公开(公告)号：EP0164923B1

公开(公告)日：1988-08-03

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

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。

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.