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公开(公告)号：US06242630B1
公开(公告)日：2001-06-05
申请号：US08908095
申请日：1997-08-11
申请人： Stefan Bade , Uwe Schoen , John Burkhard , Franz-Michael Bollenrath , Norbert Hofmann , Hermann-Josef Korte , Hartwig Rauleder , Uwe Tanger
发明人： Stefan Bade , Uwe Schoen , John Burkhard , Franz-Michael Bollenrath , Norbert Hofmann , Hermann-Josef Korte , Hartwig Rauleder , Uwe Tanger
IPC分类号： C07F708
CPC分类号： C07F7/14 , C07F7/0829 , C07F7/1876
摘要： A process for the continuous preparation of 3-halopropylorganosilanes of the general structure RbH3-a-bXaSiCH2CH2CH2Y (III), where: R is CH3, C2H5, C3H7, OCH3, OC2H5 or OC3H7, X is F, Cl, Br or I, Y is F, Cl, Br or I, and a and b are each one of the numbers 0, 1, 2 or 3 and the sum a+b is 1, 2 or 3, comprising reacting, as starting materials, an allyl halide with a silane carrying at least one H atom, wherein the starting materials are present in stoichiometric amounts or one of the starting materials is present in substoichiometric amounts, wherein the reaction carried out is a partial reaction of from 10% to 80%, on a molar basis, of the starting materials, based on either material, when both are present in stoichiometric amounts, or based on the substoichiometric material.
摘要翻译： 连续制备通常结构的3-卤代丙基有机硅烷的方法，其中R为CH 3，C 2 H 5，C 3 H 7，OCH 3，OC 2 H 5或OC 3 H 7，X为F，Cl，Br或I，Y为F，Cl，Br或I， 和b分别为数字0,1,2或3中的一个，并且和a + b为1,2或3，包括使烯丙基卤化物与携带至少一个H原子的硅烷作为原料，其中， 原料以化学计量的量存在，或者一种起始原料以亚化学计量的量存在，其中进行的反应是基于摩尔的10％至80％的起始原料的部分反应，基于任一材料 ，当两者都以化学计量的量存在时，或基于亚化学计量的材料。
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公开(公告)号：US06423858B1
公开(公告)日：2002-07-23
申请号：US09991965
申请日：2001-11-26
IPC分类号： C07F710
CPC分类号： C07F7/1892 , C07F7/20
摘要： Aminoalkylsilanes of formula I: R1R2N—(CH2)y—Si(OR3)3−nR4n (I), wherein R1 and R2 are each independently, identical of different, hydrogen, aryl, arylalkyl or C1-4-alkyl; R3 and R4 are each independently, identical or different, C1-8-alkyl or aryl; y is 2, 3 or 4 and n is 0 or 1, 2 or 3, are prepared by a process comprising: reacting an organosilane of formula II: X—(CH2)y—Si(OR3)3−nR4n (II), wherein X is Cl, Br, I or F; and R3, R4, y and n are each as defined above with ammonia or an organic amine compound of the formula: HNR1R2 (III), wherein R1 and R2 are each as defined above with at least one of R1 and R2 not being hydrogen in a liquid phase; evaporating ammonia or organic amine under reduced pressure while ammonium chloride or aminohydrochloride by-products, produced in the reaction of the first step, remains dissolved in the liquid phase; transferring the product mixture after said evaporation to another vessel operated at a lower pressure level of than the second stage, and allowing ammonium chloride or aminohydrochloride to crystallize; separating the crystalline ammonium chloride or aminohydrochloride from the crude product; and distilling the crude product to produce purified aminoalkylsilane product.
摘要翻译： 式I的氨基烷基硅烷：其中R 1和R 2各自独立地为不同的氢，芳基，芳基烷基或C 1-4 - 烷基; R 3和R 4各自独立地，相同或不同，C 1-8 - 烷基或芳基; y为2,3或4，n为0或1,2或3的方法包括：使式II的有机硅烷：其中X为Cl，Br，I或F; R 3，R 4，y和n各自如上所定义，与氨或下式的有机胺化合物：其中R 1和R 2各自如上所定义，R 1和R 2中的至少一个在液相中不是氢;蒸发氨 或有机胺，同时在第一步骤的反应中产生的氯化铵或氨基盐酸盐副产物保持溶于液相;将所述蒸发之后的产物混合物转移到在低于 第二阶段，使氯化铵或氨基盐酸盐结晶;将结晶氯化铵或氨基盐酸盐与粗产物分离; 并将粗产物蒸馏以产生纯化的氨基烷基硅烷产物。
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公开(公告)号：US06583326B2
公开(公告)日：2003-06-24
申请号：US09970856
申请日：2001-10-05
IPC分类号： C07C3768
摘要： Phenol is separated from a mixture containing hydroxyacetone, cumene, water and phenol, by fractionating the mixture in a process with a fractional distillation step and a phase separation step to provide a single phenol fraction containing less than 300 ppm of hydroxyacetone. In the work-up by distillation of cleavage product mixtures, the hydroxyacetone can be removed from the cleavage product mixture together with a phenol fraction from which the hydroxyacetone has to be removed. A process can be used for purifying cleavage product mixtures obtained in the cleavage of alkylaryl hydroperoxides such as cumene hydroperoxide. The process allows separation of phenol and acetone from mixtures obtained in the cleavage of cumene hydroperoxide.
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4.发明授权Process and apparatus for the work-up by distillation of cleavage product mixtures produced in the cleavage of alkylaryl hydroperoxides 有权在烷基芳基氢过氧化物的裂解中产生的裂解产物混合物通过蒸馏处理的方法和装置公开(公告)号：US06657087B2
公开(公告)日：2003-12-02
申请号：US09986904
申请日：2001-11-13
IPC分类号： C07C4541
摘要： The present invention claims a process and an apparatus for the work-up by distillation of cleavage product mixtures produced in the cleavage of alkylaryl hydroperoxides. Usually, in the work-up by distillation of cleavage product mixtures which are produced in the cleavage of alkylaryl hydroperoxides, the cleavage product mixture is divided into three main fractions, for which at least two distillation columns are used. The use of two distillation columns has the disadvantage that the capital costs, and also the energy costs, in these conventional processes are relatively high. By means of the inventive process for the work-up by distillation of cleavage product mixtures, the equipment requirements and the energy consumption can be markedly reduced in comparison with customary plants, since the cleavage product mixture can be resolved into the three main fractions in only one apparatus. The inventive process can be used for the work-up by distillation of cleavage product mixtures produced in the cleavage of alkylaryl hydroperoxides, in particular in the cleavage of cumene hydroperoxide. By using the inventive process it is possible to separate off phenol and acetone from a cleavage product mixture that was obtained in the cleavage of cumene hydroperoxide.
摘要翻译： 本发明要求用于通过蒸馏处理在烷基芳基氢过氧化物的裂解中产生的裂解产物混合物的方法和装置。 通常，在通过蒸馏在烷基芳基氢过氧化物的裂解中产生的裂解产物混合物的后处理中，将裂解产物混合物分成三个主要馏分，至少使用两个蒸馏塔。 使用两个蒸馏塔的缺点在于，这些常规方法中的资本成本和能源成本都相对较高。通过蒸馏裂解产物混合物的本发明方法，设备要求和 与常规植物相比，能量消耗可以显着降低，因为裂解产物混合物可以在一个装置中分解成三个主要部分。 本发明方法可用于通过蒸馏在烷基芳基氢过氧化物的切割中产生的裂解产物混合物的处理，特别是在氢过氧化枯烯的裂解中的后处理。 通过使用本发明的方法，可以从在氢过氧化枯烯的裂解中获得的裂解产物混合物中分离出苯酚和丙酮。
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5.发明授权Oxidation in the Witten-Hercules process for preparing dimethyl terephthalate 失效用于制备二甲基对苯二甲酸酯的Witten-Hercules方法中的氧化
公开(公告)号：US5869736A
公开(公告)日：1999-02-09
申请号：US949336
申请日：1997-10-14
申请人： Stefan Jelko , Anton Schoengen , Hermann-Josef Korte , Gerhard Franz , Hans-Guenther Srebny , Thomas Jostmann , Frank Steding
发明人： Stefan Jelko , Anton Schoengen , Hermann-Josef Korte , Gerhard Franz , Hans-Guenther Srebny , Thomas Jostmann , Frank Steding
CPC分类号： C07C67/39
摘要： 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.
摘要翻译： 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。
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6.发明授权
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
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。
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公开(公告)号：US5679848A
公开(公告)日：1997-10-21
申请号：US588311
申请日：1996-01-18
CPC分类号： C07C51/09
摘要： A process for the preparation of terephthalic acid (TA) from pure dimethyl terephthalate (DMT) and/or DMT intermediate product by hydrolysis in a countercurrent reactor at a conversion of greater than 99% and crystallization to give the solid product, characterized in that the sum of the stripping steam (S) and reaction water (W) satisfies the relationship L.ltoreq.S+W.ltoreq.2L, wherein (L) represents the amount of water necessary to keep the terephthalic acid (TA) produced largely in solution during the reaction and in the bottom of the reactor, and the terephthalic acid produced is crystallized in a crystallization which is free from washing stages.
摘要翻译： 一种通过在逆流反应器中以大于99％的转化率通过水解从纯对苯二甲酸二甲酯（DMT）和/或DMT中间产物制备对苯二甲酸（TA）的方法，并且结晶得到固体产物，其特征在于， 汽提蒸汽（S）和反应水（W）的总和满足关系L <= S + W
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公开(公告)号：US5614159A
公开(公告)日：1997-03-25
申请号：US419517
申请日：1995-04-10
申请人： Rudolf Modic , Hermann-Josef Korte , Anton Schoengen , Johann-Heinrich Schroeder , J org Porschen
发明人： Rudolf Modic , Hermann-Josef Korte , Anton Schoengen , Johann-Heinrich Schroeder , J org Porschen
IPC分类号： C10L3/10 , B01D53/34 , B01D53/72 , B01D53/77 , F02C3/22 , F02C3/30 , F02C6/00 , F02C3/20 , C07C51/16
摘要： In the purification of an off-gas stream originating from a process of oxidizing a liquid mixture of para-xylene with methyl para-toluate with an oxygen-containing gas under pressure, the off-gas being contaminated with at least one of an aliphatic and an aromatic impurity, which comprises expanding the off-gas stream in an expansion turbine for generating mechanical or electrical energy so as to obtain an at least partial recovery of the energy contained in the off-gas, the improvement comprising subjecting the off-gas to at least one absorption step under pressure to remove at least one component from the off-gas and subjecting the resultant off-gas stream to combustion under a pressure of more than 3 bar prior to expanding the off-gas stream in the expansion turbine.
摘要翻译： 在源自在压力下用含氧气体氧化对二甲苯与对甲苯甲酸甲酯的液体混合物的方法的废气流的净化中，废气被至少一种脂族和 芳族杂质，其包括使膨胀涡轮机中的废气流膨胀以产生机械或电能，以便获得包含在废气中的能量的至少部分回收，其改进包括使尾气处于 在压力下至少一个吸收步骤，从废气中除去至少一种组分，并在扩大膨胀涡轮机内的废气流之前，在大于3巴的压力下使得到的废气流燃烧。
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公开(公告)号：US5277878A
公开(公告)日：1994-01-11
申请号：US889339
申请日：1992-05-28
CPC分类号： B01J19/2435 , B01F3/0451 , B01F3/04836 , C07C67/39 , B01J2219/00081 , Y02P20/582
摘要： A reactor for carrying out heterogeneous-phase reactions, in particular gas/liquid reactions with a continuous liquid phase and a dispersed (discontinuous) gas phase, is described, in which, in a horizontal plane, a substantially vertically upward-directed flow of the reaction medium takes place in a first region of the reactor cross-section and a substantially vertically downward-directed flow takes place in another region of the reactor having a device for dispersing the discontinuous phase such as a dispersing screen, substantially only in the regions with upward-directed flow. The reactor is here designed in such a way that free flow of the reaction medium from regions with downward-directed flow to regions with upward-directed flow is possible in the region of the dispersing device. The preferred use of the proposed reactor is the exothermic oxidation of p-xylene and monomethyl p-toluate with air in the so-called Witten DMT process.
摘要翻译： 描述了用于进行非均相反应的反应器，特别是具有连续液相和分散（不连续）气相的气/液反应，其中在水平面中，基本上垂直向上流动的 反应介质发生在反应器横截面的第一区域中，并且在反应器的另一区域中发生基本上垂直向下的流动，其具有用于分散不连续相的装置，例如分散屏幕，基本上仅在具有 向上流动。 反应器在这里被设计成使得反应介质从具有向下流动的区域到具有向上流动的区域的区域的自由流动在分散装置的区域中是可能的。 所提出的反应器的优选用途是在所谓的Witten DMT工艺中对二甲苯和对甲苯甲酸单甲酯与空气的放热氧化。
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公开(公告)号：US5891410A
公开(公告)日：1999-04-06
申请号：US27160
申请日：1993-02-24
申请人： Rudolf Modic , Hermann-Josef Korte , Anton Schoengen , Johann-Heinrich Schroeder , Jorg Porschen
发明人： Rudolf Modic , Hermann-Josef Korte , Anton Schoengen , Johann-Heinrich Schroeder , Jorg Porschen
IPC分类号： B01D53/14 , B01D53/34 , B01D53/72 , B01D53/75 , B01D53/96 , C07C67/39 , C07C69/82 , C10L3/10 , F02C3/22 , F02C3/30 , B01D53/44
摘要： A process is disclosed for the purification of an off-gas which originates from the oxidation of xylene with air in the Witten process for the preparation of dimethyl terephthalate by subjecting the off-gas to a partial condensation step to remove constituents such as dimethyl terephthalate and xylene; then contacting the off-gas with a solvent such as para-toluic acid or a mixture of para-toluic acid and methyl benzoate so as to remove contaminants such as para-xylene out of the off-gas; then contacting the off-gas with a solvent such as methyl benzoate to remove contaminants such as methyl para-toluate out of the off-gas; then contacting the off-gas with water so as to remove contaminants such as methanol out of the off-gas, and then combusting the off-gas.
摘要翻译： PCT No.PCT / EP91 / 01577 Sec。 371日期：1993年2月24日 102（e）日期1993年2月24日PCT 1991年8月20日PCT PCT。 出版物WO92 / 03213 日期：1992年3月5日公开了在Witten工艺中用于制备二甲基对苯二甲酸二甲酯的废气净化方法，该废气源于二甲苯与空气的氧化，通过使废气进行部分冷凝步骤以除去组分 如对苯二甲酸二甲酯和二甲苯; 然后使尾气与溶剂如对甲苯甲酸或对甲苯甲酸和苯甲酸甲酯的混合物接触，以便从废气中除去诸如对二甲苯之类的污染物; 然后使废气与溶剂如苯甲酸甲酯接触，以从废气中除去污染物如对甲苯甲酸甲酯; 然后使废气与水接触，以便从废气中除去诸如甲醇的污染物，然后使废气燃烧。
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