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 The accumulation layer is kept at a slightly fluidized stable state and is smoothly withdrawn from the bottom of the column by slowly rotating an arm-type agitation blade placed in the layer or by feeding the replacing water dividedly into two trains.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。

公开(公告)号：US5679847A

公开(公告)日：1997-10-21

申请号：US642874

申请日：1996-05-06

申请人： Fumio Ohkoshi ,  Masato Inary ,  Fumiya Zaima

发明人： Fumio Ohkoshi ,  Masato Inary ,  Fumiya Zaima

IPC分类号： B01J31/04 ,  C07B61/00 ,  C07C51/265 ,  C07C63/26 ,  C07C51/16

CPC分类号： C07C51/265 ,  Y02P20/52

摘要： There is disclosed a process for producing terephthalic acid which comprises oxidizing in a liquid-phase a starting raw material comprising p-xylene incorporated with 3 to 35% by weight of p-tolualdehyde based on the same at a temperature in the range of 120.degree. to 240.degree. C. by means of a molecular oxygen-containing gas by using a lower aliphatic monocarboxylic acid as a solvent in the presence of a catalyst comprising a manganese compound having 50 to 1000 ppm by weight of manganese atoms, a cobalt compound having 50 to 2000 ppm by weight of cobalt atoms and a bromine compound having 100 to 4000 ppm by weight of bromine atoms, each based on the solvent. By virtue of the above specific constitution, it is made possible to produce high-quality terephthalic acid with a high residual rate of the lower aliphatic monocarboxylic acid as a solvent minimized in its loss, thereby enabling the production of high-quality polyester with high whiteness from the above terephthalic acid and a glycol.

摘要翻译： 公开了一种生产对苯二甲酸的方法，该方法包括在120℃的温度范围内，在液相中氧化含有3-35重量％的对甲苯甲醛的起始原料，其中包含对二甲苯。 在含有50〜1000ppm重量的锰原子的锰化合物的催化剂存在下，通过使用低级脂肪族一元羧酸作为溶剂，通过含分子氧的气体，将含有氧分子的气体，具有50〜 至2000重量ppm的钴原子和溴化合物，其中溴原子的重量为100-4000ppm。 通过上述具体的构成，可以制造具有高残留率的低级脂族一元羧酸作为溶剂使其损失最小化的高质量对苯二甲酸，从而能够生产高白度的高品质聚酯 由上述对苯二甲酸和二醇组成。

公开(公告)号：US5777161A

公开(公告)日：1998-07-07

申请号：US888419

申请日：1997-07-07

申请人： Masato Inary

发明人： Masato Inary

IPC分类号： C07C51/265 ,  C07C51/42 ,  C07C51/43 ,  C07C51/48 ,  C07C63/26

CPC分类号： C07C51/42 ,  C07C51/43

摘要： There is disclosed a process for producing highly pure terephthalic acid by the use of a dispersion medium replacement apparatus equipped with a stirring unit at the bottom portion for uniform dispersion, wherein an original slurry comprising a first dispersion medium and terephthalic acid crystals is introduced into a dispersion medium replacement apparatus at the top portion, a second dispersion medium is introduced into the apparatus at the bottom portion, a replaced slurry comprising principally the second dispersion medium and the terephthalic acid crystals is taken out from the apparatus at the bottom portion, and the first dispersion medium as a major component is taken out from the apparatus at the top portion, which process comprises maintaining a uniformly dispersed slurry at the bottom portion of the apparatus at a concentration higher than that of a slurry at the intermediate portion; maintaining the upper portion at a higher temperature in a vertical temperature distribution therein to form a temperature change zone; and controlling the feed rate of the second dispersion medium and/or the takeout rate of the replaced slurry according to the location of the temperature change zone. By virtue of the specific control system, that is, taking advantage of the temperature change zone, the apparatus can be steadily operated with ease and high reliability at a high replacement efficiency, and thus highly pure terephthalic acid is stably obtained.

摘要翻译： 公开了通过使用在底部配备有搅拌单元的分散介质置换装置来均匀分散来生产高纯度对苯二甲酸的方法，其中将包含第一分散介质和对苯二甲酸晶体的原始浆料引入到 在顶部的分散介质置换装置，在底部将第二分散介质引入装置中，主要从底部的装置中取出包含第二分散介质和对苯二甲酸晶体的置换浆料， 作为主要成分的第一分散介质从顶部的装置中取出，该方法包括以高于中间部分的浆料的浓度将均匀分散的浆料保持在装置的底部; 将其上部维持在较高的温度，并在其中形成温度变化区; 并且根据温度变化区的位置来控制第二分散介质的进料速率和/或替换的浆料的取出速率。 通过具体的控制系统，即利用温度变化区域，能够以高替换效率，容易且高可靠性地稳定地运转设备，从而稳定地得到高纯度的对苯二甲酸。

公开(公告)号：US5712412A

公开(公告)日：1998-01-27

申请号：US562764

申请日：1995-11-27

申请人： Masato Inary ,  Fumio Ohkoshi ,  Fumiya Zaima

发明人： Masato Inary ,  Fumio Ohkoshi ,  Fumiya Zaima

IPC分类号： B01D12/00 ,  C07C51/42

CPC分类号： B01D12/00 ,  C07C51/42

摘要： There are disclosed a method for replacing a dispersion medium wherein an original slurry comprising solid particles and an original dispersion medium is introduced in a dispersion medium replacement column at the top thereof, a replacing dispersion medium is introduced in the column at the bottom thereof to replace the original dispersion medium with the replacing dispersion medium, the resultant replaced slurry comprising the solid particles and the replacing dispersion medium is taken out from the column at the bottom thereof, and the original dispersion medium is taken out from the column at the top thereof, which method comprises dividing the fluid in the intermediate portion into a plurality of parallel streams, stirring the slurry in the bottom of the column to uniformize the slurry, and controlling the feed rates of the replacing dispersion medium and the replaced slurry to maintain the slurry in the bottom portion of the column at a concentration higher than that of the slurry in the intermediate portion of the column; an apparatus for carrying out the method; and a process for producing highly pure terephthalic acid from the slurry comprising an original dispersion medium and crystalline particles of terephthalic acid. The method and apparatus are capable of producing highly pure terephthalic acid at a high replacement efficiency of the dispersion medium with simplified equipment in an extremely advantageous manner.

摘要翻译： 公开了一种更换分散介质的方法，其中将包含固体颗粒和原始分散介质的原始浆料在其顶部引入分散介质置换塔中，将替代分散介质引入塔底部，以代替 具有替代分散介质的原始分散介质，从其底部的塔中取出包含固体颗粒和替代分散介质的所形成的替换浆料，并且从顶部的塔中取出原始分散介质， 该方法包括将中间部分中的流体分成多个平行的流，搅拌塔底部的浆料以使浆料均匀化，并且控制替代分散介质和更换的浆料的进料速率以将浆料保持在 柱的底部浓度高于浆料的浓度 在柱的中间部分; 用于执行该方法的装置; 以及从包含原始分散介质和对苯二甲酸的结晶颗粒的浆料中生产高纯度对苯二甲酸的方法。 该方法和装置能够以非常有利的方式以简化的设备以高分离介质的更换效率制备高纯度对苯二甲酸。

公开(公告)号：US5705682A

公开(公告)日：1998-01-06

申请号：US706890

申请日：1996-09-03

申请人： Fumio Ohkoshi ,  Masato Inary ,  Fumiya Zaima

发明人： Fumio Ohkoshi ,  Masato Inary ,  Fumiya Zaima

IPC分类号： C07C51/265 ,  C07C51/42 ,  C07C51/43 ,  C07C51/46 ,  C07C51/48 ,  C07C51/487 ,  C07C63/26 ,  C07C51/16

CPC分类号： C07C51/42 ,  C07C51/48

摘要： A process for producing highly pure terephthalic acid comprising: (a) oxidizing a p-phenylene compound in the liquid phase in the presence of acetic acid, to produce a liquid-phase oxidation product, (b) separating the liquid-phase oxidation product into the following: (i) a first mother liquid containing acetic acid and (ii) a crude terephthalic acid, (c) evaporating, in whole or in part, the first mother liquid, to produce a vapor, (d) feeding the vapor, or a condensate thereof, to an intermediate stage of a distillation tower, carrying out an azeotropic distillation and withdrawing through a bottom of the distillation tower a concentrated acetic acid, (e) subjecting the crude terephthalic acid to a refining treatment, which is a catalytic hydrotreatment, a catalytic treatment or a recrystallization, which is carried out in the presence of is water, (f) cooling and crystallizing the resultant liquid from step (e), to produce a pure terephthalic acid and a second mother liquor, (g) subjecting the second mother liquor to an extraction in the presence of an azeotrope-forming agent to extract aromatic carboxylic acids contained in second mother liquor, to produce a liquid extract, and (h) recycling the liquid extract to the distillation tower in step (d). The process can greatly reduce the effluent water treatment load and enhance the yield of the objective terephthalic acid, in addition to providing recycling of useful reactants.

摘要翻译： 一种制备高纯度对苯二甲酸的方法，包括：（a）在乙酸存在下，在液相中氧化对亚苯基化合物，以产生液相氧化产物，（b）将液相氧化产物分离成 以下：（i）含有乙酸的第一母液和（ii）粗对苯二甲酸，（c）全部或部分地蒸发第一母液，产生蒸气，（d）将蒸气， 或蒸馏塔的冷凝物，进入蒸馏塔的中间阶段，进行共沸蒸馏并通过蒸馏塔的底部抽出浓缩的乙酸，（e）使粗对苯二甲酸进行精炼处理，其是催化剂 在水存在下进行加氢处理，催化处理或重结晶，（f）冷却并使来自步骤（e）的所得液体结晶，以产生纯对苯二甲酸和第二母液，（g） 苏 在共沸物形成剂的存在下将第二母液喷射到萃取物中，以提取第二母液中所含的芳族羧酸，以产生液体提取物，和（h）在步骤（d）中将液体萃取物再循环到蒸馏塔 ）。 除了提供有用的反应物的回收之外，该方法可以大大降低流出水处理负荷并提高目标对苯二甲酸的产率。