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Performance Characteristics of Industrial waste-N330 N550 and N660 Carbon Black Hybrid Natural Rubber Composites.

Byline: Khalil Ahmed Khalid Mahmood and Sheraz Shafiq

Summary: In this research work natural rubber (NR) hybrid composite was prepared by incorporating industrial waste such as marble sludge with three different types of carbon black (CBdt) to be precise as CBN330 CBN550 and CBN660. Samples were mixed on two roll mill and vulcanized at 150 C. The effects on the curing characteristics mechanical and swelling properties of NR hybrid composites of CBdt with MS were evaluated in CBdt and hybrid combinations of MS/CBdt. It was found that gradual increment of CBdt in MS/CBdt hybrid composite decreased the scorch and cure times however the minimum and maximum torques increased with increasing CBdt in particular hybrid composite. The overall mechanical properties tended to increase however the % elongation at break resilience and abrasion loss decreased with increasing CBdt.

The swelling ratio has also been observed to be decreasing and cross link density and shear modulus increasing with CBdt i orporation.

Keywords: Hybrid composites Carbon black Marble sludge Curing characteristics Mechanical properties.

Introduction

Considering an imperative rather of polymer material natural rubber is widely used owing to its high and reversible deformability. Nevertheless the basic properties such as strength and modulus are low therefore an additional reinforcing component is essential for the practical implementation of rubber products [1-3]. Rubber is commonly reinforced with carbon black silica silicates and fibers. Carbon black (CB) is an important reinforcing material in polymers and usually improves performance related properties. Reinforcement of CB in elastomers has been investigated by numerous researchers [4-14].

At present many attention has been directed towards the hybrid filler composition in rubber compounds using varieties of two or more different kinds of filler in a polymer matrix to elucidate some innovative outcomes [15]. Among them CB-silica hybrid filler system glances to be the most popular and successful. The CB-silica dual phase filler is commercially manufactured by Cabot Corporation for the applications of truck tire [16]. The CB-silica hybrid filler system has overall improved mechanical properties compare to individual one. It also illustrates the almost favorable balance of various properties for example wet traction wear resistance and rolling resistance [17].

In our previous work the natural rubber hybrid composites were prepared by using marble sludge alone and with rice husk derived silica hybrid composites and the resultant composites showed satisfactory performance [18-20]. For further continuation of research work in said field the preparation and properties of three different kinds of carbon black along with marble sludge incorporated to natural rubber is investigated. Marble sludge is waste material remaining after cutting and polishing of large pieces of marble.

The key objective of the present exploration is to fabricate the constructive hybrid NR composite tailor-made cure characteristics mechanical swelling as well as aging properties. Thus in this work we investigated the effects of marble sludge hybrid composites with three different natures of CB namely CBN330 CBN550 and CBN660 added in natural rubber to get cost effective and good performance hybrid composites

Results and Discussion

Characterization of Marble Sludge

Marble sludge is composed of calcium/ magnesium compound in large amount and silica aluminum and iron oxide in small amount as shows in Table-1. The values obtained for metal component of MS from the complexometric titration (CaO 68.13% MgO 22.88%) gravimetric analysis (SiO2 4.26 % Al2O3 2.55 % and Fe2O3 0.585 %) and AAS (Fe2O3 0.581 % Cr2O3 0.20 % ZnO 0.23 % TiO2 0.560 % Mn 0.0059% and Sb Ni Pb and Na compound not detected) are approximately same with those obtained from WDX-ray fluorescence spectrometer.

Table-1: Analysis of MS using WDX-ray fluorescence Spectrometer.

Component###Wt (%)

###Calcium Oxide###68.6

###Magnesium Oxide###22.13

###Silica###3.89

###Aluminum Oxide###2.785

###Iron Oxide###0.603

###Chromium Oxide###0.24

###Zinc Oxide###0.20

###Titanium Oxide###0.549

Cure Characteristics

Table-2: Cure characteristics measurement of MS/CBdt hybrid NR composites.

###Cure characteristics at 150 C

MS/CBdt###Hybrid composition###Scorch time min###Cure time min###Min. Torque dNm###Max. Torqued Nm###CRI min-1

###00/00###Unfilled###2.34###4.22###0.23###2.56###0.532

###60/00###MS-60###1.67###4.55###0.39###3.45###0.348

###MS/CBN330###1.62###4.32###0.41###3.52###0.370

###50/10

###MS/CBN550###1.60###4.29###0.42###4.53###0.371

###MS/CBN660###1.57###4.26###0.44###4.57###0.371

###MS/CBN330###1.56###4.24###0.44###4.60###0.373

###40/20

###MS/CBN550###1.54###4.24###0.46###4.60###0.370

###MS/CBN660###1.54###4.21###0.48###4.62###0.374

###MS/CBN330###1.52###4.20###0.47###4.64###0.373

###30/30###MS/CBN550###1.49###4.17###0.50###4.68###0.373

###MS/CBN660###1.47###4.15###0.51###4.68###0.373

###MS/CBN330###1.40###4.10###0.52###4.70###0.370

###20/40###MS/CBN550###1.37###4.05###0.53###4.72###0.373

###MS/CBN660###1.35###4.03###0.55###4.75###0.373

###MS/CBN330###1.30###4.00###0.57###4.77###0.370

###10/50

###MS/CBN550###1.27###3.96###0.59###4.81###0.371

###MS/CBN660###1.25###3.92###0.60###4.81###0.374

###MS/CBN330###1.22###3.90###0.63###4.86###0.373

###00/60###MS/CBN550###1.18###3.86###0.64###4.88###0.373

###MS/CBN660###1.15###3.84###0.67###4.92###0.371

The CRI as shown in Table-3 has found higher values of as compare to MS filled NR composite however at higher CBdt content the CRI shows no significant effect. The hybrid filled sample with carbon black showed the highest CRI. This surveillance obviously shows the better reinforcing proficiency of all three types of carbon black in NR hybrid composite.

The minimum (ML) and maximum (MH) torque shown in Table-2 increases with gradual increases CBs amount in MS/CBdt hybrid NR composite. For a given hybrid ratio CBN330 containing hybrid ratio showed the lowest MH value. The highest MH value is scrutinized for CBN660 filled hybrid NR composite. This observation is related to the different CB in the degree of reinforcement. The highest reinforcement is observed in the case of CBN330 that is merged with its lesser particle size as

CBN330 particles in the NR matrix is more consistent which gives a better reinforcement.

Mechanical Properties

The tensile strength (TS) of MS/CBdt NR composite is shown in Fig. 1. All three type of carbon black exhibited an increasing trend up to maximum (60 phr) content. The hybrid ratio at 10/50 MS/CBN33 has optimum value as compare to other two combinations. The TS increased radically as the content of CB concentration incorporated in-place of MS in NR hybrid composite. The variation in TS is in compromise with the reinforcing aptitude of the fillers. The tensile properties dynamically depends on numerous aspects such as the filler reinforcement and rubber matrix properties filler content particle size and surface area of the filler The enhancement in TS may be caused by the very well dispersion of CBs in the NR matrix which leads to a strong interaction between the NR matrix and CB particles. These sounds-dispersed CBs might have the effect of cross linking positions therefore increasing the tensile strength [22].

The distinction in TS is in accordance with the reinforcing ability of the fillers. MS/CBN660 comprising the biggest particle size illustrates the lowest reinforcement in their corresponding hybrid composite. Similarly CBN330 having the lowest particle size in corresponding NR composite exhibit a better reinforcement level. However the CBN550 shows an intermediary behavior in their hybrid NR composite. In the particulate filled rubber matrix the fillers proceed as stress deliberators. Lesser the particle size of fillers more competent will be the stress transmitting from the matrix to the fillers [23].

A good interface between the fillers and the rubber matrix is very significant for a material to situate the stress. Under load the matrix allocates the force to the CBs that take most of the applied load.Fig. 2 demonstrates the effect of MS/CBdt content within the NR hybrid composite on 300 % modulus. The same trend as for the tensile strength was also observed for 300 % modulus. It was evidently shown that the presence of CB with MS contained NR hybrid composite has significantly improved the 300 % modulus. Hybrid NR composite reinforced with three types of CB showed a remarkable increase of modulus with gradually increasing CB. CBN330 content shows a maximum value of 300 % modulus at 10/50 MS/CBN330 which shows that the modulus increases with increase in the amount of CB in their individual hybrid system. The improvement of modulus is owing to the high modulus of CB and well dispersion exhibiting accurate stress transfer [24].

Fig. 3 illustrates the tear strength of MS with three different types of CB incorporated in NR hybrid composite. The tear strength of the composites generally depends on the nature of the filler and their hybrid composition. The same trend as for the tensile strength also observed in tear strength results. The tear strength increased with the increasing quantity of different types of CB incorporated in place of MS in NR hybrid composite as expected. A higher dispersion of the filler in the NR matrix can be observed in the maximum quantity of carbon black in 10/50 MS/CB ratio or at 60 phr CB loaded NR composite. A more uniform dispersion of CBN550 in NR matrix can be viewed. The tear strength of the hybrid composite becomes more uniform at 10/50 MS/CB phr loading compare to that at 50/10 MS/CB phr loading. This clearly supports better tear strength of MS/carbon black composite at 10/50 phr loading compare to those with lower filler content.

The % elongation at break of MS/CBdt is shown in Fig. 4. The elongation at break decreased with the increase in the quantity of different types of CBs. It may be attributable to the marked reinforcing effect of CB. As the CB content in the NR hybrid composite increases the stress level gradually increases but at the same time the strain of the hybrid composites decreased. This is because the carbon black included in the NR matrix behaves like physical cross-linking points and restrict the movement of polymer chains. This shows that the addition of carbon black makes the NR matrix stronger but more brittle.

The hardness curve for MS/CBdt is shown in Fig. 5. The hardness of the composites is another property that may be varied by the combination and the addition of filler in rubber matrix. It has been observed that the hardness of the hybrid composite increases with gradual CBs loading in all the cases of hybrid NR composite attaining highest value for MS/ CBN330 filled hybrid samples followed by CBN550 and CBN660 filled samples.

Fig. 6 illustrate the % rebound resilience of the relevant hybrid composites It is found to be lower than the unfilled NR compound and has been established to be in the sequence CBN330 greater than CBN550 greater than CBN660 comprised NR hybrid composites. The rebound resilience of the respective hybrid composites has been observed to be decreasing with the increasing amount of CBs. It may be due to the polymer chain mobility within the matrix and is lower for CBN660 filled NR hybrid composite as compare to CBN550 and CBN330 containing sample.

The abrasion resistance expressed as volume loss of unfilled MS filled and MS/CBdt hybrid NR composite have been examined and shown in Fig. 7. A higher volume loss shows the lower abrasion resistance. The unfilled NR compound has lowest volume loss however MS filled hybrid has the highest value. With gradual increase of the CB amount in MS/CBdt reduced the abrasion loss. The CBN330-filled NR hybrid composite exhibited highest abrasion resistance as compare to CBN550 and CBN660. The high value of abrasion resistance of the CBN330 containing NR hybrid composite corresponded to its highest hardness and cross-link density lowest abrasion loss [25]. Furthermore explained that the abrasion resistance of rubber vulcanizates was dependent upon their hardness and cross-link density value

Table-3: Swelling performance of MS/CBdt hybrid NR composites.

###Swelling performance

MS/CBdt Hybrid

composition###Swelling Crosslink density Shear modulus

###ratio###x 10 -4 mol/cm3###MPa

00/00###Unfilled###3.70###1.557###0.351

60/00###MS-60###2.58###2.53###0.570

###MS/CBN330###2.47###1.748###0.362

50/10###MS/CBN550###2.53###1.168###0.263

###MS/CBN660###2.55###1.428###0.322

###MS/CBN330###2.35###1.850###0.417

40/20###MS/CBN550###2.43###1.499###0.338

MS/CBN660###2.46###1.453###0.327

###MS/CBN330###2.30###1.988###0.448

###MS/CBN550###2.38###1.561###0.352

30/30

###MS/CBN660###2.42###1.580###0.356

###MS/CBN330###2.23###2.016###0.454

###MS/CBN550###2.30###1.606###0.362

20/40

###MS/CBN660###2.35###1.593###0.359

###MS/CBN330###2.19###2.183###0.492

10/50###MS/CBN550###2.27###1.697###0.382

###MS/CBN660###2.33###1.625###0.366

###MS/CBN330###2.00###2.206###0.497

###MS/CBN550###2.10###1.700###0.383

00/60

###MS/CBN660###2.18###1.626###0.366

Chemical cross-linking density is mole of effective network chain per cubic centimeter. In the present study the value of the chemical crosslink of the MS/ CBN330 filled hybrid filled NR compare with the unfilled and MS filled NR is shown in Table-3. The result shows that there was effective cross- linking of the CBdt filler with NR during vulcanization and this increase with increasing CBdt dosage in NR hybrid composite [27]. This further confirms the reality that there is better filler-rubber interaction for CBdt containing hybrid sample than the unfilled and MS filled NR composite. It has been inaugurated to be in the order CBN330 greater than CBN550 greater than CBN660 occupied NR hybrid composites

The shear modulus of MS/CBdt hybrid NR composite of hybrid composites is also given in Experimental

Materials and Test samples

The materials natural rubber (RSS-1) and carbon blacks (N330 N550 and N660) provided by Rainbow rubber industry Karachi (CBN330 high- abrasion furnace black average primary particle diameter 30 nm CBN550 fast-extruding furnace black average primary particle diameter 50 nm and CBN660 general purpose furnace black with 65 nm average primary particle diameter) have been cross linked by sulfur vulcanization. MS was collected from the marble processing industry. The MS was dried at 80 C for 24 h in the oven and then crushed in finer form. The ground MS was passed through sieve to obtain 37 m. The filled natural rubber hybrid compounds contain 00/00 60/00 50/10 40/20 30/30 20/40 10/50 and 00/60 of MS/CBs per hundred grams of rubber (phr). Furthermore to the raw rubber and filler the other constituents were Tetramethyl thiuram disulfide (a fast curing sulfur-donor accelerator) zinc oxide (ZnO and stearic acid as activator)

sulfur as curing agent 3-D imethylbutyl-N- phenyl-p-phenylenediamine (anantioxidant) 3- Dimethylbutyl-N-phenyl-p-phenylenediamine (Antioxidant) used were commercial grade and all purchased from local market.

The characterization of MWP was carried out with a XRF spectrometer (PIONEER with the Bruker AXS SPECTRA) to corroborate the composition of the MWP. XRF spectrometer result of MWP was to analyze the composition of MWP.

The formulation is presented in table 4. The composites were managed as depicted previously [28-30]. The cure characteristics of the compositions were examined as in our prior works [31 32]. Mechanical swelling and other properties of prepared hybrid composites were carried out as expressd previously via ASTM [33 34]

Table-4: Formulation Used in the Preparation of

MS/CBdt hybrid filler NR composites.###

Ingredients###Formulation phr

Natural Rubber###100###

###00:00 60:00 50:10 40:20

MS:CBdt Hybrid combination

###30:30 20:40 10:50 00:60

Zinc oxide###05###

Stearic acid###02

Tetra methylthiuram disulphide###2.4

Sulphur###1.6

Antioxidant###1.5

Conclusion

In this work the MS with CBN330 CBN550 and CBN660 hybrid NR composites were fabricated and the cure characteristics mechanical and swelling behavior were measured.

The scorch as well as cure time of the NR hybrid composite revealed a decreasing trend with increasing CBdt amount in MS/CBdt while the minimum and maximum torque exhibited an increasing tendency. The tensile strength modulus tear strength hardness cross link density and shear modulus has been found to be increased with increasing the amount of CBdt in MS/CBdt hybrid NR composite. Along with the hybrid composites the CBN330 filled hybrid models showed the highest overall properties pursued by CBN550 and CBN660 filled hybrid samples. The elongation at break resilience abrasion loss decreased and swelling ratio was established to be decreased with increasing the amount of CBdt in MS/CBdt hybrid NR composite

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Publication:Journal of the Chemical Society of Pakistan
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Date:Aug 31, 2014
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