公开(公告)号：US20110213181A1

公开(公告)日：2011-09-01

申请号：US13048644

申请日：2011-03-15

申请人： Fumiya ZAIMA ,  Masato Inari ,  Hideaki Fujita ,  Nobuo Namiki

发明人： Fumiya ZAIMA ,  Masato Inari ,  Hideaki Fujita ,  Nobuo Namiki

IPC分类号： C07C51/255

CPC分类号： C07C51/47 ,  B01J45/00 ,  B01J49/50 ,  C07C63/26

摘要： A method for producing terephthalic acid comprising: subjecting a p-phenylene compound to a liquid-phase oxidation reaction by the use of a molecular-oxygen-containing gas in the presence of a catalyst at least containing a heavy metal compound and a bromine compound, and hydrous acetic acid having a water content of 1 to 15 mass %, to thereby yield a slurry; regulating the temperature of the slurry to 35 to 140° C., to thereby cause terephthalic acid to precipitate; removing the terephthalic acid through solid-liquid separation, to thereby recover a mother liquor; and recovering the catalyst from the mother liquor through a series of operations (1) to (4), as described, for reusing at least a portion of the catalyst in the liquid-phase oxidation reaction.

摘要翻译： 一种对苯二甲酸的制造方法，其特征在于，在至少含有重金属化合物和溴化合物的催化剂的存在下，通过使用含分子氧的气体对对亚苯基化合物进行液相氧化反应， 水含量为1〜15质量％的含水乙酸，得到浆料; 将浆料的温度调节至35至140℃，从而使对苯二甲酸沉淀; 通过固液分离除去对苯二甲酸，从而回收母液; 并通过如上所述的一系列操作（1）至（4）从母液中回收催化剂，用于在液相氧化反应中重新使用至少一部分催化剂。

公开(公告)号：US08242304B2

公开(公告)日：2012-08-14

申请号：US13048537

申请日：2011-03-15

申请人： Fumiya Zaima ,  Nobuo Namiki ,  Hideaki Fujita ,  Masato Inari

发明人： Fumiya Zaima ,  Nobuo Namiki ,  Hideaki Fujita ,  Masato Inari

IPC分类号： C07C51/16 ,  C07C51/255

CPC分类号： C07C51/47 ,  C07C63/24

摘要： A method for producing isophthalic acid, comprising: subjecting a m-phenylene compound and a molecular-oxygen-containing gas to liquid-phase oxidation reaction in the presence of a catalyst comprising a heavy metal compound and a bromine compound, and hydrous acetic acid having a water content of 1 to 15 mass %, to thereby yield a slurry; regulating the temperature of the slurry to 35 to 140° C., to thereby precipitate isophthalic acid; removing the isophthalic acid through solid-liquid separation, to thereby recover a mother liquor; and recovering the catalyst from the mother liquor by following steps (1) to (4) as described.

摘要翻译： 一种间苯二甲酸的制造方法，其特征在于，在含有重金属化合物和溴化合物的催化剂的存在下，使间亚苯基化合物和含分子氧气体进行液相氧化反应， 水含量为1〜15质量％，由此得到浆料; 将浆料的温度调节至35〜140℃，由此沉淀间苯二甲酸; 通过固液分离除去间苯二甲酸，从而回收母液; 并按照如上所述的步骤（1）至（4）从母液中回收催化剂。

公开(公告)号：US08236982B2

公开(公告)日：2012-08-07

申请号：US13048644

申请日：2011-03-15

申请人： Fumiya Zaima ,  Masato Inari ,  Hideaki Fujita ,  Nobuo Namiki

发明人： Fumiya Zaima ,  Masato Inari ,  Hideaki Fujita ,  Nobuo Namiki

IPC分类号： C07C51/16 ,  C07C51/255

CPC分类号： C07C51/47 ,  B01J45/00 ,  B01J49/50 ,  C07C63/26

摘要： A method for producing terephthalic acid comprising: subjecting a p-phenylene compound to a liquid-phase oxidation reaction by the use of a molecular-oxygen-containing gas in the presence of a catalyst at least containing a heavy metal compound and a bromine compound, and hydrous acetic acid having a water content of 1 to 15 mass %, to thereby yield a slurry; regulating the temperature of the slurry to 35 to 140° C., to thereby cause terephthalic acid to precipitate; removing the terephthalic acid through solid-liquid separation, to thereby recover a mother liquor; and recovering the catalyst from the mother liquor through a series of operations (1) to (4), as described, for reusing at least a portion of the catalyst in the liquid-phase oxidation reaction.

摘要翻译： 一种对苯二甲酸的制造方法，其特征在于，在至少含有重金属化合物和溴化合物的催化剂的存在下，通过使用含分子氧的气体对对亚苯基化合物进行液相氧化反应， 水含量为1〜15质量％的含水乙酸，得到浆料; 将浆料的温度调节至35至140℃，从而使对苯二甲酸沉淀; 通过固液分离除去对苯二甲酸，从而回收母液; 并通过如上所述的一系列操作（1）至（4）从母液中回收催化剂，用于在液相氧化反应中重新使用至少一部分催化剂。

公开(公告)号：US20110213180A1

公开(公告)日：2011-09-01

申请号：US13048537

申请日：2011-03-15

申请人： Fumiya ZAIMA ,  Nobuo Namiki ,  Hideaki Fujita ,  Masato Inari

发明人： Fumiya ZAIMA ,  Nobuo Namiki ,  Hideaki Fujita ,  Masato Inari

IPC分类号： C07C51/255

CPC分类号： C07C51/47 ,  C07C63/24

摘要： A method for producing isophthalic acid, comprising: subjecting a m-phenylene compound and a molecular-oxygen-containing gas to liquid-phase oxidation reaction in the presence of a catalyst comprising a heavy metal compound and a bromine compound, and hydrous acetic acid having a water content of 1 to 15 mass %, to thereby yield a slurry; regulating the temperature of the slurry to 35 to 140° C., to thereby precipitate isophthalic acid; removing the isophthalic acid through solid-liquid separation, to thereby recover a mother liquor; and recovering the catalyst from the mother liquor by following steps (1) to (4) as described.

摘要翻译： 一种间苯二甲酸的制造方法，其特征在于，在含有重金属化合物和溴化合物的催化剂的存在下，使间亚苯基化合物和含分子氧气体进行液相氧化反应， 水含量为1〜15质量％，由此得到浆料; 将浆料的温度调节至35〜140℃，由此沉淀间苯二甲酸; 通过固液分离除去间苯二甲酸，从而回收母液; 并按照如上所述的步骤（1）至（4）从母液中回收催化剂。

公开(公告)号：US20100016629A1

公开(公告)日：2010-01-21

申请号：US12518662

申请日：2007-12-07

申请人： Fumiya Zaima ,  Masato Inari ,  Hideaki Fujita ,  Nobuo Namiki

发明人： Fumiya Zaima ,  Masato Inari ,  Hideaki Fujita ,  Nobuo Namiki

IPC分类号： C07C51/265

CPC分类号： C07C51/47 ,  B01J45/00 ,  B01J49/50 ,  C07C63/26

摘要： The invention provides a method for producing terephthalic acid, characterized by including subjecting a p-phenylene compound to liquid-phase oxidation reaction by use of a molecular-oxygen-containing gas in the presence of a catalyst at least containing a heavy metal compound and a bromine compound, and hydrous acetic acid having a water content of 1 to 15 mass %, to thereby yield a slurry; regulating the temperature of the slurry to 35 to 140° C., to thereby cause terephthalic acid to precipitate; removing the terephthalic acid through solid-liquid separation, to thereby recover a mother liquor; and recovering the catalyst from the mother liquor through a series of the following steps (1) to (4) for reusing at least a portion of the catalyst in the liquid-phase oxidation reaction: (1) an adsorption step including regulating the ratio “amount by mole of bromide ions in the mother liquor/total amount by mole of heavy metal ions in the mother liquor” to 0.6 to 3, and then exposing the mother liquor to a pyridine-ring-containing chelate resin which has been heated to 35 to 140° C., so that the resin adsorbs catalyst-derived heavy metal ions and bromide ions, and also adsorbs a carboxylic acid mixture which has been by-produced through the liquid-phase oxidation reaction, (2) an elution step (A) of exposing hydrous acetic acid having a water content of 1 to 15 mass % to the pyridine-ring-containing chelate resin which has undergone the adsorption step, thereby yielding an eluate containing the by-produced carboxylic acid mixture, (3) an elution step (B) of exposing water or hydrous acetic acid having a water content of 20 mass % or more to the pyridine-ring-containing chelate resin which has undergone the elution step (A), thereby yielding an eluate containing catalyst-derived heavy metal ions and bromide ions, and (4) a displacement step of exposing hydrous acetic acid having a water content of 1 to 15 mass % to the pyridine-ring-containing chelate resin which has undergone the elution step (B), serving as a displacement liquid, thereby regenerating the resin.

公开(公告)号：US5880313A

公开(公告)日：1999-03-09

申请号：US139677

申请日：1998-08-25

申请人： Fumiya Zaima ,  Hideaki Fujita ,  Masami Matsumoto ,  Masato Inari

发明人： Fumiya Zaima ,  Hideaki Fujita ,  Masami Matsumoto ,  Masato Inari

IPC分类号： C07C51/265 ,  C07C51/16

CPC分类号： C07C51/265

摘要： A process for continuously producing an aromatic carboxylic acid comprising oxidizing an aromatic compound substituted with alkyl groups with molecular oxygen gas in the liquid phase in a solvent containing a lower aliphatic carboxylic acid in the presence of a catalyst comprising heavy metal compounds and a bromine compound, wherein a mother liquor which is obtained after removal of crystals from a reaction liquid of the liquid phase oxidation and contains heavy metal ions and bromine ion as catalyst components is brought into contact with a chelate resin of an anion exchange type to recover the catalyst components.The catalyst components are efficiently recovered, and auxiliary agents in an amount exceeding the equivalent amount and excessive labor are not necessary.

摘要翻译： 一种连续生产芳族羧酸的方法，包括在含有重金属化合物和溴化合物的催化剂存在下，在含有低级脂肪族羧酸的溶剂中，将在液相中的分子氧气用烷基取代的芳族化合物氧化， 其中将从液相氧化反应液中除去结晶并含有重金属离子和溴离子作为催化剂组分的母液与阴离子交换型螯合树脂接触以回收催化剂组分。 有效地回收催化剂组分，并且不需要超过相当量和过量劳动量的助剂。

公开(公告)号：US20100048943A1

公开(公告)日：2010-02-25

申请号：US12520625

申请日：2007-12-07

申请人： Fumiya Zaima ,  Nobuo Namiki ,  Hideaki Fujita

发明人： Fumiya Zaima ,  Nobuo Namiki ,  Hideaki Fujita

IPC分类号： C07C51/21

CPC分类号： C07C51/47 ,  C07C63/24

摘要： The invention provides a method for producing isophthalic acid, characterized by including subjecting a m-phenylene compound to liquid-phase oxidation reaction by use of a molecular-oxygen-containing gas in the presence of a catalyst at least containing a heavy metal compound and a bromine compound, and hydrous acetic acid having a water content of 1 to 15 mass %, to thereby yield a slurry; regulating the temperature of the slurry to 35 to 140° C., to thereby cause isophthalic acid to precipitate; removing the isophthalic acid through to solid-liquid separation to thereby recover a mother liquor; and recovering the catalyst from the mother liquor through a series of the following steps (1) to (4) for reusing at least a portion of the catalyst in the liquid-phase oxidation reaction: (1) an adsorption step including regulating the ratio “amount by mole of bromide ions in the mother liquor/total amount by mole of heavy metal ions in the mother liquor” to 0.3 to 3, and then exposing the mother liquor to a pyridine-ring-containing chelate resin which has been heated to 35 to 140° C., so that the resin adsorbs catalyst-derived heavy metal ions and bromide ions, and also adsorbs a carboxylic acid mixture which has been by-produced through the liquid-phase oxidation reaction, (2) an elution step (A) of exposing hydrous acetic acid having a water content of 1 to 15 mass % to the pyridine-ring-containing chelate resin which has undergone the adsorption step, thereby yielding an eluate containing the by-produced carboxylic acid mixture, (3) an elution step (B) of exposing water or hydrous acetic acid having a water content of 20 mass % or more to the pyridine-ring-containing chelate resin which has undergone the elution step (A), thereby yielding an eluate containing catalyst-derived heavy metal ions and bromide ions, and (4) a displacement step of exposing hydrous acetic acid having a water content of 1 to 15 mass % to the pyridine-ring-containing chelate resin which has undergone the elution step (B), serving as a displacement liquid, thereby regenerating the resin.

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：US09347112B2

公开(公告)日：2016-05-24

申请号：US13579779

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 ,  C07C51/255 ,  C08K5/00 ,  C08K5/10 ,  C08K5/101 ,  C22B3/24 ,  C07C51/42 ,  C07C51/47 ,  B01J45/00 ,  C22B3/36 ,  C22B7/00

CPC分类号： C22B3/24 ,  B01J45/00 ,  C07C51/42 ,  C07C51/47 ,  C22B3/0036 ,  C22B7/006 ,  Y02P10/234 ,  Y02P20/52 ,  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 a terephthalic 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： 在生产对苯二甲酸的过程中，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使用的含吡啶环的螯合树脂时， 树脂膨胀等现象，树脂发热，产生气泡等，从而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：US20130281732A1

公开(公告)日：2013-10-24

申请号：US13881021

申请日：2011-10-25

申请人： Fumiya Zaima ,  Nirou Hoshishima ,  Kazutoshi Uozumi ,  Hideaki Fujita

发明人： Fumiya Zaima ,  Nirou Hoshishima ,  Kazutoshi Uozumi ,  Hideaki Fujita

IPC分类号： C07C51/42

CPC分类号： C07C51/42 ,  B01D61/145 ,  B01D63/066 ,  B01D65/02 ,  B01D71/024 ,  B01D2315/10 ,  B01D2321/04 ,  C07C51/43 ,  C07C63/26

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 terephthalic acid in an oxidation reaction mother liquor obtained in a process of terephthalic 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： 提供一种简单的过滤操作方法，其能够在对苯二甲酸生产过程中获得的氧化反应母液中过滤细小的对苯二甲酸的结晶的过程中长时间地进行过滤操作而不堵塞陶瓷过滤器 通过使用陶瓷过滤器的交叉流过滤。 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。