Processes for producing succinic acid from fermentation broths containing diammonium succinate

Abstract

Processes for making SA from either a clarified DAS-containing fermentation broth or a clarified MAS-containing fermentation broth that include distilling the broth under super atmospheric pressure at a temperature of >100° C. to about 300° C. to form an overhead that comprises water and ammonia, and a liquid bottoms that includes SA, and at least about 20 wt % water; cooling the bottoms to a temperature sufficient to cause the bottoms to separate into a liquid portion and a solid portion that is substantially pure SA; and separating the solid portion from the liquid portion. A method also reduces the broth distillation temperature and pressure by adding an ammonia separating and/or water azeotroping solvent to the broth.

1 . A process for making SA from a clarified DAS-containing fermentation broth comprising:
 (a) distilling the broth under super atmospheric pressure at a temperature of >100° C. to about 300° C. to form an overhead that comprises water and ammonia, and a liquid bottoms that comprises SA, and at least about 20 wt % water;   (b) cooling and/or evaporating the bottoms to attain a temperature and composition sufficient to cause the bottoms to separate into a liquid portion and a solid portion that is substantially pure SA; and   (c) separating the solid portion from the liquid portion.   
     
     
         2 . The process of  claim 1 , wherein the liquid bottoms contains at least some MAS and/or the solid portion is substantially free of succinamic acid, succinamide and succinimide. 
     
     
         3 . The process of  claim 1 , further comprising recycling the SA and water and, optionally, MAS from the liquid bottoms to the clarified broth. 
     
     
         4 . The process of  claim 1 , further comprising removing water from the liquid bottoms to increase concentration of SA in the liquid bottoms. 
     
     
         5 . The process of  claim 1 , wherein distilling the broth is carried out in the presence of an ammonia separating solvent which is at least one selected from the group consisting of diglyme, triglyme, tetraglyme, sulfoxides, amides, sulfones, polyethyleneglycol (PEG), butoxytriglycol, N-methylpyrolidone (NMP), ethers, and methyl ethyl ketone (MEK) or in the presence of a water azeotroping solvent which is at least one selected from the group consisting of toluene, xylene, methylcyclohexane, methyl isobutyl ketone, hexane, cyclohexane and heptane. 
     
     
         6 . A process for making SA from a clarified DAS-containing fermentation broth comprising:
 (a) adding an ammonia separating and/or water azeotroping solvent to the broth;   (b) distilling the broth at a temperature and pressure sufficient to form an overhead that comprises water and ammonia, and a liquid bottoms that comprises SA, and at least about 20 wt % water;   (c) cooling and/or evaporating the bottoms to attain a temperature and composition sufficient to cause the bottoms to separate into a liquid portion and a solid portion that is substantially pure SA; and   (d) separating the solid portion from the liquid portion.   
     
     
         7 . The process of  claim 6 , wherein the liquid bottoms contains at least some MAS and/or the solid portion is substantially free of succinamic acid, succinamide and succinimide. 
     
     
         8 . The process of  claim 6 , further comprising recycling the SA, water, and the solvent and, optionally, MAS from the liquid bottoms to the clarified broth. 
     
     
         9 . The process of  claim 6 , wherein distilling the broth is carried out in the presence of an ammonia separating solvent which is at least one selected from the group consisting of diglyme, triglyme, tetraglyme, sulfoxides, amides, sulfones, polyethyleneglycol (PEG), butoxytriglycol, N-methylpyrolidone (NMP), ethers, and methyl ethyl ketone (MEK) or in the presence of a water azeotroping solvent which is at least one selected from the group consisting of toluene, xylene, methylcyclohexane, methyl isobutyl ketone, hexane, cyclohexane and heptane. 
     
     
         10 . The process of  claim 6 , further comprising removing water from the liquid bottoms to increase concentration of SA in the liquid bottoms. 
     
     
         11 . A process for making SA from a clarified MAS-containing fermentation broth comprising:
 (a) distilling the broth under super atmospheric pressure at a temperature of >100° C. to about 300° C. to form an overhead that comprises water and ammonia, and a liquid bottoms that comprises SA, and at least about 20 wt % water;   (b) cooling and/or evaporating the bottoms to attain a temperature and composition sufficient to cause the bottoms to separate into a liquid portion and a solid portion that is substantially pure SA; and   (c) separating the solid portion from the liquid portion.   
     
     
         12 . The process of  claim 11 , wherein the liquid bottoms contains at least some MAS and/or the solid portion is substantially free of succinamic acid, succinamide and succinimide. 
     
     
         13 . The process of  claim 11 , further comprising recycling the SA and water and optionally MAS from the liquid bottoms to the clarified broth. 
     
     
         14 . The process of  claim 11 , further comprising removing water from the liquid bottoms to increase concentration of SA in the liquid bottoms. 
     
     
         15 . The process of  claim 11 , wherein distilling the broth is carried out in the presence of an ammonia separating solvent which is at least one selected from the group consisting of diglyme, triglyme, tetraglyme, sulfoxides, amides, sulfones, polyethyleneglycol (PEG), butoxytriglycol, N-methylpyrolidone (NMP), ethers, and methyl ethyl ketone (MEK) or in the presence of a water azeotroping solvent which is at least one selected from the group consisting of toluene, xylene, methylcyclohexane, methyl isobutyl ketone, hexane, cyclohexane and heptane. 
     
     
         16 . A process for making SA from a clarified MAS-containing fermentation broth comprising:
 (a) adding an ammonia separating and/or water azeotroping solvent to the broth;   (b) distilling the broth at a temperature and pressure sufficient to form an overhead that comprises water and ammonia, and a liquid bottoms that comprises SA, and at least about 20 wt % water;   (c) cooling and/or evaporating the bottoms to attain a temperature and composition sufficient to cause the bottoms to separate into a liquid portion and a solid portion that is substantially pure SA; and   (d) separating the solid portion from the liquid portion.   
     
     
         17 . The process of  claim 16 , wherein the liquid bottoms contains at least some MAS and/or the solid portion is substantially free of succinamic acid, succinamide and succinimide. 
     
     
         18 . The process of  claim 16 , further comprising recycling the SA, water, and the solvent and, optionally, MAS from the liquid bottoms to the clarified broth. 
     
     
         19 . The process of  claim 16 , wherein distilling the broth is carried out in the presence of an ammonia separating solvent which is at least one selected from the group consisting of diglyme, triglyme, tetraglyme, sulfoxides, amides, sulfones, polyethyleneglycol (PEG), butoxytriglycol, N-methylpyrolidone (NMP), ethers, and methyl ethyl ketone (MEK) or in the presence of a water azeotroping solvent which is at least one selected from the group consisting of toluene, xylene, methylcyclohexane, methyl isobutyl ketone, hexane, cyclohexane and heptane. 
     
     
         20 . The process of  claim 16 , further comprising removing water from the liquid bottoms to increase concentration of MAS in the liquid bottoms.