Method for preparation of n-phosphonomethylglycine

Details Method for preparation of n-phosphonomethylglycine Method for preparation of n-phosphonomethylglycine

C - Chemistry, Metallurgy

07

F

260/501.5

C07F 9/38 (2006.01)

Patent

CA 1238916

METHOD FOR PREPARATION OF N-PHOSPHONOMETHYLGLYCINE Abstract of the Disclosure An improved method of preparing N-phosphonomethylglycine in yields over 80 percent comprising: (a) hydrolyzing a phosphonate of the formula Image wherein in R, R1 and R2 are C1-C4 alkyl at a temperature between about 55°C to reflux temperature with 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 HCl in an amount sufficient to provide a mole le ratio of HCl 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 organic by-products of the hydrolysis and any organic solvent for the phosphonate from the acidic aqueous solution of N-phosphonomethylglycine either during or after the hydrolyzing step; (c) precipitating N-phos- phonomethylglycine from the acidic solution of N-phosphonamethylglycine by: (1) cooling said solution to below about 80°C; (2) raising the pH ofthe 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 agita-tion 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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