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1. 发明授权

US5286896A Process for the production of DMT-intermediate product of specific purity 失效
标题翻译：生产具有特异纯度的DMT-中间体产品的方法
公开(公告)号：US5286896A
公开(公告)日：1994-02-15
申请号：US761768
申请日：1991-08-15
申请人： Hermann-Josef Korte , Anton Miletic , Hans U. Neutzler , Anton Schoengen , Johann H. Schroeder , Ralf Wirges
发明人： Hermann-Josef Korte , Anton Miletic , Hans U. Neutzler , Anton Schoengen , Johann H. Schroeder , Ralf Wirges
IPC分类号： C07C67/52 , C07C63/26 , C07C67/39 , C07C69/82
CPC分类号： C07C67/39 , C07C67/54
摘要： 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.
摘要翻译：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。

2. 发明授权

US5338882A Process for the production of DMT-intermediate product of specific purity and pure terephthalic acid 失效
标题翻译：生产具有特异纯度的DMT-中间产物和纯对苯二甲酸的方法
公开(公告)号：US5338882A
公开(公告)日：1994-08-16
申请号：US145540
申请日：1993-11-04
申请人： Hermann-Josef Korte , Anton Miletic , Hans U. Neutzler , Anton Schoengen , Johann H. Schroeder , Ralf Wirges
发明人： Hermann-Josef Korte , Anton Miletic , Hans U. Neutzler , Anton Schoengen , Johann H. Schroeder , Ralf Wirges
IPC分类号： C07C67/52 , C07C63/26 , C07C67/39 , C07C69/82 , C07C51/09 , C07C51/43
CPC分类号： C07C67/39 , C07C67/54
摘要： 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.
摘要翻译：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。

3. 发明授权

US4642377A Process for producing terephthalic acid from p-xylene and methanol by way of dimethyl terephthalate 失效
标题翻译：通过对苯二甲酸二甲酯由对二甲苯和甲醇生产对苯二甲酸的方法
公开(公告)号：US4642377A
公开(公告)日：1987-02-10
申请号：US707579
申请日：1985-03-04
申请人： Rudolf Modic , Jorg Porschen , Anton Schoengen , Ralf Wirges
发明人： Rudolf Modic , Jorg Porschen , Anton Schoengen , Ralf Wirges
IPC分类号： C07C63/26 , C07C51/00 , C07C51/09 , C07C67/00 , C07C67/39 , C07C69/82
CPC分类号： C07C51/09 , C07C67/39
摘要： A process for the production of terephthalic acid from p-xylene and methanol by way of the dimethyl terephthalate obtained by oxidation, in the liquid phase with atmospheric oxygen in the presence of dissolved heavy metal compounds as the catalyst, of a mixture of p-xylene and a fraction containing predominantly methyl p-toluate, which fraction is recycled into the oxidation, to obtain an oxidation product containing primarily p-toluic acid and monomethyl terephthalate at a temperature of 140.degree.-170.degree. C. and under a pressure of 4-8 bar; by esterification of the oxidation product in a reactor with liquid and subsequently vaporized methanol brought to an elevated pressure, at a temperature of 220.degree.-280.degree. C. and under a pressure of 20-25 bar to obtain a raw ester containing primarily methyl p-toluate and dimethyl terephthalate; by withdrawing the raw ester fraction and a methanol-containing vapor fraction from the esterification reactor; by distillatory separation of the raw ester into a methyl p-toluate fraction and a fraction rich in terephthalic aldehyde methyl ester, which fractions are recycled into the oxidation, a raw dimethyl terephthalate fraction, and a residual fraction; and by hydrolysis of the raw dimethyl terephthalate fraction with water, obtaining the thus-formed terephthalic acid and separation of a methanol-water mixture. In this process, the methanol-containing vapor fraction and the methanol-water mixture are separated by rectification under elevated pressure and elevated temperature into a methanol-rich head fraction and an aqueous sump phase, the methanol formed at the head of the rectification stage is withdrawn in vapor phase under elevated pressure, and esterification of the oxidation product is conducted with the methanol-containing vapor brought by compression to esterification pressure and esterification temperature.
摘要翻译：通过在溶解的重金属化合物作为催化剂的存在下，在与常压氧气的液相中通过氧化获得的对二甲苯和甲醇制备对苯二甲酸的方法，将对二甲苯和主要含有对甲苯甲酸甲酯的级分，该级分被再循环到氧化中，得到主要对甲苯甲酸和对甲基苯甲酸单甲酯在140-170℃的温度和4- 8巴; 通过将反应器中的氧化产物在液体中酯化并随后蒸发的甲醇在220-280℃的温度和20-25巴的压力下进行升高的压力，得到主要含有甲基p - 对苯二甲酸二甲酯和对苯二甲酸二甲酯; 通过从酯化反应器中取出原始酯馏分和含甲醇的蒸气馏分; 通过将原料酯蒸馏分离成对甲苯甲酸甲酯馏分和富含对苯二甲酸甲酯的馏分，将这些馏分循环到氧化中，生成二甲基对苯二甲酸酯馏分和残余馏分; 并用水对生成的对苯二甲酸二甲酯部分进行水解，得到如此形成的对苯二甲酸并分离甲醇 - 水混合物。在此过程中，将含甲醇的蒸气馏分和甲醇 - 水混合物在升高的压力和升高的温度下通过精馏分离成富含甲醇的头馏分和水池，在精馏段的顶部形成的甲醇为在气相中在升高的压力下取出，氧化产物的酯化是通过压缩所产生的含甲醇的蒸气进行酯化压力和酯化温度进行的。

4. 发明授权

US4642369A Process for the production of dimethyl terephthalate from p-xylene and methanol 失效
公开(公告)号：US4642369A
公开(公告)日：1987-02-10
申请号：US707696
申请日：1985-03-04
申请人： Rudolf Modic , Jorg Porschen , Anton Schoengen , Ralf Wirges
发明人： Rudolf Modic , Jorg Porschen , Anton Schoengen , Ralf Wirges
IPC分类号： C07C69/82 , C07C51/09 , C07C67/00 , C07C67/08 , C07C67/39
CPC分类号： C07C67/08 , C07C51/09 , C07C67/39
摘要： A process for the production of dimethyl terephthalate from p-xylene and methanol by oxidation in a reactor, in the liquid phase with atmospheric oxygen in the presence of dissolved heavy metal compounds as a catalyst, of a mixture of p-xylene and a fraction containing predominantly methyl p-toluate, which fraction is recycled into the oxidation, to obtain an oxidation product containing primarily p-toluic acid and monomethyl terephthalate, at a temperature of 140.degree.-170.degree. C. and under a pressure of 4-8 bar; by esterification of the oxidation product with liquid and subsequently vaporized methanol brought to an elevated pressure, at a temperature of 220.degree.-280.degree. C. and under a pressure of 20-25 bar in a reactor to obtain a raw ester containing primarily p-toluate and dimethyl terephthalate; by withdrawing the raw ester fraction and a methanol-containing vapor fraction from the esterification stage, by distillatory separation of the raw ester into a p-toluate fraction which is recycled into the oxidation, a raw dimethyl terephthalate fraction which is subjected to further processing by recrystallization in methanol, and a residual fraction which is optionally subjected to a thermal aftertreatment or a reactive treatment with methanol and is partially recycled into the process after a subsequent working-up step by distillation. In this process, the esterification of the oxidation product is conducted with a methanol-containing vapor, brought by compression to the elevated pressure and elevated temperature required for esterification, which methanol-containing vapor has been obtained from the filtrate of the recrystallization of the raw dimethyl terephthalate fraction by vaporization or also by rectification of the methanol-containing vapor fraction and optionally additional methanol-containing process streams, under a pressure lying below the pressure utilized in the esterification reactor.

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