DE1266265B - Process for the production of glutamic acid from cell-free gas solutions - Google Patents

Description

FEDERAL REPUBLIC OF GERMANY

GERMAN

PATENT OFFICE

EDITORIAL

Int. CL:

German class:

Number:
File number:
Registration date:
Display day:

C12d

C 07 c

6b -16/02

12 q-6/01

1,266,265
A 32926 IV a / 6 b
September 25, 1959
April 18, 1968

The invention relates to a method for obtaining glutamic acid from cell-free fermentation solutions.

It is already known that the cell material made from glutamic acid containing fermentation liquids before the glutamic acid crystallizes out at pH 3.0 up to 3.5 to be separated.

It is also known to contain glutamic acid from glutamic acid and pyrrolydonecarboxylic acid To obtain molasses stillage by converting the pyrrolydonecarboxylic acid in glutamic acid, hydrolyzed with hydrochloric acid, the humic substances formed and after neutralization removed colloidal components and then the glutamic acid crystallized at pH 3.0 to 3.5 and filtered off.

Finally, it is also known that glutamine is already at pH 6.5 and a temperature of 100.degree can be converted into glutamic acid in 2 hours.

So one already has the separation of glutamic acid from fermentation liquids containing glutamic acid the cells removed.

However, it was found that the remaining carbohydrates normally contained in the fermentation liquid counteract crystallization and crystal growth. Namely, they are formed, provoked due to the remaining carbohydrates, small glutamic acid crystals of inferior crystal properties, so that the separation of the crystals becomes difficult on a technical scale. If not switched off of the remaining carbohydrates are crystals of such small needle, spindle or thin Board forms with a diameter smaller than 10 μ or with amorphous deposits educated.

If in addition to the known separation of the microorganism cells now also the remaining carbohydrates are switched off during the crystallization of the glutamic acid, the crystallization succeeds in improved degree and in good yield.

Based on the prior art, the production of glutamic acid from glutamic acid containing cell-free fermentation solutions by acidification to a pH of 3.0 to 3.5 is the one according to the invention Process characterized in that one

Process for obtaining glutamic acid
from cell-free fermentation solutions

Applicant:

Ajinomoto Co., Inc., Tokyo

Representative:

Dr. O. Faust, patent attorney,

3400 Göttingen, Am Goldgraben 26

Named as inventor:

Shinichi Motozaki,

Mei Ohno, Tokyo;

Kotaro Fujiwara, Kamakura-shi (Japan)

Claimed priority:
Japan March 18, 1959

to acidify the fermentation solution a part of the from a previous batch after separation of the pre-existing glutamic acid obtained concentrated and hydrolyzed in a manner known per se, Mother liquor freed from humic substances is used.

Since this mother liquor now has no carbohydrates, but a certain amount of pyrrolydonecarboxylic acid, Containing glutamine and soluble protein formed glutamic acid, the ratio becomes Shifted from glutamic acid to carbohydrate in favor of glutamic acid, causing crystallization the glutamic acid "is improved from the cell-free fermentation solution.

The following table gives an overview of the crystallization of glutamic acid at different Glutamic acid to carbohydrate ratios.

Ratio of glucose to glutamic acid
15: 100 25: 100 I 35: 100 45: 100

60: 100

Crystal growth rate

Ratio of the precipitated amount of crystals to the adhering mother liquor

90

28

65
35

50
48

20th

55

809 539/352

The invention is illustrated by means of the examples.

example 1

To 100 parts of glutamic acid fermentation solution with a content of 5% glutamic acid (4% as glutamic acid or their salts and 1% as pyrrolydonecarboxylic acid, glutamine, soluble protein or the like), 4% cell mass and 1.6% residual carbohydrates were added to 4 parts of diatomaceous earth and the Cells filtered off. The filtrate was gradually replaced by 15 parts of that from a previous batch Separation of the pre-existing glutamic acid obtained, concentrated and known per se Wise hydrolyzed mother liquor freed from humic substances was added, the latter 3.8 parts Contained glutamic acid and 3 parts hydrochloric acid. The pH was adjusted to 3.0. After 2 days Still at room temperature was filtered. 4.3 parts of well crystallized glutamic acid resulted. The degree of purity was 97%, calculated on dry crystals.

The filtrate, the mother liquor, was concentrated to 18 parts and 6.2 parts of concentrated hydrochloric acid added. It was heated to 110 ° C. for 3 hours and the humic substance formed was filtered off.

Most of the mother liquor filtrate was added to the fermentation solution filtrate prior to crystallization and the remaining part is neutralized and subjected to crystallization.

The total yield after such a circulation step rose to 96%, calculated on the total, Glutamic acid contained in the fermentation solution, including that which was originally present, Substances that can be converted into glutamic acid, such as pyrrolydonecarboxylic acid, glutamine and soluble protein. Of the The degree of purity of the crystals was extremely good.

Example 2

To 100 parts of glutamic acid fermentation solution with a content of 5% glutamic acid, 5% cell substance and 1% remaining sugar was added to 5 parts of humic substance in the wet state, which after the Acid treatment described below is separated from mother liquor from a previous batch and the cell mass was then filtered off. The filtrate was gradually 5 parts of concentrated obtained from a previous batch after separation of the pre-existing glutamic acid and mother liquor hydrolyzed in a manner known per se and freed from humic substances added, the latter containing 1 part glutamic acid and 1.3 parts hydrochloric acid. The pH was on 3.0 set. After standing for 2 days at room temperature, it was filtered. The yield was found 4.2 parts of glutamic acid with improved crystal property. The degree of purity was 97%, calculated on dry crystals.

The filtrate, ie the mother liquor, was concentrated to 12 parts and 4 parts of concentrated hydrochloric acid were added. It was heated to HO ⁰ C for 3 hours

ίο heated and the thus formed 5 parts of wet humic substance filtered off.

Part of the mother liquor filtrate was again used for acidification, as described above, and the remaining part neutralized and subjected to crystallization.

The total yield after this circulation procedure rose to 96%, calculated on the total content of glutamic acid in the fermentation solution, including the substances which were present in the form of pyrrolydonecarboxylic acid, glutamine and soluble protein and which can be converted into glutamic acid. The degree of purity of the crystals was just as good as in Example 1.
If an appropriate part of a concentrated mother liquor obtained from a previous batch after separation of the pre-existing glutamic acid and hydrolyzed in a manner known per se, freed from humic substances, is poured into the cell-free fermentation solution before crystallization, the ratio of the remaining amount of carbohydrates to the glutamic acid is thus increased half to a third of the original ratio in the fermentation solution is reduced and the crystallization of glutamic acid is improved.

Claims (1)

Claim: Process for the production of glutamic acid from cell-free fermentation solutions by acidification a pH of 3.0 to 3.5, characterized in that the acidification of the Fermentation solution a part of the from a previous batch after separation of the pre-existing Glutamic acid obtained concentrated and hydrolyzed in a manner known per se, of Mother liquor freed from humic substances is used. Considered publications: U.S. Patent No. 2,749,279; Kretzschmar, "Yeast and Alcohol", 1955, p. 520; H. Rauen, “Biochem. Paperback, 1956, p. 186. 809 P39 / 352 4.68 © Bundesdruckerei Berlin