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    • 2. 发明授权
    • Oxidation in the Witten-Hercules process for preparing dimethyl
terephthalate
    • 用于制备二甲基对苯二甲酸酯的Witten-Hercules方法中的氧化
    • US5869736A
    • 1999-02-09
    • US949336
    • 1997-10-14
    • Stefan JelkoAnton SchoengenHermann-Josef KorteGerhard FranzHans-Guenther SrebnyThomas JostmannFrank Steding
    • Stefan JelkoAnton SchoengenHermann-Josef KorteGerhard FranzHans-Guenther SrebnyThomas JostmannFrank Steding
    • C07C67/39C07C69/82C07C67/00
    • C07C67/39
    • A process is provided for the oxidation of p-xylene and methyl p-tolulate with oxygen-containing gases in the Witten-Hercules process for preparing dimetyl terephthalate in at least two sequentially arranged stages and in the presence of a catalyst, wherein the process involves oxidizing p-xylene and methyl p-toluate with oxygen containing gases in at least two sequential stages in the presence of a catalyst, wherein the at least two sequential stages include at least one p-xylene rich stage and at least one methyl p-toluate rich stage, wherein at least one of the following steps (a) and (b) occurs:(a) in the at least one p-xylene rich stage at least a portion of p-xylene present is oxidized in the presence of 5 to 30% by mass of methyl p-toluate, based on a total amount of oxidation mixture in the at least one p-xylene rich stage; or(b) in the methyl p-toluate rich stage at least one of methyl p-toluate or p-toluic acid is oxidized in the presence of 2 to 30% by mass of p-xylene, based on a total amount of methyl p-toluate and p-toluic acid in the methyl p-toluate rich stage.
    • 提供了一种用于在Witten-Hercules方法中用含氧气体氧化对二甲苯和甲基对氨基苯甲酸的方法,用于在至少两个顺序排列的阶段和在催化剂存在下制备对苯二甲酸二甲酯,其中所述方法涉及 在存在催化剂的情况下,在至少两个连续的阶段中使含氧气体氧化对二甲苯和对甲苯甲酸甲酯,其中所述至少两个连续步骤包括至少一个富含对二甲苯的级和至少一种对甲苯甲酸甲酯 其中发生以下步骤(a)和(b)中的至少一个:(a)在所述至少一个对二甲苯富集阶段中,存在的对二甲苯的至少一部分在5至5的存在下被氧化 30质量%的对甲苯甲酸甲酯,基于至少一个对二甲苯富集阶段的氧化混合物的总量; 或(b)在富甲苯甲酸甲酯中,基于甲基p的总量,在2-30质量%的对二甲苯的存在下,将对甲苯甲酸甲酯或对甲苯甲酸甲酯中的至少一种氧化 - 甲苯磺酸和对甲苯甲酸。
    • 3. 发明授权
    • Process for the production of DMT-intermediate product of specific purity
    • 生产具有特异纯度的DMT-中间体产品的方法
    • US5286896A
    • 1994-02-15
    • US761768
    • 1991-08-15
    • Hermann-Josef KorteAnton MileticHans U. NeutzlerAnton SchoengenJohann H. SchroederRalf Wirges
    • Hermann-Josef KorteAnton MileticHans U. NeutzlerAnton SchoengenJohann H. SchroederRalf Wirges
    • C07C67/52C07C63/26C07C67/39C07C69/82
    • 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.
    • 本发明涉及一种制备DMT中间体产品的方法及其随后对高纯度DMT和高纯度和超纯对苯二甲酸的处理。 DMT中间产物通过主要含有副产物(p-X)和对甲苯酸甲酯(p-TE)的混合物与含氧气体的液相联合氧化来制备。 所产生的酸用甲醇酯化,酯化产物分离成富含p-TE的馏分I,含有大于99wt。 %的DMT及其异构体和具有高沸点的残余物级分III,并且将p-TE馏分I再循环至氧化。 残渣馏分III的DMT含量为15〜70重量%。 %,通过在甲醇中简单溶剂重结晶纯化DMT馏分I,得到其中甲基羟基苯甲酸酯(HM-BME)和对苯二甲酸甲酯(TAE)总共低于200ppm的DMT中间产物。 随后将DMT中间产物加工成超纯DMT,通过第二次再结晶进行,随后通过在甲醇中洗涤DMT中间体产物进行对苯二甲酸处理,水解,结晶,并在必要时随后在水中洗涤。
    • 6. 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。