METHOD FOR PURIFYING 1,4-DIAMINOBUTANE Russian patent published in 2019 - IPC C07C211/09 C07C209/86 C12P13/00 C07C209/84 

FIELD: chemistry.

SUBSTANCE: invention relates to embodiments of an improved method of purifying 1,4-diaminobutane (putrescine). Method includes steps of: separating a second composition containing 1,4-diaminobutane carbonate salt from a first composition which is fermentation broth or a concentrate thereof containing 1,4-diaminobutane carbonate salt by distillation; and removing carbonate from 1,4-diaminobutane carbonate salt contained in second composition by fractional distillation to recover 1,4-diaminobutane. Distillation is carried out at steam temperature in the range of about 30 °C to 158 °C and pressure in the range of about 10 mm Hg. up to about 760 mm Hg., and pH of second composition is 10.0 or more; fractional distillation is performed at steam temperature in the interval from approximately 100 °C to 230 °C and pressure in the range from approximately 1 atm to approximately 5 atm. 1,4-diaminobutane carbonate salt is at least 1,4-diaminobutane carbonate or 1,4-diaminobutane bicarbonate. Concentrate is obtained by concentrating the fermentation broth at steam temperature in the range of about 10 °C to about 100 °C and pressure in the range of about 10 mm Hg. up to about 760 mm Hg; pH of concentrate is 10.0 or more than 2. At that, 70 wt. % or more of the carbonate salt of 1,4-diaminobutane contained in the first composition is separated during distillation. Fractional distillation is carried out using distillation column. 1,4-Diaminobutane is extracted from lower part of distillation column. Another method of purifying 1,4-diaminobutane involves the steps of: culturing a microorganism which generates 1,4-diaminobutane in a medium while providing a nitrogen source in order to obtain 1,4-diaminobutane carbonate salt; preparing fermentation broth or concentrate thereof containing 1,4-diaminobutane carbonate salt; separating a third composition comprising a carbonate salt of 1,4-diaminobutane by distilling fermentation broth or a concentrate thereof; and removing carbonate from 1,4-diaminobutane carbonate contained in third composition by fractional distillation to recover 1,4-diaminobutane. Distillation, fractional distillation and extraction of 1,4-diaminobutane are carried out as described above. Nitrogen source is at least one selected from ammonium, ammonium salt of an organic compound of a nitrogen-containing organic compound and an inorganic compound based on carbonate. Additionally, bacterial cells may be removed from the fermentation broth prior to separation of the third composition; 70 wt. % or more of 1,4-diaminobutane carbonate salt contained in the third composition is separated during distillation. pH of the third composition is 10.0 or more.

EFFECT: disclosed purification method simplifies the process by reducing the amount of the added alkaline agent, reduces formation of by-products and obtain 1,4-diaminobutane with output of 91_8–98 %.

16 cl, 2 dwg, 21 tbl, 6 ex