Process for producing of citric acid and monovalent citrate salts

• US 5,532,148 A
• Filed: 08/30/1995
• Issued: 07/02/1996
• Est. Priority Date: 08/30/1995
• Status: Expired due to Fees

• Current Assignee: NTEC, Inc.
• Original Assignee: NTEC, Inc.
• Inventors: Datta, Rathin, Bergemann, Eugene P.
• Primary Examiner(s): Lilling, Herbert J.
• Application Number:
  US08/521,210
• Time in Patent Office: 307 Days
• Field of Search: 435/144, 435/917, 435/136, 435/803
• US Class Current: 435/144
• CPC Class Codes: C12P 7/48 Tricarboxylic acids, e.g. citric acid
• CPC Class Codes: Y10S 435/80 Elimination or reduction of contamination by undersired ferments, e.g. aseptic cultivation
• CPC Class Codes: Y10S 435/917 Aspergillus niger

Abstract

A short process is disclosed for the production of citric acid in high yield and purity. Conidia of Aspergillus niger are cultured in an aqueous solution of decationized glucose syrup in a fermentation medium whose manganese(II) concentration is 2.5 to less than 20 parts per billion and whose pH value is about 1.5 to about 3.0. The fermentation medium is maintained for about 4-7 days to form citric acid and mycelia pellets in an aqueous product broth. That broth is filtered and then electrodialyzed to form a citric acid-containing aqueous broth. That broth is decolorized and ion-exchanged to remove color and inorganic ions and form an aqueous citric acid solution in which citric acid constitutes at least 98 percent of the organic acid present.

Claims

1. A process for preparing citric acid that comprises the steps of:

(a) culturing Aspergillus Niger conidia at a concentration of about 1×

10⁵ to about 1×

10⁶ conidia/mL in an aqueous solution of decationized glucose syrup to form a fermentation medium, said fermentation medium (i) containing salts suitable for germinating said conidia and forming mycelia pellets in a submerged culture, (ii) containing about 2.5 to less than 20 parts per billion Mn⁺² ions and (iii) having a pH value of about 1.5 to about 3.0;

(b) maintaining said fermentation medium at said pH value and at a temperature of about 25°

to about 35°

C. under aerobic conditions for a time period of about 4 to about 7 days to form mycelia pellets in an aqueous product broth;

(c) filtering said product broth to remove said mycelia pellets and form a clear, citric acid-containing aqueous broth;

(d) electrodialyzing said citric acid-containing aqueous broth to form a citric acid-containing aqueous concentrate; and

(e) decolorizing and ion-exchanging said citric acid-containing aqueous concentrate to remove color and inorganic ions therefrom and form an aqueous citric acid solution in which citric acid constitutes at least 98 percent of the organic acid present.

2. The process according to claim 1 wherein the concentration of Mn⁺² ions in said fermentation medium is about 3 to about 10 parts per billion.

3. The process according to claim 1 wherein said decatonized glucose syrup is present in said fermentation medium at a concentration of about 100 to about 200 g/L.

4. The process according to claim 1 wherein said fermentation is maintained for a time period of about 5 to about 6 days.

5. A process for preparing citric acid that comprises the steps of:

(a) culturing Aspergillus Niger conidia at a concentration of about 1×

10⁵ to about 1×

10⁶ spores/mL in an aqueous solution of decationized glucose syrup present at about 100 to about 200 g/L to form a fermentation medium, said fermentation medium (i) containing salts suitable for the transforming said conidia into mycelia pellets in a submerged culture, (ii) containing about 3 to about 10 parts per billion Mn⁺² ions and (iii) having a pH value of about 1.5 to about 3.0;

(b) maintaining said fermentation medium at said pH value and at a temperature of about 25°

to about 35°

C., under aerobic conditions for a time period of about 5 to about 6 days to form mycelia pellets in an aqueous product broth;

(c) filtering said product broth to remove said mycelia pellets and form a clear, citric acid-containing aqueous broth;

(d) electrodialyzing said citric-acid-containing aqueous broth to form a citric acid-containing aqueous concentrate; and

(e) decolorizing and ion-exchanging said citric acid-containing aqueous concentrate to remove color and inorganic ions and form an aqueous citric acid solution in which citric acid constitutes at least 98 percent of the organic acids present.

6. The process according to claim 5 including the further step of concentrating said aqueous citric acid solution to form an aqueous solution containing about 40 to about 80 weight percent citric acid.

7. The process according to claim 6 including the further step of recovering the citric acid as crystals.

8. The process according to claim 5 including the further step of adjusting the pH value of said citric acid-containing aqueous broth of step (d) with an alkali metal hydroxide to form an aqueous solution of a monovalent alkali metal citrate salt.

9. The process according to claim 8 including the further step of concentrating the aqueous alkali metal monovalent citrate salt solution to form an aqueous solution containing said alkali metal citrate at a concentration of about 40 to about 80 weight percent as citric acid.

10. The process according to claim 9 including the further step of recovering said alkali metal monovalent citrate salt as crystals.

11. The process according to claim 5 wherein citric acid present in said aqueous citric acid solution constitutes at least 99 percent of the organic acids present.