Synthesis of Novel Film of Poly Vinyl Alcohol Modified Guar Gum with Tamarind seed Kernel Powder and its Characterization
Shruti Panwar*, Sangeeta Loonker
Department of Chemistry, Jai Narain Vyas University, Jodhpur (Rajasthan),-342001, India.
*Corresponding Author E-mail: shrutipanwar31@gmail.com*, sangeetag@hotmail.com
ABSTRACT:
A thin film of guar gum modified with polyvinyl alcohol (PVA) was prepared with tamarind seed kernel powder (TKP) by condensation polymerization method. In this method a redox pair of ascorbic acid and potassium persulphate was used. This initiate the reaction and poly vinyl alcohol grafted over guar gum. TKP was added by changing temperature and a thin film was prepared. Characteristics of newly synthesized film was determined by Fouriour transform Infrared spectrum(FT-IR), Thermogravimetric analysis(TGA), Nuclear Magnetic Resonance(NMR), Mass spectra, Scanning Electron Microscopy(SEM), elemental analysis etc.
KEYWORDS: condensation polymerization, PVA modified guar, redox pair, NMR, SEM, MASS spectra etc.
In Today's world the more attention seeks towards the formation of green composites that are environment friendly, cause less pollutuion and having biodegradable properties. Guar gum is most suitable biopolymer1 for this purpose. It is extracted from endosperm of plant cyamopsis tetragonolobus2.It is composed of sugar galactose and mannose. A straight chain of D-mannose units, united by β (1→4) glycoside linkages and bearing a single D-galactose unit on alternate mannose jointed to it by an α (1→6) glycoside linkage.3 (fig 1)
Polyvinyl alcohol was used for making film because it is non toxic, water soluble synthetic polymer. It has good physical and chemical properties for making film.4, 5
PVA has wide applications in different fields due to its gel forming properties and bioinertness. It also have medical applications such as hemodialysis, implantable medical devices etc.6, 7, 8 PVA is used as emulsifying agent, adhesive purpose. It is also resistance to oil, grease and some solvents.9, 10
Tamarind seed kernel is an important woody perennial fruity species known for its adaptability to various climatic and edaphic conditions. India is main producer and consumer in the world.11
It is galacto-xyloglucan, isolated from seed kernel of Tamarindusindica(fig.2).Tamarind seed polysaccharide have ability to form gel over wide pH range. It has properties like high viscosity, adhesivity, pH tolerance etc.12
Fig. 1 structure of guar gum Fig. 2 structure of TKP
2 MATERIALS AND METHOD:
2.1 Materials:
Guar gum (200 mesh size)(Shri Ram Gum Industries Jodhpur), PVA, ascorbic acid, potassium persulphate(ases chemicals, jodhpur) used without further purification. Tamarind seed kernel powder, Ethanol, Methanol, sodium hydroxide (1%), ammonium hydroxide (5N) were used.
2.2 Method:
2.2.1 Synthesis of poly vinyl alcohol (PVA) grafted (-g-) guar gum:
For the grafting process, guar gum(2gm) equal amount of ascorbic acid and PVA were added in 250ml of distil water. The mixture was heated at 35͘͘͘͘.c for 30 minutes and then potassium persulphate13 was added as initiator. Allowed this mixture to rest for one hour for grafting. Now pour this mixture into large quantity of dimethyl formamide(DMF) to separate PVA-g-guar gum from the solution and wash with DMF.
2.2.2 Saponification of PVA-g- guar gum:
The grafted guar gum was saponified with 1% solution of sodium hydroxide and heated to the boiling for for one hour. This saponified guar gum separated with the help of methanol and washed with ethanol.14
2.2.3 Preparation of TKP composite with PVA-g-guar gum:
Saponified guar gums dissolved in distil water and 10ml ethanol. In another beaker TKP dissolved in 5N ammonium hydroxide. Mix both the mixture and stirred at room temperature for 18-20 hours. Mixture was heated at different temperature (30-100͘͘͘.c) so that mixture became viscous. Then the film was prepared and dried (fig.3)
Fig. 3 PVA-g-guar with TKP film
Scheme:
3 RESULTS AND DISCUSSION:
3.1 FT-IR analysis:
To analyse the functional groups and bonds present in the synthesized film, FT-IR was carried out with Bruker: Alpha’s platinum ATR single reflection spectrometer with range 4000-600cm-1. In the IR spectra (fig. 4) broad peak found at 3400-3600 cm-1was due to the stretching vibration of –OH group present in polymer backbone. Peak found at 1651 cm-1 due to stretching vibration of –CHO group in TKP. Peak at 1456 cm-1due to bending vibration of –CH3 group. Peaks near 900 cm-1was due to stretching of –CO bonds and 600-700 cm-1peak due to –CH- bonds. The above characteristic peak showed the presence of PVA and TKP with guar gum.
Fig. 4 IR spectra
3.2 TGA analysis:
TGA of the film was carried out using TGA Q 500 V 6.7 Build 203. The thermo gram (fig.5) of the film was analyzed for their thermal stability up to600.C under inert atmospheric conditions. Thermogram breaks at different temperature. First breakdown at 100͘C. here 10% weight loss occur and this was due to the loss of moisture in the film. The next breakdown was at temperature nearly 450 ͘C and this was due to the breakdown of polymer chain. Here 20% weight loss occurs. At 500͘ ͘C almost total weight loss occur. This shows that the thermal stability of the film is present at around 500͘ ͘C.
Fig. 5 TGA Thermogram
3.3 Mass analysis:
Mass spectra recorded on a JEOL-accuTOF JMS-T100LC mass spectrometer having a DART source. (fig.6) Dry Helium was used with 4 LPM flow rate for ionization at 350.C. The M+ value of the film is 391.38.
Fig. 6 Mass spectra
3.4 1H NMR analysis:
The NMR spectrum was taken by Bruker avll HD-300MHz FT-NMR.The sample for spectra (fig.7) prepared in DMSO solvent. The peak found at 0.9ppm due to –CH2- group. Peak at 3.4ppm was due to methoxy carbon (-OCH3). Peak at 2.5ppm was due to α carbon to the –CO group. Small peak at 5.3ppm was due to vinylic group. The above peak confirmed the presence of functional groups found in Guar PVA and TKP.
Fig. 7 NMR spectra
3.5 Scanning Electron Microscopy (SEM) and Elemental Analysis (EDX)
The SEM technique used to study the surface morphology of different polymers and composites. The micrograph (fig 8) of newly synthesized film was taken. It reveals that surface of the film was homogeneous and porous in nature.
Fig. 8 Scanning Electron microscopy
Elemental analysis is a process where a sample of some material is analyzed for its elemental composition such as carbon, hydrogen, nitrogen and sulphur. Elemental analysis of the film was done and found the major percentage of carbon and oxygen. Composition of newly synthesized film is given in table 1.
Table 1 Elemental analysis
|
Sr. No. |
Element |
Weight% |
Atomic % |
|
1 |
C |
37.62 |
47.56 |
|
2 |
O |
43.43 |
41.22 |
ACKNOWLEDGEMENT:
The authors are thankful to the SAIF (Sophisticated Analytical Instrument Facility) for MASS Analysis and 1H NMR analysis. Also thankful to Defense Laboratory Jodhpur (DRDO) for TGA (Sh. Shatrughan Malav, SRF) SEM, and Elemental analysis (Dr. Smita Soni).
REFERENCES:
1. Rashmi Manchanda, S.C. Arora, Rajesh Manchanda, International Journal of Pharm. Tech Research CODEN (USA): IJPRIF ISSN: 0974-4304 Vol.6, No.2, pp 412-420, April-June 2014
2. A P Gupta and Gopal Arora Der ChemicaSinica, 2012, 3(5):1191-1197 ISSN: 0976-8505 CODEN (USA) CSHIA5
3. Rajashree Chahatray, D. Sahoo, D.P. Mohanty and P.L. Nayak World Journal of Nano Science and Technology 2(1): 26-32, 2013, 2013DOI:10.5829/idosi.wjnst.2013.2.1.21136
4. Soumendra Sahoo, Rashmirekha Sahoo, Yogesh Panditrao Palve, Padmalochan Nayak, ISSN NO-2230-7885 CODEN JPBSCT J Pharm Biomed Sci.
5. T Chandy, C P Sharma. J. appl poly sci.1992; 44:2145-56
6. S K Mallapragada and N A Peppas. Journal of polymer science: part B, polymer physics, vol. 34 1996, PP.1339-1349. Doi: 10, 1002/(sici)1099-0488(199605)34:7<1339::AID-POLB15>3.0 CO;2-B
7. G. Paradossi, R. Lisi, M. Paci and V Crescenzi. Journal of polymer science: part A, polymer chemistry. Vol.34, 1996, PP.3417-3495. Doi; 10.1002/(SICI)1097-4628(199990624)72:13<1755::AID-APP 11>3.0.CO;2-R
8. J Jegal, K Lee. Journal of applied polymer science, vol. 72, 1999, PP.1755-1762. Doi:10.1002/app.1992.070441210
9. Anek Pal Gupta and Gopal Arora Journal of Materials Science and Engineering B 1 (2011) 28-33 Formerly part of Journal of Materials Science and Engineering, ISSN 1934-8959
10. R. Schell kens, C. J. Bastiaansen, Journal of Applied Polymer Science 43 (1991) 2311-2315.
11. Mohamed HA1, Mohamed BE and Ahmed KE, Mohamed, et al., J Food Process Technol 2015, 6:6
12. S. S. Shaikh, K. J. Shivsharan, R. K. Pawar, N. S. Misal, H. R. Mene, B. A. MoreInt. J. Pharm. Sci. Rev. Res., 33(1), July – August 2015; Article No. 31, Pages: 157-164 ISSN 0976 – 044X
13. Sudhir G. Warkar and A. P. Gupta Int. J. Pharm. Bio Sci. 2015 Jan.; 6(1): (P) 622 – 638 ISSN 0975-6299
14. V. Singh, S. Pandey, S. K. Singh, R. Sanghi, J Sol-Gel Technol (2008) 47:58-67 DOI 10.1007/s10971-008-1715-2
Received on 10.05.2017 Modified on 20.06.2017
Accepted on 11.07.2017 © AJRC All right reserved
Asian J. Research Chem. 2017; 10(5): 616-620.
DOI: 10.5958/0974-4150.2017.00103.1