S e p t . 2 3 , 1969 H . H . WALL.

ETAL 3 , 468, 957

PRODUCTION AND PURIFICATION OF VINYL CH LORIDE
File d J a n . 2 7. 1967
h ir e d S t a t e s Pa t e n t O
l
3 , 468, 967
PRODUCTION AND IPURIFICATION 0F
VINYL CH LORIDE
H e n r y H . Wa ll a n d Er ic P. B r e ide n b a c h , B a t on Rou g e ,
lLa . , a n d Le o A. M ille r , La k e la n d, Fia . , a s s ig n or s t o
Et h yl Cor p or a t ion , Ne w Yor k , N. Y. , a c or p or a t ion of
Vir g in ia
Con t in u a t ion - im p a r t of a p p lic a t ion S e r . No. 3 62 , 7 86,
Ap r . 2 7, 1964. Th is a p p lic a t ion J a n . 2 7, 1967, S e r .
N o. 612 , 109
lin t . Cl. ( 2 07e 17/ 3 4, 17/ 58; i ld 3 / 14
ILS . Cl. 2 60- 656 8 Cla im s
AB S TRACT 0F TH E DIS CLOS URE
Th is in v e n t ion r e la t e s t o a n ov e l p r oc e s s f or t h e p r o
du c t ion a n d p u r if ic a t ion of v in yl c h lor ide b y t h e r m a l de
c om p os it ion of dic h lor oe t h a n e a n d h ig h p r e s s u r e dis t il
la t ion of t h e p r odu c t m ix t u r e t o r e c ov e r v in yl c h lor ide .
Th e p r e s e n t in v e n t ion u t iliz e s a c om b in a t ion of du a l dis - ~
t illa t ion z on e s Wh ic h c oa c t t o c a n c e l t h e e f f e c t s of s lop p y
c u t s in e a c h z on e a n d t h u s a c h ie v e s u b s t a n t ia lly p u r e
p r odu c t s t r e a m s a n d a s u b s t a n t ia lly p u r e r e c yc le s t r e a m
Wh ile s t ill e l e c t in g a c on s ide r a b le r e f r ig e r a t ion s a v in g .
CROS S - REFERENCES To RELATED
APPLICATIONS _
Th is a p p lic a t ion is a c on t in u a t ion - in - p a r t of a p p lic a
t ion S e r . No. 3 62 , 786 le d Ap r . 2 7, 1964, a n d n ow
a b a n don e d.
B ACKGROUND OF TH E INVENTION
It is k n own t h a t v in yl c h lor ide c a n b e p r odu c e d b y
t h e r m a lly de c om p os in g e it h e r 1, 2 - dic h lor oe t h a n e or 1, 1
dic h lor oe t h a n e or b ot h in a c r a c k in g f u r n a c e a t t e m p e r a
t u r e s of a b ou t 400 C. a n d h ig h e r . Th is de c om p os it ion
in v olv e s t h e s p lit t in g ot of h ydr og e n c h lor ide f r om t h e di
c h lor oe t h a n e m ole c u le , a n d t h e r e s u lt in g m ix t u r e of r e a c t
a n t s a n d c r a c k in g p r odu c t s p r e s e n t s a di c u lt s e p a r a t ion
p r ob le m . On e dif f ic u lt y e n c ou n t e r e d in c om m e r c ia l a p
p lic a t ion s of t h e p r oc e s s is t h e e x p e n s e of c os t ly r e f r ig e r a
t ion s ys t e m s a n d r e f r ig e r a n t s n e c e s s a r y f or t h e p u r if ic a t ion
of t h e p r odu c t s t r e a m f r om t h e c r a c k in g f u r n a c e .
It is a n ob j e c t of t h is in v e n t ion t o p r ov ide a p r oc e s s
wh e r e in t h e r e q u ir e m e n t f or r e f r ig e r a t ion in t h e p r odu c t
dis t illa t ion c olu m n s is g r e a t ly m in im iz e d.
An ot h e r ob j e c t of t h is in v e n t ion is t o p r ov ide a p r oc
e s s f or t h e c om m e r c ia l p r odu c t ion of v in yl c h lor ide in a
m or e s im p le a n d e c on om ic a l m a n n e r .
S UM M ARY OF TH E INVENTION
Th is in v e n t ion r e la t e s t o a p r oc e s s f or t h e p r odu c t ion of
v in yl c h lor ide c om p r is in g in c om b in a t ion t h e s t e p s of de
c om p os in g dic h lor oe t h a n e t o p r odu c e a m ix t u r e c on t a in in g
v in yl c h lor ide , h ydr og e n c h lor ide , a n d u n r e a c t e d dic h lor o
e t h a n e ; p r e p a r in g a liq u id p or t ion a n d a g a s e ou s p or t ion
f r om s a id m ix t u r e ; dis t illin g a t le a s t p a r t of t h e liq u id
p or t ion of s a id m ix t u r e t o p r odu c e a g a s e ou s s t r e a m c on
t a in in g v in yl c h lor ide , h ydr og e n c h lor ide a n d a q u a n t it y of
u n r e a c t e d dic h lor oe t h a n e , a n d a liq u id s t r e a m c om p r is in g
s u b s t a n t ia lly p u r e u n r e a c t e d dic h lor oe t h a n e ; f u r t h e r dis
t illin g s a id g a s e ou s s t r e a m in c om b in a t ion wit h a t le a s t
p a r t of t h e g a s e ou s p or t ion of s a id m ix t u r e t o p r odu c e
a f ir s t g a s e ou s e f f lu e n t c om p r is in g s u b s t a n t ia lly p u r e h y
dr og e n c h lor ide , a s e c on d g a s e ou s e f f lu e n t c om p r is in g s u b
s t a n t ia lly p u r e v in yl c h lor ide , a n d a liq u id e iliu e n t c on
t a in in g u n r e a c t e d dic h lor oe t h a n e a n d a q u a n t it y of v in yl
c h lor ide ; a n d r e c yc lin g s a id liq u id e iiiu e n t t o b e f u r t h e r
dis t ille d wit h s a id a t le a s t p a r t of t h e liq u id p or t ion of
s a id m ix t u r e .
10
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50
60
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B RIEF DES CRIPTION OF TH E DRAWING
For a m or e c om p le t e u n de r s t a n din g of t h e p r e s e n t in
v e n t ion , r e f e r e n c e is m a de t o t h e a c c om p a n yin g dr a win g ,
wh ic h is a dia g r a m m a t ic illu s t r a t ion of a s ys t e m wh ic h
m a y b e s u it a b ly e m p loye d t o c on du c t t h e p r oc e s s a s h e r e
in a f t e r de s c r ib e d.
DES CRIPTION OF TH E PREFERRED
EM B ODIM ENTS
Dic h lor oe t h a n e ( e it h e r 1, 1- dic h lor oe t h a n e or 1, 2 - di
c h lor oe t h a n e ) is f e d b y lin e 1 in t o a t h e r m a l c r a c k in g
z on e , e . g . a f u r n a c e , wh ic h m a y b e a n u n p a c k e d r e a c t ion
v e s s e l s u p p lie d wit h h e a t in g m e a n s . Th e p r e s s u r e of t h e
g a s e ou s r e a c t a n t s wit h in t h e z on e is m a in t a in e d a t f r om
a b ou t a t m os p h e r ic p r e s s u r e t o le s s t h a n a b ou t 100 p ou n ds
p e r s q u a r e in c h g a u g e a n d p r e f e r a b ly f r om a b ou t 2 5
p ou n ds p e r s q u a r e in c h g a u g e t o a b ou t 100 p ou n ds p e r
s q u a r e in c h g a u g e . Th e t e m p e r a t u r e Wit h in t h e z on e is
g e n e r a lly m a in t a in e d a t f r om a b ou t 800 F. t o a b ou t 900
F. a n d p r e f e r a b ly f r om a b ou t 82 5 F. t o a b ou t 875 F.
Th e g a s e ou s p r odu c t s t r e a m f r om t h e t h e r m a l c r a c k in g
z on e is wit h dr a wn v ia lin e 2 a t a t e m p e r a t u r e of f r om
a b ou t 82 5 F. t o a b ou t 875 F. a n d q u e n c h e d b y a c ir
c u la t in g liq u id s t r e a m 4 f r om a q u e n c h in g z on e , e . g .
k n oc k ou t dr u m A, t o r e du c e t h e t e m p e r a t u r e of s t r e a m 2
t o a b ou t 2 50 F. a n d t h e r e b y f or m a g a s e ou s p h a s e a n d a
liq u id p h a s e . S t r e a m 4 is s u p p lie d b y c ir c u la t in g a p a r t
of t h is liq u id p h a s e . A s m a ll p a r t of s t r e a m 4 c om p r is in g
c a r b on a n d t a r s m a y b e wit h dr a wn v ia s t r e a m 5 a n d s e n t
t o wa s t e dis p os a l if n e c e s s a r y.
Th e g a s e ou s p h a s e is wit h dr a wn v ia lin e 3 f r om t h e
q u e n c h in g z on e a n d p a s s e d t o a c on de n s a t ion z on e , c _ g .
c on de n s e r B . Th e r e in t h e v a p or s t r e a m is p a r t ia lly c on
de n s e d t o a liq u id p or t ion a n d a g a s e ou s p or t ion , wh ic h
c oe x is t a s a t wo- p h a s e m ix t u r e . Th is t wo- p h a s e m ix t u r e
is p a s s e d f r om t h e c on de n s e r v ia lin e 6 in t o a dis e n g a g in g
z on e or a k n oc k ou t dr u m C Wh e r e f r om t h e liq u id p or t ion ,
wh ic h is c om p os e d p r in c ip a lly of dic h lor oe t h a n e , is r e
m ov e d v ia lin e 7. Pa r t of t h e liq u id p or t ion is r e c yc le d t o
t h e q u e n c h in g z on e v ia lin e 8 t o b e r e u n it e d wit h t h e liq u id
p h a s e . Th e r e m a in de r of s t r e a m 7 is p a s s e d v ia lin e 18
t o a dis t illa t ion z on e , p r e f e r a b ly t h ou g h n ot n e c e s s a r ily a
s in g le c olu m n , wh e r e in a p r e s s u r e of f r om a b ou t 3 0
p ou n ds p e r s q u a r e in c h g a u g e t o a b ou t 60 p ou n ds p e r
s q u a r e in c h g a u g e is m a in t a in e d. Th is Zon e is de p ic t e d in
t h e dr a win g a s a s in g le c olu m n a n d is la b e lle d t h e Di
c h lor oe t h a n e Colu m n .
Th e g a s e ou s p or t ion f r om dr u m C is Wit h dr a wn v ia
lin e 9 a t a t e m p e r a t u r e of f r om a b ou t 90 F. t o a b ou t
110 F. a n d a p r e s s u r e of f r om a b ou t 3 0 p ou n ds p e r
s q u a r e in c h g a u g e t o a b ou t 50 p ou n ds p e r s q u a r e in c h
g a u g e a n d is c om p r e s s e d t og e t h e r wit h s t r e a m 10, a g a s e
ou s s t r e a m f r om t h e Dic h lor oe t h a n e Colu m n , in a c om
p r e s s ion z on e , e . g . c om p r e s s or D, t o a p r e s s u r e of le s s
t h a n 3 00 p ou n ds p e r s q u a r e in c h g a u g e a n d p r e f e r a b ly
wit h in t h e r a n g e of f r om a b ou t 150 p ou n ds p e r s q u a r e
in c h g a u g e t o a b ou t 2 00 p ou n ds p e r s q u a r e in c h g a u g e .
In a t yp ic a l p r oc e s s r u n , s t r e a m 11 c om p r is e s a b ou t 55
p e r c e n t h ydr og e n c h lor ide , a b ou t 43 p e r c e n t v in yl c h lo
r ide a n d a b ou t 2 p e r c e n t dic h lor oe t h a n e . Th e t e m p e r a
t u r e of t h e c om p r e s s e d s t r e a m r a n g e s f r om a b ou t 3 15
F. t o a b ou t 3 3 5 F.
Th e c om p r e s s e d s t r e a m 11 is c oole d in c oolin g z on e E
t o a t e m p e r a t u r e of f r om a b ou t 50 F. t o a b ou t 150 F. ,
a n d p r e f e r a b ly f r om a b ou t 90 F. t o a b ou t 110 F. , t o
f or m a t wo- p h a s e liq u id- g a s s t r e a m , a n d t h is s t r e a m is
t r a n s m it t e d b y lin e 12 t o a f r a c t ion a t ion z on e , p r e f e r a b ly
t h ou g h n ot n e c e s s a r ily c om p r is in g t wo c olu m n s a s s h own
in t h e dr a win g . Th e f ir s t c olu m n , la b e lle d t h e H ydr og e n
Ch lor ide Colu m n , is m a in t a in e d a t a p r e s s u r e of f r om
a b ou t 150 p ou n ds p e r s q u a r e in c h g a u g e t o a b ou t 2 00
3
p ou n ds p e r s q u a r e in c h g a u g e . Th is c olu m n c on t a in s dis
t illa t ion t r a ys or t h e ir e q u iv a le n t in t h e f or m of p a c k in g . '
Th e ov e r h e a d f r om t h is c olu m n , wh ic h c on t a in s s u b s t a n
t ia lly a ll of t h e h ydr og e n c h lor ide a s a s u b s t a n t ia lly p u r e
b y- p r odu c t , is wit h dr a wn v ia lin e 13 a t a t e m p e r a t u r e of
f r om a b ou t _ 2 0 F. t o a b ou t - ' 10 F. , a n d t h e h e a v y
e n ds of t h e c olu m n c on t a in in g p r im a r ily v in yl c h lor ide
a n d s om e u n r e a c t e d dic h lor oe t h a n e a r e r e m ov e d a t a
t e m p e r a t u r e of f r om a b ou t 160 F. t o a b ou t 180 F. a n d
t r a n s m it t e d Via lin e 14 t o a s e c on d dis t illa t ion c olu m n .
Th is c olu m n , la b e lle d t h e Vin yl Ch lor ide Colu m n , is
m a in t a in e d a t a p r e s s u r e of f r om a b ou t 140 p ou n ds p e r
s q u a r e in c h g a u g e t o a b ou t 160 p ou n ds p e r s q u a r e in c h
g a u g e . Fr om t h is c olu m n t h e r e m a in in g dic h lor oe t h a n e is
wit h dr a wn a t a t e m p e r a t u r e of f r om a b ou t 190 F. t o
a b ou t 2 10 F. in a b ot t om s s t r e a m h a v in g a s u b s t a n t ia l
q u a n t it y of v in yl c h lor ide t h e r e in . Th e v in yl c h lor ide
m a y r a n g e f r om a b ou t 40 we ig h t p e r c e n t t o a b ou t 60
We ig h t p e r c e n t of t h e b ot t om s s t r e a m . Th is s t r e a m is r e
c yc le d v ia lin e 15 t o t h e r s t dis t illa t ion z on e wh ic h is '
de p ic t e d a s t h e Dic h lor oe t h a n e Colu m n in t h e dr a win g .
S u b s t a n t ia lly p u r e v in yl c h lor ide is r e c ov e r e d f r om t h e
t op of t h e s e c on d c olu m n a t a t e m p e r a t u r e of f r om a b ou t
90 F. t o a b ou t 110 F. Th is s t r e a m is r e m ov e d v ia lin e
16 a n d s e n t t o s t or a g e . It is p os s ib le t o a c h ie v e s u b s t a n
t ia lly p u r e v in yl c h lor ide a n d dic h lor oe t h a n e b y m a k in g
of f s e t t in g s lop p y c u t s in t h e Vin yl Ch lor ide a n d Di
c h lor oe t h a n e Colu m n s . Th u s , wh ile p u r e v in yl c h lor ide
is r e m ov e d v ia lin e 16, a c on s ide r a b le a m ou n t of v in yl
c h lor ide is a ls o r e m ov e d v ia lin e 15 a lon g wit h u n r e a c t e d
dic h lor oe t h a n e . Th is s lop p y c u t is of f s e t in t h e Dic h lo
r oe t h a n e Colu m n wh ic h s e p a r a t e s t h e f e e d s t r e a m s 15 a n d
18 in t o a s t r e a m 17 of s u b s t a n t ia lly p u r e dic h lor oe t h a n e
a n d a n im p u r e s t r e a m 10 c on t a in in g a q u a n t it y of dic h lo
r oe t h a n e Wh ic h is s u b s e q u e n t ly r e t u r n e d t o t h e H ydr og e n
Ch lor ide Colu m n a n d Vin yl Ch lor ide Colu m n . S t r e a m 17
f r om t h e Dic h lor oe t h a n e Colu m n is r e m ov e d a t a t e m
p e r a t u r e of f r om a b ou t 2 70 F. t o a b ou t 2 90 F. a n d
a f t e r p u r ilic a t ion m a y b e r e c yc le d t o t h e t h e r m a l c r a c k
in g z on e .
As e x p la in e d, t h e p r e s e n t in v e n t ion u t iliz e s du a l dis
t illa t ion z on e s wh ic h c oa c t t o c a n c e l t h e e l e c t s of s lop p y
c u t s in e a c h a n d t h u s a c h ie v e s u b s t a n t ia lly p u r e p r odu c t
s t r e a m s a n d a s u b s t a n t ia lly p u r e r e c yc le s t r e a m Wh ile
S t ill e i e c t in g a c on s ide r a b le r e f r ig e r a t ion s a v in g . Th e
t e r m s lop p y is a wor d p e c u lia r t o t h e a r t . B y t h is t e r m
it is m e a n t t h a t a dis t illa t ion c olu m n is op e r a t e d u n de r
s u c h c on dit ion s t h a t a s u b s t a n t ia lly p u r e p r odu c t s t r e a m
is ob t a in e d. S u c h a p r odu c t s t r e a m m a y b e e it h e r t h e
ov e r h e a d or b ot t om s of t h e c olu m n , b u t n ot b ot h , s in c e
t h e ot h e r s t r e a m f r om t h e c olu m n is im p u r e wit h s om e
q u a n t it y of t h e m a t e r ia l c om p r is in g t h e p r odu c t s t r e a m .
A s lop p y c u t is t h e op p os it e of a s h a r p c u t wh ic h
m e a n s t h a t a dis t illa t ion c olu m n is op e r a t e d u n de r s u c h
c on dit ion s a s t o ob t a in a s u b s t a n t ia lly p u r e ov e r h e a d a n d
a s u b s t a n t ia lly p u r e b ot t om s . Colu m n s u t iliz in g s h a r p
c u t s a r e dii c u lt t o c on t r ol a n d r e q u ir e c on s ide r a b le r e
f r ig e r a t ion . Th e p r e s e n t in v e n t ion a v oids t h e s e diiiic u lt ie s
b y u t iliz in g s lop p y c u t s . An d, t h r ou g h c oa c t in g dis t illa
t ion z on e s , t h e im p u r e ov e r h e a d f r om t h e r s t z on e is
t r a n s f or m e d in t h e s e c on d z on e in t o a - p u r e ov e r h e a d
a n d im p u r e b ot t om s , a n d t h e im p u r e b ot t om s f r om t h e
s e c on d z on e is r e t u r n e d t o t h e iir s t z on e t o b e t r a n s f or m e d
in t o a p u r e b ot t om s a n d a n im p u r e ov e r h e a d. H e n c e , t h e
t wo s lop p y c u t s c a n c e l ou t a n d a p u r e p r odu c t ov e r
h e a d a n d a p u r e r e c yc le b ot t om s a r e a c h ie v e d.
In or de r t h a t t h os e s k ille d in t h e a r t c a n t h u s a p p r e c ia t e
t h e p r oc e s s of t h is in v e n t ion , t h e f ollowin g e x a m p le s a r e
g iv e n b y wa y of de s c r ip t ion a n d n ot b y wa y of lim it a t ion .
Ex a m p le I
1, 2 - dic h lor oe t h a n e a t 90 p . s . i. g . a n d 3 50 F. a n d c h lo
r in e a t 90 p . s . i. g . a n d 12 0 F. we r e f e d in t o a n u n p a c k e d
c r a c k in g f u r n a c e . Th e t e m p e r a t u r e wit h in t h e f u r n a c e wa s
m a in t a in e d a t f r om a b ou t 3 50 F. t o a b ou t 850 F. A
3 , 468, 967
3 0
40
45
60
65
70
75
s t r e a m wa s wit h dr a wn f r om t h e f u r n a c e wh ic h c on t a in e d
a b ou t 3 3 p e r c e n t 1, 2 - dic h lor oe t h a n e , a b ou t 3 3 p e r c e n t
v in yl c h lor ide a n d a b ou t 3 3 p e r c e n t h ydr og e n c h lor ide
a n d s m a ll a m ou n t s of ot h e r c h lor in a t e d c om p ou n ds s u c h
a s 1, 1, 2 - t r ic h lor oe t h a n e . Th is s t r e a m f r om t h e f u r n a c e
Wa s a t a t e m p e r a t u r e of a b ou t 850 F. a n d a p r e s s u r e of
a b ou t 60 p . s . i. g . Th e s t r e a m wa s q u e n c h e d a n d f e d in t o
a k n oc k ou t dr u m . A liq u id s t r e a m f r om t h e k n oc k ou t
. dr u m a t 2 2 5 F. wa s r e c ir c u la t e d a s a q u e n c h m e diu m .
A v a p or s t r e a m f r om t h e dr u m a t 2 2 5 F. a n d 55 p . s . i. g .
wa s wit h dr a wn a n d p a s s e d t o a c on de n s e r , p a r t ia lly c on
de n s e d a n d c oole d t o a t e m p e r a t u r e of 100 F. , a n d t h e n
s e n t t o a dis e n g a g in g dr u m wh e r e in t h e s t r e a m wa s s e p a
r a t e d in t o a liq u id a n d a g a s p h a s e . Th e liq u id p h a s e wa s
c om p os e d p r im a r ily of 1, 2 - dic h lor oe t h a n e ; 70 we ig h t p e r
c e n t of t h is liq u id wa s r e c yc le d b a c k t o t h e k n oc k ou t
dr u m . Th e b a la n c e of t h e liq u id wa s p a s s e d t o a Dic h lor o
e t h a n e Colu m n wh ic h wa s op e r a t e d a t a p r e s s u r e ot "
a b ou t 50 p . s . i. g . Th e g a s e ou s p h a s e , wh ic h wa s c om p os e d
p r im a r ily of v in yl c h lor ide a n d h ydr og e n c h lor ide , wa s
p a s s e d a t a p r e s s u r e of a b ou t 45 p . s . i. g . a n d a t e m p e r a t u r e
of a b ou t 100 F. a lon g Wit h a v a p or s t r e a m f r om t h e Di
c h lor oe t h a n e Colu m n a t a t e m p e r a t u r e of 100 F. in t o a
c om p r e s s or wh e r e in t h e p r e s s u r e wa s r a is e d t o a b ou t 2 00
p . s . i. g . a n d t h e t e m p e r a t u r e wa s r a is e d t o a b ou t 3 3 5 F.
Th is c om p r e s s e d s t r e a m wa s c oole d in a h e a t e x c h a n g e r
t o a t e m p e r a t u r e of a b ou t 100 F. a n d s e n t t o a H ydr o
g e n Ch lor ide Colu m n . Th is dis t illa t ion c olu m n wa s
e q u ip p e d wit h s t a n da r d dis t illa t ion t r a ys a n d a r e u x
c on de n s e r a n d wa s op e r a t e d a t a p r e s s u r e of , 170 p . s . i. g .
S u b s t a n t ia lly p u r e h ydr og e n c h lor ide wa s r e c ov e r e d f r om
t h e ov e r h e a d of t h e c olu m n a t a t e m p e r a t u r e of _ 15 F. ;
t h e b ot t om s , c om p os e d of v in yl c h lor ide a n d 1, 2 - dic h lor o
e t h a n e a t a t e m p e r a t u r e of a b ou t 170 F. , wa s f e d in t o a
Vin yl Ch lor ide Colu m n e q u ip p e d Wt ih t r a ys a n d a r e f lu x
c on de n s e r a n d op e r a t e d a t a p r e s s u r e of 150 p . s . i. g . S u b
s t a n t ia lly p u r e v in yl c h lor ide wa s r e c ov e r e d a s t h e ov e r
h e a d a t a t e m p e r a t u r e of 100 F. Th is v in yl c h lor ide
p r odu c t c on t a in e d e s s e n t ia lly n o 1, 2 - dic h lor oe t h a n e . Th e
b ot t om s f r om t h e v in yl c h lor ide c olu m n a t a t e m p e r a t u r e
of 2 05 F. a n d c on t a in in g a b ou t 40 we ig h t p e r c e n t of
v in yl c h lor ide a n d 60 we ig h t p e r c e n t of 1, 2 - dic h lor oe t h
a n e wa s r e c yc le d t o t h e Dic h lor oe t h a n e Colu m n .
Ex a m p le 1I
Th e p r oc e s s of Ex a m p le I is r e p e a t e d s u b s t it u t in g 1, 1
dic h lor oe t h a n e f or 1, 2 - dic h lor oe t h a n e .
Th u s h a v in g f u lly de s c r ib e d t h e . in v e n t ion , wh a t is
c la im e d is : .
1. A p r oc e s s f or t h e p r odu c t ion of v in yl c h lor ide c oin
p r is in g in c om b in a t ion t h e s t e p s of :
( A) de c om p os in g dic h lor oe t h a n e t o p r odu c e a m ix t u r e
c on t a in in g v in yl c h lor ide , h ydr og e n c h lor ide , a n d
u n r e a c t e d dic h lor oe t h a n e ;
( B ) p r e p a r in g a liq u id p or t ion a n d a g a s e ou s p or t ion
b y p a r t ia lly c on de n s in g s a id m ix t u r e ;
( C) dis t illin g , a t le a s t p a r t of t h e liq u id p or t ion of s a id
m ix t u r e t o p r odu c e :
( a ) a g a s e ou s s t r e a m c on t a in in g v in yl c h lor ide ,
h ydr og e n c h lor ide a n d a q u a n t it y of u n r e a c t e d
dic h lor oe t h a n e , a n d
( b ) a liq u id s t r e a m c on s is t in g e s s e n t ia lly of s u b
s t a n t ia lly p u r e u n r e a c t e d dic h lor oe t h a n e ; V
( D) f r a c t ion a t in g s a id g a s e ou s s t r e a m in c om b in a t ion
wit h a t le a s t p a r t of t h e g a s e ou s p or t ion of s a id m ix
t u r e t o p r odu c e : l
( a ) a iir s t g a s e ou s e lu e n t c on s is t in g e s s e n t ia lly
of s u b s t a n t ia lly p u r e h ydr og e n c h lor ide ,
( b ) a s e c on d g a s e ou s e lu e n t c on s is t in g e s s e n t ia l
ly of s u b s t a n t ia lly p u r e v in yl c h lor ide , a n d
( c ) a liq u id e iu e n t c on t a in in g u n r e a c t e d di
c h lor oe t h a n e a n d a q u a n t it y of v in yl c h lor ide ;
a n d
( E) r e c yc lin g s a id liq u id e f f lu e n t t o b e f u r t h e r dis t ille d
3 , 468, 967
5
wit h s a id a t le a s t p a r t of t h e liq u id p or t ion of s a id
m ix t u r e .
2 . Th e p r oc e s s of c la im 1 wh e r e in s a id dic h lor oe t h a n e
is l, 2 - dic h lor oe t h a n e .
3 . Th e p r oc e s s of c la im 1 wh e r e in t h e p a r t ia l c on de n
s a t ion of t h e m ix t u r e b e g in s Wit h a q u e n c h b y r e c yc le d
c on de n s a t e .
4. Th e p r oc e s s of c la im 3 wh e r e in a t le a s t a p a r t of s a id
liq u id s t r e a m is r e c yc le d t o b e de c om p os e d t o s a id m ix
t u r e .
5. Th e p r oc e s s of c la im 3 wh e r e in t h e f r a c t ion a t ion
of s a id g a s e ou s s t r e a m in c om b in a t ion wit h a t le a s t a p a r t
of s a id g a s e ou s p or t ion is e i e c t e d in t wo dis t illa t ion c ol
u m n s t o p r odu c e :
( a ) s u b s t a n t ia lly p u r e g a s e ou s h ydr og e n c h lor ide f r om
t h e iir s t of t h e t wo c olu m n s ,
( b ) s u b s t a n t ia lly p u r e g a s e ou s v in yl c h lor ide f r om t h e
s e c on d of t h e t wo c olu m n s , a n d .
( c ) im p u r e liq u id dic h lor oe t h a n e c on t a in in g a s u b s t a n
t ia l q u a n t it y of v in yl c h lor ide f r om t h e s e c on d of
t h e t wo c olu m n s .
' 6. A p r oc e s s f or t h e p r odu c t ion of v in yl c h lor ide c om
p r is in g , in c om b in a t ion , t h e s t e p s of :
( A) de c om p os in g dic h lor oe t h a n e t o p r odu c e a m ix t u r e
c on t a in in g v in yl c h lor ide , h ydr og e n c h lor ide a n d u n
r e a c t e d dic h lor oe t h a n e ;
( B ) r a c t ion a t in g a t le a s t p a r t of a c on de n s e d p or t ion
of s a id m ix t u r e in a p r im a r y dis t illa t ion z on e t o
p r odu c e :
( a ) a g a s e ou s s t r e a m c om p r is in g v in yl c h lor ide ,
h ydr og e n c h lor ide a n d u n r e a c t e d dic h lor o
e t h a n e , a n d
( b ) a liq u id s t r e a m c on s is t in g e s s e n t ia lly of s u b
s t a n t ia lly p u r e u n r e a c t e d dic h lor oe t h a n e ;
( C) ir a c t ion a t in g s a id g a s e ou s s t r e a m t o p r odu c e :
( a ) a iir s t g a s e ou s e du e n t c on s is t in g e s s e n t ia lly
of s u b s t a n t ia lly p u r e h ydr og e n c h lor ide ,
( b ) a s e c on d g a s e ou s e f f lu e n t c on s is t in g e s s e n t ia l
ly of s u b s t a n t ia lly p u r e Vin yl c h lor ide , a n d
5
2 0
2 5
3 0
3 5
40
6
( c ) a liq u id e iu e n t c om p r is in g u n r e a c t e d di
c h lor oe t h a n e a n d v in yl c h lor ide ; a n d
( D) r e c yc lin g s a id liq u id e t llu e n t t o b e f u r t h e r dis t ille d
in s a id p r im a r y dis t illa t ion z on e .
7. Th e p r oc e s s of c la im 6 in c lu din g r e c yc lin g s a id
liq u id s t r e a m c on s is t in g e s s e n t ia lly of s u b s t a n t ia lly p u r e
u n r e a c t e d dic h lor oe t h a n e t o t h e de c om p os in g s t e p ( A) .
8. In t h e p r oc e s s of s e p a r a t in g v in yl c h lor ide a n d di
c h lor oe t h a n e f r om t h e m ix t u r e p r odu c e d b y low p r e s s u r e
c r a c k in g s a id dic h lor oe t h a n e t o p r odu c e v in yl c h lor ide ,
t h e im p r ov e m e n t a c c or din g t o wh ic h a t le a s t p a r t of s a id
m ix t u r e is p a r t ia lly c on de n s e d t o f or m liq u id a n d g a s e ou s
p or t ion s , a t le a s t p a r t of t h e liq u id p or t ion is s u b j e c t e d t o
a dis t illa t ion t o le a v e a s u b s t a n t ia lly p u r e dic h lor oe t h a n e
r e s idu e a n d dis t ill of f a g a s e ou s s t r e a m c om p r is in g t h e
h ydr og e n c h lor ide a n d v in yl c h lor ide c on t e n t s of s a id
liq u id p or t ion a lon g wit h s om e dic h lor oe t h a n e , t h e
g a s e ou s p or t ion of t h e p a r t ia lly c on de n s e d m ix t u r e a n d
t h e dis t ille d- of f g a s e ou s s t r e a m a r e c om b in e d a n d f r a c
t ion a t e d a t a h ig h p r e s s u r e a s c om p a r e d wit h t h e f or e
g oin g dis t illa t ion t o dr iv e of f s u b s t a n t ia lly a ll it s h ydr og e n
c h lor ide , t h e r e s idu e f r om t h a t f r a c t ion a t ion is dis t ille d
t o dis t ill of f s u b s t a n t ia lly p u r e v in yl c h lor ide a n d le a v e a
r e s idu e of dic h lor oe t h a n e c on t a in in g v in yl c h lor ide , a n d
t h e la s t m e n t ion e d r e s idu e is s u b j e c t e d t o dis t illa t ion in
a dm ix t u r e wit h t h e liq u id p or t ion of t h e p a r t ia lly c on
de n s e d r e a c t ion m ix t u r e .
Re f e r e n c e s Cit e d
UNITED S TATES PATENTS
6/ 1954 Kr e k e le r _ _ _ _ _ _ _ _ _ _ _ 2 60- 656
9/ 1962 H odg e s _ _ _ _ _ _ _ _ _ _ _ _ 2 60- 656
FOREIGN PATENTS
93 8, 82 4 10/ 1963 Gr e a t B r it a in .
B ERNARD H ELFIN, Pr im a r y Ex a m in e r
J . B OS KA, As s is t a n t Ex a m in e r
U. S . Cl. X . R.
2 , 72 4, 006
3 , 055, 955
2 03 - 75, 82