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Патент USA US2118901

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Patented May 31,1938
-
,
2,118,90
UNITED s'rA'ras PATENT ogrlc.
2,118,901
MANUFACTURE OF FLUOROHYDBO
CARBONB
Julius 861i. Leverkusen-I. a. ‘Work, as
Slim!‘ ‘01. G. Farbonindustrle
_
t
~
or
» r
cobalt, Frankiort-on-the-Main, Germany
I Nam-swing. Application February 12, rose.
881151 N0. 63,657
5 Claims; (Cl. 280-186)
This invention relates to the manufacture of
Example
The object of my present invention is to cause
1 litre of granulated activated charcoal is
stirred with an aqueous suspension of 50 grams
of mercuric oxide and-dried. The catalyst thus
?uoro-hydrocarbons.
hydrogen fluoride or an aqueous solution thereof
5 to react upon acetylene in the presence of mer
curic compounds and/or active carbons. Asmer
curic compounds there may be used, for instance,
mercuric oxide, chloride or ?uoride. In some
cases it is preferable not to use the mercury
0 catalysts as such, but to support them upon car
riers such, for instance, as activated ‘charcoals
_ which, moreover, have a catalytic e?ect by them
selves. The reaction may be carried out, for in
stance, by merely passing a gaseous mixture of
1 01 hydrogen ?uoride and acetylene over the catalyst.
The reaction sets in at ordinary temperature and
is exothermic, so that, owing to the heat liber
ated, the temperature of the catalyst rises spon
taneously, thus accelerating the reaction veloc
20 ity. Of course, it is also possible to-start the
reaction at elevated temperatures. Preferably
the gases passing over the catalyst are caused
to circulate and the resulting ?uorinated hydro
obtained is brought into an iron vessel.
fluoride is then circulated through the catalyst,
whereby the temperature is maintained at about
20 to 40° C. The
ture of the hydrogen 10
?uoride‘ may be effected in various ways, for in
stance by pumping the circulating gases before
entering the catalyst through an iron cylinder‘
containing anhydrous hydrogen ?uoride at 0° G.
A suitable amount of acetylene is admixed be‘ is
fore reaching the catalyst, and alter leaving it,
a corresponding amount of gases is. removed,
from which the ?uorinated hydrocarbons are sep—
aratecl. It is also possible to remove the prod»
ucts directly from the circulating gases, for in 20'
stance, by means of suitable solvents.
The physical constants of the products in ques
tion are the following:
tion vessel. The reaction temperature can be
regulated by varying the quantity and the com
position of the circulating gases. It is also pos
10 mm. Hg
262.8 mm. Hg
480.3 mm. Hg
30 reaction gases with indifferent gases, the per
g‘lmé?si?m. 3510:: heric ressure
“ Bollingirolnt,7cgmm.%g.
Critical temperature _____________ __°C__ + 417.5
Speci?c gravity-+265° C.._..,_____~._,_ ____ .._ =ilt6‘i5
Speci?c gravity—lll9° C-.._________.____ =il.998
Speci?c gravity-722° Cu--- ________ .. :Od?t .
1,1-di?a0rethane
4 O composition of the gas mixture and on the re
action conditions; in case acetylene is employed
in excess vinyl ?uoride is predominant; in case
the hydro?uoric acid is employed in excess the
Pressure
32 mm. Hg
444.7 mm. Hg
resulting product chie?y consists of di?uor
ethanes. The components can be separated by
fractional distillation either at ordinary tem
perature and increased pressure or at lower
temperatures and atmospheric pressure,
The products thus obtained are suitable for
various purposes, for instance, they are excellent
cooling media for refrigeration machines as they
are favorably distinguished from the correspond
ing chlorine compounds employed for this pur
55 pose by their non-poisonous nature. The new
products are further particularly valuable for the
manufacture of other ?uorinated hydrocarbons
and polymerization products.
The following example illustrates the invention
without, however, restricting it thereto:
30
I
Melting point ____________ -r _____ _._do__ —l6t.5 35
The reaction products formed depend on the
50
v
\
Pressure
sible to regulate the temperature byjmixing the
dro?uoric acid can be employed in form of an
aqueous solution or preferably in a water free
state.
/
Vinyl?uoride
carbons are removed from the gases as far as
25 possible on each return of the gases to the reac
centage of which, due tothe continuous removal
of the reaction products, increases during the
reaction. The preferred form of my invention
is to work at a temperature below about 40° 0.,
more particularly, below about 30° C. The hy
a mix
ture of gases containing acetylene and hydrogen
-
45
15:51am“;
5210s horic ressure
Boiling")8point, wgmmglg. .
Critical temperature _____________ __-°C_.. +1075
Meltingv point ____________ _.__._~__.___'do_.. -l.l.7
50
Speci?c gravity-78,8° C __.___.-____._____ =l.l2ii
Speci?c gravity 0° ___________________ ._ =0.958
Speci?c gravity+19°\-C _________ __' ____ _. =ll.9i2
Speci?c gravity-26° C_-__.._____..____._ =1.030
55
In “Handbuch der organischen Chemise” by
Beilstein IV edition, volume 1, page 186, a ?u
orethylene of a boiling point of —5l° C. is de
scribed. T’his ?gure is obviously due to a mis
take.
2
9,110,001
I claim:
to circulate through a catalyst selected from the
I. The process which comprises causing a mix
group consisting oi mercuric oxide and mercuric
ture of gaseous hydro?uoric acid and acetylene halides precipitated on a carrier, at such a rate
to circulate through a catalyst selected from the > as to prevent a rise 01' the reaction temperature
group consisting oi’ mercuric oxide and mercuric
above about 40° C.
halides at such a rate as to prevent a rise oi the
5; The process which comprises causing a mix
ture of gaseous hydro?uoric acid and acetylene
to circulate through a catalyst selected from the
group consisting of mercuric oxide and mercuric
reaction temperature above about 40° C.
2‘ The process as claimed in claim 1 wherein
mercuric ?uoride is employed as catalyst,
.
, 8. The process as claimed in claim 1 wherein - halides, precipitated on active carbon, at such a
the hydro?uoric acid is employed in a water tree . rate as to prevent a rise of the reaction tempera
state.
4. The process which comprises causing a mix
ture oi gaseous hydro?uoric acid and acetylene
ture above about 40° C.
JULIUS $61.1}.
CI
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