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7/26/2019 blend nr-br

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HEXAMETHYLENE-N,NBIS(TERT-BUTYL PEROXYCARBAMATE) AS ACROSSLINKING AGENT FOR NATURAL RUBER AND NATURAL

RUBBER/POLYBUTADIENE BLEND

D.S. OGUNNIYI*DEPARTMENT OF CHEMISTRY,

UNIVERSITY OF ILORIN,ILORIN, NIGERIA

And

C. HEPBURNINSTITUTE OF POLYMER TECHNOLOGY AND MATERIAL ENGINEERING

UNIVERSITY OF TECHNOLOGY,

LOUGHBOROUGH, LE11 3TU. UNITED KINGDOM.

ABSTRACT

The res!"s #$ "e%h!#'(%)! e)!)"(#& #$ he+)e"h-!e&eN,N/0(s"er"0"-!

2er#+-%)r0))"e HBTBP )s ) %r#ss!(&4(&' )'e&" $#r &)"r)! r00er )&5 &)"r)!

r00er62#!-0")5(e&e r00er 0!e&5 )re 2rese&"e5. S((!)r s"5(es 7ere %)rr(e5 #"

s(&' s!2hr )&5 2er#+(5e s-s"es )s %#&"r#!s. The %re %h)r)%"er(s"(%s 7ere

e)!)"e5 7("h "he M#&s)&"# Os%(!!)"(&' D(s% Rhe#e"er 7h(!e "e&s(!e shee"s 7ere

2re2)re5 )&5 s"resss"r)(& e)sree&"s (& s(2!e e+"e&s(#& 7ere se5 "#

%h)r)%"er(8e "he e%h)&(%)! 2r#2er"(es #$ "he !%)&(8e5 e!)s"#ers. I" 7)s $#&5 "h)"

"he 2r#2er"(es #0")(&e5 7("h "he )r(#s s-s"es 5e%re)se (& "he $#!!#7(&' #r5er9

s!2hr : 2er#+(5e : HBTBP. The %re e%h)&(s #$ HBTBP (& &)"r)! r00er )&5 "he

0!e&5 7)s e+2!)(&e5 )s #%%rr(&' "h#r#'h "he $ree r)5(%)! 2r#%ess.

Ke !"#d$% &)"r)! r00er, 2#!-0")5(e&e, 0!e&5, %r#ss!(&4(&'6!%)&(8)"(#&, HBTBP.*CORRESPONDING AUTHOR


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INTRODUCTION

A );#r )5)&%ee&" "# "he se #$ r00er 7)s "he 5(s%#er- #$ !%)&(8)"(#& 0-

Ch)r!es G##5-e)r (& "he U.S. (& 1


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0- 2er#+(5es. he& 5(e&e%#&")(&(&' r00ers )re %r#ss!(&4e5 0- 2er#+(5es, "he

2r#2er"(es #$ !%)&(8)"es #0")(&e5 )re (&$er(#r "# "h#se #$ !%)&(8)"es %re5 0-

s!2hr. Neer"he!ess, 2er#+(5e !%)&(8)"es #$ "hese 5(e&e r00ers, )&5 (&5ee5 #$

#"her r00ers )- 0e 5es(r)0!e (& )22!(%)"(#&s 7here %ree2 res(s")&%e (s re(re5.

Cr#ss!(&4(&' (s )!s# e$$e%"e5 0- r)5()"(#&, "he se #$ res(&s, e")! #+(5es )&5 #"her

(s%e!!)&e#s !%)&(8(&' )'e&"s. A#&' "he (s%e!!)&e#s !%)&(8(&' #r %r#ss!(&4(&'

s-s"es )re "he 0(s2er#+-%)r0))"es. He20r& re2#r"e5 "he se #$

0(s2er#+-%)r0))"es )s %r#ss!(&4(&' )'e&"s (& ' &)"r)! r00er. A!s#, "he se #$

HBTBP )s %r#ss!(&4(&' )'e&"s $#r $!#r#e!)s"#ers h)s 0ee& re2#r"e5 (& "he !("er)"re


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EXPERIMENTAL

M&'e#&$

The e!)s"#ers se5, &)"r)! r00er NR, SMR @ CV 2r#5%e5 0- M)!)-s()& N)"r)!

R00er )&5 cis2#!-0")5(e&e BR I&"e&e @ 2r#5%e5 0- E&(%he C#r2#r)"(#&, 7ere

#0")(&e5 $r# %#er%()! s#r%es. A!s#, #"her %#2#&5(&' (&'re5(e&"s 7ere s")&5)r5

)"er()!s se5 (& r00er $#r!)"(#&s )&5 7ere se5 (& %#2#&5(&' )s re%e(e5.

HBTBP 7)s 2re2)re5 )s 5es%r(0e5 (& "he !("er)"re 1?.

M M*n+

The (+(&' #$ "he )r(#s r00er 0)"%hes 7)s #& ) "7#r#!! (!! #$


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Ten$e S'#e$$-S'#&n Te$'$

The "e&s(!e s"resss"r)(& 2r#2er"(es #$ "he res!"(&' !%)&(8)"es 7ere 5e"er(&e5

)%%#r5(&' "# BS =3 P)r" A?, 1=1, s(&' T-2e ?, 500e!! s2e%(e&s.

O'e# 'e$'$

O"her "es"s (&%!5e5 "e)r s"re&'"h, 7h(%h 7)s 5e"er(&e5 )%%#r5(&' "# BS =3 2)r" A3,

1=


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%r(&'. As (" (s s)! 7("h HBTBP %res, "he %#2#&5s s" 0e %re5 !#&'er "h)& "=@

%re "(es "# e&sre "h)" "he %)r0#& 5(#+(5e e#!e5 5r(&' %re (s s$$(%(e&"!- )0s#r0e5

0- "he %)!%( h-5r#+(5e s-s"e. I" 7)s $r"her #0sere5 "h)" "he )+( "#re

)"")(&e5 (& "he NR6BR 0!e&5 7)s 're)"er "h)& 7he& NR 7)s se5 )!#&e (& )!! "he %r(&'

s-s"es. Th(s )- 0e 5e "# ) 2e%!()r("- #$ BR, 7h(%h &5er'#es s2#&")&e#s

%r#ss!(&4(&' 5r(&' !%)&(8)"(#&. I& s!2hr !%)&(8)"(#& s-s"es, BR re(res !ess

s!2hr "h)& #"her 5(e&e r00ers "# #0")(& "he #2"( %r#ss!(&4 5e&s("- 13.

P$.& P#"e#'e$ "0 1.&n2&'e$

The res!"s #$ 2h-s(%)! 2r#2er"(es #$ !%)&(8)"es 2re2)re5 $r# HBTPB %#2#&5s,

s!2hr %#2#&5s )&5 2er#+(5e %#2#&5s )re sh#7& (& T)0!es 1 ?. The 2h-s(%)!

2r#2er"(es #$ !%)&(8)"es %re5 7("h %#&e&"(#&)! %r#ss!(&4(&' )'e&"s 7ere 0e""er "h)&

"h#se #0")(&e5 $r# !%)&(8)"es %re5 7("h HBTBP. Fr"her %#2#&5(&' s"5(es 7("h

HBTBP 7#!5 0e &ee5e5 "# )4e ("s !%)&(8)"es %#2)r)0!e "# "h#se #0")(&e5 $r#

%#&e&"(#&)! %r#ss!(&4(&' s-s"es.

The )'e(&' #$ !%)&(8)"es 7)s %)rr(e5 #" &5er re!)"(e!- (!5 %#&5("(#&s ?> h#rs )"

1#C (& )(r %e!! #e& )&5 "he !%)&(8)"es se5 )s %#&"r#!s 7ere 2r#"e%"e5 7("h

)&"(#+(5)&" 7h(!e HBTBP%re5 s-s"es 7ere &2r#"e%"e5. I" 7)s $#&5 "h)" "he

re"e&"(#& #$ "e&s(!e 2r#2er"(es (& #s" HBTBP s-s"es 7)s 0e""er "h)& "h#se #$ "he

%#&"r#!s )$"er )'e(&'. Th(s )- 0e )& (&5(%)"(#& "h)" )(r#e& )'e(&' )- 0e se$! (&

(2r#(&' 2h-s(%)! 2r#2er"(es (& "h(s (&s")&%e. The %#2ress(#& se" $#r HBTBP%re5

!%)&(8)"es 7)s e+"ree!- 2##r, )s s)2!es 5(5 " sh#7 )&- re%#er-. Th(s

s''es"s "h)" "he %r#ss!(&4s #r('(&)!!- $#re5 7ere "her)!!- &s")0!e. H#7eer, "he

%#2ress(#& se" #$ HBTBP%re5 0!e&5 7)s 0e""er "h)& HBTBP%re5 &)"r)! r00er

!%)&(8)"es. The (2r#ee&" (& %#2ress(#& se" res(s")&%e )- 0e 5e "# "he

s2#&")&e#s %r#ss!(&4(&' #$ 2#!-0")5(e&e r00er. A!s#, $r"her %#2#&5(&' s"5(es


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7#!5 0e re(re5 "# (2r#e "he %#2ress(#& se" res(s")&%e #$ HBTBP%re5

!%)&(8)"es.

C#e Ce3$'#

De")(!e5 s"5(es #& %re %he(s"r- h)e " 0ee& %)rr(e5 #" (& "h(s 7#r4. H#7eer, NR

)&5 NR6BR !%)&(8)"es %re5 7("h HBTBP 7ere e+"r)%"e5 7("h h#" )%e"#&e )&5 )$"er

re#)! #$ s#!e&", "hese !%)&(8)"es 7ere "es"e5 $#r &("r#'e&. The e+"r)%"e5

!%)&(8)"es 7ere $#&5 "# %#&")(& &("r#'e&. Th(s s''es"s "h)" &("r#'e&, 2r#0)0!- $r#

)( 'r#2s, (s )"")%he5 "# "he 2#!-er )(& %h)(& #$ "he e!)s"#ers. Th(s $(&5(&' (s

s((!)r "# "h)" #$ He20r& 7h# 2r#2#se5 ) $ree r)5(%)! e%h)&(s $#r "he

%r#ss!(&4(&' #$ ' &)"r)! r00er 0- 0(s2er#+-%)r0))"es. I& "h(s e%h)&(s, (" 7)s

2r#2#se5 "h)" "he 0(s2er#+-%)r0))"e 5e%#2#ses h##!-"(%)!!- )s "he (&("()"#r

5e%#2#ses, "he $ree r)5(%)!s $#re5 )0s"r)%" h-5r#'e& $r# "he e"h-!e&e 'r#2s

)!#&' "he 2#!-er %h)(&, )&5 "he res!")&" 2#!-er r)5(%)!s (&"er)%", 5(re%"!- #r "hr#'h

"he (&"ere5()r- #$ r)5(%)! "r)2s "# $#r %r#ss!(&4s. I" 7)s )!s# s''es"e5 "h)" 0#"h

$!e+(0!e %r#ss!(&4s )&5 %)r0#&%)r0#& %r#ss!(&4s )re $#re5 $r# "he (&"er)%"(#& #$

2#!-er r)5(%)!s. The s)e e%h)&(s )s 2r#2#se5 0- He20r& , (s "h#'h" "#

)22!- (& "he 2rese&" 7#r4 7here HBTBP (s se5 )s %r#ss!(&4(&' )'e&" $#r $(!!e5 NR )&5

NR6BR %#2#&5s.

C"n.$"n

Th(s 7#r4 h)s es")0!(she5 "h)" HBTBP (s %)2)0!e #$ %r(&' $(!!e5 &)"r)! r00er )&5

&)"r)! r00er62#!-0")5(e&e %#2#&5s. A!"h#'h "he 2h-s(%)! 2r#2er"(es #$

!%)&(8)"es %re5 0- %#&e&"(#&)! %r#ss!(&4(&' s-s"es 7ere $#&5 "# 0e 0e""er "h)&

!%)&(8)"es %re5 0- HBTBP, HBTBP%re5 !%)&(8)"es "e&5 "# h)e '##5 re"e&"(#&

#$ 2r#2er"(es #& he)" )'e(&'. The e%h)&(s #$ %r#ss!(&4(&' #$ NR )&5 NR6BR (s


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2r#2#se5 "# #%%r "hr#'h h##!-"(% 5e%#2#s("(#& #$ HBTBP, (&"er)%"(#& #$ r)5(%)!s

7("h r00er, (&"er)%"(#& #$ "he res!")&" r00er r)5(%)!s, 5(re%"!- #r "hr#'h "he

(&"ere5()r- #$ r)5(%)! "r)2s )&5 s0see&" $#r)"(#& #$ %r#ss!(&4s.


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Re0e#en.e$

1. H#$$)&&, ., V!%)&(8)"(#& )&5 V!%)&(8(&' A'e&"s M)%!)re&, L#&5#&, E&'!)&5.

1=.

?. S;#"h&, I.J. )&5 A!!('er, G. (& V!%)&(8)"(#& #$ E!)s"#ers, I.J. S;#"h& )&5 G.

A!!('er E5s. R#0er" E. Fr(e'er P0!(sh(&' C#2)&-, H&"(&'"#&, Ne7 Y#r4. 1=3 >@1, ?1

. He20r&, C., B(s2er#+-%)r0))"es9 !%)&(8s(&' )'e&"s "h)" 2#ssess 0#&5

)&"(#+(5)&" 2r#2er"(es R00. #r!5 567 >=, 1=

3, ?


10/12

1?. Pe5erse&, C.J., Pre2)r)"(#& )&5 Pr#2er"(es #$ es"ers #$ Ns0s"(""e5

2er#+-%)r0)(% )%(5s J.Or'. Che.


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T)0!e 19 C#2)r(s#& #$ 2h-s(%)! 2r#2er"(es #$ NR !%)&(8)"es #0")(&e5 s(&' HBTBP%r#ss!(&4(&' )'e&" )&5 %#&"r#!s

S!2hr 2hr Per#+(5e 2hr HBTBP 2hr

NR SMR @ CV 1. 1. 1.

&O @. @. C)O >.

C)OH? .

S"e)r(% A%(5 ?.

SRF B!)%4 N? 3. 3 3

C#)r#&e Res(& @.

CBS ?.

F!e%"#! H 1. .@

S!2hr 1.@

D(%2 >C 1.@

HBTBP .

M##&e- S%#r%h )" 1?#C > (&s : > (&s ? (&s

Cre C#&5("(#&s (&s6#C =61 1>61 161@

U&)'e5 Pr#2er"(es

Te&s(!e S"re&'"h M2) ?3.@> 1.3 >.=

3 M#5!s M2) @.1? 1.< >.

E!#&')"(#&)"0re)4 @?@ 3@

Te)r S"re&'"h 4N6 3 ?.=3 h#rs )" 1 #C?@ s"r)(&

> 3?

Re"e&"(#& #$ Te&s(!e S"re&'"h =?

T)0!e ?9 C#2)r(s#& #$ 2h-s(%)! 2r#2er"(es #$ NR6BR !%)&(8)"es #0")(&e5 s(&'


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HBTBP %r#ss!(&4(&' )'e&" )&5 %#&"r#!s

S!2hr 2hr Per#+(5e 2hr HBTBP 2hr

NR SMR @ CV @. @. @.

BR I&"e&e @ @. @. @.

&O @. @. C)O >.

C)OH? .

S"e)r(% A%(5 ?.

SRF B!)%4 N? 3. 3 3

C#)r#&e Res(& @.

CBS ?.

F!e%"#! H 1. .@

S!2hr 1.@

D(%2 >C 1.3

HBTBP .

M##&e- S%#r%h )" 1?#C >@ (&s : >@ (&s ? (&s

Cre C#&5("(#&s (&s6#C 1?61 1?61 161@

U&)'e5 Pr#2er"(es

Te&s(!e S"re&'"h M2) 1>.31 .3@ >.3=

3 M#5!s M2) .< 3.= 3.1 h#rs )" 1 # C

Te&s(!e S"re&'"h M2) =.= @.>< >.?

3 M#5!s M2) .31 3. ?.1

E!#&')"(#&)"0re)4 3@ 3@ >?@

Te)r S"re&'"h 4N6 1=

C#2ress(#& Se" ?> h#rs )" 1 #C?@ s"r)(&

3 1 @3

Re"e&"(#& #$ Te&s(!e S"re&'"h =

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