Synthesis of phosphonomethyliminodiacetic acid with reduced effluent
    3.
    发明授权
    Synthesis of phosphonomethyliminodiacetic acid with reduced effluent 失效
    合成具有减少流出物的膦酰基甲基亚氨基二乙酸

    公开(公告)号:US06118022A

    公开(公告)日:2000-09-12

    申请号:US388409

    申请日:1999-09-01

    申请人: Barry A. Cullen

    发明人: Barry A. Cullen

    IPC分类号: C07F9/38

    CPC分类号: C07F9/3813

    摘要: A process for the preparation of phosphonomethylglycine in high yields is disclosed. In accordance with the process of the present invention, alkali metal IDA, such as disodium IDA, is reacted with a strong mineral acid, such as HCl, to convert the salt of IDA to IDA. The IDA is then converted to soluble IDA phosphite salt by the addition of phosphorous acid, and the alkali metal salt of the strong acid is precipitated. The phosphite salt of IDA is phosphonomethylated, such as by the addition of PCl.sub.3 and formaldehyde. Optionally, phosphorous trichloride can be hydrolyzed to provide the phosphorous acid source for phosphonomethylation of the phosphite salt.

    摘要翻译: 公开了以高产率制备膦酰基甲基甘氨酸的方法。 根据本发明的方法,碱金属IDA如IDA二钠与强无机酸如HCl反应,将IDA的盐转化为IDA。 然后通过加入亚磷酸将IDA转化为可溶性的IDA亚磷酸盐,强酸的碱金属盐沉淀。 IDA的亚磷酸盐是膦酰甲基化的,例如通过加入PCl 3和甲醛。 任选地,可以将三氯化磷水解以提供亚磷酸盐的膦酰基甲基化的亚磷酸源。

    Facile synthesis of phosphonomethylglycine from phosphonomethyliminodiacetic acid
    4.
    发明授权
    Facile synthesis of phosphonomethylglycine from phosphonomethyliminodiacetic acid 失效
    从膦酰甲基亚氨基二乙酸轻松合成膦酰基甲基甘氨酸

    公开(公告)号:US06365772B1

    公开(公告)日:2002-04-02

    申请号:US08453003

    申请日:1995-05-30

    IPC分类号: C07F922

    CPC分类号: C07F9/3813

    摘要: A process for the preparation of phosphonomethylglycine in nearly quantitative yields which eliminates the use of a noble metal co-catalyst and its concomitant problems. The oxygen-containing gas is replaced with the much more chemically active hydrogen peroxide, which in combination with activated carbon, oxidizes the PMIDA to PMG in very high yield. The amount of oxidant allowed to react with PMIDA is a function of the concentration of oxygen in the gaseous reaction products, and is controlled by monitoring that concentration. In another embodiment, the oxidizing agent is an oxygen-containing gas. In either case, the concentration of oxygen in the gaseous reaction product is monitored to determine the end point of the reaction.

    摘要翻译: 以几乎定量的产率制备膦酰基甲基甘氨酸的方法,其消除了贵金属助催化剂的使用及其伴随的问题。 含氧气体被更多的化学活性过氧化氢代替,其与活性炭结合,以非常高的产率将PMIDA氧化成PMG。 允许与PMIDA反应的氧化剂的量是气态反应产物中的氧浓度的函数,并且通过监测该浓度来控制。 在另一个实施方案中,氧化剂是含氧气体。 在任一情况下,监测气态反应产物中的氧浓度以确定反应的终点。

    Preparation of ethylenediaminetriacetic acid
    5.
    发明授权
    Preparation of ethylenediaminetriacetic acid 失效
    乙二胺三乙酸的制备

    公开(公告)号:US5449822A

    公开(公告)日:1995-09-12

    申请号:US60219

    申请日:1993-05-07

    摘要: Synthesis of ethylenediaminetriacetic acid (ED3A) or its salts is disclosed. A salt of N,N'-ethylenediaminediacetic acid (ED2AH.sub.2) is condensed with formaldehyde to form a stable 5-membered ring intermediate. The addition of cyanide across this cyclic material forms ethylenediamine N,N'-diacetic acid-N'-cyanomethyl or salts thereof (mononitrile-diacid). The nitrile in aqueous solutions may be spontaneously cyclized to form 2-oxo-1,4-piperazinediacetic acid (3KP) or salts thereof, which is the desired cyclic intermediate. In the presence of excess base, salts of ED3A are formed in excellent yield and purity. Alternatively, the starting material is ED2AH.sub.a X.sub.b, where x is a base cation, e.g., an alkali or alkaline earth metal, a is 1 to 2, and b is 0 to 1 in aqueous solutions. The reaction mixture also can be acidified to ensure complete formation of carboxymethyl-2-oxopiperazine (the lactam) prior to the reaction. Formaldehyde is added, essentially resulting in the hydroxymethyl derivative. On the addition of a cyanide source, 1-cyanomethyl-4-carboxymethyl-2-ketopiperazine (mononitrile diacid) or a salt thereof is formed. Upon the addition of any suitable base or acid, this material may be hydrolyzed to 3KP. The addition of a base will open this ring structure to form the salt of ED3A.

    摘要翻译: 公开了乙二胺三乙酸(ED3A)或其盐的合成。 N,N'-乙二胺二乙酸(ED2AH2)的盐与甲醛缩合形成稳定的5元环中间体。 在该环状物质中加入氰化物形成乙二胺N,N'-二乙酸-N'-氰基甲基或其盐(单腈 - 二酸)。 水溶液中的腈可以自发环化以形成2-氧代-1,4-哌嗪二乙酸(3KP)或其盐,其为期望的环状中间体。 在过量碱的存在下,ED3A的盐以优异的产率和纯度形成。 或者,原料为ED2AHaXb,其中x为碱性阳离子,例如碱金属或碱土金属,a为1至2,b为0至1。 反应混合物也可以酸化以确保在反应之前完全形成羧甲基-2-氧代哌嗪(内酰胺)。 加入甲醛,基本上得到羟甲基衍生物。 在加入氰化物源时,形成1-氰甲基-4-羧甲基-2-酮哌嗪(单腈二酸)或其盐。 加入任何合适的碱或酸后,该物质可水解成3KP。 添加碱将打开该环结构形成ED3A的盐。

    Process for recovering dissolved iminodiacetonitrile from effluent
liquors
    6.
    发明授权
    Process for recovering dissolved iminodiacetonitrile from effluent liquors 失效
    从流出液中回收溶解的亚氨基二乙腈的方法

    公开(公告)号:US4156096A

    公开(公告)日:1979-05-22

    申请号:US886934

    申请日:1978-03-15

    申请人: Barry A. Cullen

    发明人: Barry A. Cullen

    CPC分类号: C07C255/00

    摘要: A process for recovering iminodiacetonitrile (IDAN) values from an aqueous IDAN solution comprising: (a) extracting the aqueous IDAN solution with methylene chloride to dissolve a portion of IDAN in the methylene chloride to form a methylene chloride solution of IDAN; and (b) separating and recovering the IDAN values from the methylene chloride.In an alternative embodiment the IDAN values can be separated from the methylene chloride solution of IDAN by extracting the methylene chloride solution with an aqueous alkali metal hydroxide solution to form water-soluble dialkali metal iminodiacetate (IDAM.sub.2 wherein M is an alkali metal cation) which remains in the aqueous alkali metal hydroxide solution. The IDAM.sub.2 can be recovered from the alkali metal hydroxide solution by conventional methods (e.g., by treating with a strong acid to precipitate iminodiacetic acid (IDA)).Each extraction (the extraction with methylene chloride and the extraction with aqueous alkali metal hydroxide solution) can be conducted as a batchwise extraction or as a continuous counter-current extraction.

    摘要翻译: 从IDAN水溶液中回收亚氨基二乙腈(IDAN)值的方法,包括:(a)用二氯甲烷萃取IDAN水溶液,将部分IDAN溶解在二氯甲烷中以形成IDAN的二氯甲烷溶液; 和(b)从二氯甲烷中分离和回收IDAN值。

    Conversion of hydroxymethyl-iminodiacetic acid to
phosphonomethyl-iminodiacetic acid
    9.
    发明授权
    Conversion of hydroxymethyl-iminodiacetic acid to phosphonomethyl-iminodiacetic acid 失效
    羟甲基亚氨基二乙酸转化为膦酰基甲基亚氨基二乙酸

    公开(公告)号:US5312972A

    公开(公告)日:1994-05-17

    申请号:US969705

    申请日:1992-10-29

    申请人: Barry A. Cullen

    发明人: Barry A. Cullen

    CPC分类号: C07C227/18 C07F9/3808

    摘要: A process for preparing N-phosphonomethyl iminodiacetic acid wherein solutions of an alkali metal salt of IDA are reacted with formaldehyde so as to form the alkali metal salt of hydroxymethyliminodiacetic acid (HMIDA). The HMIDA can be subsequently reacted with a phosphorous source such as phosphorous acid to produce PMIDA in good yield.

    摘要翻译: 一种制备N-膦酰甲基亚氨基二乙酸的方法,其中IDA的碱金属盐溶液与甲醛反应形成羟甲基亚氨基二乙酸(HMIDA)的碱金属盐。 HMIDA随后可以与磷源如亚磷酸反应以产生良好的产率的PMIDA。