Abstract:
The prime objective of this dissertation is to synthesize the mesoporous materials Korean
Advanced Institute of Science and Technology-6 (KIT-6) and Santa Barbara Amorphous-15
Spherical (SBA-15-S) and utilize these mesoporous silica based materials with elastomers to
enhance the properties of tire tread compounds. Mesoporous silica based elastomers are
developed to get better physical, mechincal and thermal properties and to synthesize
materials that are environmental friendly. These filler reinforced elastomers were tested
under different conditions and the properties that were analyzed are torque, scorch time. The
combined studies of mesoporous silica based materials and elastomers showed that these
novel materials lead to promising structural and mechanical properties.
The degradation of carbon black treads have adverse effects on environment so the world is
looking for alternative materials that can replace carbon black. Silica is one of the materials
that was under observation for the last few decades but reinforcement level is not same
provided by silica as compared to carbon black. Amorphous silica and precipitated silica
have also been used in tires for many years but these tires are suffering from increased mass,
higher thickness and higher noise level. Silica can reduce the green house gas emissions as
well.
In this study meso-porous silica materials have been synthesized and utilized as fillers in
Styrene Butadiene Rubber (SBR) to investigate their effect for tire tread compounds. For
this purpose, KIT-6 is synthesized by dissolving 11.8g of HCl in 217g of deionized water
and mixing 6g of P123 in it under constant stirring. When uniform solution is formed add 6g
of 1-butanol under constant stirring at 35oC. After 1 h, add 12.8g of Tetraethyl ortho silicate
drop wise keeping the temperature constant. The resulting solution is kept under constant
stirring for 1 day at 35oC. After this the solution is shifted to Teflon bottle and placed in
oven for 1 day at 100oC for hydrothermal treatment. The obtained solution is filtered and
dried, the solid product is then calcined at 550oC for 5 h and utilized as a filler in elastomers.
SBA-15-Spherical is synthesized by dissolving 23.6g of HCl in 80g of deionized water and
adding 4g of P123 under constant stirring at 35oC. As the uniform solution is formed take
40g of deionized water and add 3.04g of KCl in it separately at 25oC. Now add this solution
to the first one and keep it under stirring for 1 h at 35oC. Then 3g of mesitylene is added and
the solution is kept under stirring for 2 h. After that 8.5g of tetraethyl ortho silicate is added
drop wise and stirred for 10 – 20mins. The solution was kept under static condition for 1 day
and then shifted to Teflon bottle and kept in oven at 100oC for 1 day. The solution is
hydrothermally treated which is then filtered and dried. The solid product retained after
filtration is calcined at 550oC for 5 h and used as a filler. The synthesized Mesoporous
silicas KIT-6 and SBA-15-Spherical are characterized by SEM-EDS, XRD, BET and FT-IR
analysis for their conformity.The surface modification of meso-porous silica materials is done by dehydrating meso porous silica for 3 h at 200oC to remove adsorbed moisture. Meso-porous silica materials are
grafted in dried toluene using 3-aminopropyltrimethoxysilane as amine source. Then 1g of
respective meso-porous material is dispersed in 50ml of dried toluene and 3ml of AP (3-
amino propyltrimethoxysilane) are added to the suspension, which is further kept under
reflux for 20 h. The solid product is recovered by filtration and repeatedly washed out with
toluene and octane and dried overnight at 80oC .
These silylated and non-silylated meso-porous silica materials are reinforced in NR (natural
rubber) to form nano composite. These nanocomposites were formed by adding 6 phr (parts
per hundred parts of rubber) of meso-porous silica into NR.
After the reinforcement of these functionalized and non-functionalized meso-porous
materials KIT-6 and SBA-15-S into natural rubber (NR) along with the curatives the thermal
and mechanical properties of these nanocomposites are determined.