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*M.S.Prasanna Kumar, *S.Sharmila, **Manivannan. *UG Student, **Assistant professor Department of polymer technology Hindustan College of Engineering Anna University, Chennai-600025 Email:,

ABSTRACT This article addresses the properties of rice husk and polypropylene composite is determined for the following ratios. PP+5% RH, PP+10% RH, PP+15% RH A suitable percentage of RH combination is suggested and recommended for the practical usage at the end of the project. Rice husk is surface modified by treating with alkali. Using PPgMA as compatibilizer. The composite is mixed and pelletized by extruder. The test samples are then prepared using injection molding. The tests conducted are 1. 2. 3. 4. 5. DSC Tensile strength Impact strength Flexural strength SEM

The properties are tabulated and presented for discussion.

Keywords: Polypropylene, Rice husk, PP-g-MA, Composite, Scanning Electron Microscopy.

1. INTRODUCTION Rice milling generates a byproduct known as husk, this surrounds the paddy grain. This husk contains about 75% of organic volatile matter and balance 25% of the weight of this husk is converted in to ash during the firing process. This husk is used as fuel in the rice mills to generate steam for the parboiling process. RH contains cellulose 35%, hemi cellulose 25%, lignin 20% and ash 17% (94% silica) by weight. It is also a very good insulator and bio degradable in nature [1]. Polypropylene is a thermoplastic material. It is manufactured from propylene gas in presence of a catalyst like titanium chloride. PP has an excellent di-electric property. PP shows low permeability to many permeants and is non toxic. PP has an excellent dielectric property and none staining in nature. It is highly resistant to most alkali, acids, organic solvents, degreasing agents and electrolytic attack. Mould shrinkage is less for PP compared to other thermoplastics. Increase in molecular weight leads to increase in melt viscosity and impact strength but lower yield strength, hardness and stiffness [2]. In present investigation RH and PP is melt blended using PP-g-MA as a bonding agent. The objective of this project is to find out the mechanical stability and the improved characters of RH-PP composite.

2. EXPERIMENTAL 2.1 MATERIALS The polypropylene (H110MA) with density of 0.910 g/cc and MFI of 11 g/10 min (measured at 230C under 2.16 kg load), obtained from Reliance pvt ltd., India was used as the base matrix for the present study. PP-g-MA (under the trade name Exxlor PO 1020) was used in this study and has a melt flow index of 125gm/10 min with percentage of MA grafting is 0.75%. 2.2 PREPARATION Surface modification of rice husk is done to improve the adhesion of agricultural fibers by chemical interaction. It can be achieved through hydrogen or covalent bonding between reactive OH groups on the thermosetting resins. Alkali treatment involves soaking the rice husk in 4% NaOH and maintaining at room temperature for 24 hours. After treatment the rice husks are rinsed thoroughly in water to remove unreached NaOH and dried completely under sunlight. Alkali treatment is viewed as one of the widely employed chemical treatment techniques for surface modification of cellulosic fibers to improve adhesion properties.

After Surface treatment, the treated rice husk and polypropylene were extruded and pelletized for the following ratios. Constant 10% PPgMA is added in all ratios. 5% RH - 85% PP, 10% RH 80% PP, 15% RH 75% PP Melt blending of PP, PP-g-MAH (10 wt %) and the RH of 5, 10, 15 % weight was carried out in an intermeshing counter rotating twin screw extruder. Prior to extrusion, the matrix polymer and the Rice husk were dehumidified in a vacuum oven at 100C for a period of 12 hours. PP and the treated rice husk are mixed manually and are fed in to the extruder. The process was
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carried out at a screw speed of 150 rpm and a temperature difference of 170 C to 190 C between feed zones to die zone, followed by granulation in a pelletizer and drying. These granules were further injection molded using injection molding machine having clamping force 800kN fitted
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with a dehumidifier at a temperature range of 195220 C and mold temperature of 80 C, for preparation of test specimens of tensile, flexural and impact strength as per ASTMD standards.

2.3 CHARACTERIZATION 2.3.1 Mechanical characterization Specimens of virgin PP and RH of required dimensions were subjected to tensile test as per ASTM D-638 using universal testing machine (UTM) LR-100K (Lloyd Instrument Ltd U.K). A cross head speed of 50mm/min and gauge length of 50mm was used for carrying out the test. Specimens of virgin PP and RH of required dimensions were taken for flexural test under three point bending using the same universal testing machine accordance with ASTM-D 790 at a cross head speed of 1.3 mm/min and a span length of 50mm. Similarly, Izod impact strength was determined from the specimens having specific dimensions with a V notch depth of 2.54 mm and notch angle of 45o as per ASTM-D 256 using impact meter 6545. For analyzing the mechanical properties test specimens were initially conditioned at 23+1o C and 55+2% RH. Four replicate specimens were used for each test and the data reported are for the average of four tests. 2.3.2 Scanning electron microscopy The morphology of the impact fractured surfaces of virgin PP and RH composite, the fracture surfaces were coated with thin layers of palladium gold of about 10 A. All specimens were examined with scanning electron microscope with an accelerating of 10kv.

2.3.3 Flow characteristics The RH-PP composite and the melt index apparatus are first pre heated. The material is loaded into the cylinder from the top and a 2.16 kg load is placed on the piston. The material is allowed to flow through the die at 230C. The initial extrudate is discarded because it may contain air bubbles and contaminants. Depending on the material or the flow rate, cuts for test are taken at different time intervals. The extrudate is weighed and the melt index values are calculated in grams per 10 minutes as per the standards of ASTM D 1238.

2.3.4 Thermal characteristics The heat flow rate to the sample is measured using a differential scanning calorimetry while the temperature of the sample in a specified atmosphere is programmed because all materials have a finite heat capacity. A small quantity of sample usually 5 to 10 mg is weighed out in to an inert capsule which is made of aluminum as per the ASTM D 3417 standards. The encapsulated sample is placed in the DSC sample holder of a DSC cell disc. In the attached control module the operator selects the temperature range and heating rate. Now the test is started and initially, constant energy input is required to heat the sample at a constant rate. This establishes a base line at a transition point; the sample requires either more or less energy depending on whether the temperature is endothermic or exothermic. A hypothetical DSC curve is displayed on the module.

3. RESULTS AND DISCUSSION 3.1 Mechanical Properties SAMPLE TENSILE STRENGTH (Kgf/cm2) 343.837 336.061 324.780 302.335 TENSILE MODULUS (Kgf/cm2) 69124.6 72537.7 74594.2 82652.3 FLEXURAL STRENGTH (Kgf/cm2) 603.13 554.17 525.46 491.98 FLEXURAL MODULUS (Kgf/cm2) 17186.67 18810 20506.67 22665.33 IMPACT STRENGTH (KJ/m2) 1.726 1.665 1.576 1.457

Virgin PP 5% RH-PP composite 10 % RH-PP composite 15 % RH-PP composite

Table 1.Mechanical properties of RH-PP composite.

The average values of both strength and modulus of tensile and flexural also strength of impact test is tabulated above. In tensile strength the average values of 5%, 10% and 15% are gradually decreased compared to the virgin polypropylene. Subsequently their tensile modulus values are increased. Also the flexural strength of the composite decreases and the flexural modulus of the composite increases compared to virgin PP. This is due to the organic nature of the RH fibers. When a composite is made between an organic and inorganic material the bonding is considerably weak. And so to overcome this situation a suitable bonding agent is added. Here PP-g-MA is added.

kgf/cm2 stress

340 330 320 310 300 290 0 2 Strain 4 % 6 8 10 Series1

(Fig 1 Tensile graph)

1000 1 0 5 10 15 10 525.46 20506.67 15 491.98 22665.33

0 603.13 17186.67

5 554.17 18810

(Fig 2 Flexural graph)

1.75 1.7 1.65 1.6 1.55 1.5 1.45 1.4 0 5 10 % of rice husk 15 20

impact strength

(Fig 3 Impact graph)

Fig 1, 2 and 3 respectively shows the stress strain curve, flexural strength & modulus and the impact strength of the RH-PP composite. From the above graphs it is clear when rice husk % increases, the tensile and flexural modulus values also increases, though the mechanical strength decreases with increased addition of the filler. 3.2 Scanning Electron Microscopy (SEM)

(a) (a) SEM image of Virgin PP (b) SEM image of 5% RH-PP composite


(c) (c) - SEM image of 10% RH-PP composite (d) - SEM image of 15% RH-PP composite


As it can be seen from the figures RH distribution into the matrix is reasonably well and no voids are found in the composites. It seems that although the cogged structure of RH in combination with using MAPP in the composite has a profound effect in creating a reasonably good interaction between the components, which have been confirmed with the mechanical studies, the bonding is not very strong and perfect because some de-bonding can also be seen on the interface of RH and the matrix. 3.3 Melt flow index MATERlAL Virgin PP 5% RH-PP Composites 10% RH-PP Composites 15% RH-PP Composites Table 1 The flow rate of the composite decreases as the percentage of incorruption of the rice husk increases. FLOW RATE 1.51 g/10 minutes 1.48 g/10 minutes 1.31 g/10 minutes 1.04 g/10 minutes

3.4 Differential scanning calorimetry The hypothetical curve obtained for the RH-PP composite and the virgin PP material is shown below. 1. Virgin PP:

(Graph 4 DSC results for virgin PP) 2. 5 % RH-PP composites:

(Graph 5 DSC results of 5 % RH-PP composites)

3. 10 % RH-PP composites:

(Graph 6 DSC results of 10% RH-PP composites) 4. 15 % RH-PP composites:

(Graph 7 DSC results of 15% RH-PP composites) These graphs explain that the melt temperature increases in the composite with the increase of percentage of RH.

4. CONCLUSION The results show that mechanical properties of the composites remained in an acceptable level even if it decreases with increase in rice husk percentage. The degradation temperature of the composite is greater than that of the virgin PP which is confirmed by the thermal analysis. The SEM results show that the interfacial adhesion in the composite is excellent. The composite is of light weight and also bio-degradable in nature. Hence we conclude that 5% RH-PP composite is the best suitable material for any light weight, bio-degradable product which needs to withstand a high temperature and where the mechanical strength is not a major criterion.

ACKNOWLEDGEMENT The authors would like to thank the Central Institute of Plastics Engineering and Technology, Chennai, India for manufacturing the RH-PP composite.The authors would also like to thank the HOD of polymer department and the staff of Hindustan College of engineering for their moral support to finish the project successfully. REFERENCES [1]. Nabi Saheb D., Jog J.P., Natural fiber polymer composites: A review, Adv. Polym. Technol., 18, 351363, 1999. [2]. Handbook of Polypropylene and Polypropylene Composites, second Edition, Marcel dekker.Inc (2003). [3] J.A.Brydson Plastic materials,Butterworth- Heinemann, oxford 6th edition 1995. [4]. Bio-degradability and Mechanical Properties of Agro-Flour Filled Polybutylene Succinate Biocomposites Hee-Soo Kim, Han-Seung Yang, Hyun-Joong Kim Laboratory of Adhesion & Bio-Composites, Major in Environmental Materials Science, Seoul National University, Seoul 151-921, South Korea [5]. Chemical and thermal stability of rice husk against alkali treatment Bwire ndazi, Christian nyahumwa and Joseph tesha Department of engineering materials, University of Dar es Salaam, Dar es salaam, Tanzania.

[6]. Flour Rice Husk as Filler in Block Copolymer Polypropylene: Effect of Different Coupling Agents By ,Mart-Ferrer and Francisco, Technical Institute of Plastics Materials, Valencia Parc Technologic, Gustavo Eiffel, 4 E-46980 Paterna, Valencia, Spain

[7]. Mechanical Properties and Water Absorption Behaviour of Chopped Rice Husk FilledPolypropylene Composites, by Mohammad Razavi-Nouri, Fatemeh Jafarzadeh-Dogouri, Abdulrasoul Oromiehie, and Amir Ershad Langroudi Faculty of Polymer Processing, Iran Polymer and Petrochemical Institute, Tehran, Iran [8]. Effects of rice husk particle size, glass fiber length, RH/GF ratio, and addition of coupling agent on the mechanical and physical properties of polypropylene-RH-GF hybrid composites. By, H. D. Rozman, A. Zuliahani, G. S. Tay