公开(公告)号：WO2021175701A1

公开(公告)日：2021-09-10

申请号：PCT/EP2021/054723

申请日：2021-02-25

Applicant: BASF SE

Inventor： SCHMIDT, Thomas ,  STAMM, Armin ,  TANG, Daniel, Dan-Tam ,  SHYMANSKA, Nataliia ,  MORMUL, Verena

IPC: C07C227/26 ,  C07C227/36 ,  C07C227/18 ,  C07C253/00 ,  C07C253/06 ,  C07C229/16 ,  C07C229/76 ,  C07C255/25

Abstract: A process for making a complexing agent with an enantiomeric excess of at least 60%, wherein said process comprises the following steps: (a) reacting an aqueous slurry of alanine with an enantiomeric excess of at least 60% with formaldehyde and hydrocyanic acid, thereby forming an aqueous solution of alanine- bisacetonitrile, (b) saponifying the alanine-bisacetonitrile from step (a) by combining the aqueous solution obtained in step (a) with an aqueous solution of alkali metal hydroxide.

公开(公告)号：WO2017220308A1

公开(公告)日：2017-12-28

申请号：PCT/EP2017/063285

申请日：2017-06-01

Applicant: BASF SE

Inventor： MUELLER, Michael Klemens ,  STAMM, Armin ,  JAEKEL, Frank ,  SUELING, Carsten

IPC: C11D3/33 ,  C07C227/00 ,  C07C229/16 ,  C11D11/00 ,  C11D11/02

Abstract: Process for making a powder or granule containing at least one chelating agent selected from alkali metal salts of methyl glycine diacetic acid (MGDA) and glutamic acid diacetate (GLDA) and iminodisuccinic acid (IDS), said process comprising the steps of (a) introducing an aqueous solution or aqueous slurry of the respective chelating agent (A) into a spray-dryer or spray-granulator, and removing most of said water by spray-drying or spray granulation using a gas with an inlet temperature of 125 to 250°C, (b) withdrawing powder or granules, respectively, from the spray-dryer or spray-granulator, respectively, (c) separating off fines from said powder or granules, wherein said fines have a maximum particle diameter of 350 µm, (d) separating off lumps from said powder or granules, wherein said lumps have a particle diameter of 1,500 µm or more, (e) milling said lumps to a maximum particle diameter of 500 µm, (f) re-introducing said fines from step (c) and milled lumps from step (e) into the spray-dryer or spray-granulator, wherein the share of fines is in the range of from 0.5 to 20 % by weight of the total chelating agent (A) withdrawn in step (b) and the share of milled lumps is in the range of from 5 to 60% by weight of the total chelating agent (A) withdrawn in step (b).

Abstract translation: 制备含有至少一种选自甲基甘氨酸二乙酸（MGDA）和谷氨酸二乙酸（GLDA）和亚氨基二琥珀酸（IDS）的碱金属盐的螯合剂的粉末或颗粒的方法，所述方法 包括以下步骤：（a）将各自螯合剂（A）的水溶液或含水浆料引入喷雾干燥器或喷雾造粒机中，并且通过喷雾干燥或使用气体喷雾造粒除去大部分所述水 （b）分别从喷雾干燥器或喷雾造粒机中分别取出粉末或颗粒，（c）分离所述粉末或颗粒中的细粒，其中所述细粒具有最大颗粒 （d）从所述粉末或颗粒中分离出块状物，其中所述块状物的粒径为1,500微米或更大，（e）将所述块状物研磨至最大粒径为500微米 ，（f）将来自步骤（c）的所述细粒再次引入， 并将来自步骤（e）的块状物研磨到喷雾干燥器或喷雾造粒机中，其中细粒的份额为在步骤（b）中提取的总螯合剂（A）的0.5-20重量％ 研磨块的份额在步骤（b）中提取的总螯合剂（A）的5至60重量％的范围内。

公开(公告)号：WO2019002022A1

公开(公告)日：2019-01-03

申请号：PCT/EP2018/066239

申请日：2018-06-19

Applicant: BASF SE

Inventor： SCHMIDT, Thomas ,  STAMM, Armin ,  REINOSO GARCIA, Marta ,  MORMUL, Verena ,  MUELLER, Michael Klemens ,  JAEKEL, Frank ,  MANNING, Jeremy

IPC: C07C227/26 ,  C07C229/16 ,  C11D3/33 ,  C11D11/02

Abstract: The present invention is directed towards a process for manufacturing a complexing agent, said process comprising the steps of (a) Providing a nitrile according to general formula (I a) or (I b) (formula I a, I b) With M being selected from alkali metal and hydrogen and combinations thereof, (b) Saponification with a total alkali amount of 2.5 to 2.9 mol of alkali metal hydroxide per mole of nitrile according to general formula (I a) or (I b), respectively, and a pH value in the range of from 9.5 to 11.5 at the end of step (b), (c) Adding an amount of alkali metal hydroxide so that the total alkali content is 2.9 to 3.1 moles per mole nitrile according to general formula(I a) or (I b), respectively, and (d) Allowing further conversion.20

公开(公告)号：WO2017102483A1

公开(公告)日：2017-06-22

申请号：PCT/EP2016/080001

申请日：2016-12-07

Applicant: BASF SE

Inventor： FRANZKE, Constanze ,  FRANZKE, Axel ,  STAMM, Armin ,  HARTMANN, Markus ,  BAUMANN, Robert

IPC: C07C227/42 ,  C07C229/04

CPC classification number: C07C227/18 ,  C07C227/10 ,  C11D3/33 ,  C07C227/42 ,  C07C229/36

Abstract: Process for manufacturing a crystalline alkali metal salt of the general formula (I) [R 1 -CH(COO)-N(CH 2 -COO) 2 ]M 1 3 (I) wherein M 1 is selected from alkali metal cations, same or different, R 1 is selected from C 1 -C 4 -alkyl and CH 2 CH 2 COOM 1 , comprising the step of (b) crystallizing said alkali metal salt from an aqueous solution containing in the range of from 5 to 30% by weight of alkali metal hydroxide, referring to said aqueous solution.

Abstract translation: 制备通式（I）的结晶碱金属盐的方法[R 1 -CH（COO）-N（CH 2）2] -COO）2 M 1 M 3（I）其中M 1选自碱金属阳离子，相同的 或者不同，R 1选自C 1 -C 4 - 烷基和CH 2 CH 2 - 包括以下步骤：（b）使所述碱金属盐从含有5至30重量％的碱金属氢氧化物的水溶液中结晶出来，指的是 所述水溶液。

公开(公告)号：WO2016180664A1

公开(公告)日：2016-11-17

申请号：PCT/EP2016/059821

申请日：2016-05-03

Applicant: BASF SE

Inventor： STAMM, Armin ,  SCHMIDT, Thomas ,  ORR, Christopher ,  MANNING, Jeremy

IPC: C07C227/18 ,  C07C229/24 ,  C09K8/035 ,  C11D3/33

CPC classification number: C07C227/18 ,  C01D1/04 ,  C07C229/16 ,  C09K8/035 ,  C11D3/33 ,  C11D11/0023

Abstract: Process for making a chelating agent according to the general formula (I), R 1 -CH(COOX 1 )-N(CH2COOX 1 ) 2 wherein R 1 is selected from hydrogen, C 1 -C 4 -alkyl, phenyl, benzyl, CH 2 OH, and CH 2 CH 2 COOX 1 , X 1 is (Μ χ Η 1-χ ), M being selected from alkali metal, x is in the range of from 0.6 to 1, said process comprising the following steps: (a) providing a solid, a slurry or a solution of a compound according to general formula (II a) R 1 -CH(COOX 2 )-N(CH 2 CN) 2 wherein X 2 is (M y H 1-y ), M being selected from alkali metal, y is in the range of from zero to 1, (b) contacting said solid or slurry or solution with an aqueous solution of alkali metal hydroxide, wherein the molar ratio of alkali metal ions to nitrile groups is in the range of from 0.6:1 to 0.95:1, (c) reacting said compound according to general formula (II a) with said alkali metal hydroxide.

Abstract translation: 制备根据通式（I）的螯合剂的方法，R1-CH（COOX1）-N（CH2COOX1）2，其中R1选自氢，C1-C4-烷基，苯基，苄基，CH2OH和CH2CH2COOX1，X1 是（ΜχH1-χ），M选自碱金属，x在0.6至1的范围内，所述方法包括以下步骤：（a）提供一般化合物的固体，浆液或溶液 式（IIa）R1-CH（COOX2）-N（CH2CN）2，其中X2是（MyH1-y），M选自碱金属，y在0至1的范围内，（b）使所述固体 或碱性金属氢氧化物水溶液的浆液或溶液，其中碱金属离子与腈基的摩尔比在0.6:1至0.95:1的范围内，（c）使通式（II）的所述化合物 a）与所述碱金属氢氧化物反应。

公开(公告)号：WO2016058875A1

公开(公告)日：2016-04-21

申请号：PCT/EP2015/073103

申请日：2015-10-07

Applicant: BASF SE

Inventor： REINOSO GARCIA, Marta ,  FRANZKE, Constanze ,  STAMM, Armin

IPC: C07C227/26 ,  C07C229/24 ,  C11D1/10

CPC classification number: C07C229/16 ,  C07C227/26 ,  C11D3/044 ,  C11D3/046 ,  C11D3/10 ,  C11D3/2079 ,  C11D3/2082 ,  C11D3/33

Abstract: Aqueous solution containing in the range of from 60.5 to 75 % by weight of a mixture of trialkalimetal salts of the L-and D-enantiomers of methyl glycine diacetic acid (MGDA), said mixture containing predominantly the respective L-isomer with an enantiomeric excess (ee) in the range of from 3 to 97%, wherein said trialkali metal salts have the general formula (I) [CH 3 -CH(COO)-N(CH 2 -COO) 2 ]K 3-x Na x (I) wherein x is in the range of from zero to 2.9.

Abstract translation: 含有60.5至75重量％的甲基甘氨酸二乙酸的L-和D-对映异构体的三碱金属盐（MGDA）的混合物的水溶液，所述混合物主要含有相应的L-异构体和对映体过量的 （ee）的范围为3-97％，其中所述三碱金属盐具有通式（I）[CH3-CH（COO）-N（CH2-COO）2] K3-xNax（I）其中x为 范围从零到2.9。

公开(公告)号：WO2009109544A1

公开(公告)日：2009-09-11

申请号：PCT/EP2009/052447

申请日：2009-03-02

Applicant: BASF SE ,  OFTRING, Alfred ,  STAMM, Armin ,  WIRSING, Friedrich ,  BRAUN, Gerold

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

IPC: C07C227/26 ,  C07C229/24

CPC classification number: C07C227/18 ,  C07C229/24

Abstract: Die vorliegende Erfindung betrifft ein Verfahren zur Herstellung von Aminodicarbonsäu- re-N,N-diessigsäuren der allgemeinen Formel I worin X unabhängig voneinander für Wasserstoff oder Alkalimetall steht und n eine Zahl 1 oder 2 bezeichnet. Weiterhin betrifft die Erfindung Aminodicarbonsäure-N,N- diessigsäuren hoher Reinheit. Das erfindungsgemäße Verfahren umfasst die folgenden Schritte: a) Umsetzung einer Aminodicarbonsäure der allgemeinen Formel Il worin X und n die zuvor genannten Bedeutungen haben, mit 0,8 bis 1,2 MoI- Äquivalenten Formaldehyd und mit 0,8 bis 1,2 Mol-Äquivalenten Blausäure; b) Umsetzung des in Schritt a) erhaltenen Reaktionsprodukts mit 0,8 bis 1,2 Mol- Äquivalenten Blausäure und mit 0,8 bis1,2 Mol-Äquivalenten Formaldehyd; c) Hydrolyse des in Schritt b) erhaltenen Reaktionsprodukts.

Abstract translation: 本发明涉及一种方法，用于Aminodicarbonsäu-重新N，通式I的N-二羧酸的制备，其中X独立地为氢或碱金属，n是数字1或第二 此外，本发明氨基二羧酸N，N-二酸类涉及高纯度。 本发明的方法包括以下步骤：a）使通式II的氨基二羧酸，其中X和n具有上述含义，与甲醛的0.8〜1.2当量的MOI和0.8〜1.2摩尔 氰化物的等同物; B）在步骤a）反应产物与氰化氢和甲醛的0.8至1.2摩尔当量0.8〜1.2摩尔当量得到的产物反应; C）水解步骤b中获得的反应产物）。