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公开(公告)号：US20230033469A1
公开(公告)日：2023-02-02
申请号：US17788968
申请日：2020-12-23
申请人： DAICEL CORPORATION
发明人： Masahiko SHIMIZU , Satoshi KUSAKABE , Ryuji SAITOU
摘要： Provided is a method capable of yielding high-purity 1,3-butylene glycol having a very low content of a high boiling point component and a low dry point, with a high recovery ratio. A method for producing 1,3-butylene glycol to yield purified 1,3-butylene glycol from a reaction crude liquid containing 1,3-butylene glycol, in which, in a high boiling point component removal column for use in the removing a high boiling point component, a charged liquid containing 1,3 -butylene glycol is distilled under conditions that (i) a reflux ratio is greater than 0.02 in a case where a concentration of 1,3-butylene glycol in the charged liquid is 95% or less, or a reflux ratio is greater than 0.01 in a case where the concentration of 1,3-butylene glycol in the charged liquid is greater than 95%, and (ii) a bottom ratio of less than 30 wt. %, high-purity 1,3-butylene glycol is distilled off from above a charging plate, and a liquid in which a high boiling point component is concentrated is extracted from below the charging plate.
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公开(公告)号：US20220354760A1
公开(公告)日：2022-11-10
申请号：US17788991
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 1,3-butylene glycol liquid feed 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：US20190263744A1
公开(公告)日：2019-08-29
申请号：US16265535
申请日：2019-02-01
申请人： Daicel Corporation
摘要： A process for producing acetic acid comprises a process comprising: (1) carbonylating methanol; (2) separating the reaction mixture into a volatile phase and a less-volatile phase; (3) distilling the volatile phase to forma first overhead rich in a lower boiling component, and an acetic acid stream rich in acetic acid; and at least one step group selected from the group consisting of the following sections (4), (9), and (15): (4) a section for separating impurities from the acetic acid stream to give purified acetic acid, (9) a section for separating the first overhead into a stream rich in acetaldehyde and a stream rich in methyl iodide, and (15) a section for absorption-treating an off-gas from the process with an absorption solvent and forming a carbon monoxide-rich stream and an acetic acid-rich stream. In this process, the concentration of oxygen in a gaseous phase of the process is controlled to less than 7% by volume and/or the concentration of oxygen in a liquid phase of the process is controlled to less than 7×10−5 g/g, and the formation of iodine is reduced. The process effectively reduces or prevents local corrosion of an inner wall of a process unit and/or line.
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公开(公告)号：US20180282253A1
公开(公告)日：2018-10-04
申请号：US15542855
申请日：2017-05-25
申请人： DAICEL CORPORATION
发明人： Masahiko SHIMIZU
摘要： There is provided a method allowing industrially efficient production of high quality acetic acid having a good potassium permanganate test value and a low impurity content without a large cost.The method for producing acetic acid according to the present invention has a carbonylation reaction step, an evaporation step and a lower boiling point component removal step, and wherein with heating of the evaporator, (i) an acetaldehyde concentration in the aqueous phase of an overhead condensate in a lower boiling point component removal column is controlled to not less than 2340 ppm by mass; and/or (ii) a methyl acetate concentration in the aqueous phase is controlled to less than 19.0% by mass and/or; (iii) a methyl acetate concentration in the organic phase of the overhead condensate in the lower boiling point component removal column is controlled to less than 38.0% by mass, and then at least a portion of the aqueous phase is treated in the acetaldehyde separation and removal step to recycle a residual liquid after the acetaldehyde separation and removal to the reaction vessel and/or the acetaldehyde separation and removal step and/or other processes.
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公开(公告)号：US20180258021A1
公开(公告)日：2018-09-13
申请号：US15542610
申请日：2017-05-25
申请人： DAICEL CORPORATION
发明人： Masahiko SHIMIZU
摘要： It is intended to provide a method capable of industrially and efficiently producing acetic acid having a good potassium permanganate test value without a large cost.A method for producing acetic acid according to the present invention is a method for producing acetic acid comprising: a carbonylation reaction step; an evaporation step; a lower boiling point component removal step; and a first overhead stream recycle step of recycling at least a portion of an aqueous phase and/or an organic phase obtained by condensing a first overhead stream obtained in the lower boiling point component removal step to a reaction vessel, wherein a crotonaldehyde concentration in a first acetic acid stream obtained in the lower boiling point component removal step is controlled to not more than 2.2 ppm by mass. The catalyst system may further contain an ionic iodide. The method for producing acetic acid may further comprise an acetaldehyde separation and removal step of distilling at least a portion of the aqueous phase and/or the organic phase obtained by condensing the first overhead stream to separate and remove acetaldehyde.
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公开(公告)号：US20200079719A1
公开(公告)日：2020-03-12
申请号：US16334659
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 yielding a good potassium permanganate test result, without costing much. The acetic acid production method according to the present invention includes a carbonylation step, a separation step, a recycling step, a liquid-liquid separation step, and an acetaldehyde-removing step of treating an object, where the object is selected from at least a part of at least one of the aqueous phase and the organic phase on the basis of a factor(s) selected from a liquid temperature in the liquid-liquid separation in the liquid-liquid separation step, an acetaldehyde concentration in at least one of the aqueous phase and the organic phase, an acetaldehyde partition coefficient, a methyl acetate concentration in at least one of the aqueous phase and the organic phase, and a methyl acetate partition coefficient. In the first acetic acid stream in the separation step, a crotonaldehyde concentration is controlled to 2.2 ppm by mass or less, and the ratio (CCR/CECR) of a crotonaldehyde concentration CCR (ppm by mass) to an 2-ethylcrotonaldehyde concentration CECR (ppm by mass) is regulated.
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公开(公告)号：US20180201564A1
公开(公告)日：2018-07-19
申请号：US15540195
申请日：2017-05-25
申请人： DAICEL CORPORATION
CPC分类号： C07C51/12 , B01D3/009 , B01D3/143 , B01D15/361 , C07C51/44 , C07C51/445 , Y02P20/127 , C07C53/08
摘要： It is intended to provide a method capable of suppressing distillation apparatus corrosion as a method for producing acetic acid, comprising the step of distilling a crude acetic acid solution containing acetic acid and an impurity having a higher boiling point than that of acetic acid to purify the acetic acid. The method for producing acetic acid of the present invention comprises the step described above, wherein the distillation of the crude acetic acid solution is performed under a condition involving a distillation column bottom temperature of not more than 165° C. An acetic acid concentration in the crude acetic acid solution to be subjected to the distillation is preferably not less than 90 mass %. Examples of the impurity having a higher boiling point than that of acetic acid include acetates, acetic anhydride, and propionic acid. A column bottom pressure of the distillation column is preferably less than 0.255 MPaG.
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公开(公告)号：US20180118651A1
公开(公告)日：2018-05-03
申请号：US15565604
申请日：2016-05-27
申请人： Daicel Corporation
摘要： A process for producing acetic acid while efficiently separating permanganate reducing compounds (PRC's) and methyl iodide is provided.PRC's are separated or removed from a mixed composition (3A) containing PRC's and methyl iodide by distilling the mixed composition in a distillation step (5) to form an overhead stream (5A), a side-cut stream (5B), and a lower stream (5C). In a distillation column of the distillation step (5), an extractant (e.g., water) extracting PRC's preferentially to methyl iodide is added to a concentration zone in which PRC's and methyl iodide are concentrated, and an extraction mixture falling from the concentration zone is withdrawn as the side-cut stream (5B).
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公开(公告)号：US20180118649A1
公开(公告)日：2018-05-03
申请号：US15540177
申请日：2017-05-25
申请人： DAICEL CORPORATION
发明人： Masahiko SHIMIZU
摘要： Provided is a method for producing acetic acid, which suppresses catalyst precipitation and accumulation in an evaporator, can efficiently recycle catalysts to a reaction vessel, and can contribute to maintenance and improvement in acetic acid productivity and securing of safety operation. In the method, the evaporator has a catalyst precipitation and accumulation prevention structure: (a) structure where inclination angle θ of inside wall surface of an inverted truncated conical cylindrical connection portion is 5° to 85°; and/or (b) structure where a vortex breaker comprising a plate-like vortex breaker main body and a leg is disposed such that the vortex breaker main body covers right above the connection portion of an evaporator bottom part to a residual liquid stream recycle line, and linear velocity r of the residual liquid stream passing through a gap between the vortex breaker main body and the evaporator bottom part is larger than 10 m/h.
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公开(公告)号：US20170260120A1
公开(公告)日：2017-09-14
申请号：US15510148
申请日：2016-11-17
申请人： DAICEL CORPORATION
发明人： Masahiko SHIMIZU , Ryuji SAITO , Hiroyuki MIURA
CPC分类号： C07C51/38 , C07C51/087 , C07C51/12 , C07C51/44 , C07C53/08
摘要： A method for producing acetic acid includes subjecting an acetic acid solution to an acetic anhydride decreasing treatment. The acetic acid solution is present typically in, or downstream from, a distillation column (5) of acetic acid production equipment (X), includes acetic acid in a concentration of 90 mass percent or more, acetic anhydride, and water, and is in such a state that an equilibrium concentration of acetic anhydride is higher than an acetic anhydride concentration. The acetic anhydride decreasing treatment includes at least one of water concentration increasing and temperature lowering so as to bring the acetic acid solution into such a state that the equilibrium concentration of acetic anhydride is lower than the acetic anhydride concentration. The acetic acid production method is suitable for yielding a high-purity acetic acid product.
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