icetcs-cug-578-page-proceedings-ksew

can be described as one in which the cooperative micelle formation process of the surfactant
is facilitated by the polymer-micelle association [39, 40]. The presence of the polymer in
solution results in a reduction of the surfactant chemical potential giving rise to surfactant
self-assembly along the polymer chain. Free micelle formation begins when the chemical
potential of the surfactant becomes equal to that for the case of micelles formation in aqueous
solution, i.e., C2 which will be dependent upon polymer concentration.
In addition to forming micelles, the surfactant can isolate its hydrophobic groups from the aqueous
phase by associating them with the hydrophobic moieties on a polymer. In particular, hydrophobic
polymers can interact strongly with nonionic surfactants. In general, anionic surfactants demonstrate a
stronger interaction with nonionic polymers than do nonionic or cationic surfactants. The reason for a
difference in cationic vs. anionic behavior may be due to the different
hydrationhydrationcharacteristics of the cationic and anionic headgroups. Anionic surfactants have
been shown to interact strongly with neutral synthetic polymers PVA (polyvinyl alcoholpolyvinyl
alcohol,), PEO (polyethylene oxide), and PVP (polyvinylpolyvinyl pyrrolidone), HPMC and PEG;
hydrophobic attraction is expected to be the primary mode of interaction since no conspicuous
electrostatic forces operate between them. However, cationic surfactants do not show the same
affinity for these polymers (nor do nonionics). They interact more strongly with more hydrophobic
polymers such as PPO (polypropylene oxide) or PVA-Ac (polyvinyl acetate). However, gemini
surfactant even cationic shows interaction with these neutral synthetic polymers as HPMC and PVP
as described in case studies.

Polymers are added to surfactants to:
1. Control the phase behavior (e.g., to solubilize water insoluble polymers).
2. Control the interfacial properties (e.g., to stabilize suspensions which depends on a
complex interplay between different pair interactions. Addition of a polymer can either
remove a surfactant from a surface or enhance its adsorption to a surface).
3. To achieve a suitable rheology (thickening and gelation effect).
4. The polymer induced micellization lead to a lower surfactant free molecules concentration and
activity (e.g., in skin formulations, free surfactant molecules cause skin irritation).

Methods to study polymer surfactant interactions

There are several techniques to study polymer-surfactant interactions such as:

1. Calorimetric Measurements

2. Nuclear Magnetic Resonance (NMR)

3. Flourescence

4. Conductivity

5. Gel Permeation Chromatography (GPC)

6. Viscosity Measurements

7. FT Infrared Spectroscopy (FTIR)

8. Surface Tension Measurements

9. Light Scattering Techniques

10. Electromotive Force (emf)

Case Studies

Case Study 1

The interactions of two gemini surfactants (16-s-16, s = 5, 6) and their conventional counterpart
cetyltrimethylammonium bromide (CTAB) with polyvinylpyrrolidones (PVP K15 and PVP K90)
have been investigated using conductivity, steady state fluorescence and viscosity techniques [41].
The results indicate that there is no PVP/CTAB complex formation if molecular weight of PVP <
15,000. Both PVP K15 and PVP K90 interact with gemini surfactants as shown in Figure-7.
Fluorescence study shows that the addition of PVP results in a decrease of the aggregation number in
all the systems investigated due to the adsorption of the PVP chain in the micelle palisade layer and
the ensuing increase of micelle ionization. The viscosity results suggest that the interactions between
the surfactants and the polymer affect both inter polymer-polymer association as well as chain
expansion [41].

Figure-7 here

Case Study 2

The interaction between a nonionic polymer, hydroxypropyl methyl cellulose (HPMC), and cationic
gemini surfactants, bis(hexadecyldimethylammonium)hexane dibromide (16-6-16),
bis(hexadecyldimethylammonium)pentane dibromide (16-5-16) and their corresponding monomeric
counterpart cetyltrimethylammonium bromide (CTAB) by using electrical conductometry,
fluorescence and viscometry methods [42]. It was found that the gemini surfactants interact strongly
with HPMC as compared to conventional surfactant CTAB. The aggregation number (Nagg) obtained
from steady state fluorescence measurement with CTAB was found to be more than with the geminis.
A significant viscosity increment was observed in case of geminis surfactant as compared to CTAB.
The rapid increase of the viscosity with surfactant concentration was, therefore, attributed to the
considerable cross links among micelles and polymers (transient network) as depicted in figure-8.

Figure-8 here

Conclusions

As a general trend, the presence of neutral polymers increases the CMC concentration for the
surfactant. The combination of surfactant and polymers improve the desired properties of the product
(surfactants are usually added to control the dispersions, flocculation and wetting properties of
suspensions while polymers are mainly added to meet rheological requirements). The surfactant-
polymer interaction can range from very strong interaction to no interaction at all. Interactions
between the surfactant and the polymer affect both inter polymer-polymer association as well as chain
expansion.

References

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Marcel Dekker Inc., New York.
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aqueous solution. Part I.—Measurement of transport numbers of cetylpyridinium and
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with some data also for cetane sulphonic acid, Trans. Faraday Soc., 32: 795-815.
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molecules. J. Am. Chem. Soc., 115: 10083.

13. Rosen MJ (1993) Selection of surfactant pairs for optimization of interfacial
properties. CHEMTECH, 23:30.

14. Menger F, Littau CA (1991) Gemini-surfactants: synthesis and properties. J. Am. Chem.
Soc., 113:1451.

15. Davis DG, Bury CR (1998) A quantitative kinetic theory of emulsion type, I.
Physical Chemistry of the Emulsifying Agent, Gas/Liquid and Liquid/Liquid
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16. Rosen MJ (2004) Surfactants and Interfacial Phenomena. 3rd edn. John Wiley, New York.
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18. Saito S (1987) Nonionic Surfactants: Physical Chemistry. Marcel Dekker, New York.
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20. Moroi Y (1992) Micelles: Theoretical and Applied Aspects. Plenum Press, New York.
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22. Evans DF, Wennerstom H (1994) The Colloidal Domain: Where Physics, Chemistry,

Biology, and Technology Meet. 1st edn, VCH Publishers, Inc.
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fjord vs. reef models. J. Am. Chem. Soc., 100: 4676.
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9: 153.
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26. Corkill JM, Goodman JF, Walker T (1967) Partial molar volumes of surface-active agents

in aqueous solution. Trans. Faraday Soc., 63: 768.
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Dodecyltrimethylammonium bromide in Water-Amino acid Systems. Indian J. Chem., 36A:
1075.
28. Luisi PL, Magid LJ (1986) Solubilization of Enzymes and Nucleic Acids in Hydrocarbon
Micellar Solution. CRC Crit. Rev. Biochem., 20: 409.
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sulphate micelles. J. Chem. Soc., Farasday Trans 1. 83: 591.
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Colloid Interface Sci., 41: 149.
31. Brackman JC, Engberts JBFN (1993) polymer-micelle interactions: Physical organic
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34. Mukerjee P (1967) The nature of the association equilibria and hydrophobic bonding in
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35. C. Gamboa C, Sepulveda L (1986) High viscosities of cationic and anionic micellar
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36. Imam T, Abe , Ikeda S (1988) Viscosity behavior of semiflexible rodlike micelles of
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40. Jonsson B, Lindma, B, Holmberg K, Kronberg B (1998) Surfactants and Polymers in
Aqueous Solutions. John Wiley & Sons, Chichester.

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and cationic gemini /conventional surfactants, Chemical Engineering Communications,
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(Hydroxypropyl) methyl Cellulose and Cationic Gemini/Conventional Surfactants Ind.
Eng.Chem. Res 51: 1227−1235.

Hydrophilic Hydrophobic
(Head Group) (Tail)

Fig.-1: Schematic representation of a surfactant monomer.

Tail Head Spacer Head Tail

Fig.-2: Schematic representation of a gemini surfactant.

Fig.-3: Schematic representation of a spherical surfactant micelle.

(A) (B) (C)

Fig.-4: Schematic presentation of normal (A), reverse (B) and mixed micelles (C). In (C),
and indicate different surfactant monomers.

Fig. -5: Schematic representation of the regions of spherical micelle.

Fig.-6: A schematic plot of the concentration dependence of the surface tension for polymer–
surfactant solutions. T1 is the critical aggregation concentration, T2' – polymer saturation with

micelles and T2 – surfactant free micelle formation.

0.06

0.5

0.05

0.4

κ (mS.cm-1) 0.04 cmc
κ (mS.cm-1)
0.3 0.03

cac

0.2 0.02 0.05 wt % PVP K 15
0.10 wt % PVP K 15
CTAB in Water 0.01 0.20 wt % PVP K 15
0.50 wt % PVP K 15
0.05 wt % PVP K 15 0.00 1.00 wt % PVP K 15
0.0
0.1 0.10 wt % PVP K 15
0.20 wt % PVP K 15
cmc 0.50 wt % PVP K 15

1.00 wt % PVP K 15 0.1 0.2 0.3

0.0 [16-6-16] (mmol.dm-3)

01234567

[CTAB] (mmol.dm-3)

rη 0.1 wt % PVP K90 + CTAB
0.5 wt % PVP K90 + CTAB
1.0 wt % PVP K90 + CTAB Fig.
0.1 wt % PVP K90 + 16-6-16
0.5 wt % PVP K90 + 16-6-16 -8
11 1.0 wt % PVP K90 + 16-6-16 Inte
10 0.1 wt % PVP K90 + 16-5-16 ract
0.5 wt % PVP K90 + 16-5-16 ion
9 1.0 wt % PVP K90 + 16-5-16 of
Water + CTAB HP
MC
8 wit

Water + 16-6-16 h
7 Water + 16-5-16 surf

6
5
4
3
2
1
0

0 50 100 150 200 250 300

[surfactant] (mmol.dm-3)

Fig. -7: Interaction of PVP with CTAB and Gemini surfactant

actant

5.SYNTHESIS AND ANTIMICROBIAL ACTIVITY OF 6-METHOXY
DERIVITIVES OF SCHIFF’S BASES

M.V.KULKARNI, N.R.LAKARE,G.K.KAKADE
Sanjivani Rural Education Society’s, Sanjivani Arts, Commerce and Science College,

Kopargaon-423601, Dist-Ahmednagar, Maharashtra, INDIA
Email: [email protected]

ABSTRACT
Four Derivatives of 6-Methoxy Schiff’s bases are synthesized. All Derivatives are
characterized by modern methods such as elemental analysis, IR spectra. All Derivatives are
found to be crystalline and coloured. From that two derivatives of Schiff’s Bases are screen
for antibacterial activity against Bacillus cereus, Escherichia coli and Staphylococcus aureus
and antifungal activity against Aspergillus Niger, Aspergillus flavus, Fusarium
oxysporum.The synthesized Schiff’s bases are found to be vast Applications in Agriculture
Field. These Schiff’s Bases are Degradable in nature.
Key Words: 6-methoxy derivatives of Aldehyde , Derivatives of Amines, IR , Antimicrobial
activity.

INTRODUCTION

Schiff bases are the compounds containing azomethine group (-HC=N-).They are
Condensation products of ketones or aldehydes with primary amines and were first
reportedBy Hugo Schiff in 1864. Schiff bases derived from aromatic amines and aromatic
aldehydes have a wide variety of applications in many fields, for example, biological,
inorganic, and analytical chemistry [1–4]. In addition, Schiff bases and heterocyclic ring are
important class of compounds in medicinal and pharmaceutical field [5–8]. Recently, in our
previous work, Schiff bases show biological properties including antibacterial, antifungal
antitumor, analgesic, and anti-inflammatory activities [9–18]. In view of these observations
and in continuation of previous work in Schiff’s base chemistry, we synthesized some new
imide and Schiff’s base derivatives containing rings for the evaluation of antimicrobial
activity.
Schiff bases having oxime derivatives have been reported to possess anti-inflammatory
activity. It has been suggested that azomethine linkage might be responsible for the biological
activities of Schiff’s bases. Schiff bases have appeared to be an important intermediate in a
number of enzymatic reactions involving interaction of enzyme with amino or carbonyl group
of the substrate. In the lysine class, represented by fructose diphosphate aldolase, an

intermediate Schiff base is formed between α-amino group of lysine of enzyme and a
carbonyl group of substrate. Another important role of Schiff base structure is a
transamination. Transaminases are found in mitochondria and cytosine of eukaryotic cells.

REVIEW OF LITERATURE

Schiff bases have significant importance in chemistry; especially in the developmentof
Schiff base complexes, because Schiff base ligands are potentially capable of forming
stable complexes with metal ions. Many Schiff base complexes show excellent catalytic
activity in various reactions at high temperature (>100 °C) and in the presence of moisture.
Over the past few years, there have been many reports on their applications in homogeneous
and heterogeneous catalysis, hence the need for a review article highlighting the catalytic
activity of Schiff base complexes realized.
Schiff bases have been used extensively as ligands in the field of coordination chemistry,
some of the reasons are that the intramolecular hydrogen bonds between the (O) and the (N)
atoms which play an important role in the formation of metal complexes and that Schiff base
compounds show photochromism and thermochromism in the solid state by proton transfer
from the hydroxyl (O) to the imine (N) atoms
Schiff bases have appeared to be an important intermediate in a number of enzymatic
reactions involving interaction of enzyme with amino or carbonyl group of the substrate. In
the lysine class, represented by fructose diphosphate aldolase, an intermediate Schiff base is
formed between α-amino group of lysine of enzyme and a carbonyl group of substrate
Another important role of Schiff base structure is a transamination.

EXPERIMENTAL

General
A Schiff base is nitrogen analog of an Aldehyde or Ketone in which the C=O group is replace
by C=N-R group .It is usually formed by the condensation of an aldehyde or ketone with
primary amine according to the following scheme-

Scheme-1here
Schiff’s bases those contain aryl substituent’s substantially more stable and readily
synthesized than alkyl substituent’s which are relatively unstable.
The formation of Schiff’s base from an aldehyde or ketone is a reversible reaction and
generally takes place under acid or base catalyst.

Scheme-2 here
The mechanism of Schiff’s base formation is another variation of the theme of nucleophillic
addition to the carbonyl group. In this case nucleophile is amine.In the first part of the

mechanism,the amine reacts with the aldehyde or ketone to give an unstable addition
compound called Carbinolamine.
Typically the dehydration of the Carbinolamine is the rate determining step of schiff’s base
formation and this is why the reaction is catalysed by mild acid.The schiff’s base formation is
really a sequence of two types of reactions,i.e addition followed by elimination.

Other way to synthesized of Schiff’s base:-

1. By treatment of active hydrogen compounds with nitroso compound.

2. Primary amines add to triple bond to gives enamines which tautomerizes to the more
stable imines.

3. By the addition of ammonia to aldehyde or ketone.

4. Addition of amines to aldehydes or ketones.

Among above methods,Third method is convenient, because,

a) Gives high yield.

b) Products are highly pure.

c) Easy to synthesis.

Brief outline of method

New Schiff bases have been synthesized from the condensation reaction of 6-methoxy-2-
naphthaldehyde and 3-Chloro-benzamine in dry ethanol with 3-4 drop of H2SO4. Mixture is
refluxed for 2 hrs. Then Mixture cooled and poured on ice cold water. The resulting solid was
filtered dried and recrystallized from ethanol.The formation of 6-methoxy 2-naphthalidine
aniline derivatives were confirmed by the
Following tests:-

1. Negative 2, 4-dinitrophenyl hydrazine test.
2. Negative diazotization test.
3. Lassiagnes test for nitrogen is positive.

Scheme-3 here
Table-1 here

ANTIMICROBIAL ACTIVITY

The antimicrobial activities of some synthesized compounds were determined by agar diffusion

method as recommended by Genome Life Sciences, Aurangabad. The compounds were evaluated for

antimicrobial activity. The compound A and B were assayed for antibacterial activity against Bacillus

cereus, Escherichia coli and Staphylococcus aureus and antifungal activity against Aspergillus Niger,

Aspergillus flavus, Fusarium oxysporum by agar well diffusion assaynand fungal broth method assay

respectively.

The zone of inhibition was measured in mm and was compared with standard drug. DMSO was used

as blank and Ampicillin was used as antibacterial standard and Grysofulvin was used as antifungal

standard. Both the compounds were tested at 50 µg/ml and 100 µg/ml concentration.

The antimicrobial screening data revealed that compound A was found to be moderate active against

Bacillus cereus and Staphylococcus aureus at 100 µg concentration, where as compound B was found

to be moderate active at 50 µg and 100 µg concentration.Data is provided in Table-2.

Antifungal activity data revealed that compound A showed reduced growth against Aspergillus Niger,
Aspergillus flavus, Fusarium oxysporum where as compound B was highly active against Aspergillus
Niger. Data is provided in Table-3.

Table-2 here
Table-3 here
Figure-1 here
Figure-2 here
INTERPRETATION OF IR SPECTRA OF THE DERIVED COMPOUND OF
SCHIFF’S BASE

• IR spectra of compounds A, B and C show stretch between 1600-1625 cm-1.
• Which confirms the presence of C=N bond in the above compounds.

Figure-3 here
CONCLUSION

Successfully synthesized New Schiff’s bases and Study their Antimicrobial activity. The synthesized
compounds were tested for their antimicrobial activity against three microorganisms and the minimal
inhibitory concentrations (MICs) of the tested compounds were determined by the dilution method.
The antimicrobial screening showed that these newly synthesized compounds have good antimicrobial
activities than known drug.

REFERENCES

1. P. Singh, R. L. Goel, and B. P. Singh, “8-acetyl-7-hydroxy-4-methyl coumarin as a
gravimetric reagent for Cu2+ and Fe3+,” Journal of the Indian Chemical Society, vol. 52, pp.
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2. B. F. Perry, A. E. Beezer, R. J. Miles, B. W. Smith, J. Miller, and M. G.
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4. M. Rahman, M. A. Mridha, and M. A. Ali, “Transition metal complexes of the
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5. P. Sah, N. Saraswat, and M. Seth, “Synthesis of phthalyl substituted imidazolones
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2011. View at Scopus

6. A. E. Amr, N. M. Sabry, M. M. Abdalla, and B. F. Abdel-Wahab, “Synthesis,
antiarrhythmic and anticoagulant activities of novel thiazolo derivatives from methyl 2-
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7. A. S. Said, A. E. Amr, N. M. Sabry, and M. M. Abdalla, “Analgesic, anticonvulsant
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+R NH2 1 O 2 R
C
R C R NR + H2O

R

R---Alkyl or Aryl group

Scheme-1

1 O 2 OH R N R + H2O
12
+R NH2 R R R
RR
NHR

Scheme-2
H

O R

H3C O + H2N

3-4 drops of H2SO4 Reflux for 2 hrs

N
H

Scheme-3

Table-1 MELTING POINTS AND YIELDS OF 6-METHOXY-2-NAPHTHYLIDINE

ANILINES

S.No. Name of compound Structure M. Yield

P%
0C

A 6-methoxy-2- N
naphthylidine-3-chloro-
benzamine 138 87

O
CH3

B 6-methoxy-2- O Cl
naphthylidine-3-chloro- CH3 N
benzamine
O 98 85
C 6-methoxy-2- CH3
naphthylidine-3-chloro- H3C
benzamine N

149 88

D 6-methoxy-2- O N
naphthylidine-3-chloro- CH3
benzamine 110 90

O CH3

TABLE-2: ANTIBACTERIAL ACTIVITY

Zone of Inhibition(mm)

Bacteria used Positive Negative Negative A B
Bacillus cereus control control control
(DMSO) (Water) 50 100
12 16 µl µl
50 100 09 13
µl µl

00 00 00 00 00 12

Escherichia coli 18 22 00 00 00 00 00 00 00 10

Staphylococcus 16 16 00 00 00 00 00 10 00 00
aureus

TABLE-3: ANTIFUNGAL ACTIVITY OF CHEMICAL COMPOUNDS AGAINST PLANT
PATHOGENIC FUNGI

Sr.No Compounds Aspergillus flavus Aspergillus Niger Fusarium
oxysporum
1A RG RG
-ve RG RG
2B +ve +ve
3 -ve control +ve

4 Grysofulvin +ve
(+ve control)
-ve -ve -ve
Legend: +ve-Growth
-ve- No Growth
RG- Reduced Growth

Compound A

Compound B
Compound C
Fig.-1: Images Showing Antibacterial Activity

Compound-A

Compound-B

Compound-C
Fig.-2: Images Showing Antifungal Activity

Compound A
Compound B

Compound C
Fig.-3: IR Spectra

6. BIOCONVERSION OF GLYCEROL TO 1,3-PROPANEDIOL AND IT’S
APPLICATION

Mandar Karve, Jay J Patel, Nirmal K Patel*
Department of Chemical Sciences, Natubhai V. Patel College of Pure and Applied Sciences,

Vallabh Vidhyanagar, Anand, Gujarat, India

e-mail: [email protected]

ABSTRACT:

Excess waste glycerol obtained from biodiesel production is becomes environmental problem and
economical concern due to its growing surplus. In this present work various
microorganism viz. E-coli (Escherichia coli), Citrobacter, Klebsiella, Lactobacillus, Enterobacter and
Clostridium strain were used to convert waste glycerol in to 1,3-propanediol (1,3-PDO) in aerobic
condition. Where E-coli give the best result among those various microorganisms is used.
1,3-propanediol obtained by bioconversion of waste glycerol using E-coli was used in the production
of saturated as well as unsaturated polyester resin which can be used as moulding as well as in coating
industry. Resulting 1,3-propanediol and polyester resin were characterized by Infrared spectroscopy
and Gas chromatography.

Keywords: Bioconversion, Escherichia Coli, Crude glycerol, 1,3-propanediol.

INTRODUCTION:

Glycerol is polyol compound contain three hydroxyl groups in its structure. It is a colorless
compound which is generally soluble in all alcohols, ethyl acetate and dioxane. It is insoluble in ether,
benzene and chloroform. [1] Glycerol finds applications in the paint, automotive, cosmetic, food,
tobacco, pharmaceutical, pulp, paper, leather and textile industries. [2]

Nowadays glycerol waste is obtained as a by-product during the manufacturing of biodiesel.
[3] Biodiesel is a very important product for now and a future aspect, but the production cost of
biodiesel is very high and disposal of this crude glycerol may add some additional cost. As the
petroleum resources are decreases day by day, the use of biodiesel may helpful not only in protection
of environment but also alternative for petroleum products. [4,5] If the crude glycerol from biodiesel
industry shall be utilized for further application then cost cutting in biodiesel production is possible
which may lead to make use of it as substitute of petrol and diesel. [6,7] Crude glycerol can be use to
obtain various products like carbon dioxide, 1,2-propanediol, 1,3-propanediol, succinic acid, ethanol,
xylitol, propionate, hydrogen. The same can be carried out by chemical as well as biological route. [8]
Higher pressure and temperature is required in chemical synthesis which leads process costly and
difficult to proceed. [9,10] On the other hand, fermentation or microbial conversion of crude glycerol

produces the high value product like 1,2-propanediol, 1,3-propanediol, lactic acid, acetic acid and
dihydroxyacetone. [11] Also, microbial route carried out at or slightly above room temperature and
atmospheric pressure. [12] Microbial conversion of glycerol into 1,3-propanediol can be done using
microorganisms like E. Coli, Bacillus spices, A. Niger, Pseudomonas and yeast in aerobic as well as
anaerobic conditions, toxic by-product will not generate using E-coli and most of that microorganism
need vitamin B12 as a cofactor which increases costs of 1,3-PDO production where E-coli do not need
vitamin B12 which solve problem of high production cost. 1, 3-propanediol can be formulated into
composites, adhesives, laminates, powder coating, UV-cured coatings, mouldings, solvents and as an
anti-freeze agent. [13,14] It can be used in manufacturing of polyester, polyurethane and polyol. Most
importantly the production of 1,3-propanediol is increased because it can be utilized for development
of a biodegradable polymer poly (trimethylene terephthalate), which having unique physiochemical
properties in the fiber industry and other applications in cosmetics, foods, lubricants and medicines.
[15,16]

There so in the present work bioconversion of crude glycerol into 1,3-PDO was carried out
and the resulting 1,3-PDO was utilized for the synthesis of saturated and unsaturated polyester resin.
1,3-PDO was analyzed by gas chromatography (G.C.).

MATERIAL AND METHODS:
Materials

Phthalic anhydride, maleic anhydride, 1,3-PDO, PTSA (para toluene sulfonic acid), propylene
glycol, Potassium hydroxide (KOH) and medium composition were purchased from Sigma Aldrich
while solvents viz. Xylene, ethyl acetate and chloroform were purchased from Merck India Private
Ltd.
Methods
Bioconversion of Crude Glycerol to 1, 3-propanediol

Bioconversion of crude glycerol was carried out using E-coli. The medium consisted of
K2HPO4 - 2.0gm, KH2PO4 - 2.00gm, MgSO4 - 1.0gm, CaCl2 - 0.4gm, FeCl3 - 1.0gm, NH4NO3 -1.0gm,
glycerol - 100ml composition per litre of distilled water. The medium was sterilized in an autoclave
at 150 rpm for 30 minutes. E-coli was added in 250 ml flasks containing 150 ml medium. The flask
was incubated at 250C for 6 days.
Separation

In the first step, separation of biomass from aqueous solution and 1,3-PDO by filtration is
carried out. This 1,3-PDO is isolated by distillation and solvent extraction process. In extraction
process 1, 3-propanediol can be isolated from glycerol-water mixture using ethyl acetate or
chloroform as solvents because 1, 3-propanediol is miscible with it, so 1,3-PDO was extracted in a
solvent which was further evaporated to separating out 1, 3-propanediol.

Gas Chromatography

The resulting 1,3-PDO was characterized by Gas chromatograph (GC) using Perkin Elmer
auto system XL instrument using capillary column.

Synthesis of Polyester Resin

Different polyester can be synthesized by esterification of 1,3-propanediol with various
dicarboxylic acids in the presence of a catalyst. In our present work, we used phthalic anhydride,
1,3-PDO and PTSA as catalyst for saturated polyester resin and for unsaturated polyester resin maleic
anhydride was used with the same materials which were used for saturated polyester resin synthesis.

In three neck flask add 13.28gm phthalic anhydride, 11.73ml 1, 3-propanediol, 0.2gm PTSA
as catalyst and 10ml xylene as solvent. Using motor stirrer material was mixed properly. Now raise
the temperature gradually up to 800C than increases up to 160-1800C. Din and stark apparatus
attached with three neck flask contains 10ml of xylene which helps to remove water from the system.
Acid value can be calculated at regular interval of process using the following method.

Acid value Determination

At regular interval sample from the above process was taken and titrated against a standard
alcoholic KOH solution. Note down the burette reading and find out the acid value by following
equation (1).

୆.ୖ. ଡ଼ ୒ ଡ଼ ହ଺.ଵ .............. (1)
Acid value =

୛ୣ୧୥୦୲ ୭୤ ୲୦ୣ ୱୟ୫୮୪ୣ ୲ୟ୩ୣ୬

Where, N = Normality of the alcoholic KOH solution.

IR Spectroscopy

The resulting polyester sample was characterised by IR spectroscopy using Perkin Elmer
spectrum GX instrument by KBr pallet method.

RESULT AND DISCUSSION

Effect of Temperature

During the esterification process, temperature plays a very important role. If the temperature was
kept around 1800C to 2000C for 4 hrs reaction time, than product may thermally decompose. More
specifically at the higher temperature sublimation of phthalic anhydride may occur. Ultimately there
was shortage of one of the important constituent was taking place. Due to this reason acid values do