公开(公告)号：EP1881957B1

公开(公告)日：2011-08-17

申请号：EP06743390.4

申请日：2006-05-02

Applicant: BASF SE

Inventor： OFTRING, Alfred ,  BRAUN, Gerold ,  WIRSING, Friedrich ,  STAMM, Armin ,  BALDENIUS, Kai-Uwe

IPC: C07C227/26 ,  C07C229/16

CPC classification number: C07C227/26 ,  C07C229/16

Abstract: The invention relates to a method for producing a light-coloured methylglycine-N,N-diethanoic acid trialkali metal salt with a low by-product content, by the alkaline hydrolysis of methylglycine diacetonitrile, said method comprises steps that are carried out in the order (a) to (f): (a) mixing of the methylglycine diacetonitrile with an aqueous alkali lye at a temperature of = 30 °C; (b) the aqueous alkali methylglycine diacetonitrile suspension is then reacted at a temperature ranging between 10 and 30 °C for a period of 0.1 to 10 h, to form a solution; (c) the solution obtained in step (b) is then reacted at a temperature ranging between 30 to 40 °C for a period of 0.1 to 10 h; (d) optionally the solution obtained in step (c) is reacted at a temperature ranging between 50 and 80 °C for a period of between 0.5 and 2 h; (e) optionally the solution obtained in step (c) or (d) is reacted at a temperature ranging between 110 and 200 °C for a period of between 5 and 60 min; (f) hydrolysis and isolation of ammonia from the solution obtained in step (c), (d) or (e) by stripping at a temperature of between 90 and 105 °C.

公开(公告)号：EP2705022B1

公开(公告)日：2017-12-06

申请号：EP12716431.7

申请日：2012-04-25

Applicant: BASF SE

Inventor： OFTRING, Alfred ,  WEBER, Maxim ,  BRAUN, Gerold ,  LAUTERBACH, Arnulf

IPC: C07C227/42 ,  C07C229/04

CPC classification number: C07C227/42 ,  C07C229/04

公开(公告)号：EP2262760B1

公开(公告)日：2017-08-30

申请号：EP09716225.9

申请日：2009-03-02

Applicant: BASF SE

Inventor： OFTRING, Alfred ,  STAMM, Armin ,  WIRSING, Friedrich ,  BRAUN, Gerold

IPC: C07C227/18

CPC classification number: C07C227/18 ,  C07C229/24

公开(公告)号：EP2694468A1

公开(公告)日：2014-02-12

申请号：EP12711135.9

申请日：2012-03-20

Applicant: BASF SE

Inventor： OFTRING, Alfred ,  BRAUN, Gerold ,  LAUTERBACH, Arnulf

IPC: C07C227/26 ,  C07C229/16

CPC classification number: C07C227/26 ,  C07C229/16

Abstract: The invention relates to a method for producing aqueous solutions of methylglycine-N,N-diacetic acid trialkali metal salts at a high yield and purity using Strecker synthesis, starting from an aqueous solution of α-alanine, by reacting same with formaldehyde and hydrocyanic acid in an aqueous solution to form α-alanine N,N-diacetonitrile in a reaction unit, and saponifying same with a base to form the corresponding methylglycine-N,N-diacetic acid trialkali metal salt. The method is characterized in that the α-alanine is partially neutralized, and the addition of formaldehyde and hydrocyanic acid for reacting into α-alanine-N,N-diacetonitrile is controlled such that the concentration of free hydrocyanic acid in the liquid reaction mixture is limited at all times so that secondary reactions, in particular into formaldehyde cyanohydrin, including subsequent reactions of the formaldehyde cyanohydrin as well as the polymerization of hydrocyanic acid occur only to such an extent that the specification requirements for the methylglycine-N,N-diacetic acid trialkali metal salt, in particular with respect to the nitrilotriacetic acid content and color, are met.

Abstract translation: 本发明涉及使用Strecker合成法，从α-丙氨酸的水溶液开始，通过与甲醛和氢氰酸反应，以高产率和纯度生产甲基甘氨酸-N，N-二乙酸三烷基金属盐的水溶液的方法 在水溶液中在反应单元中形成α-丙氨酸N，N-二乙腈，并用碱皂化，形成相应的甲基甘氨酸-N，N-二乙酸三碱金属盐。 该方法的特征在于α-丙氨酸被部分中和，并且控制加入甲醛和氢氰酸以反应成α-丙氨酸-N，N-二乙腈，使得液体反应混合物中游离氢氰酸的浓度为 所有时间都受到限制，使得二次反应，特别是甲醛氰醇，包括甲醛氰醇的后续反应以及氢氰酸的聚合仅发生到甲基甘氨酸-N，N-二乙酸的规范要求 三碱金属盐，特别是关于次氮基三乙酸含量和颜色。

公开(公告)号：EP2262760A1

公开(公告)日：2010-12-22

申请号：EP09716225.9

申请日：2009-03-02

Applicant: BASF SE

Inventor： OFTRING, Alfred ,  STAMM, Armin ,  WIRSING, Friedrich ,  BRAUN, Gerold

IPC: C07C227/26 ,  C07C229/24

CPC classification number: C07C227/18 ,  C07C229/24

Abstract: The present invention relates to a method for the production of aminodicarboxylic acid-N,N,diacetic acids of the general Formula I, wherein X independently of one another represents hydrogen or an alkali metal and n represents a number 1 or 2. Furthermore, the invention relates to aminodicarboxylic acid-N,N-diacetic acids of high purity. The inventive method comprises the following steps: A.) reacting an aminodicarboxylic acid of the general Formula II, wherein X and n have the aforementioned meanings, with 0.8 to 1.2 mole equivalents of formaldehyde and with 0.8 to 1.2 mole equivalents of hydrocyanic acid; b) reacting the reaction products of step a) with 0.8 to 1.2 mole equivalents of hydrocyanic acid and with 0.8 to 1.2 mole equivalents of formaldehyde; c) hydrolyzing in the reaction product obtained in step b).

Abstract translation: 提供了制备式（I）的氨基二羧酸N，N-二乙酸的方法，其中X独立地为氢或碱金属，n为1或2.具有高纯度的氨基二羧酸-N，N-二乙酸 可以产生。 该方法包括：a）使氨基二羧酸与0.8至1.2摩尔当量的甲醛和0.8至1.2摩尔当量的氢氰酸反应; b）使a）的反应产物与0.8至1.2摩尔当量的氢氰酸和0.8至1.2摩尔当量的甲醛反应; c）在b）中得到的反应产物中水解。

公开(公告)号：EP2694468B1

公开(公告)日：2017-01-18

申请号：EP12711135.9

申请日：2012-03-20

Applicant: BASF SE

Inventor： OFTRING, Alfred ,  BRAUN, Gerold ,  LAUTERBACH, Arnulf

IPC: C07C227/26 ,  C07C229/16

CPC classification number: C07C227/26 ,  C07C229/16

公开(公告)号：EP2705022A1

公开(公告)日：2014-03-12

申请号：EP12716431.7

申请日：2012-04-25

Applicant: BASF SE

Inventor： OFTRING, Alfred ,  WEBER, Maxim ,  BRAUN, Gerold ,  LAUTERBACH, Arnulf

IPC: C07C227/42 ,  C07C229/04

CPC classification number: C07C227/42 ,  C07C229/04

Abstract: What is proposed is a process for preparing a crystalline L-MGDA tri-alkali metal salt by crystallization from an aqueous solution thereof which has been obtained by Strecker synthesis proceeding from L-α-alanine, by reaction with formaldehyde and hydrogen cyanide to give L-α-alanine-N,N-diacetonitrile and subsequent alkaline hydrolysis of the L-α-alanine-N,N-diacetonitrile to give the L-MGDA tri-alkali metal salt, which is characterized in that a temperature of 150°C is not exceeded in the course of alkaline hydrolysis.

Abstract translation: 所提出的是一种制备结晶L-MGDA三碱金属盐的方法，该方法是通过从由Strecker合成从L-α-丙氨酸进行的水溶液中结晶，通过与甲醛和氰化氢反应得到L -α-丙氨酸-N，N-二乙腈，随后碱性水解L-α-丙氨酸-N，N-二乙腈，得到L-MGDA三碱金属盐，其特征在于温度为150℃ 在碱性水解过程中不超过。

公开(公告)号：EP1581481B1

公开(公告)日：2008-10-01

申请号：EP03782412.5

申请日：2003-12-16

Applicant: BASF SE

Inventor： OFTRING, Alfred ,  BRAUN, Gerold

IPC: C07C253/10 ,  C07C255/46

CPC classification number: C07C253/10 ,  C07C2601/14 ,  C07C255/46

Abstract: The invention relates to a method for producing 3-cyano-3,5,5- trimethylcyclohexanone (isophorone nitrile) by reacting isophorone with hydrogen cyanide in the presence of a base as a catalyst. A special sulfonic acid or a special carboxylic acid is added to the resulting raw isophorone nitrile product which is then distilled. The invention further relates to the use of a special sulfonic acid or a special carboxylic acid as a neutralizing agent prior to distilling a raw isophorone nitrile product which is obtained by reacting isophorone with hydrogen cyanide in the presence of a base as a catalyst in order to prevent precipitations during neutralization of the base used as a catalyst with an acid.