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Патент USA US2410890

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Patented Nov'. 12, 1946
2,410,890
UNITED STATES PATENT
OFFICE
' 2,410,890
METHOD OF PRODUCING CATALYST
Ralph Burgess Mason, Baton Rouge, La., assignor
to Standard Oil Development Company, a cor
poration of Delaware
No Drawing. Application J une'15, 1944,
Serial No. 540,549
1 Claim. (Cl. 252-254)
1
Table 1
The present invention relates to the novel fea
tures hereinafter disclosed in the speci?cation
and claim.
MoOa.Mg0.ZnO
The catalytic reduction of nitroaromatic Com
Catalyst
pounds to the corresponding aromatic amines has
‘
Sul?ded (A)
Reduced (B)
been accomplished heretofore. One of the im
portant problems involved in the successful com
Method of pretreat- Hydro__ Glass tube__ Glass tube.
mercial production of aromatic amines has to do
Wt. percent catalyst
33 _____ __ 33 _________ ._ 38
with the provision of a suitable catalyst for the
(on fee .
Diluent
______________
__
Xylene.
Xylene .... _. Alfkylate safety
operation. I have discovered a class of catalysts 10
ue.
which are eminently suitable for catalyzing the
Volumepercentdiluent. 80 ..... __
_ 80.
reduction of aromatic nitro compounds such as
Pressure, lbs/sq. in___“ 2,600. _
_ 2,600.
men .
nitro benzene, nitro toluene, nitro xylene, etc.,
Temperature,°F ____ _.
450 ____ __
Wt. percent conversion
100 ____ __
_
450.
13.
of feed.
to form the corresponding aromatic amine. These
catalysts consist of a mixture of metallic oxides 15
In sul?ding the catalyst, the same was treated
partially sul?ded. Preferably, the catalyst con
with a stream of gas containing nitrogen and hy
sists of a mixture of molybdenum oxide, mag
drogen sul?de in a glass tube. Any other con
nesium oxide and zinc oxide, partially sul?ded.
venient method of introducing sulfur into the
Brie?y, these catalysts consist of active hydro
genation catalysts admixed with the oxides of 20 catalyst may, of course, be used. In particular,
a good method for sul?ding the catalyst is to treat
calcium or magnesium, the latter being the spac
the oxide mixture with the hydrogen sul?de con
ing or supporting agent. In the preferred modi
?cation of my invention I have secured excellent
results with a partially sul?ded mixture of molyb
taining gas at a temperature of about 850° to 900°
F. at approximately one atmosphere pressure
denum oxide, magnesium oxide and zinc oxide, 25 whereupon the catalyst acquires about 15 to 25
weight per cent sulfur. Another method is to
form the sul?ded catalyst in situ in the reducing
superiority of the partialIY sul?ded catalyst.
zone. In the foregoing table the designation
The main object of my invention, therefore,
“Glass tube” means that the catalyst is sul?ded
has to do with improvements in catalysts suitable
and hereinafter I shall set forth data showing the
for use in the reduction of aromatic nitro com
pounds.
30 in a tube outside the reactor while the term
“Hydro” means that the sul?ding is accomplished
in the reactor. The term “Reduced” means that
Other and further objects of my invention will
the catalyst was treated with hydrogen but not
appear in the following more detailed description
‘with HzS or other form of sulfur.
and claim.
My catalyst is adapted for use in a continuous
35
In preparing the catalyst I proceed in a pre
process where the feed stock comprising a nitro
ferred modi?cation as follows:
aromatic passes continuously through a bed of
17 parts of MgO were mixed dry with 30‘ parts
catalyst. Thus for example, I may carry out the
of ZnO and 53 parts of M003, the parts being by
process in the type of apparatus shown in the
weight and su?icient water was added to make a 40 application of Cecil L. Brown, U. S. Serial No.
498,695, ?led August 14, 1943.
paste. The paste was dried at 250° F. and ex
Numerous modi?cations of my invention will
' truded to form rods say 1% of an inch in diameter
suggest themselves to those who are familiar with
and about 1A of an inch in length. Of course, the
this art.
size of the shaped bodies may vary considerably.
Instead of extruded rods, my catalyst may be in 45 What I claim is:
The method of forming a catalyst suitable for
the form of lumps, granules, pellets, pills, or any
promoting
the reduction of nitro aromatic com
convenient shape.
pounds which comprises mixing about 1''! parts of
In order to show the value of the foregoing par
MgO with 30 parts of ZnO, and 53 parts of M002,
tially sul?ded catalyst consisting of an equimo
adding su?‘lcient water to make a paste, drying
50
lecular mixture of molybdenum oxide, magnesium
the paste at about 250° F., extruding the paste to
oxide and zinc oxide, I made three runs in which
form shaped bodies, and thereafter sul?ding the
I reduced nitro xylene, in the presence of excess
catalyst by treating it with a volatile sul?de at
hydrogen over the amount theoretically required,
temperatures within the range of from 850° F. to
two (under A) in which the catalyst was partially 55 900° F. at one atmosphere pressure until the cata
sul?ded, and in the other (under B) the cata
lyst acquires from about 15-25 weight per cent of
lyst was not sul?ded. The operating conditions
sulfur,
RALPH BURGESS MASON.
and the results are set forth in. the table below:
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