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    Method for preparation of N-phosphonomethylglycine
    3.
    发明公开
    Method for preparation of N-phosphonomethylglycine 失效
    Verfahren zur Herstellung von N-膦酰基甲基甘氨酸。

    公开(公告)号：EP0164923A2

    公开(公告)日：1985-12-18

    申请号：EP85303444.5

    申请日：1985-05-16

    Applicant: STAUFFER CHEMICAL COMPANY

    Inventor： Dinizo, Stephen Edward ,  Djafar, Roger Rachid

    IPC: C07F9/38

    CPC classification number: C07F9/3813

    Abstract: An improved method of preparing N-phosphonomethylglycine in yields over 80 percent comprising: (a) hydrolyzing a phosphonate of the formula
    wherein in R, R' and R 2 are C 1 -C 4 alkyl at a temperature between about 55°C to reflux temperature water in an amount sufficient to provide a mole ratio of water to phosphonate within a range of abut 10:1 to about 60:1 and HCI in an amount sufficient to provide a mole ratio of HCI to phosphonate within a range of about 2:1 to about 4:1 or higher to yield an acidic aqueous solution of N-phosphonomethylglycine; (b) removing volatile phosphonate from the acidic aqueous solution of N-phosphonomethylglycine either during or after the hydrolyzing step; (c) precipitating N-phosphonomethylglycine from the acidic solution of N-phosphonomethylglycine by: (1) cooling said solution to below about 80°C; (2) raising the pH of the said solution to within a range of about 1.0 to about 1.8; (3) seeding the solution with 2-4 ppm solid N-phosphonomethylglycine with agitation; and (4) further cooling said solution to about 25°C and continuing agitation and cooled for about 1.5 hours; (d) recovering the precipitated N-phosphonomethylglycine from its mother liquor; and (e) washing the recovered N-phosphonomethylglycine with water to remove impurities and ammonium chloride.

    Abstract translation: 一种改进的N-膦酰基甲基甘氨酸的制备方法，其产率高于80％，包括：（a）水解式CHEM的膦酸酯，其中在R 1，R 2和R 2中的C 1 -C 4烷基在约 55℃至回流温度的水，其量足以提供约10:1至约60:1范围内的水与膦酸酯的摩尔比，并且HCl的量足以提供HCl与膦酸盐的摩尔比在 范围为约2:1至约4:1或更高，得到N-膦酰基甲基甘氨酸的酸性水溶液; （b）在水解步骤期间或之后从N-膦酰基甲基甘氨酸的酸性水溶液中除去挥发性膦酸酯; （c）通过以下步骤从N-膦酰基甲基甘氨酸的酸性溶液中沉淀N-膦酰基甲基甘氨酸：（1）将所述溶液冷却至低于约80℃; （2）将所述溶液的pH提高到约1.0至约1:8的范围内; （3）搅拌下用2-4ppm固体N-膦酰基甲基甘氨酸接种溶液; 和（4）将所述溶液进一步冷却至约25℃并继续搅拌并冷却约1.5小时; （d）从其母液中回收沉淀的N-膦酰基甲基甘氨酸; 和（e）用水洗涤回收的N-膦酰基甲基甘氨酸以除去杂质和氯化铵。

    Method of preparation and use of solid, phytoactive compositions
    4.
    发明公开
    Method of preparation and use of solid, phytoactive compositions 失效
    制备和使用固体，物理组合物的方法

    公开(公告)号：EP0256608A3

    公开(公告)日：1989-03-08

    申请号：EP87201554.0

    申请日：1987-08-17

    Applicant: STAUFFER CHEMICAL COMPANY

    Inventor： Djafar, Roger Rachid ,  Benke, Alan Henry

    IPC: A01N25/14 ,  A01N57/20

    CPC classification number: C07F9/3813 ,  A01N25/30 ,  A01N57/20 ,  A01N2300/00

    Abstract: A method for the preparation of a solid, phytoactive composition comprising: (a) reacting an acid form of a phytoactive N-phosphonomethyl-­N-carboxylmethyl compound with a liquid amine to form the amine salt of said N-phosphonomethyl-N-carboxylmethyl compound; (b) admixing said amine salt of said N-phosphonomethyl-N-carboxylmethyl compound with a molten surfactant, the surfactant being solid at ambient temperatures; and (c) cooling said mixture to a temperature below the melting point of the sur­factant to form a composition comprising said surfactant and said amine salt of N-phosphonomethyl-N-carboxylmethyl compound interdispersed in the matrix thereof and which is solid at ambient temperatures.

    Method of preparation and use of solid, phytoactive compositions
    5.
    发明公开
    Method of preparation and use of solid, phytoactive compositions 失效
    Verfahren zur Herstellung und Verwendung fester，pflanzenwirksamer Zusammensetzungen。

    公开(公告)号：EP0256608A2

    公开(公告)日：1988-02-24

    申请号：EP87201554.0

    申请日：1987-08-17

    Applicant: STAUFFER CHEMICAL COMPANY

    Inventor： Djafar, Roger Rachid ,  Benke, Alan Henry

    IPC: A01N25/14 ,  A01N57/20

    CPC classification number: C07F9/3813 ,  A01N25/30 ,  A01N57/20 ,  A01N2300/00

    Abstract: A method for the preparation of a solid, phytoactive composition comprising: (a) reacting an acid form of a phytoactive N-phosphonomethyl-­N-carboxylmethyl compound with a liquid amine to form the amine salt of said N-phosphonomethyl-N-carboxylmethyl compound; (b) admixing said amine salt of said N-phosphonomethyl-N-carboxylmethyl compound with a molten surfactant, the surfactant being solid at ambient temperatures; and (c) cooling said mixture to a temperature below the melting point of the sur­factant to form a composition comprising said surfactant and said amine salt of N-phosphonomethyl-N-carboxylmethyl compound interdispersed in the matrix thereof and which is solid at ambient temperatures.

    Abstract translation: 一种制备固体植物组合物的方法，包括：（a）将酸形式的植物活性N-膦酰基甲基-N-羧基甲基化合物与液体胺反应，形成所述N-膦酰基甲基-N-羧基甲基化合物的胺盐 ; （b）将所述N-膦酰基甲基-N-羧基甲基化合物的所述胺盐与熔融的表面活性剂混合，所述表面活性剂在环境温度下为固体; 和（c）将所述混合物冷却至低于表面活性剂熔点的温度，以形成包含所述表面活性剂和所述N-膦酰基甲基-N-羧甲基化合物的胺盐的组合物，其分散于其基质中，并且在环境温度下为固体。

    Method for preparation of N-phosphonomethylglycine
    7.
    发明公开
    Method for preparation of N-phosphonomethylglycine 失效
    制备N-磷杂双环十六烷基的方法

    公开(公告)号：EP0164923A3

    公开(公告)日：1986-04-16

    申请号：EP85303444

    申请日：1985-05-16

    Applicant: STAUFFER CHEMICAL COMPANY

    Inventor： Dinizo, Stephen Edward ,  Djafar, Roger Rachid

    IPC: C07F09/38

    CPC classification number: C07F9/3813

    Abstract: An improved method of preparing N-phosphonomethylglycine in yields over 80 percent comprising: (a) hydrolyzing a phosphonate of the formula
    wherein in R, R' and R 2 are C 1 -C 4 alkyl at a temperature between about 55°C to reflux temperature water in an amount sufficient to provide a mole ratio of water to phosphonate within a range of abut 10:1 to about 60:1 and HCI in an amount sufficient to provide a mole ratio of HCI to phosphonate within a range of about 2:1 to about 4:1 or higher to yield an acidic aqueous solution of N-phosphonomethylglycine; (b) removing volatile phosphonate from the acidic aqueous solution of N-phosphonomethylglycine either during or after the hydrolyzing step; (c) precipitating N-phosphonomethylglycine from the acidic solution of N-phosphonomethylglycine by: (1) cooling said solution to below about 80°C; (2) raising the pH of the said solution to within a range of about 1.0 to about 1.8; (3) seeding the solution with 2-4 ppm solid N-phosphonomethylglycine with agitation; and (4) further cooling said solution to about 25°C and continuing agitation and cooled for about 1.5 hours; (d) recovering the precipitated N-phosphonomethylglycine from its mother liquor; and (e) washing the recovered N-phosphonomethylglycine with water to remove impurities and ammonium chloride.

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