Professional Documents
Culture Documents
Cao-Su-Hoa-Hoc-Va-Cong-Nghe - Rubber-Curing - (Cuuduongthancong - Com)
Cao-Su-Hoa-Hoc-Va-Cong-Nghe - Rubber-Curing - (Cuuduongthancong - Com)
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Rubber Curing
Systems th
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• Over the years three special types of cure
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systems have been developed. They are:
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• efficient vulcanisation (EV) systems,
ng
co
• semi-efficient vulcanisation (SEV)
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systems and
th
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• conventional vulcanisation (CV) systems.
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The levels of accelerator and sulfur in CV,
SEV and EV systems are shown in Table 1
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Measuring Cure
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The curve exhibits a number of features
which are used to compare cure:
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- Maximum torque MH.
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- tS2, T2 or T5 : there is a delay or
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induction time before the torque or
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resistance value begins to rise.
th
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- T90 : is the time for the torque to
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increase to:
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90/100(MH − ML)+ ML
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Cure rate: A rise in the value of torque
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with time, the slope of the curve, gives
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the measure of cure rate. Sometimes cure
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rates of various cure systems are
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compared with T90−ts2 data
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Test Equipment and Conditions
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• Cure characteristics were determined
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using an MDR 2000EA rheometer.
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• Test specimens were vulcanised by
an
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compression molding at temperatures and
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times indicated.
o
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according to ISO 37
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• tear strength according to ISO 34/1.
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• DIN abrasion ISO 4649.
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• fatigue to failure ASTM 4482/85.
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• hardness according to ISO 48.
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• Ageing of the test specimens was carried
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out in a ventilated air oven at 100 C for 3
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• Heat build up and permanent set after dynamic
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loading were determined using a Goodrich
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Flexometer (Load 11 kg or 22 kg; stroke 0.445
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cm, frequency 30 Hz, start temperature 100 C)
according to ISO 4666/3-1982.
th
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• Dynamic mechanical analysis was carried out
o
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2231.
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• Vulcanisate network structure was
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determined by equilibrium swelling in
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toluene using the method reported by Ellis
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and Welding. The volume fraction
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• (Vr) obtained was converted into the
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crosslinks.
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• The proportions of mono-, di-, and
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polysulfidic crosslinks in the vulcanisates
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were determined using thiol amine
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chemical probes.
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an
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• Following the cleavage of the poly- and
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disulfidic crosslinks, the samples were
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characteristics were determined according
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to ASTM 2229-85.
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Curing Systems
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Curing systems can be classified into four
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categories.
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Sulfur Curing Systems
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Accelerators
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Accelerators may be classified in several
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ways:
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(a) inorganic or organic
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(b) acidic or basic
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Functionally, accelerators can also be
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classified into two broad categories:
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Primary accelerators:
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Primary accelerators are mercapto based
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accelerators, generally efficient and confer
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good processing safety to the rubber
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compounds, exhibiting a broad vulcanisation
an
th
plateau with relatively low crosslink density.
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• Secondary accelerators:
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Some rubber compounds use only one
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accelerator but most contain two, a primary at
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about 1 phr and a secondary (or booster) at
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0.1 to 0.5 phr.
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These combinations cause faster vulcanisation
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• NR and SBR compounds with MBTS/DPG
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as the control. The secondary accelerators
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also change the network structures. The
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polysulfidic crosslinks are converted to
th
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monosulfidic exhibiting heat stability.
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Sulfur Donors
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• Aside from the sulfur itself, sulfur bearing
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compounds that liberate sulfur at the
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vulcanisation temperature can be used as
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vulcanising agents.
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Cures for Speciality Elastomers
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• The curing systems used to vulcanise
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speciality elastomers such as EPDM, CR,
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IIR and NBR are different than those used
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to cure NR, SBR, BR and its blends
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• The former elastomers are less
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Cure Systems for EPDM
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Cure Systems for Nitrile
Rubber
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• Cure systems for nitrile rubber are
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somewhat analogous to those of NR, SBR
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or BR except that magnesium carbonate
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(MC) treated sulfur is usually used to aid
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sulphur dispersion into the polymer.
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Cure Systems for
Polychloroprene
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• CR can be vulcanised in the presence of
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zinc oxide alone, but magnesium oxide is
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necessary to confer scorch resistance.
an
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• Along with the metal oxides, TMTD, DOTG
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and sulfur are used. This is a good
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dimensional stability.
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Cure Systems for Butyl and
Halobutyl Rubber
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• The low degree of unsaturation
.c
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requires the use of ultra accelerators,
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such as thiuram or dithiocarbamate.
an
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Phenolic resins, bisazoformates , and
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quinone derivatives can also be employed.
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• Sulfur crosslinks have limited stability at
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elevated temperatures and can rearrange
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to form new crosslinks.
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• Resin cure systems provide C-C crosslinks
th
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and heat stability.
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Halobutyl Rubber
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Peroxide Cure Systems
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Peroxide Vulcanisation of
EPDM
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• Peroxide vulcanisation of EPDM is growing
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in popularity because of enhanced ageing
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resistance.
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• A comparison of sulfur and peroxide cure
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systems for EPDM is shown in Table 32 .
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• Apart from peroxide type and the amount
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of peroxide incorporated in compounds,
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the efficiency of crosslinking depends on
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coagents.
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• The commercially important ones are:
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- Maleimide type: N,N -phenyl maleimide
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- Allylic type: triallyl cyanurate (TAC)
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triallyl isocyanurate (TAIC)
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- Methacrylate type: zinc dimethacrylate
th
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- Acrylate type: ethylene glycol diacrylate
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zinc diacrylate
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polybutadiene resin
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Sulfur Free Curing Systems
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Some special vulcanising agents can cure
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diene rubbers such as NR, SBR and BR.
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Phenolic Curatives,
Benzoquinone
Derivatives and Bismaleimides
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• Diene rubbers can be vulcanised by the
co
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action of phenolic compounds like phenol-
th
formaldehyde resin (5-10 phr). Resin
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cured NR offers good set properties
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• Resin curing of SBR and BR imparts
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excellent cut growth and abrasion
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resistance.
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• Resin cured nitrile rubber shows high
th
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fatigue life and high relaxation.
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A high diene rubber can also be vulcanised
ng
by the action of a dinitrosobenzene, made in
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situ by the oxidation of a quinonedioxime
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Vulcanisation by Triazine
Accelerators
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• The triazine accelerators are more
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effective than the thiazole accelerators
co
and produce highly reversion resistant
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vulcanisates.
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Urethane Crosslinkers
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• Natural rubber can be crosslinked by a blocked
.c
diphenyl methane diisocyanate to produce
ng
urethane crosslinks.
co
• The crosslinking agent dissociates into two
an
th
quinonedioxime molecules and one diphenyl
ng
methane diisocyanate.
o
•
du
group.
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Other Crosslinking Agents
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• There exist a considerable number of
.c
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compounds containing labile chlorine
co
which bring about sulfurless vulcanisation
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at levels of approximately 3 phr.
th
ng
• Basic chemicals such as lead oxides and
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New Developments
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• Maintaining properties and performance
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throughout a rubber product’s service life
co
is directly related to maintaining the
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integrity of the vulcanisate structure under
th
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both thermal and thermal oxidative
o
conditions.
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• Two additives have allowed compounders
.c
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to forget this compromise, namely
co
hexamethylene-1,6-bisthiosulfate (HTS), a
an
post vulcanisation stabiliser and 1,3-
th
ng
bis(citraconimidomethyl) benzene (BCI-
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Some Practical Examples with
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Varying Cure Systems
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Tyres
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Tread
Steel belts
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Carcass plies
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Black sidewall
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Inner liner
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Apex Veneer coverstrip
th
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Bead
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White sidewall
Chafer
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Rim cushion
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Tread
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• Trying to balance the three main
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apparently conflicting needs of wear, wet
ng
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grip and rolling resistance
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• The cure system should be CV/SEV.
th
Accelerators used are sulfenamide class
ng
(TBBS, CBS, MBS).
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RADIAL TRUCK TREAD FORMULATION
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Ingredients phr
.c
NR 100
ng
ZnO 5
co
Stearic acid 2
an
TBBS 1.5
Sulfur
th 1.5
ng
N-234 55
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Aromatic oil 8
6 PPD 2
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TMQ 1.5
PVI 0.1
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Perkalink 900
om
• Perkalink 900 is an antireversion agent
.c
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which provides long term heat stability in
co
sulfur vulcanized compounds by
an
substituting stable, flexible carbon-carbon
th
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crosslinks for the sulfur crosslinks that are
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• Silica as a reinforcing filler is being used
om
more extensively in the tyre industry to
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provide improved tear resistance and
ng
decreased rolling resistance.
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• In order to maximise these benefits the
an
silane coupling agent bis-(3-
th
ng
triethoxysilylpropyl) tetrasulfide (TESPT) is
o
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often employed.
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• A passenger tread containing silica needs a
.c
ng
cure system based on sulfenamide/sulfur
co
(SEV/CV system) and guanidine activators
an
(DPG).
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Aircraft tread requires a high modulus, better
abrasion resistance and low heat generation.
om
The above requirements could be satisfied by using
.c
a CV/SEV cure system with DCBS as accelerator
ng
and insoluble sulfur (IS) as crosslinker.
co
an
th
For achieving high modulus, HMT and a resorcinol
ng
system is used.
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Tread Base or Sub Tread
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• A natural rubber rich undertread layer can
.c
ng
enhance the adhesion between belt or
co
cap-ply and tread.
an
• The cure system needs better flexibility
th
ng
and low heat generation. Typically the
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Belts
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• In radial tyres, sets of belts or breakers made
.c
ng
from brass coated steel cords are layed at
co
alternate bias angles.
an
• to provide a trellising effect, to stiffen the area
th
under the tread and also to prevent growth
ng
under inflation or high speed rotation.
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• The design of the belt package should
om
give a smooth ride with minimum energy
.c
loss, but with sufficient stiffness to
ng
prevent undue movement within the
co
contact area causing irregular or rapid tyre
an
wear.
th
ng
• The cure package is composed of a slow
o
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.c
ng
1,6- bis(thiosulfate), disodium salt dihydrate)
co
improves adhesion characteristics under
an
ageing environments.
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Sidewall
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• Sidewall compounds cover the thinnest
.c
ng
part of the tyre where most flexing occurs
co
as the tyre deflects.
an
• They therefore need to have a high
th
ng
degree of flex resistance and good
o
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age resistance.
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• Sidewall compounds contain additional
om
ingredients to prevent oxidative or ozone
.c
attack since this part of the tyre will be
ng
particularly exposed to the sun and the
co
an
elements.
th
• The cure system should be CV or between
o ng
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CV/SEV.
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Carcass
om
• The cure system of choice for a carcass
.c
ng
compound is based on a scorch resistant
co
cure package.
an
• thermally stable, insoluble sulfur and
th
ng
bloom resistant adhesion additives are
o
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required.
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• the cure system suitable for this
.c
ng
application is based on a slow accelerator
co
such as DCBS with a high amount of
an
insoluble sulfur (generally 4-5 phr).
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Bead
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• require high modulus and good adhesion
.c
ng
to steel wires.
co
• High modulus is achieved by using
an
th
resorcinol/HMMM or phenol formaldehyde
ng
resins.
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Apex
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• The apex components provide the gradual
.c
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shape and stiffness reduction from the
co
rigid bead coil to the flexible mid-sidewall
an
of the tyre.
th
ng
• These components need to be very hard
o
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component endings.
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Cap-Ply
om
• act as a barrier layer between the tread and the
.c
casing to restrict migration of chemicals from
ng
the tread into the belt.
co
• requires high modulus and good adhesion
an
th
behaviour. ng
• The cure system used to achieve the target
o
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om
.c
ng
co
an
th
o ng
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Inner Liner
om
• Zinc oxide with MBTS and a small amount
.c
ng
of sulfur is used to crosslink halobutyl
co
rubber.
an
th
o ng
du
u
cu
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om
.c
ng
co
an
th
o ng
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Industrial Rubber Products
om
.c
ng
co
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th
o ng
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Conveyor Belt Cover - NR
om
• flex resistance, abrasion resistance and low
.c
heat build up.
ng
co
• In order to achieve better flex resistance, a
an
conventional cure package is recommended
th
(however, such a system suffers from the
o ng
adverse effects of heat generation).
du
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om
.c
ng
co
an
th
o ng
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om
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ng
co
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• The antireversion agent has no effect on
om
scorch resistance and time to optimum cure.
.c
• The compound containing the antireversion
ng
agent maintains a torque level close to the
co
maximum.
an
th
• The antireversion effect is also evident in the
o ng
stability of vulcanisate properties following
du
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.c
ng
co
an
th
o ng
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om
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Engine Mount - NR
om
• The essential performance properties for an
.c
engine mount are low heat build up and low
ng
dynamic compression set.
co
• a cure system comprising of sulfenamide
an
•
th
(moderate loading, 1.2-1.7 phr) with sulfur (2-
ng
2.5 phr) is recommended.
o
•
du
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om
• In spite of this modified cure system
.c
(CBS/TMTD/S), the properties are still not
ng
co
optimum, particularly with regard to heat
an
build up.
th
• The addition of an antireversion agent
ng
might provide advantage and with this in
o
du
studied.
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ng
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Tank Pad – NR/SBR/BR Blend
om
• The required properties for a tank pad are heat
.c
ng
stability, low heat generation, improved flex and
co
good compression set.
an
• This can be achieved by selecting a cure
th
package between SEV and towards an EV cure.A
ng
combination of a sulfenamide with a thiazole is
o
du
suitable.
u
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om
• The sulfur loading is generally high to
.c
address the improved flex requirements.
ng
co
• Because of high sulfur loadings, the
an
system suffers from the adverse effects of
heat and reversion resistance. th
ng
• Perkalink 900 is active in compounds
o
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om
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ng
co
an
th
o ng
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o ng
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o ng
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Oil Seal - NBR
om
• The general requirement for oil seal applications is
.c
ng
oil resistance, low compression set, high elongation
co
and good heat stability.
an
• In order to achieve this, a cure system comprising
th
of MBTS/TMTD and sulfur is preferred.
ng
•
o
TMTD is used in a small amount so that
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om
• In order to keep high elongation, the amount
.c
ng
of sulfur should not be too low.
co
• Compression can be negatively affected if
an
th
the sulfur loading is too high.
ng
• The heat stability can be improved by
o
du
Perkalink 900.
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Concluding Remarks
om
• Cure systems play an important role in
.c
ng
achieving the performance requirements
co
of rubber articles.
an
• Antireversion chemicals constitute a class
th
ng
of such materials, and can improve service
o
du
performance.
u
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• Cure systems, however, paint only part of
om
the picture with regard to the manufacture
.c
of rubber articles.
ng
• polymers and fillers are equally important
co
in meeting performance requirements.
an
th
• In addition, compound mixing and
o ng
processing play a critical role in
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