Investigation of aluminahydrate as a fire retardant in silica filled rubber floor-tiles. 1 A research project thesis submitted in partial fulfillment of the degree of Master of Science in Polymer Technology. B y Kama! Asoka Rajapaksha. • 'ijSfjrV Of M0.RATUWA, m W •• M Polymer Technology Division, Department of Chemical Engineering, University of Moratuwa, Sri Lanka. September 2004. Univers i ty of M o r a t u w a 82709 S 2 7 0 9 Th c c Is 67709 D E C L A R A T I O N I h e r e b y d e c l a r e tha t th i s s u b m i s s i o n is a resu l t o f a w o r k c a r r i e d ou t by m e a n d to t h e b e s t o f m y k n o w l e d g e . It c o n t a i n s n o m a t e r i a l p r e v i o u s l y w r i t t e n o r p u b l i s h e d b y a n o t h e r p e r s o n n o r m a t e r i a l w h i c h h a s b e e n a c c e p t e d f o r t h e a w a r d o f a n y d e g r e e o r a c c e p t a b l e q u a l i f i c a t i o n o f a Un i ve rs i t y , o r o t h e r i ns t i t u te o f h i g h e r l e a r n i n g , e x c e p t w h e r e t h e r e f e r e n c e t o t h e m a t e r i a l is m a d e . I K A R a j a p a k s h a S e p t e m b e r 2 0 0 4 . i # n ACKNOWLEDGEMENT I a m g r a t e f u l t o m y s u p e r v i s o r s Mr. K. S u b r a m a n i u m ( M S c c o u r s e c o - o r d i n a t o r , s e n i o r lec tu re r , d e p a r t m e n t o f C h e m i c a l E n g i n e e r i n g ) a n d M r . S h a n t h i k o r a t o t a ( O p e r a t i o n a l D i r e c t o r K i n e t i c s (Pv t ) L t d . B i y a g a m a ) f o r t he i r g u i d a n c e , p a t i e n c e s h o w n t h r o u g h o u t t h e p ro jec t . M y e s p e c i a l t h a n k s t o Mr. S h a n t h i k o r a t o t a , f o r s u p p o r t i n g m e b y p r o v i d i n g a l l t h e r e q u i r e d m a t e r i a l s a n d fac i l i t i es . I w o u l d l i ke t o t h a n k a l l t h e d i v i s i o n a l m a n a g e r s a n d e x e c u t i v e s a n d l a b o r a t o r y s ta f f o f m y f i r m . k i n e t i c s ( P v t ) L t d . B i y a g a m a f o r t h e i r g r e a t s u p p o r t g i v e n t o m e in a l l m y e x p e r i m e n t a l w o r k s . M y s p e c i a l t h a n k s a r e d u e t o t h e f a c t o r y m a n a g e r a n d o t h e r s ta f f o f A r p i t a l i a n C o m p a c t S o l e s (Pv t ) L t d , B i y a g a m a , f o r t he i r a s s i s t a n c e in o f f e r i n g s o m e tes t r esu l t s o f m y e x p e r i m e n t a l w o r k s . I w o u l d a l s o l i ke t o t h a n k a l l t h e l i b ra ry m e m b e r s o f IT I ( f o r m e r C I S I R ) f o r p r o v i d i n g m e t h e r e q u i r e d fac i l i t i es w i t h o u t a n y res t r i c t i on . F i n a l l y m y t h a n k s a r e d u e t o m y p a r e n t s , f a m i l y m e m b e r s , a n d m y f r i e n d s fo r t he i r f u l l es t s u p p o r t g i v e n m e t o p r e p a r a t i o n o f t h i s t h e s i s . A B S T R A C T T h e f l a m e - r e t a r d a n t c h e m i c a l s , w h i c h c o m m e r c i a l l y f i n d a p p l i c a t i o n s in r u b b e r s , a r e c o n s i d e r e d t o b e t o x i c c h e m i c a l s , b e c a u s e o f t h e l i be ra t i on o f t he i r h a r m f u l vo la t i l e b y p r o d u c t s , w h e n r u b b e r s a r e o n f i re . F r o m t h e r e s e a r c h w o r k s in t h e r e c e n t p a s t it h a s b e e n e s t a b l i s h e d t ha t t h e • c h e m i c a l , a l u m i n a h y d r a t e is o n e o f t h e s a f e s t a n d e n v i r o n m e n t a l l y f r i e n d l y f l a m e r e t a r d a n t s . A s a resu l t , t h e a p p l i c a t i o n o f t h i s c h e m i c a l a s a f l a m e - r e t a r d a n t in r u b b e r s a n d p l a s t i c s is o n t h e r i se , a t p r e s e n t pa r t i cu l a r l y in t h e d e v e l o p e d w e s t e r n c o u n t r i e s . T h u s in v i e w o f u t i l i z i ng th i s c h e m i c a l in loca l i ndus t r i es , a s a f l a m e r e t a r d a n t e s p e c i a l l y in t h e s i l i ca f i l l e r a d d e d r u b b e r f l oo r - t i le c o m p o u n d s , a n a t t e m p t h a s b e e n m a d e in th i s w o r k , to e v a l u a t e t h e c h e m i c a l f o r i ts f i r e r e t a r d a n t p r o p e r t y in t he i r v u l c a n i z a t e s . T h e s t u d y r e v e a l s t ha t t o o b t a i n o p t i m u m f l a m e r e t a r d a n c e in t h e r u b b e r f l oo r t i les , t h e c o n v e n t i o n a l r u b b e r c o m p o u n d s c o n t a i n i n g 4 0 p h r p r e c i p i t a t e d s i l i ca s h o u l d b e i n c o r p o r a t e d w i t h a t l eas t 1 0 5 p h r o f a l u m i n a h y d r a t e in p l a c e o f 5 p h r o f t h e m i x t u r e o f c h l o r i n a t e d p a r a f f i n w a x a n d a n t i m o n y t r i ox ide . IV TABLE OF CONTENTS Page No Declaration ii A c k n o w l e d g e m e n t iii A b s t r a c t iv T a b l e o f C o n t e n t s v L is t o f f i g u r e s V i i L is t o f t a b l e s V i i i Chapter 1 - Introduction. 1.1 F l a m e s p r e a d i n g in r u b b e r a n d p r e v e n t i n g f i r e r e t a r d a n t s 2 1.2 A i m o f t h e p ro jec t 9 1.3 M e t h o d o f a p p r o a c h 9 1.4 H i s t o r i c a l r e v i e w o f p r e v e n t i o n o f f i r e 1 0 1.5 T h e p r e s e n t s i t u a t i o n o f f i r e a n d its p r e v e n t i o n 12 Chapter 2 - Experimental. 2.1 M a t e r i a l c h o s e n 14 2 .2 P r e p a r a t i o n o f r u b b e r c o m p o u n d s 2 0 2 . 3 P r o c e s s a b i l i t y t es t s 2 2 2 . 4 P h y s i c a l t e s t i n g o f v u l c a n i z a t e s 2 2 2 .4 .1 T e n s i l e p r o p e r t i e s 2 3 2 . 4 . 2 H a r d n e s s 2 5 2 .4 .3 A b r a s i o n r e s i s t a n c e 2 5 2 .5 M e t h o d s o f t e s t i n g f l a m e r e t a r d a n t p r o p e r t y o f a l u m i n a h y d r a t e a d d e d r u b b e r v u l c a n i z a t e s . 2 7 2 .5 .1 C o m b u s t i b i l i t y tes t i n c l i n e d at 4 5 ° a n g l e p o s i t i o n 2 7 2 .5 .2 C o m b u s t i b i l i t y tes t - in ve r t i ca l p o s i t i o n 2 9 2 . 5 . 3 C o m b u s t i b i l i t y tes t - i n h o r i z o n t a l p o s i t i o n 3 0 2 . 5 . 4 S m o k e m e a s u r e m e n t tes t 3 1 4 v s Chapter 3 - Test results - Tables 3.1 T e s t r esu l t s o f p r o c e s s a b i l i t y c h a r a c t e r i s t i c 3 5 3 .2 t o 3 .3 T e s t r e s u l t s o f p h y s i c a l tes t o f v u l c a n i z a t e s 3 6 3 .4 t o 3 .6 T e s t r esu l t s o f c o m b u s t i b i l i t y 3 8 3 .7 A s s e s s m e n t t es t r e s u l t s o f s m o k e d e n s i t y 4 1 3 .8 C l a s s e s o b t a i n e d f r o m tes t r esu l t s 4 2 % 3 .9 A S T M S t a n d a r d b u i l d i n g s 4 3 Test results - Graphs 3.1 G r a p h o f R h e o m e t e r c h a r a c t e r i s t i c s 3 4 3 .2 G r a p h o f p r o c s s a b i l i t y c h a r a c t e r i s t i c 4 4 3 .3 - 3 .4 G r a p h s o f p h y s i c a l tes t o f v u l c a n i z a t e s 4 5 3 . 5 - 3 . 7 G r a p h s o f c o m b u s t i b i l i t y 4 7 * 3 .8 G r a p h o f s m o k e d e n s i t y 5 0 Chapter 4 - Results and discussion. 4 .1 R e s u l t s a n d D i s c u s s i o n . 5 2 4 . 2 C o n c l u s i o n 5 9 4 . 3 F u r t h e r w o r k t o b e d o n e 6 0 4 . 4 A p p e n d i x 1 , 1 1 , 111 6 1 * 4 . 5 R e f e r e n c e s 6 7 4 VI \ L I S T O F F I G U R E S P a g e N o . F i g u r e 2 .1 S k e t c h f o r G o t e c h t e s t i n g M a c h i n e s I n c . - R h e o m e t e r t e s t e r 2 2 F i g u r e 2 . 2 S k e t c h f o r T e n s i l e s t r e n g t h tes t p i e c e s . 2 4 F i g u r e 2 . 3 D u r o m e t e r - R u b b e r h a r d n e s s tes te r . 2 5 F i g u r e 2 .4 D I N a b r a d e r - R u b b e r a b r a s i o n r e s i s t a n c e tes ter . 2 6 F i g u r e 2 .5 T h e tes t a p p a r a t u s f o r c o m b u s t i b l e t e s t s - s a m p l e p o s i t i o n e d 4 5 ° . 2 8 F i g u r e 2 . 6 T h e tes t a p p a r a t u s f o r c o m b u s t i b l e t e s t s - i n ve r t i ca l p o s i t i o n . 2 9 F i g u r e 2 .7 D e t e r m i n a t i o n o f r a te o f b u r n i n g h o r i z o n t a l - Lef t : F r o n t v i e w , R igh t : s i d e v i e w 3 0 F i g u r e 2 . 8 A r a p a h o e s m o k e b o x tes t a p p a r a t u s 3 1 F i g u r e 3.1 R h e o m e t e r g r a p h 3 4 F i g u r e 3 . 2 a T e s t e r e s u l t s - t e n s i l e s t r e n g t h 4 4 F i g u r e 3 . 2 b T e s t r e s u l t s - m o d u l u s at 3 0 0 % e l o n g a t i o n 4 4 F i g u r e 3 . 2 c T e s t r e s u l t s - e l o n g a t i o n a t b r e a k 4 4 F i g u r e 3 .3 H a r d n e s s tes t r e s u l t s 4 5 F i g u r e 3 .4 A b r a s i o n r e s i s t a n c e tes t r e s u l t s 4 6 F i g u r e 3 .5 R e s u l t s o f c o m b u s t i b i l i t y t e s t - 4 5 ° a n g l e 4 7 F i g u r e 3 .6 R e s u l t s o f c o m b u s t i b i l i t y tes t - ve r t i ca l p o s i t o n 4 8 F i g u r e 3 .7 R e s u l t s o f c o m b u s t i b i l i t y t es t - h o r i z o n t a l p o s i t o n 4 9 F i g u r e 3 .8 R e s u l t s o f s m o k e d e n s i t y 5 0 F i g u r e 4 . 1 a , b c o m p a r i s i o n o f t s 2 a n d t 9 0 w i t h w o r k i n g l imi t f o r d i f f e ren t f o r m u l a t i o n s 5 4 , 5 5 F i g u r e 4 . 1 c , d c o m p a r i s i o n o f M L a n d M H w i t h w o r k i n g l imi t f o r d i f f e ren t f o r m u l a t i o n s 5 5 , 5 6 VLT L i s t o f T a b l e s P a g e No . T a b l e 1.1 E s t i m a t e d c o n s u m p t i o n o f f i r e r e t a r d a n t s in t h e U S A in y e a r 2 0 0 0 . 12 T a b l e 2.1 F o r m u l a t i o n s fo r r u b b e r c o m p o u n d s . 21 T a b l e 3.1 R e s u l t s o f t e n s i l e s t r e n g t h , m o d u l u s a t 3 0 0 % a n d e l o n g a t i o n 35 T a b l e 3 .2 H a r d n e s s tes t r esu l t s 36 T a b l e 3 .3 A b r a s i o n r e s i s t a n c e tes t r esu l t s 37 T a b l e 3 .4 R e s u l t s o f c o m b u s t i b i l i t y t es ts - 4 5 ° p o s i t i o n 38 T a b l e 3 .5 R e s u l t s o f c o m b u s t i b i l i t y t e s t s - ve r t i ca l p o s i t i o n 39 T a b l e 3 .6 R e s u l t s o f c o m b u s t i b i l i t y t e s t s - h o r i z o n t a l p o s i t i o n 40 T a b l e 3.7 R e s u l t s o f s m o k e d e n s i t y 41 * T a b l e 3 .8 C l a s s e s o b t a i n e d f r o m t h e tes t r e s u l t s 42 T a b l e 3 .9 A S T M s t a n d a r d b u i l d i n g c o d e s 43 T a b l e 4 . 1 w o r k i n g l im i ts o f p r o c e s s i n g c h a r a c t e r i s t i c s 52 T a b l e 4 . 2 S t a n d a r d v a l u e s o f p h y s i c a l c h a r a c t e r i s t i c s r e q u i r e d fo r f l o o r t i l es 52 T a b l e 4 . 3 S t a n d a r d a n d m o d i f i e d r u b b e r f l o o r t i l e f o r m u l a t i o n s 53 T a b l e 4 . 4 R h e o m e t e r d a t a fo r p r e p a r e d r u b b e r c o m p o u n d m ix 54 v m