United S ta tes Pa tent [ 1 9 1

Hundeck et a l .
4 , 7 7 4 , 3 7 3
S ep . 2 7 , 1 9 8 8
[ 1 1 ] Pa tent Number:
[ 4 5 ] Da te o f Pa tent:
[ 5 4 ] PROCES S FOR MAKING
1 , 2 -DICHLOROETHANE
[ 7 5 ] Inv ento rs : J o a ch im Hundeck, B o nn; Ha ra l d
S ch ul z , Erf ts ta dt; Ha ns Hennen,
Hiirth , a l l o f Fed. Rep . o f Germa ny
[ 7 3 ] As s ig nee: Ho ech s t Aktieng es el l s ch a f t,
Fra nkf urt a m Ma in, Fed. Rep . o f
Germa ny
[ 2 1 ] Ap p l . No . : 5 5 4 , 5 8 6
[ 2 2 ] Fil ed: No v . 2 3 , 1 9 8 3
[ 3 0 ] Fo reig n Ap p l ica tio n Prio rity Da ta
Dec. 8 , 1 9 8 2 [ DE] Fed. Rep . o f Germa ny . . . . . . . 3 2 4 5 3 6 6
[ 5 1 ] Int. 0 1 . 4 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . c0 7 c 1 7 /0 2
[ 5 2 ] us . ( :1 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 7 0 /2 5 4 ; 5 7 0 /2 4 4 ;
5 7 0 /2 4 7
[ 5 8 ] Fiel d o f S ea rch . . . . . . . . . . . . . . . . . . . . . . . . 5 7 0 /2 5 4 , 2 4 4 , 2 4 7
[ 5 6 ] Ref erences Cited
U. S . PATENT DOCUMENTS
3 , 2 2 2 , 4 0 8 1 2 /1 9 6 5 S mith . . . . 1 1 . . . . . . . . . 5 7 0 /2 4 4
4 , 3 4 7 , 3 9 1 8 /1 9 8 2 Ca mp bel l . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 7 0 /2 5 4
FOREIGN PATENT DOCUMENTS
3 1 6 8 2 /1 9 6 6 J a p a n . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 7 0 /2 5 4
8 1 9 4 2 0 9 /1 9 5 9 United King do m 1 1 8 6 7 4 2 4 /1 9 7 0 United King do m . . . . . . . . . . . . . . . . 5 7 0 /2 5 4
Prima ry Exa miner-Ho wa rd T. Ma rs
[ 5 7 ] AB S TRACT
Th e dis cl o s ure rel a tes to a p ro ces s f o r ma king 1 , 2
dich l o ro eth a ne by rea cting eth yl ene with ch l o rine in a
s o l v ent in th e p res ence o f a ca ta l ys t, a t a temp era ture o f
a bo ut 2 0 to 2 0 0 C. a t a tmo s p h eric o r el ev a ted p res
s ure, a nd dis til l a tiv el y s ep a ra ting th e 1 , 2 -dich l o ro eth a ne
f ro m th e ch l o rina tio n mixture. Th e dis cl o s ure p ro v ides
mo re p a rticul a rl y f o r th e ca ta l ys t us ed to be a n a nh y
dro us tetra ch l o r0 f erra te( l -) o r a s ubs ta nce ca p a bl e o f
f o rming a tetra ch l o ro f erra te( l -) in th e rea ctio n mixture.
2 Cl a ims , N0 Dra wing s
4 , 7 7 4 , 3 7 3
1
PROCES S FOR MAKING 1 , 2 -DICHLOROETHANE
It is kno wn th a t 1 , 2 -dich l o ro eth a ne ca n be ma de by
rea cting eth yl ene with ch l o rine in l , 2 -dich l o ro eth a ne a s
a s o l v ent a nd rea ctio n medium. Th e p rincip a l by-p ro
duct o bta ined in th is rea ctio n is l , l , 2 -trich l o ro eth a ne '
wh ich o rig ina tes f ro m a s ubs titutio n rea ctio n dich l o ro
eth a ne is s ubj ected to . In o rder to o bv ia te th is s ubs titu
tio n rea ctio n, us e is ma de o f ca ta l ys ts wh ich co mp ris e
ch l o rides o f th e el ements bel o ng ing to g ro up s IV to VI
o f th e Perio dic S ys tem, a nd a re p a rtia l l y us ed in th e
p res ence o f o xyg en; mo re es p ecia l l y, a nh ydro us iro n
( III) ch l o ride wh ich is rea dil y a cces s ibl e a nd inexp en
s iv e is us ed.
Th e res ul ting crude ca ta l ys t-co nta ining dich l o ro eth
a ne is no rma l l y ta ken f ro m th e rea ctio n v es s el , trea ted
with wa ter o r a n a queo us a l ka l i meta l s o l utio n s o a s to
be f reed f ro m ca ta l ys t a nd h ydro g en ch l o ride co nta ined
in it, a nd dis til l a tiv el y wo rked up in kno wn ma nner.
Th e us e o f FeCl 3 a s a ca ta l ys t in th e a dditio n ch l o rina
tio n o f eth yl ene enta il s certa in a dv ers e ef f ects . In th e
p res ence o f wa ter, f o r exa mp l e, FeCl 3 h a s co rro s iv enes s
f o r meta l l ic ma teria l s s uch a s th o s e no rma l l y us ed f o r
ma king rea cto rs , co l umns o r h ea t exch a ng ers p ro v ided
o f co urs e th a t th es e co me into co nta ct th erewith . Need
l es s to s a y, ch l o rine o f co mmercia l p urity wh ich is no r
ma l l y us ed f o r ef f ecting th e ch l o rina tio n a l wa ys co n
ta ins tra ces o f mo is ture, a nd h ydro g en ch l o ride o rig i
na ting f ro m undes ira bl e s ide rea ctio ns .
Wh enev er it is des ira bl e f o r th e h ea t energ y s et f ree
during th e ch l o rina tio n o f eth yl ene to be util iz ed, it is
inv a ria bl y neces s a ry f o r th e rea ctio n to be ca rried o ut a t
temp era tures h ig h er th a n th e bo il ing p o int o f dich l o ro
eth a ne a t a tmo s p h eric p res s ure. In v iew o f th e f a ct th a t
co rro s iv enes s increa s es co ns idera bl y with increa s ing
temp era tures , it is indis p ens a bl e to ef f ect th e ch l o rina
tio n rea ctio n in a p p a ra tus l ined with co rro s io n-res is ta nt
ma teria l s wh ich na tura l l y a f f ect th e co mmercia l a ttra c
tiv enes s o f th e entire p ro ces s .
We h a v e no w f o und th a t a nh ydro us tetra ch l o ro f er
ra tes wh en us ed a s ca ta l ys ts in th e p ro ductio n o f 1 , 2
dich l o ro eth a ne a re o f co ns idera bl y reduced co rro s iv e
nes s th a n FeCl 3 f o r rea cto rs wh ich th ems el v es a re no t
co rro s io n p ro o f . In a dditio n to th is , th es e co mp o unds
h a v e been f o und f a v o ra bl y to in? uence by-p ro duct
f o rma tio n wh ich is reduced.
Th e p res ent inv entio n rel a tes mo re p a rticul a rl y to a
p ro ces s f o r ma king 1 , 2 -dich l o ro eth a ne by rea cting eth
yl ene with ch l o rine in a s o l v ent in th e p res ence o f a
ca ta l ys t a nd, if des ired, a n a g ent inh ibiting by-p ro duct
f o rma tio n, a t a temp era ture o f a bo ut 2 0 to 2 0 0 C. a t
a tmo s p h eric o r el ev a ted p res s ure, a nd dis til l a tiv el y s ep
a ra ting th e 1 , 2 -dich l o ro eth a ne f ro m th e ch l o rina tio n
mixture, wh ich co mp ris es : us ing , a s th e ca ta l ys t, a n
a nh ydro us tetra ch l o ro f erra te ( l -) o r a s ubs ta nce ca p a bl e
o f f o rming a tetra ch l o ro f erra te ( l -) in th e rea ctio n mix
ture.
A p ref erred f ea ture p ro v ides f o r th e ca ta l ys t to be a
tetra ch l o ro f erra te ( l -) th e ca tio n o f wh ich is a n a l ka l i
meta l o r a l ka l ine ea rth meta l o r a mmo nium io n. It h a s
a l s o been f o und p ref era bl e to us e th e ca ta l ys t in a co n
centra tio n o f a bo ut 0 . 0 0 5 to 0 . 5 weig h t %, ca l cul a ted a s
iro n( III) ch l o ride a nd ba s ed o n th e qua ntity o f s o l v ent.
A f urth er p ref erred f ea ture p ro v ides f o r th e s o l v ent
to be 1 , 2 -dich l o ro eth a ne a nd f o r o xyg en o r a ir to be
us ed a s th e inh ibito r.
2 0
3 0
4 0
4 5
5 0
5 5
6 5
2
Th e f o l l o wing s ta tements a re intended f urth er to
il l us tra te th e p ro ces s o f th is inv entio n.
Th e ca ta l ys ts s uita bl e f o r us e in th e p ro ces s o f th is
inv entio n ba s ica l l y co mp ris e a l l th o s e tetra ch l o ro f er
ra tes ( 1 -) wh ich h a v e a s o l ubil ity in th e s o l v ent, e. g .
dich l o ro meth a ne, s uf f icient f o r ca ta l yz ing th e rea ctio n.
Us e ca n mo re s p eci? ca l l y be ma de o f th e f o l l o wing
co mp o unds :
a mmo nium tetra ch l o ro f erra te ( l -) ( NH4 FeCl 4 )
s o dium tetra ch l o ro f erra te ( l ) ( Na FeCl 4 )
p o ta s s ium tetra ch l o ro f erra te ( l ) ( KFeCl 4 )
ma g nes ium-bis [ tetra ch l o ro f erra te ( l -) ] ( M g [ FeCl 4 ] 3 )
Th e ca ta l ys ts ca n be p ro duced in cus to ma ry ma nner.
Th e ca ta l ys ts ca n be p ro duced in cus to ma ry ma nner.
Anh ydro us a mmo nium tetra ch l o ro f erra te ( 1 -) ca n, f o r
exa mp l e, be o bta ined by mel ting a mixture o f s to ich io
metric p ro p o rtio ns o f a mmo nium ch l o ride a nd a nh y
dro us iro n( III) ch l o ride.
Th e ca ta l ys t s h o ul d g enera l l y be dis s o l v ed o r s us
p ended in th e s o l v ent p l a ced in a rea cto r. It is a l s o p o s s i
bl e h o wev er f o r th e ca ta l ys t to be p rep a red o uts ide th e
rea ctio n s o l utio n a nd f o r it to be s ucces s iv el y intro
duced into th e rea cto r. S til l f urth er, it is p o s s ibl e to
intro duce a nh ydro us FeCl 3 a nd a s eco nd a nh ydro us
co mp o nent s o l ubl e in th e rea ctio n medium a nd ca p a bl e
o f f o rming th e tetra ch l o ro f erra te into th e s o l v ent ini
tia l l y a dmitted to th e rea cto r. It is ? na l l y p o s s ibl e to
p rep a re th e tetra ch l o ro f erra te ( l -) in th e rea ctio n mix
ture by intro ducing e. g . ( NH4 ) 2 FeCl 5 . H2 O o r a tetra
ch l o ro f erra te ( 2 -) into th e rea ctio n mixture, a nd by
o xydiz ing th is l a tter a nio n in th e rea ctio n medium to
g iv e a tetra ch l o ro f erra te ( l -) .
Th e p res ent ca ta l ys ts ' ca n be s a id to co mp a re f a v o r
a bl y with th e p rio r a rt ca ta l ys ts ina s much a s th ey a re o f
co ns idera bl y reduced co rro s iv enes s f o r rea cto rs ma de
up o f no t co rro s io n p ro o f meta l s , co mp a red with th e
co rro s iv enes s enco untered in th e p rio r a rt meth o ds f o r
ma king 1 , 2 -dich l o ro eth a ne. It wa s a l s o f o und th a t a p a rt
f ro m mino r p ro p o rtio ns o f l , l , 2 -trich l o ro eth a ne ( a s th e
? rs t s ubs titutio n p ro duct) a nd a co rres p o nding mino r
p ro p o rtio n o f h ydro g en ch l o ride, p ra ctica l l y no f urth er
by-p ro ducts a re being f o rmed under th e p ro ces s co ndi
tio ns s el ected in a cco rda nce with th is inv entio n. Th e
rea ctio n s o l utio n rema ins cl ea r ev en a f ter rea ctio n o v er
a p ro l o ng ed p erio d p ro v ided th a t th e s o l utio n h a s a m
mo nium tetra ch l o ro f erra tes ( l -) co nta ined in it. It is
ev en p o s s ibl e f o r rea ctio n mixture rendered da rk during
th e rea ctio n to re-a s s ume a l ig h ter co l o ra tio n during th e
f urth er co urs e o f th e rea ctio n, up o n th e a dditio n o f th e
co mp o unds s p eci? ed h ereina bo v e. Th e p res ent p ro ces s
? na l l y ens ures a n a l mo s t qua ntita tiv e co nv ers io n ra te a t
h ig h s p a ce/time-yiel ds .
Th e p ro ces s o f th is inv entio n ca n be ca rried o ut, f o r
exa mp l e, in th e l o o p rea cto r des cribed in DE-OS No . 2 4
2 7 0 4 5 o r a ny o th er s uita bl e rea cto r.
Th e f o l l o wing Exa mp l es il l us tra te th e inv entio n.
EXAMPLES 1 -4
Abo ut 2 . 0 kg 1 , 2 -dich l o ro eth a ne co nta ining f ro m 0 . 1
to 0 . 3 weig h t % o f o ne o f th e dis s o l v ed ca ta l ys ts s p eci
? ed in th e Ta bl e h ereina f ter wa s intro duced into a g l a s s
l o o p rea cto r wh ich h a d a ca p a city o f a bo ut 2 l iters . Th e
a s cending p o rtio n o f th e rea cto r l o o p wa s p ro v ided
with a l a yer o f p a cking ma teria l . Dis p o s ed bel o w th e
l a yer o f p a cking ma teria l s o a s to o p en into th e rea cto r
4 , 7 7 4 , 3 7 3
3
were eth yl ene, ch l o rine a nd a ir inl ets f o r th e intro duc
tio n o f a bo ut 6 0 l /h ea ch o f eth yl ene a nd ch l o rine a nd
1 5 l /h a ir. Th e rea cto r l iquid wa s circul a ted in th e rea c
to r s ys tem in a cco rda nce with th e p rincip l e underl ying
a ma mmo uth p ump . During th e rea ctio n, a temp era ture
o f a bo ut 7 7 C. wa s f o und to es ta bl is h in th e rea ctio n
mixture.
Dich l o ro eth a ne in v a p o r f o rm wh ich ca me f ro m th e
rea cto r wa s co ndens ed in a wa ter co o l er a rra ng ed
a bo v e th e rea cto r. B y mea ns o f a co ndens a te dis tribut
ing mea ns , a co ndens a te p o rtio n co rres p o nding to th e
qua ntity p ro duced wa s ta ken f ro m th e co o l er wh il s t
co ndens a te in exces s wa s recycl ed to th e rea ctio n z o ne.
B y mea ns o f a co o l ing tra p , a f urth er dich l o ro eth a ne
p o rtio n wa s s ep a ra ted f ro m is s uing g a s wh ich co ns is ted
s ubs ta ntia l l y o f inert g a s es . Crude dich l o ro eth a ne with
th e co mp o s itio n indica ted in th e Ta bl e h ereina f ter wa s
o bta ined in a n a v era g e yiel d o f 2 6 7 g p er h o ur. In th is
co nnectio n, it s h o ul d be bo rne in mind th a t th e g a s
qua ntities intro duced were determined j us t by mea ns o f
f l o w meters . Des p ite th e f a ct th a t a s teel s tructure wa s
p l a ced in th e rea cto r, th e iro n co ntent o f th e rea ctio n
mixture rema ined unch a ng ed.
EXAMPLE 5
Th e p ro cedure wa s a s in Exa mp l e 1 but 2 0 7 2 g l , 2
dich l o ro eth a ne co nta ining 1 . 6 g dis s o l v ed FeCl ; wa s
intro duced into th e rea cto r. Th e s o l utio n co nta ined
0 . 0 7 6 weig h t % FeCl g , determined co l o rimetrica l l y.
Th e qua ntities o f eth yl ene a nd ch l o rine intro duced in
th e p res ence o f a ir underwent rea ctio n ins ide th e rea c
to r to g iv e crude dich l o ro eth a ne co nta ining 0 . 1 8 weig h t
% 1 , 1 , 2 -trich l o ro eth a ne.
Next, th e rea ctio n s o l utio n wa s a dmixed with 0 . 5 g
Mg Cl z . Th e exp eriment wa s co ntinued o v er a 4 week
co ntinuo us o p era tio n p erio d a nd a bo ut 2 6 5 g /h crude
p ro duct wa s o bta ined. Des p ite th e f a ct th a t a s teel s truc
ture wa s p l a ced in th e rea cto r, th e iro n co ntent o f th e
rea ctio n mixture rema ined unch a ng ed.
l , 2 -dich l o ro eth a ne wh ich wa s o bta ined in th e co n
dens er ( p ro duct A) a nd th e l iquid reta ined in th e rea cto r
( p ro duct B ) were a na l yz ed a nd th e f o l l o wing res ul ts
were o bta ined:
Pro duct A Pro duct 1 3
( wg t %) ( wg t %)
C2 H5 Cl < 0 . 0 0 2 < 0 . 0 0 2
l , 2 -EDC 9 9 . 9 7 9 9 . 8 4
1 , 1 , 2 -ETC 0 . 0 2 1 0 . 0 8 9
HCl < 0 . 0 0 l -
f urth er co mp o nents 0 . 0 0 7 0 . 0 7
EDC = LZ-dich l o ro eth a ne
ETC = l . l , 2 ' trich l o ro eth a ne
EXAMPLE 6
Th e p ro cedure wa s a s des cribed in Exa mp l e 5 but
2 1 5 5 g l , 2 -dich l o ro eth a ne co nta ining 1 . 7 g dis s o l v ed
iro n( III) ch l o ride wa s intro duced into th e rea cto r. Th e
s o l utio n co nta ined 0 . 0 8 3 weig h t % FeCl 3 , determined
co l o rimetrica l l y. Th e qua ntities o f eth yl ene a nd ch l o
rine intro duced in th e p res ence o f a ir underwent rea c
tio n ins ide th e rea cto r to g iv e crude dich l o ro eth a ne
co nta ining 0 . 1 2 weig h t % l , l , 2 -trich l o ro eth a ne.
Next, th e rea ctio n s o l utio n wa s a dmixed with 0 . 6 g
Na Cl a nd with a dditio na l l , 2 -dich l o ro eth a ne. l , 2
dich l o ro eth a ne ( p ro duct A) wa s o bta ined in th e co n
2 0
2 5
4 5
5 5
6 0
6 5
4
dens er. It wa s a na l yz ed a nd th e f o l l o wing res ul ts were
o bta ined.
Pro duct A
( \ v g t 7 r)
CZH5 Cl < 0 . 0 o 2
l , 2 -EDC 9 9 . 9 7
1 , 1 , 2 -ETC 0 . 0 2 5
HC] < 0 . 0 0 l
f urth er co mp o nents 0 . 0 0 4
Af ter co ntinuo us o p era tio n o v er a p erio d o f 1 0 da ys ,
a f urth er 1 . 7 g FeCl 3 a nd 0 . 6 g Na Cl were intro duced
into th e rea cto r l iquid s o th a t th e s o l utio n no w co n
ta ined 0 . 1 6 4 weig h t % iro n( III) ch l o ride. Pro duct A
o bta ined in th e co ndens er wa s a na l yz ed a nd th e f o l l o w
ing res ul ts were o bta ined:
Pro duct A
( wg t %)
C2 H5 Cl < 0 . 0 0 2
l , 2 -EDC 9 9 . 9 8
1 , 1 , 2 -ETC 0 . 0 1 2
HCI 0 . 0 0 1
f urth er co mp o nents 0 . 0 0 4
Af ter co ntinuo us o p era tio n o v er a f urth er p erio d o f 7
da ys , th e rea cto r l iquid wa s a dmixed o nce a g a in with
1 . 7 g FeCl g , a nd 0 . 6 g Na Cl s o th a t th e s o l utio n no w
co nta ined 0 . 2 4 8 wg t % iro n( III) ch l o ride. Pro duct A
o bta ined in th e co ndens er a nd th e rea cto r l iquid ( p ro d
uct B ) were co mp o s ed a s f o l l o ws :
Pro duct A Pro duct B
( wg t %) ( wg t %)
C3 H5 Cl < 0 . 0 0 2 < 0 . 0 0 2
1 . 2 -EDC 9 9 . 9 7 9 9 . 8 1
1 , 1 , 2 -ETC 0 . 0 1 8 0 . 0 6 8
HCl < 0 . 0 0 l
f urth er co mp o nents 0 . 0 0 4 0 . 1 2
EXAMPLE 7
A mixture o f 4 3 4 1 g l , 2 -dich l o ro eth a ne a nd 3 . 3 g
FeCl 3 wa s intro duced into a s tirring v es s el wh ich h a d a
v o l ume o f 5 l iters . Th e FeCl 3 -co ntent, determined co l
o rimetrica l l y, wa s 0 . 0 7 6 weig h t %. Next, 1 . 1 g Na g CO;
wa s a dded to th e s o l utio n wh ich wa s s tirred ma g neti
ca l l y. 6 0 l /h ch l o rine g a s a nd 1 5 l / h a ir were intro duced
th ro ug h a ? rs t inl et, a nd 6 0 l /h eth yl ene wa s intro duced
th ro ug h a s eco nd inl et p ro v ided with a f rit into th e f eed
mixture.
Dich l o ro eth a ne in v a p o r f o rm wh ich ca me f ro m th e
rea cto r wa s co ndens ed in a wa ter co o l er a rra ng ed
a bo v e th e rea cto r. B y mea ns o f a co ndens a te dis tribut
ing mea ns , a co ndens a te p o rtio n co rres p o nding to th e
qua ntity o f dich l o ro eth a ne p ro duced wa s ta ken f ro m
th e co o l er wh il s t co ndens a te in exces s wa s recycl ed into
th e rea ctio n z o ne. B y mea ns o f a co o l ing tra p , a f urth er
co ndens a te p o rtio n wa s s ep a ra ted f ro m th e is s uing g a s
co ns is ting s ubs ta ntia l l y o f inert g a s es .
Pro duct A o bta ined in th e co ndens er wa s a na l yz ed
a nd th e f o l l o wing res ul ts were o bta ined:
4 , 7 7 4 , 3 7 3
-co ntinued
Pro duct A Pro duct A
( wg t %) ( wg t 7 ( 7 )
C1 H5 Cl < 0 . 0 0 2 5 l , l . 2 -ETC 0 . 0 3
1 , 2 -EDC 9 9 . 9 6 l -l Cl 0 . 0 0 1
1 , 1 , 2 -ETC 0 0 3 1 f urth er co mp o nents 0 . 0 0 3
l -l Cl 0 . 0 0 2
f urth er co mp o nents 0 . 0 0 5 v
TAB LE
Ana l ys is o f crude p ro duct ( wg t %)
Furth er
Exa mp l e Ca ta l ys t A C1 H5 Cl l , 2 -EDC l , l , 2 -ETC HCl co mp o nents
I NH4 FeCl 4 0 . 1 5 0 . 0 0 4 9 9 . 9 3 0 . 0 6 0 . 0 0 2 0 . 0 0 3
2 ( CH3 ) ; NHFeCl 4 0 . 1 3 9 9 . 8 6 0 . 1 3 0 . 0 l 0 . 0 0 6
3 Na FeCl 4 0 . 1 4 < 0 . 0 0 2 9 9 . 9 4 0 . 0 3 0 . 0 0 2 0 . 0 0 5
4 KFeCl 4 0 . 2 4 < 0 . 0 0 2 9 9 . 8 6 0 . 1 3 0 . 0 0 3 0 . 0 0 6
A = Co ncentra tio n o f ca ta l ys t, ca l cul a ted a s FeCl g
Af ter o p era tio n o v er a p erio d o f 6 0 h o urs , th e s o l u
tio n wa s dil uted with 1 , 2 -dich l o ro eth a ne s o th a t its
iro n( III) ch l o ride co ntent s til l wa s 0 . 0 2 8 wg t %, deter
mined co l o rimetrica l l y. Af ter o p era tio n f o r a f urth er 4 0
h o urs , p ro duct A o bta ined in th e co ndens er wa s a na
l yz ed, a nd th e f o l l o wing res ul ts were o bta ined:
Pro duct A
( wg t %)
C2 l -l 5 Cl < 0 . 0 0 2
LZ-EDC 9 9 . 9 6
2 0
2 5
3 0
3 5
4 5
5 5
6 0
6 5
We cl a im:
1 . In th e p ro ces s f o r ma king 1 , 2 -dich l o ro eth a ne by
rea cting eth yl ene with ch l o rine in a s o l v ent in th e p res
ence o f a ca ta l ys t, a t a temp era ture o f a bo ut 2 0 to 2 0 0
C. a t a tmo s p h eric o r el ev a ted p res s ure, a nd dis til l a tiv el y
s ep a ra ting th e 1 , 2 -dich l o ro eth a ne f ro m th e ch l o rina tio n
mixture, th e imp ro v ement wh ich co mp ris es : us ing , a s
th e ca ta l ys t, a n a nh ydro us tetra ch l o ro f erra te ( l -) o r a
s ubs ta nce ca p a bl e o f f o rming a tetra ch l o ro f erra te ( 1 -) in
th e rea ctio n mixture in a co ncentra tio n o f a bo ut 0 . 0 0 5 to
0 . 5 weig h t %, ca l cul a ted a s iro n( III) ch l o ride a nd ba s ed
o n th e qua ntity o f s o l v ent, th e ca tio n o f th e tetra
ch l o ro f erra te ( l -) being a n a l ka l i meta l o r a l ka l ine ea rth
meta l o r a mmo nium io n.
2 . Th e p ro ces s a s cl a imed in cl a im 1 , wh erein th e
s o l v ent is 1 , 2 -dich l o ro eth a ne.
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