The invention relates to a preparation method of 3-guanidino
propanoic acid. The preparation method comprises the following steps of: adding 3-aminopropionic acid to
methanol, thereby obtaining a solution a at 15 DEG C; putting monocyanamide into
methanol, thereby obtaining a solution b; feeding the solution b to the solution a, thereby obtaining a solution c at a temperature within 15 DEG C and PH in the range from 7.5 to 8.0; performing vacuum concentration on the solution c and filtering at -5 DEG C, thereby obtaining a crude product of
sodium 3-
guanidine propionate; preparing the crude product into an
aqueous solution of
sodium 3-
guanidine propionate, thereby obtaining a solution d2; filling H type weakly acidic cation exchange resin into an
ion exchange column, and feeding the solution d2 into the
ion exchange column and detecting no 3-guanidino
propanoic acid; blending the exchange solution collected by the step e and performing decompression concentration on the exchange solution, feeding
methanol, reducing the temperature to -10 DEG C for
crystallization, thereby obtaining a crystalline mixed liquid f; and then filtering and
drying the crystalline mixed liquid f to obtain 3-guanidino
propanoic acid. The problem of removing
sodium ions during the production of 3-guanidino propanoic acid is solved through exchange treatment of the weakly acidic cation exchange resin; as methanol is taken as a
solvent, the utilization and
recovery cost of the
solvent is lower and the preparation method is
safer to operate; side-reactions are few; the 3-guanidino propanoic acid is extracted by
ion resin exchange; and the yield of the 3-guanidino propanoic acid is 76.0% and the purity of the 3-guanidino propanoic acid is 99.0%.