The Effect of Alkanolamide Addition on Cure and Tensile Properties of Unfilled Natural Rubber Compounds

  

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  The effect of alkanolamide addition on cure and tensile properties of unfilled natural rubber compounds

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  2 ₁ Department of Chemical Engineering, University of Sumatera Utara, Medan, Indonesia ₂ School of Materials and Mineral Resources Engineering Universiti Sains Malaysia Penang, , ,

  Rubber additives are classified into curative and non-curative additives. Curative additives play

an important role in determining the cure characteristics of rubber compounds. They affect the rate and

nature of the vulcanization process. In rubber technology, the popular curative additives are sulphur or

other vulcanizing agents, zinc oxide, stearic acid and accelerators.

  1. Introduction In rubber technology, rubber recipe is the heart of rubber compounding which contains a group

of base rubber and rubber additives [1]. Each of them has a specific function either in proces Rubber or blend of rubbers will provide rubbery behavior to

^57]

the compound ; rubber additives such as fillers can cheapen the cost of rubber products , modify

^[57]

modulus and processing properties ; plasticisers are used to reduce viscosity, enhance deformability

and alter properties; vulcanizing agents can crosslink the rubber chains; and accelerators are

something that improve the action of vulcanizing agents to speed up the resultant crosslinking.

  torque differences, tensile modulus and tensile h of up to 0.6 phr of ALK loading and ^[13] then decreased with further increases in the ALK loading. Scanning electron microscopy ^[23] (SEM) proved that 0.6 phr loading of ALK in the NR compound s exhibited the greatest matrix ^[13] tearing line and surface roughness which correlated to a higher tensile strength of the NR compound.

  1.0 phr. It was found that the addition of ALK exhibited shorter scorch and cure times and ^[14] higher elongation at break of the unfilled NR compounds The ALK also exhibited higher . ^[13]

  Bleach DeodoPalm Stearin ( RBDPS) and diethanolamine, and incorporated into the ed unfilled-NR compound as a new rubber additive . The ALK loadings were 0 . 2, 0.4, 0.6, 0.8 and ^[33]

  Malaysia E-mail: indradanas@yahoo.com Abstract. Effect of alkanolamide (ALK) addition on cure and tensile properties of unfilled natural rubber (NR) compounds was investigated. The ALK was synthesized from Refined ^[33]

  1 , H Ismail

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  I Surya

  223 T alkanolamide addition on cure and tensile properties of he effect of unfilled natural rubber compounds

  IOP Conf. Series: Materials Science and Engineering (2017) 012012 doi:10.1088/1757-899X/223/1/012012

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  Innovation in Polymer Science and Technology 2016 (IPST 2016)

  A lot of studies on curative additives have reported by some researchers. Coran studied on

concentration effect of stearic acid, a palm oil fatty acid, on NR [2-3]. He found that the specific rate

^[47]

of vulcanization is decreased if the concentration of stearic acid is increased . Poh and Tang reported

that the scorch time increases with the stearic acid content for all the rubbers investigated [4]. Barton

and Hart reported that modulus values improve as the lauric acid content increases. The addition of

lauric acid also improved the physical properties of the vulcanisates [5]. Ismail and Ruhaizat reported

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that the concentration of palm oil fatty acid affected not only the curing characteristics and but also the

mechanical properties of the unfilled and calcium carbonate filled NR compounds [ 6-7]. The diamine

salt of fatty acid, referred to as a multifunctional additive (MFA), can also be util curative

_[14]

additive in filled NR compounds. The MFA improved the cure characteristics and mechanical

properties of the silica-filled NR compounds [ 8] and white rice husk ash-filled NR compounds [9].

  In this study, the effect of the addition of Alkanolamide (ALK on the cure and tensile )

properties of the unfilled-NR compounds was investigated. The ALK is considered as a relatively new

rubber additive, and it was prepared from Refined Bleached Deodorized Palm Stearin (RBDPS) and

ethanolamine. Compared to others, this additive has unique nature of molecule which is structured by

the combination of hydrophobic long chain hydrocarbon and hydrophilic amide as visualized in Figure

1.

2. Experimental Method

  2.1. Materials _[16] NR grade SMR L was used and obtained from Guthrie (M) Sdn. Bhd., Seremban, Malaysia. Other

compounding ingredients such as sulphur, zinc oxide, stearic acid , N-isopropyl-N'-phenyl-p-

phenylenediamine (IPPD) and Mercapto Benzothiazolyl disulfide (MBTS) were supplied by Bayer

_[22]

(M) Ltd. , Sdn. Bhd., Petaling Jaya, Selangor, Malaysia. All materials were used as supplied. The ALK

was synthesized in laboratory using Refined Bleach ed Deodorized Palm Stearin (RBDPS) and

diethanolamine. Its molecular structure is shown in Figure 1.

  O CH CH OH

  2

  2 (CH ) C CH

  2

  14

  3 N CH CH OH

  2

  2 _[16] Figure 1. The molecular structure of alkanolamide

  2.2. Compounding _[16] A semi-efficient vulcanization system was used for the compounding. The recipe for the preparation of the NR compound is given in Table 1.

• _* Table 1. The composition of the NR compound

  Ingredients Content (phr) NR (SMR L) 100.0 Zinc oxide

  5.0 Stearic acid

  2.0 IPPD

  2.0 MBTS

  1.5 Sulphur

  1.5 _{[34] *} ALK 0.0; 0.2; 0.4; 0.6; 0.8; 1.

  parts per hundred parts of rubber Innovation in Polymer Science and Technology 2016 (IPST 2016) _[16]

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The compounding procedure was done in accordance with the American Society for Testing and

_[78]

Material (ASTM) Designation D 3184 80. Table 2

  The compounding was done on a two-roll mill.

• – – shows the designation and composition of the NR-based recipes used in this study.

  Table 2. The designation and composition of the unfilled NR based recipes Designation Composition Unfilled NR/ALK (phr) A/0.0 (Control) Unfilled NR 100/0.0 B/0.2 Unfilled NR/ALK 100/0.2 C/0.4 Unfilled NR/ALK 100/0.4 D/0.6 Unfilled NR/ALK 100/0.6 E/0.8 Unfilled NR/ALK 100/0.8 F/1.0 Unfilled NR/ALK 100/1.0 _[16]

2.3. Cure Characteristics

  The cure characteristics of the rubber compounds were obtained using a Monsanto Moving Die

Rheometer (MDR 2000) which was employed to determine the scorch time (ts ), cure time (t ) a

_[39]

  2

  90

torque difference o tested at 150

C. The rubber compounds were subsequently compression-moulded using a stainless

  o steel mould at 150

  C, with a pressure of 10 MPa and applying a laboratory hot-press based on respective curing times . _[25]

  2.4. Tensile Properties _[14] Dumbbell-shaped samples were cut from the moulded sheets according to ASTM D 412-93. _[14]

Tensile tests were performed at a crosshead speed of 500 mm/min . Tensile tests were carried out with

a universal tensile machine Instron 3366 to determine the tensile properties in terms of tensile strength

(TS), stresses at 100% and 300% elongations (M100, M300) and elongation at break (EB).

  2.5. Scanning Electron Microscopy (SEM) The tensile fractured surfaces of the compounds were examined by using a Zeiss 5VP _[43]

scanning electron microscope (SEM). All the surfaces were examined after first sputter coating with

gold to avoid electrostatic charging and poor image resolution . _[14]

3. Results and Discussion [13] 3 .

  1. Effect of Alkanolamide on Cure Characteristics and Crosslink Density _[13] Effect of ALK on the cure characteristics of the unfilled NR compound is showed in Table 3. The

scorch and cure times decreased with increased ALK loading . It was a cure enhancement which

indicated ALK acted as a co-curing agent (secondary accelerator) in the curing. The amine content of Innovation in Polymer Science and Technology 2016 (IPST 2016)

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the ALK caused the rubber compound more basic. Alkaline substances tend to improve the cure rate

[10].

  Table 3. The cure characteristics and tensile properties of unfilled NR compounds with and without ALK Cure characteristics Tensile properties

  Compounds ts ^{2 , min. t 90 , min. M H L M100 M300 TS EB} −M

  (dN.m) (MPa) (MPa) (MPa) (%) A/0.0

  4.59

  7.13 4.77 0.538 1.235 17.7 1070.0 B/0.2

  4.52

  7.05 4.85 0.544 1.236 19.3 1095.7 C/0.4

  4.24

  6.65 4.97 0.561 1.311 19.5 1116.5 D/0.6

  3.96

  6.45 5.21 0.586 1.364 20.1 1141.5 E/0.8

  3.74

  6.00 5.12 0.545 1.267 18.4 1154.0 1.0

  3.73

  5.83 4.89 0.516 1.231 16.5 1172.0 M L = Minimum torque; M H = Maximum torque; M H L = Torque difference A/0.0 = Unfilled NR without ALK .

  −M _[25] B/0.2; C/0.4; D/0.6; E/0.8; F/1.0 = Unfilled NR with ALK.

  The addition of up to 0. 6 phr of ALK increased the torque difference (M H L ). Further −M

increases in the ALK loading decreased the torque difference. Torque difference represents shear

dynamic modulus which indirectly related to the crosslink density of a rubber compound [11-14]. The

addition of ALK affected the torque difference of the rubber compounds or the crosslink density of the

rubber vulcanisate. It was due to the acti on of the ALK as a secondary accelerator which enhanced the

state of curing process. _[13] The reduction of crosslink density beyond 0. 6 phr loading was due to the softening or

lubricating effect of the excessive ALK which dissolved a the elemental sulphur and hence

_[45]

reduced crosslink density. This explanation was supported with the morphology study of the tensile

fractured surface of the E/0. 8 with excessive ALK. In Figure 2(D), it seemed smooth wits

_[13]

matrix tearing and surface roughness. It indicated the more pronounced lubricating effect of the

excessive ALK (15] . _[44]

3.2. Effect of Alkanolamide on Tensile Properties

  Effect of ALK loading on the tensile properties of the unfilled NR vulcanisates is shown in

Table 3. The addition of 0.2 phr ALK produced vulcanisate B/0.2 with higher EB. Increasing the ALK

loading caused further increases in the percentage of EB or the extensibility of the rubber vulcanisate.

This was due to the function of ALK as an internal plasticiser which modified flexibility or

distensibility of rubber vulcanisate.

  The addition of ALK increased the M100 and M300 up to maximum level at 0.6 phr and

decreased with further increases in the ALK loading. The results of tensile strength also exhibit similar

trend. Tensile modulus and tensile strength are dependent only on degree of crosslink [8, 13]. The

improvement of those properties was attributed to higher degree of crosslink (as indicated by a higher Innovation in Polymer Science and Technology 2016 (IPST 2016)

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value of torque difference). The deterioration of those properties was due the excessive amount of

ALK which dissolved other curatives and hence reduced degree of crosslink density (as indicated by a

lower value of torque difference). As discussed earlier, crosslink density of a rubber compound is

indicated by torque difference value. The greater the torque difference, the higher is the degree or total

crosslink densit [11, 13 y ]. _[31]

3.3. Scanning Electron Microscopy (SEM )

  Figure 2 shows the SEM micrographs of the tensile fractured surfaces of the unfilled NR

compounds with and without ALK. Compared to A/0.0 (Figure 2A), t he fractured surfaces of C/0.4

and D/0.6 (Figure 2B and 2C, respectively) show many larger discontinuous slip tear lines with path

deviation indicating a higher energy requirement to cause failure. As a consequence, it led to increased

_[22]

resistance to crack propagation and thus, caused an increase in crosslink density. Otherwise the

fractured surface of E/0. 8 (Figure 2D) exhibits the least matrix tearing and surface roughness which

presumably correlated lo

_[14]

  

Ismail et al. and Nabil et al., (2013)[15]. They reported that an increase in crosslink density was

responsible for the roughness and matrix tearing line of the fractured surface.

  [13]

  Figure 2. SEM micrographs of the failure fracture surface of unfilled NR compound at a magnification of 200

  X, (A) A/0. 0, (B) C/0.4, (C) D/0.6, and (D) E/0.8 It was demonstrated that ALK can be utilised as a new curative additive in unfilled NR

compounds. ALK can be function as secondary accelerator which enhanced the cure rate. ALK also Innovation in Polymer Science and Technology 2016 (IPST 2016) _[23]

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enhanced the torque difference, crosslink density, tensile modulus and tensile strength especially up to

0. 6 phr. ALK also can be function as internal plasticiser which enhanced the EB

4. Conclusions

  _[13]

Alkanolamide can function as a curative additive in unfilled natural rubber co mpounds. Results

indicate that alkanolamide can be utiliz ed as a secondary accelend a plasticiser in the unfilled

_[13]

natural rubber compounds . The incorporation of alkanolamide enhanced the cure rate , reduced the

scorch time and improved the flexibility by increasing the elongation at break. The incorporation of

alkanolamide also enhanced tensile properties and crosslink density of the unfilled natural rubber

vulcanisate especially up to 0.6 phr loading.

  Acknowledgements The authors would like to thank Universiti Sains Malaysia, for providing the research facilities for carrying out the experiment and for making this research work possible.

  References

[1] Dick JS 2001 Rubber Technology Compounding and testing for performance Hamser Munich.

[2] Coran A 1964 Rubber Chem Technol

37 3 689-697.

[3] Coran A 1965 Rubber Chem Technol 38 1 1-14. [4] Poh BT and Tang W 1995 J Appl Polym Sci 55 3 537-542. [5] Barton BC and Hart EJ 1953 Rubber Chem Technol 26 3 510-521. [6] Ismail H and Ruhaizat T 1998 Polym-Plast Technol 37 4 483-494. [7] Ismail H and Ruhaizat TA 1997 Iran Polym J 2 97-104.

  6 [8] Ismail H and Chia H 1998 Polym Test 17 3 199-210. [9] Ismail H et al 1999 Eur Polym J 35 8 1429-1437. [10] Surya I et al 2014 Polym Test 40 24-32. [11] Teh PL et al 2004 Eur Polym J 40 11 2513-2521. [12] Ismail H and Shaari SM 2010 Polym Test 29 872-878. [13] Surya I et al 2015 Polym Test 42 208-214. [14] Surya I and Ismail H 2016 Polym Test 50 276-282. [15] Surya I, Ismail H and ARashid A 2013 Polym Test 32 1313-1321.