公开(公告)号：US6013831A

公开(公告)日：2000-01-11

申请号：US69815

申请日：1998-04-30

申请人： Hiroshi Machida ,  Fumiya Zaima ,  Kengi Nakaya ,  Kazuo Tanaka

发明人： Hiroshi Machida ,  Fumiya Zaima ,  Kengi Nakaya ,  Kazuo Tanaka

IPC分类号： C07C51/265 ,  C07C67/08 ,  C07C67/52 ,  C07C67/48

CPC分类号： C07C67/08 ,  C07C51/265 ,  C07C67/52

摘要： A process for the production of high-purity dimethyl 2,6-naphthalenedicarboxylate, which comprises esterifying 2,6-naphthalenedicarboxylic acid obtained by liquid phase oxidation of 2,6-dialkylnaphthalene with molecular oxygen in the presence of an oxidation catalyst, with methanol and then purifying a crude ester formed by the esterification, the crude ester being purified in the presence of an aromatic hydrocarbon as a solvent, in which impurities contained in a reaction product obtained by the esterification of 2,6-naphthalenedicarboxylic acid prepared by the liquid phase oxidation of 2,6-dialkylnaphthalene are effectively removed with simple procedures, oxidation catalyst metals are recovered, a crystal of naphthalenedicarboxylic acid formed by the oxidation of dialkylnaphthalene and/or its oxide derivative can be easily separated, and the oxidation catalyst to be brought into the step of producing dimethyl naphthalenedicarboxylate is recovered in the process of the production of naphthalenedicarboxylic acid and effectively used in the process of the production of naphthalenedicarboxylic acid.

摘要翻译： 一种制备高纯度2,6-萘二甲酸二甲酯的方法，其包括在氧化催化剂存在下，通过用分子氧将2,6-二烷基萘液相氧化得到的2,6-萘二羧酸与甲醇和 然后纯化通过酯化形成的粗酯，粗酯在作为溶剂的芳族烃存在下纯化，其中通过由液相制备的2,6-萘二甲酸酯化得到的反应产物中所含的杂质 通过简单的方法有效地除去2,6-二烷基萘的氧化，回收氧化催化剂金属，可以容易地分离通过二烷基萘和/或其氧化物衍生物的氧化形成的萘二甲酸的结晶，并将氧化催化剂 在生产n的过程中回收生产二甲基萘二甲酸二甲酯的步骤 邻苯二甲酸二羧酸，有效用于生产萘二羧酸的方法。

公开(公告)号：US06541662B2

公开(公告)日：2003-04-01

申请号：US10021430

申请日：2001-12-19

申请人： Hiroshi Machida ,  Ko Kedo ,  Fumiya Zaima

发明人： Hiroshi Machida ,  Ko Kedo ,  Fumiya Zaima

IPC分类号： C07C6109

CPC分类号： C07C51/36 ,  C07C61/12 ,  C07C61/125 ,  C07C61/09

摘要： A process for producing a hydrogenation product of aromatic carboxylic acid which comprises continuously producing the hydrogenation product of aromatic carboxylic acid by hydrogenating an aromatic carboxylic acid having a melting point of 250° C. or higher in a solvent in the presence of a solid catalyst, wherein the hydrogenation is conducted in a condition such that substantially the entire amount of the aromatic carboxylic acid of a raw material is dissolved in the solvent by recycling a portion of a reaction liquid taken out of a reactor into the reactor. An aromatic carboxylic acid having a high melting point and hardly soluble in solvents can be hydrogenated at a suitable reaction temperature in accordance with a continuous process without using a great amount of a solvent and the reaction product of the object compound can be produced very efficiently.

摘要翻译： 一种芳族羧酸的氢化产物的制造方法，其特征在于，在固体催化剂存在下，通过在溶剂中氢化熔点为250℃以上的芳香族羧酸，连续制造芳香族羧酸的氢化物， 其特征在于，氢化反应是将从反应器中取出的反应液的一部分再循环到反应器中，将原料的芳香族羧酸的总量全部溶解在溶剂中的方式进行。 可以在不使用大量溶剂的情况下，根据连续方法在合适的反应温度下氢化不溶于溶剂的高熔点，并且可以非常有效地制备目标化合物的反应产物。

公开(公告)号：US06268528B1

公开(公告)日：2001-07-31

申请号：US09432783

申请日：1999-11-03

申请人： Hiroshi Machida ,  Fumiya Zaima ,  Masato Inari ,  Hiroshi Watanabe ,  Emiko Yokose

发明人： Hiroshi Machida ,  Fumiya Zaima ,  Masato Inari ,  Hiroshi Watanabe ,  Emiko Yokose

IPC分类号： C07C5116

CPC分类号： C07C51/265 ,  C07C63/38

摘要： Dialkylnaphthalene is oxidized to naphthalenedicarboxylic acid in a lower aliphatic carboxylic acid solvent in the presence of a catalyst comprising a cobalt compound, a manganese compound and a bromine compound having an atomic ratio of manganese to cobalt of 0.03 to 0.5. The catalyst is supplied to the oxidation reaction zone so that the total amount of cobalt and manganese is 0.025 to 0.1 gram atom based on 1 gram mol of the dialkylnaphthalene. An oxidation product slurry is subjected to solid-liquid separation when the concentration of the naphthalenedicarboxylic acid in the slurry is 8 to 30% by weight. The process prevents the by-production of benzotricarboxylic acid such as trimellitic acid, thereby drastically reducing the incorporation of heavy metal complexes with trimellitic acid into naphthalenedicarboxylic acid crystals. The process optionally includes the addition of a polymer flocculant, this forming crystal aggregates with a large particle size and facilitating the separation of the crystals from the mother liquor.

摘要翻译： 在包含钴化合物，锰化合物和原子比为锰与钴的溴化合物的催化剂存在下，在低级脂族羧酸溶剂中将二烷基萘氧化成萘二羧酸为0.03〜0.5。 将催化剂供应到氧化反应区，使得钴和锰的总量基于1克摩尔的二烷基萘为0.025至0.1克原子。 当浆料中萘二甲酸的浓度为8〜30重量％时，氧化产物浆液进行固液分离。 该方法防止苯三甲酸如偏苯三酸的副产物，从而大大降低了与偏苯三酸的重金属络合物与萘二甲酸晶体的结合。 该方法任选地包括加入聚合物絮凝剂，这种形成晶体具有大粒径的聚集体并且有利于晶体与母液的分离。

公开(公告)号：US08957247B2

公开(公告)日：2015-02-17

申请号：US13579823

申请日：2011-02-18

申请人： Fumiya Zaima ,  Hideaki Fujita

发明人： Fumiya Zaima ,  Hideaki Fujita

IPC分类号： C07C51/16 ,  C07C51/42 ,  C07C51/47 ,  B01J45/00

CPC分类号： C07C51/42 ,  B01J45/00 ,  C07C51/47 ,  C07C63/26

摘要： In pretreating a pyridine ring-containing chelate resin which is used in the step for adsorption and collection of a heavy metal ion and a bromide ion derived from a catalyst from the oxidation reaction mother liquid in the process of producing an aromatic carboxylic acid, there may occur phenomena such as swelling of the resin, heat generation of the resin, and air bubbles generation, thereby causing fracture and deterioration of the resin. As a first treatment, Br− conversion, under a certain condition, of a pyridine ring-containing chelate resin with an aqueous solution of hydrobromic acid is performed, and then as a second treatment, replacement with acetic acid solvent is performed, thereby making it possible to prevent fracture and deterioration of the resin.

摘要翻译： 在制造芳族羧酸的方法中，在从氧化反应母液中预处理用于吸附和收集来自氧化反应母液的催化剂的重金属离子和溴离子的步骤中的含吡啶环的螯合树脂时， 发生树脂膨胀，树脂发热，产生气泡等现象，导致树脂的断裂和劣化。 作为第一处理，在一定条件下，使用含有吡啶环的螯合树脂与氢溴酸水溶液进行Br-转化，然后作为第二处理，进行乙酸溶剂置换，从而使其 可以防止树脂的断裂和劣化。

公开(公告)号：US20100012887A1

公开(公告)日：2010-01-21

申请号：US12304415

申请日：2007-06-08

申请人： Masato Inari ,  Fumiya Zaima

发明人： Masato Inari ,  Fumiya Zaima

IPC分类号： C09K3/00

CPC分类号： C07C51/43 ,  B01D9/004 ,  B01D9/0045 ,  C07C51/47 ,  C07C63/26

摘要： A method of replacing a first dispersion medium in a starting slurry composed of the first dispersion medium and a terephthalic acid crystal with a second dispersion medium. The starting slurry is tangentially fed to a vertically extending cylindrical portion of a cyclone-shaped nozzle disposed at an upper portion of a replacement tank of a dispersion medium replacement apparatus, from a tangential direction of the cylindrical portion. The fed starting slurry moves circularly along an inner wall of the cylindrical portion. The slurry circularly moving is then discharged from an opening which is disposed at a vertically lower end of the cylindrical portion and dispersed in a second dispersion medium which is fed from a lower portion of the replacement tank. The replaced slurry composed of the terephthalic acid crystal and the second dispersion medium is mainly discharged from the lower portion of the replacement tank, and the first dispersion medium is mainly withdrawn from the upper portion of the replacement tank.

摘要翻译： 用第二分散介质代替由第一分散介质和对苯二甲酸晶体组成的起始浆料中的第一分散介质的方法。 将起始浆料切向地供给到设置在分散介质置换装置的更换罐的上部处的旋转形喷嘴的垂直延伸的圆柱形部分，该圆筒部分从圆柱形部分的切线方向。 进料的起始浆料沿圆柱形部分的内壁圆周移动。 然后，从设置在圆筒部的垂直下端的开口排出循环移动的浆料，并分散在从更换槽的下部供给的第二分散介质中。 由对苯二甲酸晶体和第二分散介质构成的替换浆料主要从更换槽的下部排出，第一分散介质主要从更换槽的上部排出。

公开(公告)号：US20100004484A1

公开(公告)日：2010-01-07

申请号：US12374835

申请日：2007-07-19

申请人： Masato Inari ,  Fumiya Zaima

发明人： Masato Inari ,  Fumiya Zaima

IPC分类号： C07C51/43

CPC分类号： C07C51/42 ,  C07C51/43 ,  C07C63/24

摘要： A method of replacing a first dispersion medium in a starting slurry composed of the first dispersion medium and isophthalic acid crystals with a second dispersion medium. The starting slurry is tangentially fed to a vertically extending cylindrical portion of a cyclone-shaped nozzle disposed at an upper portion of a replacement tank of a dispersion medium replacement apparatus, from a tangential direction of the cylindrical portion. The fed starting slurry moves circularly along an inner wall of the cylindrical portion. The slurry circularly moving is then discharged from an opening which is disposed at a vertically lower end of the cylindrical portion and dispersed in a second dispersion medium which is fed from a lower portion of the replacement tank. The replaced slurry composed of isophthalic acid crystals and the second dispersion medium is mainly discharged from the lower portion of the replacement tank, and the first dispersion medium is mainly withdrawn from the upper portion of the replacement tank.

摘要翻译： 将由第一分散介质和间苯二甲酸晶体构成的起始浆料中的第一分散介质用第二分散介质置换的方法。 将起始浆料切向地供给到设置在分散介质置换装置的更换罐的上部处的旋转形喷嘴的垂直延伸的圆柱形部分，该圆筒部分从圆柱形部分的切线方向。 进料的起始浆料沿圆柱形部分的内壁圆周移动。 然后，从设置在圆筒部的垂直下端的开口排出循环移动的浆料，并分散在从更换槽的下部供给的第二分散介质中。 由间苯二甲酸晶体构成的替代浆料和第二分散介质主要从更换槽的下部排出，第一分散介质主要从更换罐的上部排出。

公开(公告)号：US07071362B2

公开(公告)日：2006-07-04

申请号：US10924811

申请日：2004-08-25

申请人： Tomohiro Sugawara ,  Fumiya Zaima ,  Atsushi Okoshi ,  Kinji Kato ,  Masato Inari

发明人： Tomohiro Sugawara ,  Fumiya Zaima ,  Atsushi Okoshi ,  Kinji Kato ,  Masato Inari

IPC分类号： C07C47/28 ,  C07C47/32

CPC分类号： C07D317/12 ,  C07C45/59 ,  Y02P20/55 ,  C07C47/32

摘要： In the production of an alicyclic aldehyde, a starting aromatic aldehyde is converted into an aromatic acetal for protecting the formyl group. The aromatic ring of the aromatic acetal is then hydrogenated to convert the aromatic acetal into an alicyclic acetal, which is then hydrolyzed to cleave the acetal protecting group to obtain the aimed alicyclic aldehyde.

摘要翻译： 在制备脂环醛时，将起始芳族醛转化成芳族缩醛以保护甲酰基。 然后将芳族缩醛的芳环加氢以将芳族缩醛转化为脂环族缩醛，然后将其水解以切割缩醛保护基以获得目标脂环族醛。

公开(公告)号：US09266810B2

公开(公告)日：2016-02-23

申请号：US13881022

申请日：2011-10-25

申请人： Fumiya Zaima

发明人： Fumiya Zaima

IPC分类号： C07C51/47 ,  B01D71/02 ,  B01D61/14 ,  B01D65/02 ,  B01D63/06

CPC分类号： C07C51/47 ,  B01D61/145 ,  B01D63/066 ,  B01D65/02 ,  B01D71/024 ,  B01D2321/04 ,  C07C63/26 ,  C07C63/24

摘要： Provided is a simple filtering operation method capable of conducting a filtering operation without clogging in a ceramic filter for a long period of time, in the operation of filtering fine crystals of an aromatic carboxylic acid in an oxidation reaction mother liquor obtained in a process of an aromatic carboxylic acid production by a cross-flow filtration using the ceramic filter. The present invention can be accomplished by conducting an operation for filtering the fine crystals and a back washing operation with a filtrate while maintaining a flowing circulation operation of the oxidation reaction mother liquor under predetermined conditions.

摘要翻译： 提供了一种简单的过滤操作方法，其能够在陶瓷过滤器中长时间地进行过滤操作而不会堵塞在过滤中获得的氧化反应母液中的芳族羧酸的微细晶体的操作 使用陶瓷过滤器通过交叉流过滤生产芳香族羧酸。 本发明可以通过在保持预定条件下的氧化反应母液的循环操作的同时进行用于过滤细晶的操作和用滤液进行反洗操作来实现。

公开(公告)号：US08247605B2

公开(公告)日：2012-08-21

申请号：US12374835

申请日：2007-07-19

申请人： Masato Inari ,  Fumiya Zaima

发明人： Masato Inari ,  Fumiya Zaima

IPC分类号： C07C51/42

CPC分类号： C07C51/42 ,  C07C51/43 ,  C07C63/24

摘要： A method of replacing a first dispersion medium in a starting slurry composed of the first dispersion medium and isophthalic acid crystals with a second dispersion medium. The starting slurry is tangentially fed to a vertically extending cylindrical portion of a cyclone-shaped nozzle disposed at an upper portion of a replacement tank of a dispersion medium replacement apparatus, from a tangential direction of the cylindrical portion. The fed starting slurry moves circularly along an inner wall of the cylindrical portion. The slurry circularly moving is then discharged from an opening which is disposed at a vertically lower end of the cylindrical portion and dispersed in a second dispersion medium which is fed from a lower portion of the replacement tank. The replaced slurry composed of isophthalic acid crystals and the second dispersion medium is mainly discharged from the lower portion of the replacement tank, and the first dispersion medium is mainly withdrawn from the upper portion of the replacement tank.

摘要翻译： 将由第一分散介质和间苯二甲酸晶体构成的起始浆料中的第一分散介质用第二分散介质置换的方法。 将起始浆料切向地供给到设置在分散介质置换装置的更换罐的上部处的旋转形喷嘴的垂直延伸的圆柱形部分，该圆筒部分从圆柱形部分的切线方向。 进料的起始浆料沿圆柱形部分的内壁圆周移动。 然后，从设置在圆筒部的垂直下端的开口排出循环移动的浆料，并分散在从更换槽的下部供给的第二分散介质中。 由间苯二甲酸晶体构成的替代浆料和第二分散介质主要从更换槽的下部排出，第一分散介质主要从更换罐的上部排出。

公开(公告)号：US5684187A

公开(公告)日：1997-11-04

申请号：US639966

申请日：1996-04-29

申请人： Fumio Ohkoshi ,  Masato Inary ,  Fumiya Zaima

发明人： Fumio Ohkoshi ,  Masato Inary ,  Fumiya Zaima

IPC分类号： C07C51/487 ,  C07C51/43 ,  C07C63/26 ,  C07C51/42

CPC分类号： C07C51/43

摘要： There is disclosed a process for producing highly pure terephthalic acid by converting a slurry of terephthalic acid crystals in acetic acid solvent which crystals are obtained by liquid-phase oxidation of p-alkylbenzene, into a slurry thereof in water solvent by mother liquor replacement and then subjecting the latter slurry to a catalytic hydrogenation treatment which process comprises the steps of introducing the slurry of terephthalic acid crystals in acetic acid into a mother liquor replacement column at the top portion; forming an accumulation layer of the terephthalic acid crystals at the bottom portion by the sedimentation of the crystals; feeding replacing water sufficient for the formation of upward rising stream of water to the inside of the column at the bottom portion; and withdrawing the accumulation layer of the crystals from the bottom portion of the column. The accumulation layer is kept at a slightly fluidized stable state and is smoothly withdrawn from the bottom of the column by slowly rotating an arm-type agitation blade placed in the layer or by feeding the replacing water dividedly into two trains.

摘要翻译： 公开了通过将通过液相氧化对烷基苯获得的结晶的乙酸溶剂中的对苯二甲酸晶体的浆料转化成其在水溶剂中的浆液，通过母液置换，生产高纯对苯二甲酸的方法，然后 对后一种浆料进行催化加氢处理，该方法包括以下步骤：将对苯二甲酸晶体的淤浆在乙酸中引入到顶部的母液置换塔中; 通过晶体的沉淀在底部形成对苯二甲酸晶体的堆积层; 将足够的水替换为在塔底部向上升起的水流形成塔的内部; 并从柱的底部排出晶体的积聚层。 蓄积层保持在稍微流化的稳定状态，并且通过缓慢旋转放置在该层中的臂式搅拌叶片或通过将替代水分成两部分进料来平缓地从塔的底部排出。