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1
Introduction
Citric acid is produced by the fungi Aspergillus niger in an
aerob fermenter. For the product recovery of citric acid the
fermentation medium has to be taken out of the reactor. In
the continuous process it would not be economical and
ecological to discharge the fermentation broth after
product recovery took place. Therefore a recirculation of
the fermentation broth is recommended. For this purpose
a four stage process was created. Part 1 of the article
dealt with the fermentation stage of the process especially the continuous fermentation. This part deals with
the product recovery and the recirculation of the fermentation broth.
2
Extraction stage
The citric acid which is produced by the fungi Aspergillus
niger in the fermentation stage is soluted in the fermenReceived: 4 February 1997
S. Wieczorek, H. Brauer
Technische Universitat Berlin, Institut fur Verfahrenstechnik,
Strae des 17. Juni 136, D-10623 Berlin, Germany
Correspondence to: H. Brauer
2.1
Extractant
Tertiary amines are very efcient binders for organic acids. They form an amine-acid complex with the organic
acid. For the experiments tri-dodecylamine was choosen as
a tertiary amine. To improve the solubility of this amineacid complex in the extractant octanol as a polar component was added to the extractant. Low viscosity and low
density promote phase separation. Therefore cerosin was
given to the extractant. Experiments were carried out in
the spray column to nd out the best combination of the
three components for the extraction of citric acid from the
fermentation broth. For the study an articial fermentation broth with the following composition was used: citric
acid 40 kg/m3, fructose 40 kg/m3, glucose 40 kg/m3 and
KH2PO4 0.3 kg/m3. The results can be seen in Fig. 2. The
distribution coefcient is given for different compositions
of the extractant. The curves have basically the same
shape. The distribution coefcient increases with increasing amount of octanol because the amine-acid complex
has to be soluted in the extractant. If the percentage of
octanol gets higher than 35% the distribution coefcient
decreases. This is a result of the smaller percentage of
cerosin as dilutent in the extractant. The curve given for an
extractant with 40% tri-dodecylamine shows the smallest
values for the distribution coefcient because of the
smallest amount of cerosin in the extractant. The highest
distribution coefcient is obtained for the extractant with
30% of tri-dodecylamin. For the following experiments a
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composition of 35% octanol, 35% cerosin and 30% tridodecylamine was choosen.
2.2
Treatment of the recycled fermentation broth
The extractant has a low solubility in water and therefore
parts of it are transferred into the fermentation reactor
after the extraction process. To examine the inuence of
each component of the extractant on citric acid production
experiments in shaken asks were carried out. The resulting two phase system was mixed with a magnetic
stirrer to reach the equilibrium state and only the aqueous
phase was given to the shaken asks. The fermentations in
the shaken asks were started with an inoculum of Aspergillus niger. To see the inuence of the components on
citric acid production a standard fermentation without any
extractant components prepared. In Fig. 3 one can see the
citric acid concentration in the different asks as a function of fermentation time. The highest citric acid concentration of 22 kg/m3 was reached by the standard
3
Reextraction stage
In the reextraction stage the citric acid is removed from
the extractant and the extractant is regenerated. The
loaded extractant is mixed with an aqueous solution of trisodiumcitrat. One or two sodium ions leave the tri-sodiumcitrat to displace the amine in the amine-acid complex.
The two phase system consists of the unloaded extractant
and a mixture of mono- and di-sodiumcitrat. They are
separated in a settler. The aqueous phase is mixed with
soda lye to form tri-sodiumcitrat. A part of it is used for
the reextraction and the other part is converted into
crystallin citric acid in the product stage. In the reextraction stage the citric acid concentration in the extractant
could be reduced from 34.5 kg/m3 to 0.6 kg/m3. To be
recycled into the extraction stage the extractant needs
further cleaning. The regeneration is done by mixing the
extractant with an aqueous solution of strong soda lye.
Then the two phases are separated in a settler and the
aqueous phase is discharged as waste. For an economic
process it is of importance that the extractant can be used
a lot of times without loosing its ability to extract citric
Conclusion
It could be shown that a continuous fermentation with
4
recirculation of the fermentation broth after product reContinuous fermentation with recirculation
The details of a continuous fermentation have been dis- covery was run for 55 days with very good results. The
cussed in part one of the article. To see the inuence of the extraction stage causes the problem that parts of the exrecirculation of the fermentation broth the fermentation tractant dissolve in the aqueous phase. The necessary
cleaning of the recirculated fermentation broth was
has to run for a long time. This can be achieved by the
fermentation process with dilution of the biosuspension achieved with activated carbon. A regeneration of the extractant could be done for more than 30 times.
which has been explained in part one. The dilution is
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achieved by replacing 16 dm of the 20 dm biosuspension
in the reactor with fermentation medium. The fermenta- References
tion time from one exchange to the other is called period 1. Daniel, S.; Brauer, H.: Bioverfahrenstechnische Untersuchung der
of production. In Fig. 5 the curve of the citric acid conabsatzweisen und kontinuierlichen Produktion von Zitronensaure
centration for a fermentation with four periods of proim Hubstrahlbioreaktor; VDI-Forschungsheft; VDI-Verlag, Dusseldorf 1994
duction can be seen. For comparison the result of a
batchwise fermentation is indicated as well. The continu- 2. Greger, W.; Grueger, A.: Biotechnologie-Lehrbuch der ange-
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