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1. 发明授权

US6028215A Process for preparing esters of carboxylic acids 失效
标题翻译：制备羧酸酯的方法
公开(公告)号：US6028215A
公开(公告)日：2000-02-22
申请号：US109767
申请日：1998-07-06
申请人： Bernd Bessling , Bernd Lohe , Rudiger Welker , Walter Disteldorf , Jean Werner Knab
发明人： Bernd Bessling , Bernd Lohe , Rudiger Welker , Walter Disteldorf , Jean Werner Knab
IPC分类号： B01J31/08 , B01D3/00 , B01D3/14 , B01J8/04 , B01J19/24 , B01J19/32 , C07B61/00 , C07C67/08 , C07C67/54 , C07C69/14 , C07C69/16
CPC分类号： C07C67/08 , B01D3/009 , B01D3/14 , B01J19/32 , B01J8/0453 , C07C67/54 , B01J2208/00814 , Y02P20/127
摘要： A process for preparing esters from alcohol and carboxylic acid by a) feeding a mixture, comprising at least alcohol and/or carboxylic acid as educts, into a distillation column with separated sections containing reactive and conventional internals, wherein the reactive internals are arranged below the inlet of the mixture and conventional internals are arranged above the inlet of the mixture, b) reaction of the alcohol and the carboxylic acid in the reactive internals in presence of a catalyst, c) distillative separation of the evolving reaction mixture into the higher boiling ester and a lower boiling azeotrope containing alcohol, water and ester, wherein the ester accumulates in the bottom and the azeotrope is removed overhead, d) separation of the azeotrope in a phase separator in an aqueous phase and in an organic phase and the organic phase to be returned to the top of the column, wherein in step b) a heterogenous catalyst is utilized and in step c) the ester is taken off above the bottom as pure product between further conventional internals which differ in their arrangement from those in step a) and which are arranged above the inlet of a circulating evaporator.
摘要翻译：一种由醇和羧酸制备酯的方法，其方法是：a）将含有至少醇和/或羧酸的混合物作为离子液体进料到具有包含反应性和常规内部物质的分离部分的蒸馏塔中，其中反应性内部件布置在混合物入口和常规内件布置在混合物入口的上方，b）在催化剂存在下，醇和羧酸在反应性内件中的反应，c）将放出的反应混合物蒸馏分离成高沸点酯和含有醇，水和酯的低沸点共沸物，其中酯积聚在底部，共沸物在塔顶除去，d）将相分离器中的共沸物在水相和有机相中分离，并将有机相分离成返回到塔的顶部，其中在步骤b）中使用异种催化剂，并且在步骤c）中，将酯从t上方取出他作为在其布置方式与步骤a）中不同的另外的常规内件之间的纯产品底部，并且布置在循环蒸发器的入口上方。

2. 发明授权

US08901344B2 Production of carboxylic acid esters by stripping with alcohol vapor 有权
标题翻译：用醇蒸汽汽提生产羧酸酯
公开(公告)号：US08901344B2
公开(公告)日：2014-12-02
申请号：US13140274
申请日：2009-12-15
申请人： Jarren Peters , Walter Disteldorf , Katrin Friese , Thomas Schäfer , Oliver Bey
发明人： Jarren Peters , Walter Disteldorf , Katrin Friese , Thomas Schäfer , Oliver Bey
IPC分类号： C07C67/08 , B01D19/00 , B01D3/38 , B01D3/36
CPC分类号： B01D19/0015 , B01D3/36 , B01D3/38 , C07C67/08 , C07C69/80
摘要： The invention relates to a method for producing carboxylic acid esters by reacting a reaction mixture, comprising a carboxylic acid and/or a carboxylic acid anhydride, and an alcohol in a reaction system having one or more reactors, wherein reaction water is distilled off as an alcohol/water azeotrope with the exhaust vapor. In addition, the reaction mixture is treated with superheated alcohol vapor. The method allows the production of esters having a low acid number.
摘要翻译：本发明涉及通过在具有一个或多个反应器的反应体系中使包含羧酸和/或羧酸酐的反应混合物与醇反应制备羧酸酯的方法，其中反应水作为酒精/水与排气蒸气共沸。此外，反应混合物用过热醇蒸气处理。该方法允许生产具有低酸值的酯。

3. 发明授权

US07385075B2 Method for producing esters of multibasic acids 有权
标题翻译：生产多元酸酯的方法
公开(公告)号：US07385075B2
公开(公告)日：2008-06-10
申请号：US10416465
申请日：2001-11-13
申请人： Walter Disteldorf , Günther Golfier , Bernd Morsbach , Kurt Schwirten
发明人： Walter Disteldorf , Günther Golfier , Bernd Morsbach , Kurt Schwirten
IPC分类号： C07C69/76
CPC分类号： C07C67/08 , C07C67/54 , C07C69/44 , C07C69/80
摘要： A process is described for preparing esters of an acid component selected from among polybasic C4-C10 carboxylic acids and an alcohol component selected from among C3-C12 alkanols or from among C3-C12 alkanediols, the alkyl chain of which may have interruption by from 1 to 3 oxygen atoms, by a) heating at boiling point, in a reaction zone and in the presence of an esterification catalyst, a mixture essentially consisting of the acid component or of an anhydride thereof and of the alcohol component, b) using rectification to separate the vapor comprising alcohol and water into an alcohol-rich fraction and a water-rich fraction, and c) returning the alcohol-rich fraction into the reaction zone and conducting the water-rich fraction out of the process. The process is simple to carry out and permits rapid achievement of essentially quantitative conversion.
摘要翻译：描述了一种制备选自多元醇C 4 -C 10羧酸和选自C 3 -C 10羧酸的醇组分的酸组分的酯的方法， C 1 -C 12烷醇或C 3 -C 12烷二醇，其烷基链可能具有中断1至3个氧原子，通过a）在沸点加热，在反应区和酯化催化剂存在下，基本上由酸组分或其酸酐和醇组分组成的混合物，b）使用精馏将将含有醇和水的蒸汽加入富含醇的馏分和富含水的馏分中，以及c）将富含醇的馏分返回到反应区中，并将富含水的馏分导出该过程。该过程很简单，可以快速实现基本的定量转化。

4. 发明授权

US4550208A Preparation of 4,4'-diaminobenzophenones 失效
标题翻译： 4,4'-二氨基二苯甲酮的制备
公开(公告)号：US4550208A
公开(公告)日：1985-10-29
申请号：US673938
申请日：1984-11-21
申请人： Walter Disteldorf , Wolfgang Eisfeld , Rolf-Dieter Kohler
发明人： Walter Disteldorf , Wolfgang Eisfeld , Rolf-Dieter Kohler
IPC分类号： C07C67/00 , C07C213/00 , C07C225/22 , C07D209/48 , C07C97/10
CPC分类号： C07D209/48
摘要： 4,4'-diaminobenzophenones of the formula I ##STR1## where the rings A and B can be further substituted, are prepared by a process in which a compound of the formula II ##STR2## where the rings A, B and E can be substituted, is oxidized with aqueous nitric acid in the presence of nitrobenzene or of an alkanoic acid and under superatmospheric pressure, and the reaction product is cleaved.The process according to the invention gives the compounds of the formula I in high yield and purity.
摘要翻译：环A和B可以进一步被取代的式Ⅰ“（IMAGE）的4,4'-二氨基二苯甲酮通过其中环A，B和E环可以是式取代的，在硝基苯或链烷酸存在下，在超大气压下，用硝酸水溶液氧化，反应产物被裂解。根据本发明的方法以高产率和纯度给出了式I化合物。

5. 发明授权

US4207255A Manufacture of very pure halonaphthalic acid anhydrides 失效
标题翻译：制造非常纯的卤代二氢酸酐
公开(公告)号：US4207255A
公开(公告)日：1980-06-10
申请号：US850239
申请日：1977-11-10
申请人： Wolfgang Eisfeld , Walter Disteldorf , Albert Hettche
发明人： Wolfgang Eisfeld , Walter Disteldorf , Albert Hettche
IPC分类号： C07D311/92 , C07C51/31 , C07C63/34
CPC分类号： C07C51/316
摘要： Pure halonaphthalic acid anhydrides are prepared from haloacenaphthenes by oxidation with nitric acid in a mixture of aliphatic carboxylic acid, water and nitric acid in the presence of vanadate, with or without further metal salts, at an elevated temperature and the reaction product is isolated and subjected to an oxidative after-treatment with hypochlorite in aqueous solution at a pH of from 9 to 12 at an elevated temperature. The products are intermediates for the manufacture of optical brighteners.
摘要翻译：纯的卤代邻苯二甲酸酐通过在酸酐存在下，在有或者没有其它金属盐的情况下，用硝酸在脂族羧酸，水和硝酸的混合物中进行氧化由卤代苊制备，并将反应产物分离并进行在升高的温度下在pH为9至12的水溶液中用次氯酸盐进行氧化后处理。该产品是制造荧光增白剂的中间体。

6. 发明授权

US07183233B2 Method for separating an esterification catalyst 有权
标题翻译：分离酯化催化剂的方法
公开(公告)号：US07183233B2
公开(公告)日：2007-02-27
申请号：US10523284
申请日：2003-07-23
申请人： Kurt Schwirten , Walter Disteldorf , Günther Golfier , Jarren Peters
发明人： Kurt Schwirten , Walter Disteldorf , Günther Golfier , Jarren Peters
IPC分类号： C07C67/48 , B01J20/31
CPC分类号： C07C67/58 , C07C67/60 , C07C69/80
摘要： Process for removal of the esterification catalyst by separation from a crude plasticizer ester obtained by reacting a dicarboxylic acid with C8–C13 alcohols, by treating the crude ester with an aqueous alkali solution in the range from 10 to 100° C. and then separating the aqueous alkaline phase comprising the hydrolyzed esterification catalyst by gravitational phase separation, by treating the crude ester, prior to or during the phase separation, with a salt of a di- or polyvalent metal, or with a mixture of these salts.
摘要翻译：通过与通过使二羧酸与C 8 -C 13醇反应获得的粗增塑剂酯分离来除去酯化催化剂的方法，通过用水碱溶液在10至100℃的范围内，然后通过重力相分离来分离包含水解酯化催化剂的水性碱性相，通过在相分离之前或期间，用二酯的盐处理粗酯，或多价金属，或与这些盐的混合物。

7. 发明授权

US4537987A Preparation of pure monoesters of adipic acid 失效
标题翻译：己二酸纯单酯的制备
公开(公告)号：US4537987A
公开(公告)日：1985-08-27
申请号：US629766
申请日：1984-07-11
申请人： Heinz-Walter Schneider , Wolfgang Richter , Walter Disteldorf , Rudolf Kummer
发明人： Heinz-Walter Schneider , Wolfgang Richter , Walter Disteldorf , Rudolf Kummer
IPC分类号： B01J31/00 , B01J31/20 , B01J31/24 , C07B61/00 , C07C67/313 , C07C67/38 , C07C67/39 , C07C69/44 , C07C69/67
CPC分类号： C07C67/39
摘要： Pure monoesters of adipic acid are prepared by a process in which(a) a pentenoate is reacted with carbon monoxide and hydrogen at from 90.degree. to 140.degree. C. and under from 5 to 300 bar in the presence of a carbonyl complex of cobalt or of rhodium, and a 5-formylvalerate is separated off, and(b) the 5-formylvalerate thus obtained is oxidized with molecular oxygen, or with a gas containing this, at from 20.degree. to 100.degree. C. under from 1 to 10 bar.
摘要翻译：己二酸的纯单酯通过以下方法制备，其中（a）戊烯酸酯与一氧化碳和氢气在90至140℃和5至300巴下在钴或羰基络合物存在下反应的铑，并分离出5-甲酰基戊酸酯，（b）将所得的5-甲酰基戊酸酯用分子氧或含有该气体的气体在20至100℃下在1至10巴。

8. 发明申请

US20110251419A1 METHOD FOR REGENERATION OF RAW ESTER 有权
标题翻译：再生原始方法
公开(公告)号：US20110251419A1
公开(公告)日：2011-10-13
申请号：US13140239
申请日：2009-12-15
申请人： Katrin Friese , Walter Disteldorf , Mannheim Germany , Günther Golfer
发明人： Katrin Friese , Walter Disteldorf , Mannheim Germany , Günther Golfer
IPC分类号： C07C67/58
CPC分类号： C07C67/58 , C07C67/60 , Y02P20/584 , C07C69/80
摘要： The invention relates to a raw ester of an esterification reaction catalyzed by a metal-containing esterification catalyst generated by a) mixing the raw ester at a temperature T of more than 100° C. under a pressure p that is equal to or greater than the vapor pressure of water at the temperature T with an aqueous base, b) relaxing the ester-base mixture and evaporating water, c) mixing the obtained fluid phase with water forming a water-in-oil emulsion, d) distilling water out of said emulsion and e) filtering the ester. Said method results in esters having low acid value and residues accrue in easily filterable form in the solid catalyst residues.
摘要翻译：本发明涉及由含金属的酯化催化剂催化的酯化反应的原料酯，其通过以下步骤生成：a）在大于100℃的温度T下，在等于或大于蒸馏水，c）将得到的流体相与形成油包水乳液的水混合，d）将水从所述的水溶液中蒸出，乳液和e）过滤酯。所述方法导致具有低酸值和残留物的酯在固体催化剂残余物中易于过滤形式产生。

9. 发明申请

US20050240053A1 Method for separating an esterification catalyst 有权
标题翻译：分离酯化催化剂的方法
公开(公告)号：US20050240053A1
公开(公告)日：2005-10-27
申请号：US10523284
申请日：2003-07-23
申请人： Kurt Schwirten , Walter Disteldorf , Gunther Golfier , Jarren Peters
发明人： Kurt Schwirten , Walter Disteldorf , Gunther Golfier , Jarren Peters
IPC分类号： C07C67/58 , C07C67/60 , C07C67/48
CPC分类号： C07C67/58 , C07C67/60 , C07C69/80
摘要： Process for removal of the esterification catalyst by separation from a crude plasticizer ester obtained by reacting a dicarboxylic acid with C8-C13 alcohols, by treating the crude ester with an aqueous alkali solution in the range from 10 to 100° C. and then separating the aqueous alkaline phase comprising the hydrolyzed esterification catalyst by gravitational phase separation, by treating the crude ester, prior to or during the phase separation, with a salt of a di- or polyvalent metal, or with a mixture of these salts.
摘要翻译：通过与通过使二羧酸与C 8 -C 13醇反应获得的粗增塑剂酯分离来除去酯化催化剂的方法，通过用水碱溶液在10至100℃的范围内，然后通过重力相分离来分离包含水解酯化催化剂的水性碱性相，通过在相分离之前或期间，用二酯的盐处理粗酯，或多价金属，或与这些盐的混合物。

10. 发明授权

US06437170B1 Mixture of diesters of adipic or phthalic acid with isomers of nonanols 有权
标题翻译：己二酸或邻苯二甲酸二酯与壬醇异构体的混合物
公开(公告)号：US06437170B1
公开(公告)日：2002-08-20
申请号：US09449395
申请日：1999-11-26
申请人： Lucien Thil , Boris Breitscheidel , Walter Disteldorf , Edgar Zeller , Marc Walter , Bernd Morsbach , Knut Dornik
发明人： Lucien Thil , Boris Breitscheidel , Walter Disteldorf , Edgar Zeller , Marc Walter , Bernd Morsbach , Knut Dornik
IPC分类号： C07C6976
CPC分类号： C08K5/11 , C07C67/08 , C07C69/44 , C07C69/80 , C08K5/05 , C08K5/12 , C08L27/06
摘要： The mixture described is a mixture of isomeric nonanol diesters of a dicarboxylic acid, selected from the class consisting of a mixture of diesters of adipic acid in the 1H NMR spectrum of which, observed in CDCl3, the ratio of the area under the resonance signals at chemical shifts in the range from 1.0 to 2.0 ppm with respect to TMS to the area under the resonance signals at chemical shifts in the range from 0.5 to 1.0 ppm with respect to TMS is from 1.20 to 5.00 and a mixture of diesters of phthalic acid, in the 1H NMR spectrum of which, observed in CDCl3, the ratio of the area under the resonance signals at chemical shifts in the range from 1.1 to 3.0 ppm with respect to TMS to the area under the resonance signals at chemical shifts in the range from 0.5 to 1.1 ppm with respect to TMS is from 1.00 to 4.00. The diesters of adipic and phthalic acid are suitable as plasticizers for PVC-based molding compositions and have high compatibility, a low cold crack temperature, low torsional rigidity and/or high thermal stability.
摘要翻译：所述的混合物是二羧酸的异构壬醇二酯的混合物，其选自在1 H NMR光谱中己二酸二酯的混合物，其在CDCl 3中观察到的共振信号下的面积比例相对于TMS，1.0〜2.0ppm范围内的化学位移相对于TMS，化学位移为0.5〜1.0ppm的共振信号下的面积为1.20〜5.00，邻苯二甲酸二酯，在1H NMR谱中，在CDCl3中观察到，在化学位移下的共振信号下的面积相对于TMS的1.1至3.0ppm范围内的化学位移下的共振信号下的面积的比例在己二酸和邻苯二甲酸的二酯适用于PVC基成型组合物的增塑剂，具有高相容性，低冷裂纹温度，低扭转度刚性和/或高热稳定性。

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