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1. 发明授权

US06329535B1 Process for preparing esterified chroman compounds 失效
标题翻译：酯化色满化合物的制备方法
公开(公告)号：US06329535B1
公开(公告)日：2001-12-11
申请号：US09692313
申请日：2000-10-20
申请人： Horst Weigel , Steffen Krill , Hans Joachim Hasselbach , Klaus Huthmacher
发明人： Horst Weigel , Steffen Krill , Hans Joachim Hasselbach , Klaus Huthmacher
IPC分类号： C07D31176
CPC分类号： C07D311/72 , C07C67/00 , Y02P20/582 , C07C69/017 , C07C69/16 , C07C69/157
摘要： A process for preparing esterified chroman compounds from 2,6,6-trimethylcylohex-2-ene-1,4-dione, wherein the esterified intermediates are reacted directly to give the desired chroman derivatives without an additional purification step.
摘要翻译：从2,6,6-三甲基环己-2-烯-1,4-二酮制备酯化色满化合物的方法，其中酯化的中间体直接反应得到所需的苯并二氢吡喃衍生物，无需额外的纯化步骤。

2. 发明授权

US6150563A Aliphatic alkanals with improved storage stability and method of improving the storage stability 有权
标题翻译：具有改善储存稳定性的脂肪族链烷烃和提高储存稳定性的方法
公开(公告)号：US6150563A
公开(公告)日：2000-11-21
申请号：US134562
申请日：1998-08-14
申请人： Hans Joachim Hasselbach , Klaus Huthmacher , Katja Kelm , Horst Weigel
发明人： Hans Joachim Hasselbach , Klaus Huthmacher , Katja Kelm , Horst Weigel
IPC分类号： C07C45/86 , C07C47/02 , C07C319/26 , C07C323/22 , C07C47/00
CPC分类号： C07C323/22 , C07C45/86
摘要： Aliphatic alkanals with a water content of greater than 300 ppm which are stable in storage, and a method of improving the storage stability of these aliphatic alkanals, especially of substituted, sulfur-containing alkanals. The formation of oligomers, polymers and condensation products from elimination reactions and oxidation and the subsequent reactions of the products formed results in undesired impurities that are largely prevented by the addition of an organic acid that forms metal complexes and, optionally, alkanolamines or trialkanolamines.
摘要翻译：水分大于300ppm的脂肪族链烷烃，其储存稳定，以及提高这些脂肪族链烷烃，特别是取代的含硫链烷烃的储存稳定性的方法。由消除反应和氧化形成的低聚物，聚合物和缩合产物以及所形成的产物的后续反应导致不期望的杂质，其通过加入形成金属络合物的有机酸和任选的烷醇胺或三链烷醇胺而大大地被防止。

3. 发明授权

US06797827B2 Process for the preparation of alpha-amino acids by hydrolysis of hydantoins at elevated pressure and elevated temperature 有权
标题翻译：通过在升高的压力和升高的温度下水解乙内酰脲来制备α-氨基酸的方法
公开(公告)号：US06797827B2
公开(公告)日：2004-09-28
申请号：US10630094
申请日：2003-07-30
申请人： Martin Körfer , Dieter Buss , Horst Weigel , Christoph Weckbecker , Hans Joachim Hasselbach , Klaus Huthmacher
发明人： Martin Körfer , Dieter Buss , Horst Weigel , Christoph Weckbecker , Hans Joachim Hasselbach , Klaus Huthmacher
IPC分类号： C07D23386
CPC分类号： C07C319/20 , C07C227/24 , C07C323/58 , C07C229/08 , C07C229/36
摘要： A process for the preparation of &agr;-amino acids by hydrolysis of hydantoins in the presence of water and at least one metallic oxide under conditions such that all the starting materials are completely dissolved in the water as a result of high pressure and high temperature and only one further phase is present in the reactor in addition to the metallic oxide phase.
摘要翻译：一种在水和至少一种金属氧化物的存在下水解乙内酰脲来制备α-氨基酸的方法，使得所有起始物质由于高压和高温而完全溶解在水中，只有在除了金属氧化物相之外，在反应器中还存在一个相。

4. 发明申请

US20150051421A1 PROCESS FOR THE PREPARATION OF METHIONINE 有权
标题翻译：制备甲硫氨酸的方法
公开(公告)号：US20150051421A1
公开(公告)日：2015-02-19
申请号：US14386165
申请日：2013-02-26
申请人： Martin Koerfer , Hans Joachim Hasselbach , Stefan Reichert , Harald Jakob , Christoph Weckbecker , Klaus Huthmacher , Horst Krull , Bernd Drapal , Rainer Peter
发明人： Martin Koerfer , Hans Joachim Hasselbach , Stefan Reichert , Harald Jakob , Christoph Weckbecker , Klaus Huthmacher , Horst Krull , Bernd Drapal , Rainer Peter
IPC分类号： C07C319/12 , C07C323/52
CPC分类号： C07C319/28 , C07C319/12 , C07C319/20 , C07C319/26 , C07C323/52 , Y02P20/142 , C07C323/58
摘要： The invention relates to a process for the preparation of D,L-methionine, in which carbon dioxide is fed to an aqueous potassium methioninate solution obtained by hydrolysis of 5-(2-methylmercaptoethyl)hydantoin, in order to precipitate out crude methionine, which is separated off and purified, where, for the purposes of purification, an aqueous solution of the separated-off crude methionine is prepared and subjected to a recrystallization, characterized in that the solution from which the recrystallization takes place contains potassium ions and also a crystallization additive, where the crystallization additive is a nonionic or anionic surfactant, or a mixture of different nonionic or anionic surfactants, and that the recrystallization takes place by introducing a 60 to 110° C.-hot methionine solution into a 35 to 80° C.-warm methionine suspension, the temperature of which is lower than that of the introduced solution, the temperature of the methionine suspension being maintained between 35 and 80° C. during the addition.
摘要翻译：本发明涉及一种制备D，L-甲硫氨酸的方法，其中将二氧化碳加入到通过5-（2-甲基巯基乙基）乙内酰脲的水解获得的甲硫氨酸钾水溶液中，以沉淀出粗蛋氨酸，分离纯化，其中，为了纯化的目的，制备分离的粗制甲硫氨酸的水溶液并进行重结晶，其特征在于进行重结晶的溶液含有钾离子并且还具有结晶添加剂，其中结晶添加剂是非离子或阴离子表面活性剂，或不同的非离子或阴离子表面活性剂的混合物，并且通过将60至110℃的热甲硫氨酸溶液引入35至80℃进行重结晶。 - 温血蛋氨酸悬浮液，其温度低于引入溶液的温度，甲硫氨酸悬浮液的温度维持在在加入过程中在35和80℃之间。

5. 发明授权

US09156782B2 Process for the preparation of methionine 有权
标题翻译：制备甲硫氨酸的方法
公开(公告)号：US09156782B2
公开(公告)日：2015-10-13
申请号：US14386165
申请日：2013-02-26
申请人： Martin Koerfer , Hans Joachim Hasselbach , Stefan Reichert , Harald Jakob , Christoph Weckbecker , Klaus Huthmacher , Horst Krull , Bernd Drapal , Rainer Peter
发明人： Martin Koerfer , Hans Joachim Hasselbach , Stefan Reichert , Harald Jakob , Christoph Weckbecker , Klaus Huthmacher , Horst Krull , Bernd Drapal , Rainer Peter
IPC分类号： C07C319/12 , C07C319/20 , C07C319/26 , C07C319/28 , C07C323/52
CPC分类号： C07C319/28 , C07C319/12 , C07C319/20 , C07C319/26 , C07C323/52 , Y02P20/142 , C07C323/58
摘要： The invention relates to a process for the preparation of D,L-methionine, in which carbon dioxide is fed to an aqueous potassium methioninate solution obtained by hydrolysis of 5-(2-methylmercaptoethyl)hydantoin, in order to precipitate out crude methionine, which is separated off and purified, where, for the purposes of purification, an aqueous solution of the separated-off crude methionine is prepared and subjected to a recrystallization, characterized in that the solution from which the recrystallization takes place contains potassium ions and also a crystallization additive, where the crystallization additive is a nonionic or anionic surfactant, or a mixture of different nonionic or anionic surfactants, and that the recrystallization takes place by introducing a 60 to 110° C.-hot methionine solution into a 35 to 80° C.-warm methionine suspension, the temperature of which is lower than that of the introduced solution, the temperature of the methionine suspension being maintained between 35 and 80° C. during the addition.
摘要翻译：本发明涉及一种制备D，L-甲硫氨酸的方法，其中将二氧化碳加入到通过5-（2-甲基巯基乙基）乙内酰脲的水解获得的甲硫氨酸钾水溶液中，以沉淀出粗蛋氨酸，分离纯化，其中，为了纯化的目的，制备分离的粗制甲硫氨酸的水溶液并进行重结晶，其特征在于进行重结晶的溶液含有钾离子并且还具有结晶添加剂，其中结晶添加剂是非离子或阴离子表面活性剂，或不同的非离子或阴离子表面活性剂的混合物，并且通过将60至110℃的热甲硫氨酸溶液引入35至80℃进行重结晶。 - 温血蛋氨酸悬浮液，其温度低于引入溶液的温度，甲硫氨酸悬浮液的温度维持在在加入过程中在35和80℃之间。

6. 发明授权

US6126972A Process for the preparation of aqueous sodium methioninate solutions and use of those solutions in the production of a granulate 有权
标题翻译：用于制备甲硫氨酸钠水溶液的方法，并使用这些溶液来生产颗粒
公开(公告)号：US6126972A
公开(公告)日：2000-10-03
申请号：US309278
申请日：1999-05-11
申请人： Martin Korfer , Lutz Rohland , Wolfram Binder , Hans Joachim Hasselbach , Hans Christian Alt , Klaus Huthmacher , Heidemarie Kniesel
发明人： Martin Korfer , Lutz Rohland , Wolfram Binder , Hans Joachim Hasselbach , Hans Christian Alt , Klaus Huthmacher , Heidemarie Kniesel
IPC分类号： A23K1/16 , A23K1/22 , C07C319/20 , C07C319/28 , C07C323/58 , A23K1/18 , C07C321/00
CPC分类号： C07C319/28 , C07C319/20 , C07C323/58 , Y10S426/807
摘要： A process for the preparation of aqueous sodium methioninate solutions having a low sodium carbonate content from the crude hydrolysis mixtures obtained in the hydrolysis of 5-(.beta.-methylmercaptoethyl)-hydantoin with from 1.1 to 6 equivalents of sodium hydroxide and/or sodium carbonate, by separating off sodium carbonate monohydrate while heating, and granulates subsequently prepared from those solutions by various processes.
摘要翻译：一种从1.1至6当量氢氧化钠和/或碳酸钠水解5-（β-甲基巯基乙基） - 乙内酰脲得到的粗水解混合物制备具有低碳酸钠含量的甲硫氨酸钠水溶液的方法，通过在加热时分离出碳酸钠一水合物，然后通过各种方法从这些溶液中制备颗粒。

7. 发明授权

US07179938B2 Process for the preparation of methionine 有权
标题翻译：制备甲硫氨酸的方法
公开(公告)号：US07179938B2
公开(公告)日：2007-02-20
申请号：US10497949
申请日：2002-08-06
申请人： Christoph Weckbecker , Horst Krull , Jürgen Bilz , Klaus Huthmacher , Hans Joachim Hasselbach
发明人： Christoph Weckbecker , Horst Krull , Jürgen Bilz , Klaus Huthmacher , Hans Joachim Hasselbach
IPC分类号： C07C323/00 , C07C57/00
CPC分类号： C07C319/20 , C07C319/26 , C07C319/28 , C07C323/58
摘要： The invention relates to a process for the preparation of methionine of high bulk density, in which a mixture which comprises a compound which has a foaming action and a compound which influences the crystallization is added to the hydrolysis solution, and to the mixture itself.
摘要翻译：本发明涉及一种制备高堆积密度的甲硫氨酸的方法，其中将包含具有发泡作用的化合物和影响结晶的化合物的混合物加入到水解溶液中，以及混合物本身。

8. 发明授权

US6146612A Method for recovering sulfuric acid from sulfate salts 有权
标题翻译：从硫酸盐中回收硫酸的方法
公开(公告)号：US6146612A
公开(公告)日：2000-11-14
申请号：US206948
申请日：1998-12-08
申请人： Hans Albrecht Hasseberg , Hans Joachim Hasselbach , Klaus Huthmacher , Volker Hafner , Harald Heinzel
发明人： Hans Albrecht Hasseberg , Hans Joachim Hasselbach , Klaus Huthmacher , Volker Hafner , Harald Heinzel
IPC分类号： B01D53/34 , B01D53/50 , B01D53/77 , C01B17/58 , C01B17/74 , C07C319/20 , C07C319/28 , C07C323/52 , C07C323/60
CPC分类号： C07C319/20 , C01B17/585 , C01B17/745 , C07C319/28
摘要： A process is provided for the recovery of sulfuric acid from NH.sub.4 HSO.sub.4 and (NH.sub.4).sub.2 SO.sub.4 salts produced from the sulfuric acid hydrolysis of methylmercaptopropionaldehyde (MMP) cyanohydrin to produce 2-hydroxy-4-methylthiobutyric acid (MHA), which can be used as an additive in animal feed. The sulfate salts are combusted in a furnace to produce sulfur dioxide; the sulfur dioxide is contacted with an aqueous solution containing sulfuric acid and hydrogen peroxide, where the sulfur dioxide is converted into sulfuric acid. The product sulfuric acid is recovered.
摘要翻译：提供了从甲基巯基丙醛（MMP）氰醇的硫酸水解产生的NH 4 HSO 4和（NH 4）2 SO 4盐中回收硫酸以产生2-羟基-4-甲硫基丁酸（MHA）的方法，其可以用作动物饲料添加剂。硫酸盐在炉中燃烧以产生二氧化硫; 二氧化硫与含有硫酸和过氧化氢的水溶液接触，其中二氧化硫被转化成硫酸。产物硫酸被回收。

9. 发明授权

US09464045B2 Process for the preparation of methionine 有权
标题翻译：制备甲硫氨酸的方法
公开(公告)号：US09464045B2
公开(公告)日：2016-10-11
申请号：US14850207
申请日：2015-09-10
申请人： Martin Koerfer , Hans Joachim Hasselbach , Stefan Reichert , Harald Jakob , Christoph Weckbecker , Klaus Huthmacher , Horst Krull , Bernd Drapal , Rainer Peter
发明人： Martin Koerfer , Hans Joachim Hasselbach , Stefan Reichert , Harald Jakob , Christoph Weckbecker , Klaus Huthmacher , Horst Krull , Bernd Drapal , Rainer Peter
IPC分类号： C07C319/28 , C07C319/20 , C07C319/26 , C07C319/12 , C07C323/52
CPC分类号： C07C319/28 , C07C319/12 , C07C319/20 , C07C319/26 , C07C323/52 , Y02P20/142 , C07C323/58
摘要： This disclosure relates to a process for preparing D,L-methionine by feeding carbon dioxide to an aqueous potassium methioninate solution obtained by hydrolysis of 5-(2-methylmercaptoethyl)hydantoin, in order to precipitate out crude methionine, which is separated off and purified. In this process an aqueous solution of the separated-off crude methionine is purified by recrystallization from a solution containing potassium ions and also a crystallization additive. The crystallization additive is a nonionic or anionic surfactant, or a mixture of different nonionic or anionic surfactants. The recrystallization occurs by introducing a 60 to 110° C.-hot methionine solution into a 35 to 80° C.-warm methionine suspension, a temperature of which is lower than that of the introduced solution, such that the temperature of the methionine suspension being maintained between 35 and 80° C. during the addition. The crystallization additive is a sorbitan fatty acid ester or a mixture of different sorbitan fatty acid esters.
摘要翻译：本公开涉及通过将二氧化碳供给到通过水解5-（2-甲基巯基乙基）乙内酰脲获得的甲硫氨酸钾水溶液以便沉淀出粗蛋氨酸的方法来制备D，L-甲硫氨酸，其分离和纯化。在该方法中，分离的粗甲硫氨酸的水溶液通过从含有钾离子的溶液和结晶添加剂中重结晶来纯化。结晶添加剂是非离子或阴离子表面活性剂，或不同的非离子或阴离子表面活性剂的混合物。通过将60〜110℃的甲硫氨酸溶液导入35〜80℃的甲硫氨酸悬浮液中，其温度低于引入的溶液的温度，使得甲硫氨酸悬浮液的温度在添加期间保持在35和80℃之间。结晶添加剂是脱水山梨糖醇脂肪酸酯或不同脱水山梨糖醇脂肪酸酯的混合物。

10. 发明授权

US6140536A Process for obtaining 2-hydroxy-4-methylthiobutyric acid (MHA) 有权
标题翻译：获得2-羟基-4-甲硫基丁酸（MHA）的方法
公开(公告)号：US6140536A
公开(公告)日：2000-10-31
申请号：US91796
申请日：1998-09-01
申请人： Hans Albrecht Hasseberg , Hans Joachim Hasselbach , Klaus Huthmacher , Volker Hafner , Harald Heinzel , Barbara Jager
发明人： Hans Albrecht Hasseberg , Hans Joachim Hasselbach , Klaus Huthmacher , Volker Hafner , Harald Heinzel , Barbara Jager
IPC分类号： C07C319/20 , C07C319/28 , C07C323/52 , C07C315/00
CPC分类号： C07C319/28 , C07C319/20
摘要： A method for the isolation of 2-hydroxy-4-methylthiobutyric acid (MHA), wherein MHA is isolated from a reaction mixture obtained by addition of hydrogen cyanide (HCN) to methylmercaptopropionaldehyde (MMP) and hydrolysis by sulphuric acid of the methylmercaptopropionaldehyde cyanohydrin (MMP-CH) thus obtained. The reaction mixture is brought into contact in a liquid/liquid extraction system with an organic solvent substantially immiscible with water, in order to form an extraction solution which contains the solvent and the MHA transferred out of the reaction mixture. By bringing the salt content of the reaction mixture, prior to the liquid/liquid extraction, to a concentration of about >50 wt. % (wt./wt.), preferably >55 wt. %, referred to the sum of the inorganic constituents of the reaction mixture, the coordinated use of energy in the total system is improved, the evaporation of strongly corrosive solutions is avoided, the efficiency of the hydrolysis step is increased and the distribution coefficients during the extraction are improved. The MHA is isolated as the extract from this extraction solution by evaporation, and may be used as animal feed supplement.
摘要翻译： PCT No.PCT / EP96 / 05437 Sec。 371日期：1998年9月1日 102（e）1998年9月1日PCT PCT 1996年12月5日PCT公布。公开号WO97 / 23452 日期1997年7月3日分离2-羟基-4-甲硫基丁酸（MHA）的方法，其中MHA是通过将氰化氢（HCN）加入到甲基巯基丙醛（MMP）中并通过硫酸水解而获得的反应混合物中分离的的甲基巯基丙醛氰醇（MMP-CH）。使反应混合物在液/液萃取系统中与基本上与水不混溶的有机溶剂接触，以形成含有溶剂和从反应混合物中转移的MHA的萃取溶液。通过使液体/液体萃取之前的反应混合物的盐含量达到约> 50wt。％（重量/重量），优选> 55重量％％，是指反应混合物的无机成分之和，改善了总体系中能量的协调使用，避免了强腐蚀性溶液的蒸发，提高了水解步骤的效率，提高了分散系数提取提高。通过蒸发将MHA作为来自该提取溶液的提取物分离，并且可以用作动物饲料添加剂。

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