Bioseparation Citric Acid

8/11/2019 Bioseparation Citric Acid

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BKB4493 BIOSEPARATIONENGINEERING

2013/14-IICASE STUDY

PROCESS OF PRODUCING THE

BIO-PRODUCTS:CITRIC ACID


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GROUP MEMBERS

O RAFIDAH BT MOHAMED ALI

HANAPIAH KE11019O AHMAD IZZAT BIN ZULKEFLK

KE11036

O OOI CHEE BENG KE11047

O CHONG SOO LING KE11060

O NURUL AIN BINTI IBRAHIM KE12004


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IntroductionO one of weak organic acids (a

tricarboxylic acid) widely used as

preservative and conservative in

food.

O

additional flavor to increase sourtaste to foods and drinks. Other

uses are for cleaning and chelating

agent, for cosmetics and

pharmaceuticals, as well as

industrial and construction.O universal intermediate product of

metabolism and its traces are

found in virtually all plants and

animals.


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Figure 1.1 shows 3D structure of citric acid. (www.myorganicchemistry.wikispaces.com)


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Citric acid can be produced byfermentation process by

Aspergillus niger, a commonmicroorganism that is efficient toproduce this acid.

Prior to fermentation process,citric acid was isolated fromcitrus fruits such as ORANGEand LEMONSwhere the juiceswere treated with calcium

hydroxide to precipitate calciumcitrate, which was isolated andconverted back to the acid usingsulfuric acid (Verhoff, 2005)


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Chemical propertiesAlso known as: Citro, citrate, 77-92-9, Aciletten, Citretten, Anhydrous

citric acid, Chemfill, Hydrocerol A (www.chemicalbook.com)

Molecular formula C6H8O7

Molecular weight

192.12352

Melting point

307.4 F

Specific Gravity/Density:

1.665 g/cm3

pH

1.7 (10% soln)Density

1.542

Refractive index

1.493~1.509

Storage temp. Store at room temperature

Solubility

H2O: 1 M at 20 C, clear, colorless

Form

gritWater Solubility

750 g/L (20 C)

Sensitivity

Hygroscopic

Stability

Stable. Incompatible with bases, strong

oxidizing agents, reducing agents, metal

nitrate


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Physical properties usually can be found in white crystalline powder

and is described as colorless, odorlesscrystals withan acid taste.

denser than water and water soluble.

The pure material is moisture sensitive as it will

undergoes slow hydrolysis.

reacts with oxidizing agents, bases, reducingagents and metal nitrates. Reactions with metal

nitrates are potentially explosive. Heating to the

point of decomposition causes emission of acrid

smoke and fumes.

Certain measures must be implemented while

handling citric acid in laboratory. Inhalation of dustirritates nose and throat and contact with eyes

causes irritation. Whilst exposed with fire it will

melts and decomposes. Although, the reaction is

not hazardous


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Applications in industry Citric acid can be found abundantly and its uses are dominantly

in food manufacturing

The largest industrial application of citric acid is for making

detergents.

In liquid detergents, sodium citrate (salts from citric acid) is usedas a builder,to increase the effectiveness of the surfactants, due

to its high solubility and bio-degradability.

While in the form of powdered detergents, sodium citrate is used

as a co-builder and processing aid. Sodium citrate also

contributes alkalinity to enhance surfactant performance. The

environmentally friendly nature of sodium citrate is a majorfactor in the use of citrates in the detergent industry.


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Applications in industry

Used in plating operations, where it is used as a

chelating agent to control the deposition rate of

metals in both electroplating and electrolysis

plating.

The pharmaceutical industry - as a flavoringand

stabilizing agent in multiple pharmaceutical

preparations. The largest use of citric acid in the

pharmaceutical industry though is for the

effervescent effect it produces when combined

with bicarbonates or carbonates in antacids anddentifrices


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10 m3 of

water per

tonne of

acid

milk of lime containingcalcium oxide (180

250 kg/m3)

120150 minutes.

For 15 minutes


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If crystallization is performed at

temperatures below 36.5C, the

citric acid mono-hydrate isformed and above this transition

temperature citric acid anhydrate

may be obtained.

temperaturebelow 40C (to

avoid

caramelization),

concentrated

sulphuric

acid (60

70 percent)


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MICROORGANISM

Aspergillus Niger (A. niger) is the microorganism of choicefor citric acid production.

Advantages compared to other microorganism of bacteria,

yeast and fungi:

ease of handling

ability to ferment a variety of cheap raw materials

high yields

(Schuster et al., 2002; Grewal et al., 1995)


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NUTRIENT MEDIA

O Carbon source: sweet potato starch hydrolyzate (SPSH) - 153.77

g/L

O Diammonium hydrogen phosphate [(NH4)2HPO4, DAHP] -

3.55 g/L

O Potassium dihydrogen phosphate [KH2PO4, PDHP] - 2.58

g/L

O MgSO4.7H2O (0.10 g/L)

(Sankpal et al., 2000)


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FERMENTATION PROCEDURE

1. 50 mL of SPSH was measured into 250 mL Duran flasks.

2. Nutrients were added appropriately.

3. The pH of the medium was adjusted using 36.5 g/L HCl and 80 g/LNaOH buffer solutions.

4. 5% volume fraction of inoculum size was added aseptically to the

flask, which was placed on a clean table for surface fermentation.

5. Fermentation duration and condition - 8 days and pH of 6.


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FILTRATIONO Recovery of citric acid from the surface

process starts with filtration to separate

the mycelium from the culture liquid and

washing of mycelial cake, which may still

contain a significant fraction of the citricacid produced.

O Filtration of the mycelium from the

submerged process may require the use

of filter aids due to formation of slimy

polysaccharides as by-products


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PRECIPITATION

CaOH is

added.

Vacuum

filtration

Dissolve withdilute H2SO4.

Filtration

(Pazouki and Panda, 1998)

Objective: To purify the citric acid.Inlet: Citric Acid and Lime (CaOH)

Outlet: Citric Acid


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SOLVENT EXTRACTIONO Amine extraction =method of separation of

carboxylic or hydroxy carboxylic acid fromaqueous solution.

O CA is readily extracted into a number of

organic solvents, such as high-molecular-weight aliphatic amines (Pazouki andPanda 1998).

O Wenneresten (1980, 1983) found thattertiary amines were effective extractantsfor CA.


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O ADVANTAGE= consuming negligible

amounts of mineral acids and bases andproduction of salt by-products.

O Solvent extraction method with tertiary

amines can be further refined for the

technically feasible extraction of CA at pilotscale


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CRYSTALLIZATION

Figure : A forced circulating crystallizer . ( Dyke, 2004)

Objective: To remove the impurities (salt) and ease of storage

Inlet = Citric Acid

Outlet= Citric Acid


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EQUIPMENTS HOLLOW FIBER TUBULAR

MEMBRANE

SPIRAL WOUND MEMBRANE FILTER


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O When your ultrafiltrationinvolve suspended solids,

bacteria, or highconcentrations ofmacromolecules, hollow fibermembranes is used to clarify,concentrate, and purify

process streams.O These high-tech membranes

are widely used in submergedmembrane bioreactor

systems, industrial andmunicipal water treatment,and a variety of industrialapplications.

HOLLOW

FIBERTUBULAR

MEMBRANE


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O This design is with a shell and tubearrangement with polymeric

membranes cast on the inside ofplastic or porous paper componentswith lengths from 0.6 - 6.4 m(Tamime, 2013).

O The feed of the module is passedthrough the tubes, accommodatingradial transfer of permeate to theshell side.

O A single module can consist of 50 tothousands of hollow fibres. Thediameter of each fibre ranges from0.6 3 mm with the feed flowing inthe tube and the product permeatecollected radially on the outside(Munir, 1998).


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Hollow Fiber Tubular Membranes

Source : http://www.kochmembrane.com/Learning-Center/Configurations/What-are-Hollow-Fiber-Membranes.aspx


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O The advantage of having self-supporting

membranes is easier to clean to its ability

to be back-flushed.

O The disadvantage - Replacement costs

however are high, as one faulty fibre will

require the whole bundle to be replaced.

O Considering the tubes are of small diameter,

using this design also makes the system

prone to blockage.


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SPIRAL WOUND MODULE

O The designs of a spiral wound membraneconsist of membrane envelopes (leaves) andfeed spacers which wound around a perforatedcentral collection tube.

O Feed solution passes axially down the moduleacross the membrane envelope.

O A portion of the feed solution permeates into themembrane envelope, where it spirals toward the

center and exits through the collection tube

(Scott et al., 1996).


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O - These modules were designed in an effort to pack as

much membrane surface as possible into a given

volume (Senthilmurugan et al., 2005).

O Small scale spiral wound modules consist of a single

membrane leaf wrapped around the collection tube.

O In the large membrane area module, using single

membrane leaf might generate large pressure drop due

to the longer path taken by the permeate to reach the

central collection tube.

O Multiple short leaves have been utilized to keep the

pressure in the module in a manageable level (Van der

Meer and van Dijk, 1997).


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Spiral Wound Membrane Module (Scott et al., 1996)


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REFERENCES

1. Cheryan, Munir (1998). Ultrafiltration and Microfiltration Handbook. CRC Press.

2. Dyke, S. (2004). Enhanced Forced Circulation: The Continued Solution to High Solids Black LiquorCrystallization. Il USA: HPD, Plainfield.

3. E. Betiku, O. A. Adesina. (2013). Statistical approach to the optimization of citric acid production usingfilamentous fungus Aspergillus niger grown on sweet potato starch hydrolyzate.Biomass and Bioenergy,55, 350-354.

4. E. Schuster, N. Dunn-Coleman, J. C. Frisvad, P. W. V. Dijck. (2002). On the safety of Aspergillus niger - areview.Appl. Microbiol. Biotechnol., 59(4-5), 426-435.

5. Frank H. Verhoff (2005), "Citric Acid", Ullmann's Encyclopedia of Industrial Chemistry, Weinheim: Wiley-VCH

6. H. S. Grewal, K. L. Kalra. (1995). Fungal production of citric acid.Biotechnol. Adv., 13(2), 209-234.

7. Membrane Processing: Dairy and Beverage Applications [Hardcover] by A. Y. Tamime (2013)

8. N. V. Sankpal, A. P. Joshi, B. D. Kulkarni. (2000). Nitrogen-dependent regulation of gluconic and/or citricacid production by Aspergillus niger.J. Microbiol. Biotechnol., 10(1), 51-55.

9. Pazouki, M., & Panda, T. (1998). Recovery of citric acid - a review.Bioprocess Engineeing 19, 435-439.

O


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Bioseparation Citric Acid