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    • 13. 发明授权
    • Process for producing highly pure terephthalic acid
    • 高纯度对苯二甲酸生产方法
    • US5684187A
    • 1997-11-04
    • US639966
    • 1996-04-29
    • Fumio OhkoshiMasato InaryFumiya Zaima
    • Fumio OhkoshiMasato InaryFumiya Zaima
    • C07C51/487C07C51/43C07C63/26C07C51/42
    • C07C51/43
    • 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 The accumulation layer is kept at a slightly fluidized stable state and is smoothly withdrawn from the bottom of the column by slowly rotating an arm-type agitation blade placed in the layer or by feeding the replacing water dividedly into two trains.
    • 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。
    • 16. 发明授权
    • Process for the production of DMT-intermediate product of specific
purity and pure terephthalic acid
    • 生产具有特异纯度的DMT-中间产物和纯对苯二甲酸的方法
    • US5338882A
    • 1994-08-16
    • US145540
    • 1993-11-04
    • Hermann-Josef KorteAnton MileticHans U. NeutzlerAnton SchoengenJohann H. SchroederRalf Wirges
    • Hermann-Josef KorteAnton MileticHans U. NeutzlerAnton SchoengenJohann H. SchroederRalf Wirges
    • C07C67/52C07C63/26C07C67/39C07C69/82C07C51/09C07C51/43
    • C07C67/39C07C67/54
    • The invention relates to a process for the production of a DMT intermediate product as well as its working up to fibregrade DMT and to medium pure and pure terephthalic acid. The DMT intermediate product is moreover produced by combined oxidation of a predominantly para-xylene (p-X) and para-toluic acid methyl ester (p-TE) containing mixture in liquid phase with an oxygen containing gas, esterification of the acids being produced with methanol, distillative or rectificative separation of the esterification products being produced into a p-TE rich fraction I, a fraction II containing more than 99% by weight DMT and its isomers and a high boiling residue fraction III as well as feeding back the p-TE fraction I into the oxidation, with the residue fraction III having a DMT content of 15 to 70% by weight and the DMT fraction II being purified by single solvent recrystallisation in methanol to form the DMT intermediate product to such an extent that the amounts of hydroxymethylbenzoic acid methyl ester (HM-BME) and terephthalic acid methyl ester (TAE) in the DMT intermediate product amount together to less than 200 ppm.
    • 本发明涉及一种生产DMT中间产物以及其加工成纤维分级DMT和中纯纯对苯二甲酸的方法。 此外,DMT中间体产物通过主要在对二甲苯(pX)和对甲苯甲酸甲酯(p-TE)的液相混合物与含氧气体的组合氧化产生,所述酸与甲醇的酯化反应 ,产生的酯化产物的蒸馏或精馏分离成富含p-TE的馏分I,含有大于99重量%DMT及其异构体的馏分II和高沸点残渣馏分III,以及将p-TE 馏分I进入氧化,其中残余物馏分III的DMT含量为15至70重量%,DMT馏分II通过在甲醇中的单一溶剂重结晶纯化以形成DMT中间产物,使得羟甲基苯甲酸的量 DMT中间体产物中的酸甲酯(HM-BME)和对苯二甲酸甲酯(TAE)的含量一起低于200ppm。
    • 18. 发明授权
    • Improved process for recovery of purified terephthalic acid
    • 改进纯化对苯二甲酸的回收方法
    • US5175355A
    • 1992-12-29
    • US810725
    • 1991-12-18
    • Debra J. StreichDiane J. GrazianoSandra K. SchillerRoger J. Grimm
    • Debra J. StreichDiane J. GrazianoSandra K. SchillerRoger J. Grimm
    • C07C63/26C07C51/42C07C51/43C07C51/47C07F9/46
    • C07F9/46C07C51/43
    • A process is disclosed for preparation of purified terephthalic acid containing 200 ppmw or less of p-toluic acid. A filter cake of purified terephthalic acid is prepared by filtering, under a differential pressure of about or greater than 0.5 psi over the system pressure and a temperature within the range of from about 100.degree. C. to about 205.degree. C., an aqueous slurry of purified terephthalic acid containing a solution of p-toluic acid. The aqueous solution of p-toluic acid remaining in the filter cake of purified terephthalic acid is displaced from the filter cake by water under a pressure gradient over the system pressure at a temperature within the range of from about 100.degree. C. to about 205.degree. C. Pressure flash evaporation of water remaining in the filter cake occurs upon release of the system pressure to lower pressure with consequent lower temperature. The crystalline terephthalic acid product containing 200 ppmw or less p-toluic acid can be dried under atmospheric pressure. Purified terephthalic acid is useful for the manufacture of polyesters from which clothing and related goods are made.
    • 公开了一种制备含有200ppmw或更少的对甲苯甲酸的纯对苯二甲酸的方法。 纯化的对苯二甲酸的滤饼通过在系统压力和约100℃至约205℃范围内的温度下在约或大于0.5psi的压差下过滤来制备,水性浆料 的含对苯甲酸溶液的纯对苯二甲酸。 保留在纯化对苯二甲酸的滤饼中的对甲苯甲酸的水溶液在压力梯度下在压力梯度下在约100℃至约205℃的温度范围内从水中从滤饼中移出。 C.将系统压力释放到较低压力并随之降低温度时,会发生残留在滤饼中的水的压力闪蒸。 含有200ppmw以下的对甲苯甲酸的结晶对苯二甲酸产物可以在大气压下干燥。 纯化的对苯二甲酸可用于制造服装和相关商品的聚酯。
    • 19. 发明授权
    • Extraction process for removal of impurities from terephthalic acid
filtrate
    • 从对苯二甲酸滤液中除去杂质的萃取方法
    • US4939297A
    • 1990-07-03
    • US361176
    • 1989-06-05
    • Larry W. BrowderJames C. MedlinArt T. Spaugh, Jr.
    • Larry W. BrowderJames C. MedlinArt T. Spaugh, Jr.
    • C07C63/26B01J31/40C07C51/42C07C51/48
    • C07C51/42C07C51/48Y02P20/52
    • A method for removing impurities from an oxidative terephthalic acid synthesis mother liquor containing acetic acid, water, corrosion metals, a metal catalyst and organic impurities, comprising the steps of (a) removing from the mother liquor by evaporation from 50-95% of the acetic acid and water contained therein; (b) adding an amount of water to the concentrated mother liquor sufficient to dissolve the metal catalyst and form an aqueous mixture; (c) extracting the aqueous mixture by counter-current extraction with a substantially water-insoluble organic solvent, to produce a lighter phase containing the organic solvent, a minor amount of the water, acetic acid and the organic impurities and a heavier phase containing a major amount of the water, corrosion metals and the metal catalyst, and; (d) removing the corrosion metals from the heavier phase by heating and filtering, and; (e) removing the organic impurities from the lighter phase by distillation.
    • 一种从含有乙酸,水,腐蚀金属,金属催化剂和有机杂质的氧化对苯二甲酸合成母液中除去杂质的方法,包括以下步骤:(a)通过蒸发从母液中除去50-95% 其中含有乙酸和水; (b)向浓缩母液中加入足够量的水以溶解金属催化剂并形成含水混合物; (c)通过用基本上不溶于水的有机溶剂逆流萃取来提取含水混合物,以产生含有有机溶剂,少量水,乙酸和有机杂质的较浅相,以及含有 主要量的水,腐蚀金属和金属催化剂,以及; (d)通过加热和过滤从较重的相中除去腐蚀金属; (e)通过蒸馏从较轻的相中除去有机杂质。