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HIGH-PURITY ETHYLHEXYL-ACRYLATEANDPREPARATION METHODUSING THE Dec. 2 9 , 2010 (KR) . . . . . . . . . . . . . . . . . . . . . . 10-2010-0138235SAME P u b l i c a t i o n C l a s s i ? c a t i o n( 7 1 ) A p p l i c a n t s z S u n g Kyu E E , D a e j e o n ( K R ) ; J o o nHo S H I N , D a e j e o n ( K R ) ; J o n g Ku ( 5 1 ) I n t - C lL E E , D a e j e o n ( K R ) ; S u n g Kyun KIM, C07C 7 / 5 4 ( 2 0 0 6 - 0 1 )D a e j e o n ( K R ) B01D / 1 4 ( 2 0 0 6 . 0 1 )

( 5 2 ) US. C l .( 7 2 ) I n v e n t o r s : Sung Kyu LEE, Daejeon K R ) ; Joon CPC . . . . . . . . . . . . . . . C 0 7 C 7 / 5 4 ( 2 0 1 3 . 0 1 ) ; B 0 1 D 3 / 1 4 1Ho S H I N , D a e j e o n ( K R ) ; J o n g Ku ( 2 0 1 3 . 0 1 )LEE, Daejeon K R ) ; Sung Kyun KIM, USPC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 0 3 / 9 9 ; 2 0 2 / 1 5 8D a e j e o n ( K R ) ( 5 7 ) ABSTRACT( 7 3 ) A s s l g n e e : LG CHEM LTD S e o u l ( K R ) The p r e s e n t i n v e n t i o n r e l a t e s t o a d i v i d i n g W a l l c o l u m n f o r

_ p r e p a r i n g h i g h - p u r i t y 2 - e t h y l h e X y l - a c r y l a t e , and a method( 2 1 ) A p p l ' NO 1 3 / 9 2 9 5 2 0 f o r d i s t i l l i n g 2 - e t h y l h e X y l - a c r y l a t e . T h e i v i d i n g W a l l c o l u m n_ of h e present invention provides an f f e c t having tWo d i s t i l( 2 2 ) F l l e d ' J u n ' 2 7 2 0 1 3 l a t i o n c o l u m n s t h r o u g h o n e d i s t i l l a t i o n c o l u m n , t h e r e b y h a v

R e l a t e d U A p p l i c a t i o n Data i n g a n e f f e c t o f e d u c i n g e n e r g y compared o t h e c o n v e n t i o n a lp r o c e s s i n g d e v i c e i n p r e p a r i n g h i g h - p u r i t y 2 - e t h y l h e x y l( 6 3 ) C o n t i n u a t i o n o f a p p l i c a t i o n N o . PCT/KR2011/ a c r y l a t e a n d a n e f f e c t o f r e d u c i n g e q u i p m e n t c o s t s o f t h e

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US 2013/0284586 A 1

DIVIDINGWALL COLUMN OR PREPARINGHIGH-PURITY ETHYLHEXYL-ACRYLATEAND PREPARATIONMETHOD SING THE

SAMETECHNICAL FIELD

[ 0 0 0 1 ] The r e s e n t i n v e n t i o n r e l a t e s t o a d i v i d i n g W a l l c o lumn o r p r e p a r i n g h i g h - p u r i t y 2 - e t h y l h e x y l - a c r y l a t e ( E H A )and a p r e p a r a t i o n method s i n g t h e s a m e .

BACKGROUND ART[ 0 0 0 2 ] Since v a r i o u s raW m a t e r i a l s such a s crude o i l a r et y p i c a l l y m i x t u r e s o f many compounds i n many ases, s u c hv a r i o u s raW a t e r i a l s a r e o f t e n u s e d a f t e r b e i n g s e p a r a t e d i n t oc o m p o u n d s , i n s t e a d o f i r e c t l y i n d u s t r i a l l y u s e d . A e p r e s e nt a t i v e p r o c e s s from among h e m i c a l p r o c e s s e s f o r s e p a r a t i n ga mixture s a d i s t i l l a t i o n p r o c e s s . I n g e n e r a l , s i n c e a d i s t i l l at i o n p r o c e s s s e p a r a t e s a raW m a t e r i a l i n t o a h i g h b o i l i n gcomponent n d a loW o i l i n g c o m p o n e n t , When h e number fcomponents o f a m i x t u r e t o be s e p a r a t e d i s n , t h e number fd i s t i l l a t i o n c o l u m n s s n - l Which s o b t a i n e d by u b t r a c t i n g 1from t h e number ( n ) . T h a t i s , a p r o c e s s f o r s e p a r a t i n g ah i g h - p u r i t y p r o d u c t from c r u d e raW a t e r i a l i n t h e convent i o n a l d i s t i l l a t i o n i n d u s t r y m o s t l y u s e s a s t r u c t u r e i n Which 2d i s t i l l a t i o n c o l u m n s a r e c o n t i n u o u s l y a r r a n g e d .[ 0 0 0 3 ] A s shoWn n F I G . 1 , a c o n v e n t i o n a l d i s t i l l a t i o n p r oc e s s u s e s a 2-column method of s e p a r a t i n g a loW b o i l i n gcomponent D n a ? r s t column 1 1 , a n d s e p a r a t i n g a mediumb o i l i n g component S a n d a h i g h b o i l i n g component B i n as e c o n d column 2 1 .[ 0 0 0 4 ] A o m p o s i t i o n p r o ? l e i n a ? r s t column n a convent i o n a l 2 column i s t i l l a t i o n method Which s a t y p i c a l p r o c e s so f i s t i l l i n g a l c o h o l s i s shoWn n F I G . 2 . A s shoWn n F I G . 2 ,t h e medium o i l i n g component B s g e n e r a l l y r e - m i x e d i n al o W e r p a r t o f t h e ? r s t c o l u m n . I n p a r t i c u l a r , When 2 - e t h y lh e x y l - a c r y l a t e (EHA) s s e p a r a t e d a s a medium o i l i n g comp o n e n t , a c o m p o s i t i o n p r o ? l e i n t h e ? r s t column s shoWn nF I G . 3 . As shoWn n F I G . 3 , e v e n When - e t h y l h e x y l - a c r y l a t ei s u s e d , i t can be s e e n t h a t a r e - m i x i n g phenomenon c c u r s i na l o W e r p a r t of h e ? r s t column.[ 0 0 0 5 ] A l t h o u g h t h e c o n v e n t i o n a l d i s t i l l a t i o n p r o c e s s maye a s i l y c o n t r o l a c o m p o s i ti o n o f a p r o d u c t , t h e c o n v e n t i o n a ld i s t i l l a t i o n p r o c e s s h a s p r o b l e m s i n t h a t a medium b o i l i n gcomponent s r e - m i x e d and i l u t e d i n a ? r s t d i s t i l l a t i o n c o lumn. T h i s r e m i x i n g e f f e c t l e a d s t o a d d i t i o n a l l y u n n e c e s s a r ye n e r g y c o n s u m p t i o n s b e c a u s e o f a t h e r m a l i n e f ? c i e n c y .[ 0 0 0 6 ] I n o r d e r o s o l v e t h e s e p r o b l e m s , many t u d i e s h a v ebeen done on a neW i s t i l l a t i o n s t r u c t u r e . A e p r e s e n t a t i v ea t t e m p t t o i m p r o v e s e p a r a t i o n e ? i c i en c y t h r o u g h a t h e r m a l l ycoupled t r u c t u r e i s a P e t l y u k d i s t i l l a t i o n column t r u c t u r e a sshoWn i n F I G . 4 . A e t l y u k d i s t i l l a t i o n column i n c l u d e s ap r e - f r a c t i o n a t o r 1 2 and a main column 22 Which a r e t h e rm a l l y c o u p l e d t o e a c h o t h e r s u c h t h a t a l o W b o i l i n g compon e n t a n d a h i g h b o i l i n g component a r e ? rs t s e p a r a t e d i n t h ep r e - f r a c t i o n a t o r 1 2 , a n d t h e n a t o p p o r t i o n and a b o t t o mp o r t i o n o f t h e p r e - f r a c t i o n a t o r 1 2 a r e r e s p e c t i v e l y l o a d e d n t oin?oW l a t e s o f t h e main column 2 2 , and loW o i l i n g comp o n e n t D , a medium o i l i n g c o m p o n e n t S , a n d a h i g h b o i l i n gcomponent B a r e s e p a r a t e d from one a n o t h e r i n t h e maincolumn 2 . I n t h e P e t l y u k i s t i l l a t i o n column t r u c t u r e , s i n c ea d i s t i l l a t i o n c u r v e i n t h e P e t l y u k d i s t i l l a t i o n column s s i m il a r t o a n e q u i l i b r i u m d i s t i l l a t i o n c u r v e , e n e r g y e f ? c i e n c y i sh i g h . H o W e v e r , i t i s n o t e a s y t o d e s i g n a p r o c e s s and p e r a t e

O c t . 3 1 , 2 0 1 3

t h e P e t l y u k d i s t i l l a t i o n c o l u m n , a n d t i s p a r t i c u l a r l y d i f ? c u l tt o b a l a n c e a p r e s s u r e i n t h e P e t l y u k d i s t i l l a t i o n c o l u m n .

DISCLOSURET e c h n i c a l Problem

[ 0 0 0 7 ] The p r e s e n t i n v e n t i o n i s d i r e c t e d t o p r o v i d i n g ad i v i d i n g W a l l c o l u m n o r p r e p a r i n g h i g h - p u r i t y 2 - e t h y l h e x y la c r y l a t e (EHA) a n d a p r e p a r a t i o n method s i n g t h e s a m e .

T e c h n i c a l S o l u t i o n[ 0 0 0 8 ] One s p e c t o f h e p r e s e n t i n v e n t i o n p r o v i d e s a d i v i di n g W a l l column i n c l u d i n g a main column i n c l u d i n g : a cond e n s e r ; a r e b o i l e r ; and a d i v i d i n g W a l l , W h e r e i n t h e maincolumn s divided i n t o a t o p Z o n e , an upper in?oW Z o n e , anupper out?oW Z o n e , a loWer in?oW Z o n e , a loWer out?oWZ o n e , and a bottom Z o n e , and i n c l u d e s a t l e a s t one in?oWs t r e a m and t l e a s t t h r e e out?oW s t r e a m s , Wherein a c h of h ea t l e a s t one in?oW stream s a stream t h a t a feed c o n t a i n i n gc r u d e 2 - e t h y l h e x y l - a c r y l a t e (EHA) ?oWs i n t o a n in?oWm i d d l e p l a t e Where t h e upper in?oW Zone and t h e l o W e rin?oW Zone of h e main column o n t a c t each t h e r , and one rmore of t h e out?oW s t r e a m s i s a stream of 2 - e t h y l h e x y la c r y l a t e , a n d a m e t h o d o f r e p a r i n g i g h - p u r i t y 2 - e t h y l h e x y la c r y l a t e u s i n g t h e d i v i d i n g W a l l c o l u m n .

A d v a n t a g e o u s E f f e c t s[ 0 0 0 9 ] A i v i d i n g W a l l c o l u m n a c c o r d i n g t o t h e p r e s e n ti n v e n t i o n ma y p r o v i d e a n e f f e c t o f h a v i n g tWo d i s t i l l a t i o ncolumns u s i n g o n e d i s t i l l a t i o n c o l u m n , and may r e d u c ee n e r g y c o n s u m p t i o n a n d e q u i p m e n t c o s t s When o m p a r e d oa c o n v e n t i o n a l p r o c e s s a p p a r a t u s f o r p r e p a r i n g h i g h - p u r i t y2 - e t h y l h e x y l - a c r y l a t e ( E H A ) .

DESCRIPTION OF DRAWINGS[ 0 0 1 0 ] FIG. 1 i s a s c h e m a t i c vieW i l l u s t r a t i n g a convent i o n a l d i s t i l l a t i o n p r o c e s s o f p r e p a r i n g h i g h - p u r i t y 2 - e t h y lh e x y l - a c r y l a t e ( E H A ) .[ 0 0 1 1 ] F I G . 2 s h o W s a g r a p h i l l u s t r a t i n g a c o m p o s i t i o np r o ? l e i n a ? r s t column n a d i s t i l l a t i o n p r o c e s s of 2-columnm e t h o d .[ 0 0 1 2 ] F I G . 3 s h o W s a g r a p h i l l u s t r a t i n g a c o m p o s i t i o np r o ? l e o f 2 - e t h y l h e x y l - a c r y l a t e i n t h e ? r s t c o l u m n i n t h ed i s t i l l a t i o n p r o c e s s o f t h e 2-column m e t h o d .[ 0 0 1 3 ] F I G . 4 i s a s c h e m a t i c vieW l l u s t r a t i n g a s t r u c t u r e ofa P e t l y u k d i s t i l l a t i o n c o l u m n .[ 0 0 1 4 ] F I G . 5 i s a s c h e m a t i c vieW l l u s t r a t i n g a s t r u c t u r e ofa d i v i d i n g W a l l column a c c o r d i n g t o an embodiment of h ep r e s e n t i n v e n t i o n .[ 0 0 1 5 ] F I G . 6 s h o W s a g r a p h i l l u s t r a t i n g a c o m p o s i t i o np r o ? l e i n a column f t h e d i v i d i n g W a l l column f F I G . 5 .[ 0 0 1 6 ] F I G . 7 s a s c h e m a t i c vieW i l l u s t r a t i n g a p r o c e s s ofd i s t i l l i n g 2 - e t h y l h e x y l - a c r y l a t e u s i n g t h e d i v i d i n g W a l l c o lumn f FIG. 5.[ 0 0 1 7 ] F I G . 8 i s a s c h e m a t i c vieW i l l u s t r a t i n g a p r o c e s s ofd i s t i l l i n g 2 - e t h y l h e x y l - a c r y l a t e u s i n g a d i s t i l l a t i o n c o l u m n o fa 2-column method.

BEST MODE OF THE INVENTION[ 0 0 1 8 ] A i v i d i n g W a l l c o l u m n a c c o r d i n g t o t h e p r e s e n ti n v e n t i o n i n c l u d e s a main column i n c l u d i n g a c o n d e n s e r , ar e b o i l e r , a n d a d i v i d i n g W a l l , W h e r e i n t h e main column s


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divided i n t o a t o p Zone, an upper in?ow Zone, an upper o u t?ow Zone, a lower in?ow Zone, a lower out?ow Zone, and abottom Z o n e , and i n c l u d e s a t l e a s t one in?ow stream and a tl e a s t t h r e e out?ow s t r e a m s , wherein each of h e at l e a s t onein?ow stream i s a s t r e a m t h a t a f e e d F c o n t a i n i n g crude2 - e t h y l h e x y l - a c r y l a t e (EHA) ?ows i n t o a n in?ow m i d d l ep l a t e NR1 where h e upper in?ow Zone and h e l o w e r in?owZone of h e main column o n t a c t each t h e r , and one or m o reof h e a t l e a s t t h r e e out?ow s t r e a m s i s a s t r e a m of 2 - e t h y lh e x y l - a c r y l a t e .[ 0 0 1 9 ] The i v i d i n g w a l l column s e q u i v a l e n t t o a P e t l y u kd i s t i l l a t i o n column i n a thermodynamic a s p e c t , b u t i s d i f f e re n t from h e P e t l y u k d i s t i l l a t i o n column n a s t r u c t u r a l a s p e c tb e c a u s e a d i v i d i n g w a l l i s p r o v i d e d i n a column o i n t e g r a t e ap r e - f r a c t i o n a t o r i n a main c o l u m n . S i n c e t h e d i v i d i n g w a l lcolumn n a t u r a l l y s o l v e s a d i ? i c u l t y i n b a l a n c i n g a p r e s s u r ebetween h e p r e - f r a c t i o n a t o r and h e main column and a d i f? c u l t y n p e r f o r m i n g a n o p e r a t i o n , a n o p e r a t i o n may e a c i l it a t e d . A l s o , s i n c e two i s t i l l a t i o n columns a r e i n t e g r a t e d i n t oo n e , i n v e s t m e n t c o s t s ma y be s i g n i ? c a n t l y r e d u c e d .[ 0 0 2 0 ] A l s o , a d i v i d i n g w a l l column a c c o r d i n g t o t h ep r e s e n t i n v e n t i o n i n c l u d e s a main column i n c l u d i n g a cond e n s e r , a r e b o i l e r , a n d a d i v i d i n g w a l l , w h e r e i n t h e maincolumn s divided i n t o a t o p Z o n e , an upper in?ow Z o n e , anupper out?ow Z o n e , a lower in?ow Z o n e , a lower out?owZ o n e , and a bottom Z o n e , wherein a f e e d F c o n t a i n i n g crude2 - e t h y l h e x y l - a c r y l a t e ?ows n t o a n in?ow m i d d l e p l a t e NR1where h e upper in?ow Zone and h e lower in?ow Zone of h emain column o n t a c t e a c h o t h e r , a l o w e r b o i l i n g componentD ows u t i n t h e t o p Z o n e , a h i g h b o i l i n g component B ?owso u t i n t h e bottom Z o n e , and a medium o i l i n g component S?ows o u t t o an out?ow middle p l a t e NR2 where t h e upperout?ow Zone and t h e lower out?ow Zone c o n t a c t each t h e r .The medium o i l i n g c o m p o n e n t may e s u b s t a n t i a l l y 2 - e t hy l h e x y l - a c r y l a t e .[ 0 0 2 1 ] The f e e d F m a y have a 2 - e t h y l h e x y l - a c r y l a t e cont e n t g r e a t e r t h a n o r e q u a l t o 80 wt %.[ 0 0 2 2 ] F I G . 5 i s a s c h e m a t i c view i l l u s t r a t i n g a d i v i d i n gw a l l column a c c o r d i n g t o an embodiment o f t h e p r e s e n ti n v e n t i o n . R e f e r r i n g t o F I G . 5 , t h e d i v i d i n g w a l l columni n c l u d e s a main column , and condenser 31 and a r e b o i l e r4 1 r e s p e c t i v e l y c o n n e c t e d t o a n u p p e r p l a t e and l o w e r p l a t eo f t h e main column .[ 0 0 2 3 ] The c o n d e n s e r 3 1 i s a d e v i c e f o r d e p r i v i n g e v a p or a t i o n h e a t of mixture n a g a s e o u s state and condensing t h em i x t u r e . A o n d e n s e r used n a c o n v e n t i o n a l c h e m i c a l e n g in e e r i n g s y s t e m may b e u s e d w i t h o u t l i m i t a t i o n . A l s o , t h er e b o i l e r 41 i s a d e v i c e f o r p r o v i d i n g e v a p o r a ti o n h e a t to am i x t u r e i n a l i q u i d s t a t e and e v a p o r a t i n g t h e m i x t u r e . Ar e b o i l e r u s e d i n a c o n v e n t i o n a l c h e m i c a l e n g i n e e r i n g s y s t e mma y be s e d w i t h o u t l i m i t a t i o n .[ 0 0 2 4 ] The main column may e r o u g h l y d i v i d e d n t o s i xZ o n e s . A op Zone 100 r e f e r s t o an upper a r e a of t h e maincolumn 1 w i t h no i v i d i n g w a l l . An pper in?ow Zone 200 sone of r e a s d i v i d e d by d i v i d i n g w a l l and s u b - a r e a l o c a t e dover a stream of an in?ow component ( f e e d ) . An pper o u t? ow Zone 300 s one of h e a r e a s d i v i d e d by h e d i v i d i n g w a l land s a sub-area l ocated over a stream of an out?ow compon e n t . A ower in?ow Zone 400 s one of h e a r e a s d i v i d e d byt h e d i v i d i n g w a l l and s a s u b - a r e a l o c a t e d u n d e r t h e s t r e a m o ft h e in?ow component. A ower out?ow Zone 500 s one of h ea r e a s d i v i d e d by t h e d i v i d i n g w a l l and s a s u b - a r e a l o c a t e d

O c t . 3 1 , 2 0 1 3

under t h e s t r e a m o f t h e out?ow component. A l s o , a bottomZone 6 0 0 r e f e r s t o a lower r e a of h e main column 1 with nod i v i d i n g w a l l .[ 0 0 2 5 ] A l s o , t h e main column 1 h a s a t l e a s t one in?owstream and at l e a s t t h r e e out?ow s t r e a m s . The at l e a s t onein?ow stream i n c l u d e s a stream t h a t a feed P which s crude2 - e t h y l h e x y l - a c r y l a t e ?ows n t o a n in?ow m i d d l e p l a t e NR1where t h e upper in?ow Zone 200 and t h e lower in?ow Zone400 of h e main column c o n t a c t each t h e r . The t l e a s t t h r e eout?ow s t r e a m s ma y n c l u d e s t r e a m s i n c l u d i n g a low o i l i n gcomponent D owing o u t i n t h e t o p Z o n e 1 0 0 , a h i g h b o i l i n gcomponent B ?owing o u t i n t h e bottom Zone 6 0 0 , and amedium b o i l i n g component S ?owing o u t to an out?owmiddle l a t e NR2 where h e u p p e r out?ow Zone 300 and h elower out?ow Zone 500 c o n t a c t each o t h e r . I n t h i s c a s e , t h emedium b o i l i n g component S ?owing o u t t o t h e out?owm i d d l e p l a t e NR2 may b e s u b s t a n t i a l l y 2 - e t h y l h e x y l - a c r yl a t e .[ 0 0 2 6 ] The t e r m c r u d e 2 - e t h y l h e x y l - a c r y l a t e f e e d u s e dh e r e i n which s a mixture having 2 - e t h y l h e x y l - a c r y l a t e a s amain component e f e r s t o a t a r g e t m a t e r i a l t o be i s t i l l e d i n ad i s t i l l a t i o n p r o c e s s , and t h e t e r m m a i n c o m p o n e n t u s e dh e r e i n r e f e r s t o one component which i s i n c l u d e d i n t h el a r g e s t a m o u n t among e s p e c t i v e c o m p o n e n t s o f h e m i x t u r e .I n o r d e r o o b t a i n i g h - p u r i t y 2 - e t h y l h e x y l - a c r y l a t e , t i s p r e fe r a b l e t h a t a c r u d e 2 - e t h y l h e x y l - a c r y l a t e f e e d h a s a h i g h e r2 - e t h y l h e x y l - a c r y l a t e c o n t e n t . I n o r d e r t o o b t a i n h i g h - p u r i t y2 - e t h y l h e x y l - a c r y l a t e g r e a t e r t h a n o r e q u a l t o 9 9 wt %, t i sp r e f e r a b l e t h a t a c r u d e 2 - e t h y l h e x y l - a c r y l a t e f e e d h a s a 2 - e t hy l h e x y l - a c r y l a t e c o n t e n t g r e a t e r t h a n o r e q u a l t o 80 wt %.[ 0 0 2 7 ] A l s o , t h e e x p r e s s i o n s u b s t a n t i a l l y 2 - e t h y l h e x y la c r y l a t e means t h a t a m i x t u r e may be r e g a r d e d a s s u b s t a nt i a l l y 2 - e t h y l h e x y l - a c r y l a t e . I n d e t a i l , t h e e x p r e s s i o n s u bs t a n t i a l l y 2 - e t h y l h e x y l - a c r y l a t e means t h a t a m i x t u r e h a s2 - e t h y l h e x y l - a c r y l a t e a s a main component, h a s a h i g h e r2 - e t h y l h e x y l - a c r y l a t e c o n t e n t t h a n a f e e d , and a s a 2 - e t h y lh e x y l - a c r y l a t e component e x c e e d i n g a t l e a s t 9 0 wt %.[ 0 0 2 8 ] A i v i d i n g w a l l p r o c e s s h a s a n a d v a n t a g e o f l o w e re n e r g y consumption t h a n a c o n v e n t i o n a l p r o c e s s u s i n g twoc o n t i n u o u s d i s t i l l a t i o n columns due o a s t r u c t u r a l d i f f e r e n c e .I n t h e d i v i d i n g w a l l c o l u m n , s i n c e s p a c e s d i v i d e d b y t h ed i v i d i n g w a l l a c t a s a p r e - f r a c t i o n a t o r , a composition of al i q u i d i s almost same a s an e q u i l i b r i u m d i s t i l l a t i o n curve duet o s e p a r a t i o n o f a h i g h b o i l i n g component a n d a l o w b o i l i n gc o m p o n e n t , a n d t h e r m o d y n a m i c e ? i c i e n c y f o r s e p a r a t i o n i si m p r o v e d d u e t o s u p p r e s s i o n o f r e - m i x i n g .[ 0 0 2 9 ] The upper in?ow Zone and t h e lower in?ow Zones u b s t a n t i a l l y a c t a s a p r e - f r a c t i o n a t o r of c o n v e n t i o n a l p r oc e s s . That s , t h e upper in?ow Zone and h e lower in?ow Zonemay be c o l l e c t i v e l y r e f e r r e d t o a s a p r e - s e p a r a t i o n a r e a . Af e e d ?owing i n t o t h e p r e - s e p a r a t i o n a r e a i s s e p a r a t e d i n t o al o w b o i l i n g c o m p o n e n t a n d a h i g h b o i l i n g c o m p o n e n t . Someo f h e l o w b o i l i n g c o m p o n e n t a n d h e h i g h o i l i n g c o m p o n e n ts e p a r a t e d i n t h e p r e - s e p a r a t i o n a r e a ?ows i n t o t h e t o p Z o n e ,and some ?ows back i n t o t h e upper out?ow Zone and t h elower out?ow Zone t o be e - d i s t i l l e d .[ 0 0 3 0 ] The upper out?ow Zone and h e lower out?ow Zonea c t a s a main column of c o n v e n t i o n a l p r o c e s s . That s , t h eupper out?ow Zone and t h e lower out?ow Zone may be c o ll e c t i v e l y r e f e r r e d t o a s a main s e p a r a t i o n a r e a . A ow o i l i n gcomponent a n d a medium b o i l i n g component a r e m a i n l ys e p a r a t e d i n a n u p p e r p o r t i o n o f t h e d i v i d i n g w a l l o f t h e mains e p a r a t i o n a r e a , a n d a medium o i l i n g component and h i g h


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b o i l i n g c o m p o n e n t a re m a i n l y s e p a r a t e d n a l o w e r p o r t i o n o ft h e d i v i d i n g W a l l o f t h e main s e p a r a t i o n a r e a .[ 0 0 3 1 ] I n d e t a i l , a c o m p o s i t i o n p r o ? l e i n t h e d i v i d i n g W a l lcolumn f F I G . 5 i s shoWn n F I G . 6 .[ 0 0 3 2 ] T h e l o W b o i l i n g c o m p o n e n t D a s s e s t h r o u g h t h et o p Zone of h e main column and h e c o n d e n s e r , and some oft h e l o W b o i l i n g c o m p o n e n t D s p r o d u c e d i n t o a l o W b o i l i n gp r o d u c t D nd h e r e m a i n i n g r e t u r n s a s a l i q u i d ?ux LD o t h et o p Z o n e o f t h e main o l u m n . A l s o , t h e h i g h b o i l i n g compon e n t B a s s e s t h r o u g h t h e bottom Zone of h e main columna n d t h e r e b o i l e r , a n d some f h e h i g h b o i l i n g component B sp r o d u c e d i n t o a h i g h b o i l i n g p r o d u c t a n d t h e r e m a i n i n gr e t u r n s a s a vapor ? u x VB o t h e bottom Zone of t h e mainc o l u m n .[ 0 0 3 3 ] A e s i g n o f a t h e r m a l l y c o u p l e d i s t i l l a t i o n c o l u m nsystem h a v i n g a d i v i d i n g W a l l i s based on a d e s i g n of ac o n v e n t i o n a l t h e r m a l l y c o u p l e d d i s t i l l a t i o n column a n d ad e s i g n o f a d i s t i l l a t i o n column a v i n g a minimum number fp l a t e s . S i n c e s e p a r a t i o n e f ? c i e n c y o f a d i s t i l l a t i o n column smaximized When a l i q u i d c o m p o s i t i o n a l d i s t r i b u t i o n o f i st i l l a t i o n p l a t e s i n t h e d i s t i l l a t i o n column s s i m i l a r t o a n e q u il i b r i u m d i s t i l l a t i o n c u r v e , a minimum-plate d i s t i l l a t i o n s y stem s ? r s t d e s i g n e d u n d e r t h e a s s u m p t i o n t h a t a d i s t i l l a t i o nc o l u m n s o p e r a t e d b y h a n d l i n g a p r e - r e ? u x . T h a t s , t h e u p p e rin?oW Zone and h e loWer in?oW Zone r e designed under h eassumption h a t c o m p o s i t i o n s of f e e d and l i q u i d a t a f e e din?oW p l a t e a r e t h e same. I n t h e upper out?oW Zone and t h el o W e r out?oW o n e , a c o m p o s i t i o n o f l i q u i d from h e middlet o t h e t o p i s c a l c u l a t e d by a c a s c a d e method o r d e s i g n i n g a ne q u i l i b r i u m c o m p o s i t i o n s t a r t i n g f r o m a c o n c e n t r a t i o n o f amedium o i l i n g p r o d u c t . I n t h e l o W e r out?oW Z o n e a c t i n g a sa main o l u m n , a c o m p o s i t i o n o f a l i q u i d i s c a l c u l a t e d fromt h e middle o t h e bottom s i n g a c a s c a d e method f c a l c u l a ti n g a n e q u i l i b r i u m c o m p o s i t i o n s t a r t i n g f r o m a c o n c e n t r a t i o no f h e medium o i l i n g p r o d u c t .[ 0 0 3 4 ] The number o f p l a t e s o f e a c h o f t h e u p p e r in?oWZone and h e loWer in?oW Zone Which c t a s a p r e - f r a c t i o n a t o rand h e upper out?oW Zone and h e loWer out?oW Zone Whicha c t a s a main column ma y be o b t a i n e d by c a l c u l a t i n g t h enumber f p l a t e s h a v i n g a c o m p o s i t i o n o f a p r o d u c t a n d t h enumber o f f e e d in?oW p l a t e s from a d i s t r i b u t i o n o f t h eo b t a i n e d l i q u i d c o m p o s i t i o n . S i n c e t h e number f l a t e s i s a ni d e a l t h e o r e t i c a l p l a t e n u m b e r , t h e a c t u a l number f l a t e s i nt h e d i v i d i n g W a l l column m a y a r y a c c o r d i n g t o a commond e s i g n s t a n d a r d .[ 0 0 3 5 ] I n t h e d i v i d i n g W a l l c o l u m n a c c o r d i n g o t h e p r e s e n te m b o d i m e n t , t h e number f l a t e s p r o v i d e d n e a c h o f h e t o pZ o n e , t h e upper in?oW o n e , t h e upper out?oW o n e , t h e loWerin?oW o n e , t h e loWer out?oW o n e , and h e bottom Zone mayr a n g e from 90 o 1 4 0 % of t h e o r e ti c a l p l a t e number Which sc a l c u l a t e d from a d i s t i l l a t i o n c u r v e . When t h e number ofp l a t e s i s l e s s t h a n 9 0 % o f t h e c a l c u l a t e d t h e o r e t i c a l p l a t en u m b e r , a l o W b o i l i n g component a n d a h i g h b o i l i n g compon e n t ma y o t b e W e l l s e p a r at e d i n t h e p r e - s e p a r a t i o n a r e a , andWhen h e number f p l a t e s e x c e e d s 1 4 0 , e n e r g y consumpt i o n r e d u c t i o n i s no l o n g e r i n c r e a s e d i n an a r e a having aminimum e ? u x r a t i o , r e s u l t i n g i n a n i n c r e a s e i n i n v e s t m e n tc o s t s .[ 0 0 3 6 ] A l s o , a l e n g t h o f t h e d i v i d i n g W a l l p r o v i d e d i n t h emain column s d e t e r m i n e d a c c o r d i n g t o a p l a t e number alc u l a t e d a c c o r d i n g to d i s t i l l a t i o n c u r v e s of h e upper in?oWZone and h e loWer in?oW o n e , o r t h e upper out?oW Zone andt h e loWer out?oW Z o n e . While t h e r e a r e v a r i o u s methods ofo b t a i n i n g a t h e o r e t i c a l p l a t e number and a r e ? u x amount by

O c t . 3 1 , 2 0 1 3

d e t e r m i n i n g a s p a c i n g o f t h e d i v i d i n g W a l l u s i n g a n e q u i l i brium i s t i l l a t i o n c u r v e method on a l i q u i d composition i t ht h e p r e - s e p a r a t i o n a r e a and h e main s e p a r a t i o n a r e a When ano p t i m a l s p a c i n g o f t h e d i v i d i n g W a l l i s d e s i g n e d i n t h e d i v i di n g W a l l c o l u m n , a t h e o r e t i c a l p l a t e number s o b t a i n e d u s i n ga Fenske-UnderWood metho d i n t h e p r e s e n t i n v e n t i o n . TheFenske-UnderWood method s W e l l knoWn o one f o r d i n a r ys k i l l i n t h e a r t .[ 0 0 3 7 ] A e n g t h o f t h e d i v i d i n g W a l l may a n g e f r o m 4 0 t o8 5 % o f a t o t a l t h e o r e t i c a l p l a t e number o f t h e t o p Z o n e , t h eupper in?oW Z o n e , t h e l o W e r out?oW Z o n e , and t h e bottomZone a l c u l a t e d from d i s t i l l a t i o n c u r v e . When h e l e n g t h oft h e d i v i d i n g W a l l i s l s s t h a n 40%, some o f a loW b o i l i n gcomponent i n t h e p r e - s e p a r a t i o n a r e a ma y ?oW doWn fromt h e p r e - s e p a r a t i o n a r e a and be n t r o d u c e d i n t o a p r o d u c t i n t h emain c o l u m n . When h e l e n g t h o f t h e d i v i d i n g W a l l e x c e e d s85%, t i s d i f ? c u l t to m a i n t a i n a smooth e q u i l i b r i u m How o fl i q u i d / v a p o r s t a t e s o f l o W b o i l i n g / m e d i u m b o i l i n g compon e n t s a n d l i q u i d / v a p o r s t a t e s o f medium o i l i n g / h i g h b o i l i n gc o m p o n e n t s i n t h e d i v i d i n g W a l l c o l u m n , t h e r e b y m a k i n g i td i f ? c u l t t o manufacture a d i s t i l l a t i o n column.[ 0 0 3 8 ] A o n d i t i o n f o r o p e r a t i n g t h e d i v i d i n g W a l l c o l u m nf o r p r e p a r i n g h i g h - p u r i t y 2 - e t h y l h e x y l - a c r y l a t e i s a s f o l l o W s .[ 0 0 3 9 ] F o r e x a m p l e , a t e m p e r a t u r e o f t h e t o p Z o n e p r e f e ra b l y r a n g e s from 88 t o 9 8 C . a t a p r e s s u r e of h e t o p Zone of1 5 t o 2 5 t o r r . When h e t e m p e r a t u r e o f h e t o p Zone s l e s s t h a n8 8 C . , a l o W b o i l i n g component may ?oW doWn from t h ep r e - s e p a r a t i o n a r e a , t h e r e b y b a d l y a f f e c t i n g p r o d u c t p u r i t y .When h e t e m p e r a t u r e o f t h e t o p Z o n e e x c e e d s 9 8 C . , a h i g hb o i l i n g c o m p o n e n t ( H e a v i e s ) may ?oW p f r o m t h e p r e - s e p ar a t i o n a r e a , t h e r e b y b a d l y a f f e c t i n g p r o d u c t p u r i t y .[ 0 0 4 0 ] A e m p e r a t u r e o f t h e b o t t o m Z o n e p r e f e r a b l y r a n g e sfrom 138 t o 148 C . at a p r e s s u r e ofthe t o p Zone of 1 5 t o 25t o r r . When h e t e m p e r a t u r e of h e bottom Zone i s l e s s t h a n1 3 8 C . , a medium b o i l i n g component may ?oW d o W n ,t h e r e b y r e d u c i n g p r o d u c t i v i t y . When h e t e m p e r a t u r e o f t h eb o t t o m Z o n e e x c e e d s 1 4 8 C . , t h e h i g h b o i l i n g c o m p o n e n t( H e a v i e s ) may a t e r a l l y ?oW a l o n g W i t h t h e medium o i l i n gc o m p o n e n t .[ 0 0 4 1 ] A l s o , a t e m p e r a t u r e o f h e out?oW i d d l e p l a t e NR2Which s l o c a t e d a t a p o s i t i o n Where t h e upper out?oW Zoneand t h e loWer out?oW Zone c o n t a c t each o t h e r and t o Whicht h e medium o i l i n g c o m p o n e n t S ?oWs u t p r e f e r a b l y r a n g e sfrom 124 t o 134 C . at a p r e s s u r e ofthe t o p Zone of 1 5 t o 25t o r r . When h e t e m p e r a t u r e o f h e out?oW i d d l e p l a t e NR2 sl e s s t h a n 1 2 4 C . , i t i s n o t e a s y t o remove a loW b o i l i n gc o m p o n e n t . When t h e t e m p e r a t u r e o f t h e out?oW m i d d l ep l a t e NR2 x c e e d s 1 3 4 C . , i t i s n o t e a s y t o remove a h i g hb o i l i n g c o m p o n e n t , t h e r e b y g r e a t l y a f f e c t i n g p r o d u c t p u r i t y .[ 0 0 4 2 ] When h e d i v i d i n g W a l l column s d e p r e s s u r i Z e d o rp r e s s u r i z e d , t h e t e m p e r a t u r e r a n g e s may e c h a n g e d . I n g e ne r a l , a s a p r e s s u r e i n c r e a s e s , an upper temperature i m i t andl o W e r t e m p e r a t u r e l i m i t t e n d t o i n c r e a s e .[ 0 0 4 3 ] F o r e x a m p l e , When a p r e s s u r e o f t h e t o p Zone i sa b o u t 1 5 t o r r , a t e m p e r a t u r e of h e t o p Zone m a y a n g e froma b o u t 83 t o a b o u t 9 3 C . , a t e m p e r a t u r e of h e bottom Zonem a y a n g e from b o u t 1 3 5 t o a b o u t 1 4 5 C . , and t e m p e r a t u r eo f h e out?oW i d d l e p l a t e NR2 ay a n g e from b o u t 120 oa b o u t 1 30 C .[ 0 0 4 4 ] I n a d d i t i o n , When p r e s s u r e o f t h e t o p Zone s a b o u t30 o r r , a t e m p e r a t u r e of h e t o p Zone m a y a n g e from b o u t 9 5t o a b o u t 1 0 5 C . , a t e m p e r a t u r e of h e bottom Zone ma y a n g e


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from a b o u t 140 t o a b o u t 1 5 0 C . , and a t e m p e r a t u r e of h eout?ow i d d l e p l a t e NR2 ay a n g e from b o u t 1 2 8 t o a b o u t1 3 8 0 C .[ 0 0 4 5 ] T a b l e 1 shows an upper t e m p e r a t u r e l i m i t and al o w e r t e m p e r a t u r e l i m i t a c c o r d i n g t o a p r e s s u r e .

TABLELower e m p e r a t u r e U p p e r t e m p e r a t u r el i m i t ( 0 C . ) l i m i t ( 0 C . )P 1 20 torr

Top Zone 8 8 98Bottom Zone 138 1 4 8Out?ow i d d l e p l a t e NR2 1 2 4 134

P 1 15 torr

Top Zone 8 3 93Bottom Zone 135 145Out?ow i d d l e p l a t e NR2 1 2 0 1 3 0

P 1 30 torr

Top Zone 9 5 105Bottom Zone 140 150Out?ow i d d l e p l a t e NR2 1 2 8 1 3 8

[ 0 0 4 6 ] A e l a t i o n s h i p between t e m p e r a t u r e and p r e s s u r ei n t h e d i v i d i n g w a l l column c c o r d i n g o t h e p r e s e n t i n v e n t i o nmay e de?ned s i n g E q u a t i o n s 1 t o 3 .[ 0 0 4 7 ] A e m p e r a t u r e of t h e t o p Zone ma y r a n g e from alower temperature i m i t T a t o an upper temperature i m i t T2aa c c o r d i n g t o E q u a t i o n 1 .

L o w e r t e m p e r a t u r e l i m i t : T 1 a : 0 . 0 2 P 2 + 1 . 7 P + 6 2U p p e r e m p e r a t u r e l i m i t : T 2 a : 0 . 0 2 P 2 + 1 . 7 P + 7 2 ( 1 ) ,

where Tm nd 2 0 a r e t e m p e r a t u r e s ( C . ) , and P s a p r e s s u r eo f t h e t o p Z o n e ( t o r r ) , p r o v i d e d t h a t 1 s P s 7 0 .[ 0 0 4 8 ] A e m p e r a t u r e of h e bottom Zone m a y a n g e fromlower temperature i m i t T b t o an upper temperature i m i t T 2 1 ,a c c o r d i n g t o E q u a t i o n 2 .

L o w e r t e m p e r a t u r e l i m i t : T 1 b : 0 . 0 2 6 7 P 2 + 1 . 5 3 3 3 P +118

U p p e r t e m p e r a t u r e l i m i t : T 2 b : 0 . 0 2 6 7 P 2 + 1 . 5 3 3 3 P +1 2 8 ( 2 ) ,

where 1 1 , a n d 2 1 , a r e t e m p e r a t u r e s ( C . ) , a n d P s a p r e s s u r eo f t h e t o p Z o n e ( t o r r ) , p r o v i d e d t h a t 1 s P s 7 0 .[ 0 0 4 9 ] A l s o , a t e m p e r a t u r e o f h e out?ow i d d l e p l a t e NR2which s l o c a t e d at a p o s i t i o n where t h e upper out?ow Zoneand t h e lower out?ow Zone c o n t a c t each o t h e r and to whicht h e medium o i l i n g component S ?ows u t ma y a n g e fromlower temperature i m i t T c t o an upper temperature i m i t T26a c c o r d i n g t o E q u a t i o n 3 .

L o w e r t e m p e r a t u r e l i m i t : T 1 C : 0 . 0 2 6 7 P 2 + 1 . 7 3 3 3 P +100

U p p e r t e m p e r a t u r e l i m i t : T 2 C : 0 . 0 2 6 7 P 2 + 1 . 7 3 3 3 P +1 1 0 ( 3 ) ,

where 1 6 a n d T 2 6 a r e t e m p e r a t u r e s ( C . ) , a n d P s a p r e s s u r eo f t h e t o p Z o n e ( t o r r ) , p r o v i d e d t h a t 0 . 1 s P s 7 0 .[ 0 0 5 0 ] A t h e r m a l l y c o u p l e d d i s t i l l a t i o n c o l u m n s y s t e mh a v i n g a d i v i d i n g w a l l a c c o r d i n g t o t h e p r e s e n t i n v e n t i o n h a sa n o b j e c t i v e o f i m p r o v i n g e f ? c i e n c y o f i s t i l l i n g a 3 - c o m p on e n t m i x t u r e , and h a s a n e f f e c t o f h a v i n g two d i s t i l l a t i o nc o l u m n s by r o v i d i n g t h e d i v i d i n g w a l l i n a main column oform s p a c e s which u n c t i o n a s a p r e - f r a c t i o n a t o r and a main

O c t . 3 1 , 2 0 1 3

column h a v i n g a l i q u i d c o m p o s i t i o n d i s t r i b u t i o n s i m i l a r t ot h a t o f a h i g h - e ? i c i e n c y e q u i l i b r i u m d i s t i l l a t i o n s y s t e m .[ 0 0 5 1 ] A l s o , t h e p r e s e n t i n v e n t i o n p r o v i d e s a method o fp r e p a r i n g 2 - e t h y l h e x y l - a c r y l a t e u s i n g t h e d i v i d i n g w a l l c o lumn. The method may p r e p a r e h i g h - p u r i t y 2 - e t h y l h e x y la c r y l a t e b y p r o v i d i n g a c r u d e 2 - e t h y l h e x y l - a c r y l a t e f e e d t ot h e d i v i d i n g w a l l c o l u m n a n d s e p a r a t e l y d i s t i l l i n g 2 - e t h y lh e x y l - a c r y l a t e .[ 0 0 5 2 ] The i v i d i n g w a l l column n c l u d e s th e main columni n c l u d i n g t h e c o n d e n s e r , t h e r e b o i l e r , a n d t h e d i v i d i n g w a l l ,w h e r e i n t h e main column s d i v i d e d i n t o t h e t o p Z o n e , t h eupper in?ow Z o n e , t h e upper out?ow Z o n e , t h e lower in?owZ o n e , t h e lower out?ow Z o n e , and t h e bottom Z o n e , andi n c l u d e s at l e a s t one in?ow stream and at l e a s t t h r e e out?ows t r e a m s , wherein each of h e a t l e a s t one in?ow stream s as t r e a m h a t t h e f e e d F c o n t a i n i n g c r u d e 2 - e t h y l h e x y l - a c r y l a t e?ows i n t o t h e in?ow m i d d l e p l a t e NR1 where t h e u p p e rin?ow Zone and t h e lower in?ow Zone of h e main columnc o n t a c t each o t h e r , and t h e a t l e a s t t h r e e out?ow s t r e a m si n c l u d e s t r e a ms t h a t t h e low o i l i n g component D ows u t t ot h e t o p Z o n e , t h e h i g h b o i l i n g component B ?ows o u t t o t h ebottom o n e , and h e medium o i l i n g component S ?ows u tt o t h e out?ow middle l a t e NR2 here h e upper out?ow oneand t h e l o w e r out?ow Zone c o n t a c t each o t h e r , and t h emedium b o i l i n g component S ?owing o u t t o t h e out?owm i d d l e p l a t e NR2 may b e s u b s t a n t i a l l y 2 - e t h y l h e x y l - a c r yl a t e .

MODES OF THE INVENTION[ 0 0 5 3 ] H e r e i n a f t e r , e x e m p l a r y e m b o d i m e n t s o f h e p r e s e n ti n v e n t i o n w i l l b e d e s c r i b e d i n d e t a i l . H o w e v e r , t h e p r e s e n ti n v e n t i o n i s n o t l i m i t e d t o t h e e x e m p l a r y embodiments d i sc l o s e d b e l o w , b u t c a n b e implemented n v a r i o u s f o r m s .

E m b o d i m e n t a n d C o m p a r a t i v e E x a m p l e[ 0 0 5 4 ] A i v i d i n g w a l l column was d e s i g n e d , m a n u f a ct u r e d , a n d o p e r a t e d i n o r d e r t o v e r i f y a p e r f o r m a n c e o f as y s t e m a c c o r d i n g to t h e p r e s e n t i n v e n t i o n . I t was o u n d fromt h e o p e r a t i o n o f t h e d i v i d i n g w a l l column h a t a d e s i r e d p r o du c t c o m p o s i t i o n was o b t a i n e d . F o r a c o m p a r a t i v e e x a m p l e ,c o n v e n t i o n a l 2 d i s t i l l a t i o n c o l u m n s h a v i n g no d i v i d i n g w a l lwere u s e d , and f o r an embodiment, 1 d i s t i l l a t i o n columnh a v i n g a d i v i d i n g w a l l was s e d .[ 0 0 5 5 ] F I G S . 7 and 8 a r e s c h e m a t i c v i e w s i l l u s t r a t i n g t h eembodiment o f t h e p r e s e n t i n v e n t i o n a n d t h e c o m p a r a t i v ee x a m p l e , r e s p e c t i v e l y . F I G . 7 i l l u s t r a t e s a d i v i d i n g w a l l c o lumn c c o r d i n g t o t h e embodiment o f t h e p r e s e n t i n v e n t i o n .F I G . 8 i l l u s t r a t e s a c o n v e n t i o n a l d i s t i l l a t i o n column n c l u d i n gt w o c o l u m n s a c c o r d i n g t o t h e c o m p a r a t i v e e x a m p l e . I n F I G S .7 and , r e f e r e n c e n u m e r a l s 1 t o 8 d e n o t e i n d i v i d u a l s t r e a m si n t h e e m b o d i m e n t a n d t h e c o m p a r a t i v e e x a m p l e .[ 0 0 5 6 ] T h e e m b o d i m e n t a n d t h e c o m p a r a t i v e e x a m p l e h a v et h e o r e t i c a l p l a t e numbers as shown i n T a b l e 2 , a n d e x p e r imental r e s u l t s a r e shown i n T a b l e s 3 and . T a b l e 3 shows ac o n d i t i o n and c o m p o s i t i o n f o r e a c h s t r e am a c c o r d i n g t o t h eembodiment. a b l e 4 shows c o n d i t i o n and composition o re a c h s t r e a m a c c o r d i n g t o t h e c o m p a r a t i v e e x a m p l e .


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US 2013/0284586 A 1 O c t . 3 1 , 2 0 1 3

TABLE TABLET h e o r e t i c a l C o m p a r a t i v e R e d u c e d

I t e m p l a t e number e x a m p l e amount ReducEmbodiment T O P 1 9 1 . 1 ? 1 0 0 8 F i r s t S e c o n d E m b o d i - (MMK t i o nUpper ln?OW Z 0 1 1 6 200 9 column column Sum ment c a l / h r ) r a t e ( )

Upper u t f l o W Zone 300 1 0LoWer in?oW Zone 400 1 8 Energy 0 . 3 9 0 . 1 9 0 . 5 8 0 . 4 3 0 . 1 5 2 5 . 9LoWer u t f l o W Zone 500 5 consumptionBottom Zone 600 1 5 (MMK

C o m p a r a t i v e F i r s t c o l u m n 1 8 c a l / h r )e x a m p l e S e c o n d column 2 0

[ 0 0 5 9 ] T h e c o m p a r a t i v e e x a m p l e u s i n g t h e c o n v e n t i o n a ld i s t i l l a t i o n column i n c l u d e s tWo columns and f o u r h e a tTABLE e x c h a n g e r s W h e r e a s t h e d i v i d i n g W a l l c o l u m n a c c o r d i n g t othe embodiment may include one column and tWo heat

Embodi Streamnumber . . . . .e x c h a n g er s . A c c o r d l n g l y , l n v e s t m en t c o s t s o f t h e d 1 v 1 d 1 n gm e n t 1 2 3 4 5 Wall column according t o t h e embodiment of t h e p r e s e n tC o n d i t i o n T e m p e r a t u r e 5 0 . 0 5 5 . 2 5 5 . 2 7 7 . 2 9 3 . 9

( C - )i n v e n t i o n m a y be a b o u t 30 oWer h a n t h o s e of h e convent i o n a l d i s t i l l a t i o n c o l u m n . I n p a r t i c u l a r , an e n e r g y r e d u c t i o n

P r e s s u r e 1 4 7 1 _ 1 3 5 _ @ 3 5 _ @ 6 9 ; ; 9 Q _ @ r a t e of h e d i v i d i n g W a l l column according o t h e embodiment( t o n ) o f t h e p r e s e n t i n v e n t i o n i s a b o u t 25.9% l o W e r t h a n t h a t o f t h ef l u x ( k g / h r ) 5 1 2 9 . 6 8 0 6 3 . 5 6 1 0 . 0 3 9 2 0 . 0 5 9 9 . 6 Conventional d i s t i l l a t i o n ColumnCom- LoW o 1 l 1 n g 1 5 . 0 0 7 5 . 0 0 7 5 . 0 0 0 . 0 0 0 . 0 0p o s i t i o n p o i n t ( W t )Medium 8 1 . 1 0 2 5 . 0 0 2 5. 0 0 1 0 0 . 0 0 7 6 . 9 0 DESCRIPTION OF REFERENCE NUMERALSb l Z g W t ) [ 0 0 6 0 ] 1 : m a i n c o l u m nH i g h b o i l i n g 3 . 90 0 . 0 0 0 . 0 0 0 . 0 0 2 3 . 1 0 [ 0 0 6 1 ] 1 1 ; ? r s t columnp o i n t ( W t ) [ 0 0 6 2 ] 2 1 ' s e c o n d columnS ( t ) 1 0 0 100 100 100 100 _um W [ 0 0 6 3 ] 1 2 : p r e - f r a c t l o n a t o r

[ 0 0 6 4 ] 2 2 : main columnTABLE

C o m p a r a t i v e S t r e a m numberexample 1 2 3 4 5 6 7C o n d i t i o n Temperature 6 0 . 0 5 5 . 2 55 . 2 8 4 . 7 6 2 . 5 6 2 6 9 6 5

( C - )P r e s s u r e 1 4 7 1 . 1 3 5 . 0 3 5 . 0 2966.7 3 5 . 0 3 5 . 0 1 0 0 . 0( t o r r )f l u x ( k g / h r ) 6 1 2 9 . 6 6 4 6 4 . 9 6 1 0 . 0 4 5 1 9 . 6 3 9 5 9 . 2 3 9 2 0 . 0 6 9 9 . 6

Composition LoW 1 5 . 0 0 7 5 . 0 0 7 5 . 0 0 0 . 0 0 0 . 0 0 0 . 0 0 0 . 0 0b o i l i n gp o i n t ( W t )M ediu m 8 1 . 1 0 2 5 . 0 0 2 5. 0 0 9 5 . 1 0 1 0 0 . 0 0 1 0 0 . 0 0 7 7 . 0 0b o i l i n gp o i n t ( W t )High 3 . 9 0 0 . 0 0 0 . 0 0 4 . 9 0 0 . 0 0 0 . 0 0 2 3 . 0 0b o i l i n gp o i n t ( W t )Sum W t %) 1 0 0 1 0 0 1 0 0 1 0 0 1 0 0 1 0 0 1 0 0

[ 0 0 5 7 ] When a b l e 3 and T a b l e 4 a r e compared i t h e a c h [ 0 0 6 5 ] 3 1 : c o n d e n s e ro t h e r , When t h e d i v i d i n g W a l l column a c c o r d i n g t o t h e [ 0 0 6 6 ] 4 1 1 r e b O i l e re m b o d i m e n t W a s u s e d , h i g h - p u r i t y 2 - e t h y l h e x y l - a c r y l a t e o f [ 0 0 6 7 ] 5 1 3 d 1 v 1 d 1 n g W a l l9 9 . 9 Wt as more e ? i c i e n t l y o b t a i n e d d u e to r e m o v a l o f [ 0 0 6 8 ] 1 0 0 : t O P Z O I _ 1 er e - m i x i n g a n d a n i n c r e a s e i n s e p a r a t io n e ? i c i e nc y . An d d i - [ 0 0 6 9 ] 2 0 0 : u p p e r In?ow Z o n et i o n a l r e c c l i n r o c e s s of e c t i f i n 2 - e t h l h e x l - a c l a t e i s [ 0 0 7 0 ] 3 0 0 : upper Out?ow Zoned d d y gp _ y d g _ y h y b [ 0 0 7 1 ] 4 0 0 : l o W e r i n ? o W Z o n er e u c e u e t o an n c r e a s e 1n p r o u c t p u r 1 t y , t e r e y 1 m p r o v - [ 0 0 7 2 ] 5 0 0 : l o w e r Out?ow Z o n emg r o d u c n v l t y - [ 0 0 7 3 ] 6 0 0 : bottom Z O n e[ 0 0 5 8 ] I n d d i t i o n , T a b l e 5 s h o W s a r e s u l t o b t a i n e d b y m e a - [ 0 0 7 4 ] NR1: i n ? o w m i d d l e P l a t es u r i n g e n e r g y c o n s u m p t i o n a c c o r d i n g o t h e e m b o d i m e n t a n d [ 0 0 7 5 ] NR2I O u t ? o w m l d d l e P l a t et h e c o m p a r a t i v e e x a m p l e ( c o n v e n t i o n a l ) a n d c a l c u l a t i n g a [ 0 0 7 6 ] F : f e e d ( r a W m a t e r i a l )r e d u c t i o n r a t e . [ 0 0 7 7 ] B : h i g h b o i l i n g c o m p o n e n t


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US 2013/0284586 A 1

[ 0 0 7 8 ] D : l o W b o i l i n g c o m p o n e n t[ 0 0 7 9 ] S : medium o i l i n g c o m p o n e n t

INDUSTRIAL PPLICABILITY[ 0 0 8 0 ] A i v i d i n g W a l l c o l u m n a c c o r d i n g t o t h e p r e s e n ti n v e n t i o n may e v a r i o u s l y u s e d i n ? e l d s u s i n g 2 - e t h y l h e x y la c r y l a t e ( E H A ) .

1 . A i v i d i n g W a l l column o m p r i s i n g a main column comp r i s i n g : ac o n d e n s e r ;

a r e b o i l e r ; anda d i v i d i n g W a l l ,Wherein t h e main column s d i v i d e d i n t o a t o p Z o n e , an

upper in?oW o n e , an upper out?oW o n e , a loWer in?oWZ o n e , a loWer out?oW Z o n e , and a bottom Z o n e , andcomprises a t l e a s t one in?oW s t r e a m and a t l e a s t t h r e eout?oW s t r e a m s ,

Wherein h e at l e a s t one in?oW stream s a stream h a t a feedc o n t a i n i n g c r u d e 2 - e t h y l h e X y l - a c r y l a t e ?oWs i n t o a nin?oW i d d l e p l a t e Where h e upper in?oW Zone and h eloWer in?oW Zone of t h e main column c o n t a c t eacho t h e r , and one r mo r e of h e out?oW streams s a streamo f - e t h y l h e X y l - a c r y l a t e .

2 . The d i v i d i n g W a l l column o f c l a i m 1 , W h e r e i n a loWb o i l i n g component ?oWs o u t i n t h e t o p Z o n e , a h i g h b o i l i n gcomponent B oWs u t i n t h e bottom o n e , a medium o i l i n gcomponent ?oWs o u t t o an out?oW middle p l a t e Where t h eupper out?oW Zone and h e loWer out?oW Zone c o n t a c t eacho t h e r , a n d t h e medium o i l i n g c o m p o n e n t ? o W i n g o u t t o t h eo u t ? o W m i d d l e p l a t e i s 2 - e t h y l h e X y l - a c r y l a t e .

3 . The i v i d i n g W a l l column o f c l a i m 1 , W h e r e i n t h e f e e dh a s a 2 - e t h y l h e X y l - a c r y l a t e c o n t e n t g r e a t e r t h a n o r e q u a l t o 80Wt %.

4 . The i v i d i n g W a l l column f c l a i m 1 , W h e r e i n t h e numb e r o f p l a t e s p r o v i d e d i n e a c h o f t h e t o p Z o n e , t h e u p p e rout?oW Z o n e , t h e loWer in?oW Z o n e , t h e l o W e r out?oW Z o n e ,and t h e bottom Zone of h e main column a n g e s from 90 t o1 4 0 % of t h e o r e t i c a l p l a t e number a l c u l a t e d from a d i s t i ll a t i o n curve.

O c t . 3 1 , 2 0 1 3

5 . The i v i d i n g W a l l column f l a i m , W h e r e i n a l e n g t h o ft h e d i v i d i n g W a l l i s d e t e r m i n e d a c c o r d i n g t o t h e number o fp l a t e s i n c l u d e d i n t h e u p p e r in?oW Zone and h e l o W e r in?oWZ o n e , or t h e upper out?oW Zone and h e loWer out?oW Z o n e .

6 . The i v i d i n g W a l l column f l a i m , W h e r e i n a l e n g t h o ft h e d i v i d i n g W a l l r a n g e s from 40 o 8 5 % of t o t a l t h e o r e t i c a lp l a t e number f h e t o p Z o n e , t h e u p p e r in?oW o n e , t h e l o W e rout?oW o n e , and h e bottom Zone Which s c a l c u l a t e d fromd i s t i l l a t i o n curve.7 . The i v i d i n g W a l l column f l a i m , W h e r e i n a t e m p e r at u r e of h e t o p Zone ranges from loWer temperature i m i t TMt o a n u p p e r t e m p e r a t u r e l i m i t T 2 0 s a t i s f y i n g E q u a t i o n 1 :

Where Tm nd 2 0 a r e t e m p e r a t u r e s ( C . ) , and P s a p r e s s u r ei n t h e t o p Z o n e ( t o r r ) , p r o v i d e d t h a t l s P s 7 0 .8 . The i v i d i n g W a l l column f l a i m , W h e r e i n a t e m p e r at u r e of h e bottom Zone a n g e s from loWer temperature i m i tT 1 1 , t o a n u p p e r t e m p e r a t u r e l i m i t T 2 1 , s a t i s f y i n g E q u a t i o n 2 :

Where 1 1 , a n d 2 1 , a r e t e m p e r a t u r e s ( C . ) , a n d P s a p r e s s u r ei n t h e t o p Z o n e ( t o r r ) , p r o v i d e d t h a t l s P s 7 0 .9 . The i v i d i n g W a l l column f l a i m , W h e r e i n a t e m p e r at u r e o f an out?oW i d d l e p l a t e Which s p r o v i d e d t a p o s i t i o nWhere t h e upper out?oW Zone and t h e loWer out?oW Zonec o n t a c t e a c h o t h e r and o Which medium o i l i n g component?oW s o u t r a n g e s from a loWer t e m p e r a t u r e l i m i t T16 t o anu p p e r t e m p e r a t u r e l i m i t T 2 6 s a t i s f y i n g E q u a t i o n 3 :

Wherein T 6 and 2 6 a r e t e m p e r a t u r e s ( C . ) , and P s a p r e ss u r e i n t h e t o p Z o n e ( t o r r ) , p r o v i d e d t h a t l s P s 7 0 .1 0 . A e t h o d o r p r e p a r i n g 2 - e t h y l h e X y l - a c r y l a t e u s i n g t h ed i v i d i n g W a l l column f c l a i m 1 .

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(2013) us20130284586 dividing wall column for preparing high-purity 2 ethylhexyl-acrylate

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