provided is a method capable of industrially efficiently producing acetic acid yielding a good potassium permanganate test result, without costing much. In the acetic acid production method, (1) by-produced acetaldehyde is industrially advantageously removed from a process stream, and (2) a crotonaldehyde concentration in an acetic acid stream from a light ends column is controlled to a specific level or lower, and/or a reflux ratio at a second distillation column is controlled to 0.1 or more. In addition, (3) the method includes the step of subjecting at least one of an aqueous phase and an organic phase of a light ends column overhead condensate to distillation in a crotonaldehyde-removing column; the light ends column is operated at a reflux ratio of 2 or more (when the aqueous phase is refluxed); and the crotonaldehyde-removing column is operated so as to meet a specific condition(s).
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公开(公告)号：US20200172461A1
公开(公告)日：2020-06-04
申请号：US16071337
申请日：2018-03-27
申请人： DAICEL CORPORATION
发明人： Masahiko SHIMIZU
摘要： Provided are a method and an acetic acid production method, each of which can effectively restrain or prevent local corrosion of an inner wall of a process unit and/or line and can lower a formic acid concentration in an acetic acid product. The method produces acetic acid by a process including (1) a reaction step and (A) a separation step. In the reaction step (1), methanol is carbonylated with carbon monoxide in the presence of a catalytic system, acetic acid, methyl acetate, and water, where the catalytic system includes a metal catalyst and methyl iodide. In the separation step (A), the reaction mixture resulting from the reaction step is separated, using at least one selected from evaporators and distillation columns, into a stream containing the catalyst, an acetic acid stream rich in acetic acid, and a stream rich in lower-boiling components as compared with the acetic acid stream. In this method, an oxygen concentration is controlled by at least one of (a) controlling the oxygen concentration in a gaseous phase in the process to less than 7 percent by volume, and (b) controlling the oxygen concentration in a liquid phase in the process to less than 7×10−5 g/g. In addition, a formic acid concentration in the liquid phase in the process is controlled to 500 ppm by mass or less. Thus, the formation of at least one of iodine and formic acid is restrained.
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公开(公告)号：US20200123093A1
公开(公告)日：2020-04-23
申请号：US16334673
申请日：2018-05-29
申请人： DAICEL CORPORATION
发明人： Masahiko SHIMIZU
摘要： Provided is a method for industrially efficiently producing acetic acid that yields a good potassium permanganate test result, without enormous cost. A light ends column (first distillation column) is operated with a reflux ratio at a specific level or more, a distillation column (crotonaldehyde-removing column) is provided for treating an organic phase of an overhead condensate from the light ends column, and the crotonaldehyde-removing column is operated under such conditions as to meet at least one of conditions (i) to (iii) as follows: (i) a reflux ratio at the distillation column is 0.01 or more; (ii) at the distillation column, the ratio of a crotonaldehyde concentration in a distillate to a crotonaldehyde concentration in a charge liquid is less than 1; and (iii) at the distillation column, the ratio of a crotonaldehyde concentration in bottoms to a crotonaldehyde concentration in the charge liquid is greater than 1. The crotonaldehyde concentration in an acetic acid stream (first acetic acid stream) resulting from light ends removal in the light ends column is controlled at a specific level or less, and/or the reflux ratio at a dehydration column (second distillation column) is controlled at a specific level or more, and at least one of the ratios CCR/CECR and CCR/CBA in at least one of the first acetic acid stream and an acetic acid-rich stream resulting from further purification of the first acetic acid stream is lowered, to give an acetic acid product that yields a better potassium permanganate test result.
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公开(公告)号：US20200123090A1
公开(公告)日：2020-04-23
申请号：US16334654
申请日：2018-05-29
申请人： DAICEL CORPORATION
发明人： Masahiko SHIMIZU
摘要： Provided is a method that can industrially efficiently produce acetic acid yielding a good potassium permanganate test result, without costing much. The method includes an acetaldehyde-removing step by which by-produced acetaldehyde is industrially advantageously removed. The method also includes the step of subjecting at least one of an aqueous phase and an organic phase of a light ends column overhead condensate to distillation in a crotonaldehyde-removing column. The light ends column is operated at a reflux ratio of 2 or more (when the aqueous phase is refluxed). The crotonaldehyde-removing column is operated so as to meet at least one of conditions (a-i) to (a-iii) as follows: (a-i) a reflux ratio at the distillation column is 0.01 or more; (a-ii) at the distillation column, the ratio of a crotonaldehyde concentration (ppm by mass) in a distillate to a crotonaldehyde concentration (ppm by mass) in a charge liquid is less than 1; and (a-iii) at the distillation column, the ratio of a crotonaldehyde concentration (ppm by mass) in bottoms to a crotonaldehyde concentration (ppm by mass) in the charge liquid is greater than 1.
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公开(公告)号：US20190151769A1
公开(公告)日：2019-05-23
申请号：US16193595
申请日：2018-11-16
申请人： Daicel Corporation
CPC分类号： B01D3/40 , B01D3/148 , B01D3/36 , B01D3/4255 , B01D3/4261 , C07C51/12 , C07C51/44 , C07C53/08
摘要： A process for separating or removing permanganate reducing compounds (PRC's) from a first mixture containing at least one PRC, methyl iodide, and water comprises the steps of: feeding the first mixture to a feed port of a distillation column, and distilling and separating the first mixture into an upper stream and a lower stream, wherein the distillation of the first mixture forms a second mixture at an upper position than the feed port, and the process further comprises the steps of: withdrawing the second mixture as the upper stream, and withdrawing the lower stream from a lower position than the feed port.
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公开(公告)号：US20230087989A1
公开(公告)日：2023-03-23
申请号：US17788823
申请日：2020-12-23
申请人： DAICEL CORPORATION
摘要： A high-purity 1,3-butylene glycol product that is colorless and odorless (or almost colorless and odorless), unlikely to cause coloration and odor over time, and/or unlikely to cause an acid concentration increase over time when the product is left in a state containing water is provided. A 1,3-butylene glycol product containing 1,3-butylene glycol, wherein, after the 1,3-butylene glycol product has been kept at 180° C. for 3 hours in air atmosphere, at least one of contents of compounds represented by the following Formula (A) or (B) is less than 8 ppm. In the following formula, R1 to R4 are the same as or different from each other, and each of R1 to R4 is a hydrogen atom, an alkyl group which has from 1 to 4 carbon atoms and may be substituted with a hydroxy group, or an alkenyl group which has from 2 to 4 carbon atoms and may be substituted with a hydroxy group.
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公开(公告)号：US20230046811A1
公开(公告)日：2023-02-16
申请号：US17789093
申请日：2020-12-23
申请人： DAICEL CORPORATION
IPC分类号： C07C29/80 , C07C29/60 , B01D3/42 , C07C29/141
摘要： Provided is a method capable of manufacturing high-purity 1,3-butylene glycol having a high potassium permanganate test value, a very low content of low boiling point components, and a high initial boiling point with a high recovery rate.
A method for manufa.cturing 1,3-butylene glycol is a method for obtaining purified 1,3-butylene glycol from a crude reaction liquid containing 1,3-butylene glycol. In a dehydration column used in the dehydration step, a liquid feed containing 1,3-butylene glycol and water with an acetaldehyde content of 1000 ppm or lower and a crotonaldehyde content of 400 ppm or lower is distilled, and a liquid concentrated with a low boiling point component containing water is distilled off from above a feed plate; and in a product column used in the product distillation step, a 1,3-butylene glycol liquid feed having an acetaldehyde content of 500 ppm or lower and a crotonaldehyde content of 200 ppm or lower is distilled under a condition of a reflux ratio of higher than 0.1.
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