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Патент USA US2407814

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Patented Sept. 17, 1946
UNITED STATES PATENT OFFICE
2,407,813
PROCESS FOR MANUFACTTIRE 0F
SUPPORTED CATALYSTS
Harry A. Cheney, Oakland, Calif., assignor ‘to
Shell Development Company, San Francisco,
Calif., a corporation of Delaware
NoDrawing. Application June 21, 1943,
1
Serial No. 491,723
8 Claims. (Cl. 252—253)
2
H
This invention relates to the manufacture of
supported catalysts and relates more particularly
to the manufacture of catalysts comprising at
starting materials in the production of such prod
ucts as synthetic rubber and aviation fuels, ren
ders these catalysts exceedingly valuable. Of
least one metal of group VIII in combination with
these catalysts those comprising cobalt and/or
activated carbon which have been found to be
nickel in combination with activated carbon are
particularly effective in the conversion of ole?nic
particularly outstanding in their ability to effect
hydrocarbons to the lower boiling of the linear
this desirable reaction. Catalysts comprising co
polymers thereof, although they can be employed
balt are somewhat preferred over those compris
also in other types of hydrocarbon conversions.
ing nickel since they enable the conversion of the
Catalysts comprising elements of group VIII 10. ole?nic hydrocarbon to the lower boiling of the
?nd application’in a wide variety of processes,
linear polymers thereof at temperatures below
particularly those involving the conversion of hy
about 250° C. and preferably not substantially in
drocarbons such as,,for example, hydrogenation,
excess of about 150° C., whereas those comprising
polymerization, dehydrogenation, isomerization,
nickel generally require somewhat higher tem
gas pyrolysis, aromatization, etc. These metals 15, peratures, for example, up to about 350°C" to at
in a limited number of cases are used per se in
tain equivalent results.
relatively large fragments, pieces or chunks.
Methods heretofore generally employed in the
Most catalytic processes, however, require their
preparation of these catalysts comprise the im
usage in dispersed or ?nely-divided form de
pregnation of the carrier material with a solution
posited upon suitable support materials. Support 2O of a compound of an element of group VIII and
materials which may be employed comprise ma
subsequent heating of the resulting mixture at
terials of porous structure such as activated car
atmospheric pressure to effect decomposition of
bon, pumice, ?re brick, as well as synthetically
the deposited compound. Though variations in
prepared or naturally-occurring siliceous or alu
the method of preparing these catalysts have
minous materials such as, for example, clays, 25 heretofore been disclosed, such methods have
bentonite, bauxite, diatomaceous earth, silica gel,
generally been handicapped by serious disadvan
Activated Alumina, active or activated blends or
tages. The resultant catalysts are generally lack
compounds of silica and alumina, etc.. These
ing in uniformity with‘respect to activity. An
various types of carrier materials, though individ
other disadvantage is the often total absence of a
ually applicable as supports for the catalyst in a
particular characteristic such as, for example,
number of varying reactions, are, however, not
in the case of catalysts comprising an element of
equivalent. It has been found that character
group VIII and activated carbon, the ability to
istics of the catalysts are often dependent upon
catalyze the conversion of ole?ns to the lower
the nature of the particular support material
boiling of the linear polymers thereof,
employed and that the catalytic effect of the ele
The particular characteristic of the resultant
ments of group VIII may be modi?ed or changed 3.5, catalyst, it has been found, is dependent not only
by judicious selection of the particular support
upon the particular element of group VIII and
material combined therewith.
particular support material chosen but also upon
It has been found that catalysts comprising an
the particular compound of the element of group
element of group VIII in combination with acti
VIII used as a starting material. Thus, catalysts
vated carbon possess the ability of catalyzing the
conversion of ole?nic hydrocarbons to a product
comprising cobalt and/or nickel prepared by
which can be made to predominate in one or sev
eral of the lower boiling of the linear polymers
thereof at temperatures below about 350° C. A
particularly advantageous characteristic of this
catalyst combination is the ability to convert
even the lower boiling of the ole?nic hydrocar
bons, such as ethylene and propylene, to the
lower boiling of the linear polymers thereof to a
degree not possessed by other types of available
polymerization catalysts. Their ability to pro
mote the, conversion of ethylene and, propylene
to products predominating in butylene and hex
combining an activated carbon with a salt such
as the acetate and chloride of these metals and
subsequent reduction of these compounds pro
45 duces a catalyst possessing little, if any, ability
to promote’ the conversion of ethylene to the
lower boiling of the linear polymers thereof. On
the other hand, when utilizing a salt such as, for
example, a salt obtained by the interaction of
an element of group VIII with an oxygen-con
taining mineral acid such as, for example, cobalt
nitrate, nickel nitrate, etc., as starting materials,
the resulting catalysts possess‘ these desirable
characteristics to a surprising degree. However,
ylene, respectively, materials highly desirable as 55 in the production of the catalyst utilizing a salt
a
0
2,407,8ié
4
tion. The rotating type of apparatus is preferred
particularly prone to undergo spontaneous igni
not only because it enables the uniform distri
bution of the element of group VIII of the
periodic table throughout the porous mass but
methods utilized heretofore, often results in a
spontaneous decomposition to varying degrees, CI because it enables the attainment of more effec
tive mixing of the components without attrition
of the salt, thereby not only producing materials
to vany substantial‘degree of the‘ porous materials.
ineffective as catalysts but presenting serious
It furthermore enables more uniform heating of’
hazards. vWhen the production of some mate
the mixture, thereby providing more effective
rial in the absence of marked spontaneous de-"
control of the rate ,of decomposition as well as
composition is attained by such methods, the re‘
tion during heating, such as the nitrates, es
' pecially when conducted on a large-scale by
‘the more e?icient removal of decomposition
products and volatilized materials from the mass
under treatment.
sulting product nevertheless generally consists
of a substantial proportion which does not possess
the desired characteristic activity,‘ and‘ a1 remain
In preparing the'catalysts in accordance with
ing portion which is devoid to a markedv degree of
' uniformity with respect to composition and cata
' ‘the invention a suitable inorganic porous mate
lytic activity. This, it is found, is due toat least
a substantial degree to overheating of portions of
the catalyst resulting from spontaneous. ignition,
which though present to a lesser and‘ localized
degree is, nevertheless, often unavoidably en 20
countered to an’ undesirable‘ extent in’ methods of
catalyst preparation resorted to heretofore.
t is an object of the present invention to pro
vide ‘an improved method for the more eiiicient
rial, for examplaa porous granular carbon mag
terial, such as the activated vegetable or animal
charcoals as prepared and activated by various
commercial suppliers, is introduced into a sealed
vessel, preferably of the rotating type. Suction
is thereuponapplied to‘ reducethe'pressure with
in the vessel to subatmospheric pressure, for-“ex
ample, in the range of from about 1 to about
25 mm. of mercury.
While maintaining the sub‘
preparation of catalytic materials comprising an 25 atmospheric' pressure a compound of ‘an element
element of group VIII and a porous inorganic
of group VIII of the periodic table capable of
support material wherein the above disadvantages
are obviated to at least a substantial degree.
Another object of the invention is the provision
of an'improved method for the more vefficient
undergoing decomposition under the application
manufacture of catalysts comprising an element
of group VIII in combination with activated
carbon having greater uniformity with respect to
composition and‘ catalytic activity than those‘ ob
of heat is introduced into the vessel.
The'form in which‘ the compound of the ele
ment of group VIII is introduced into the vessel
will depend upon‘ the physical ‘characteristics ‘of
the particular compound used as ‘well as the na
ture ofthe catalyst ultimately desired. Thus; the
compound may be introduced in the form of‘a
A still 35 suspension in a suitable liquid; medium, or as a
further object of the invention is the provision
In the preparation of catalysts suitable for the
of ‘an improved method for the more e?icient pro
' tained by methods available heretofore.
solution‘.
duction of catalysts comprising cobalt and/or
nickel" in combination with activated carbon, par
ticularly effective in the conversion of ole?nic
hydrocarbons "to the 10Wer boiling of the linear
polymers thereof. Other objects ‘and advantages
of‘ the invention will become apparent from the
following description thereof.
.
I
conversion of ole?nic hydrocarbons to'the" lower
boiling of the linear polymers thereof at relatively
low temperatures, it is preferred'to’utilize the salt
' of an element of group VIIIfand' ‘an oxygen
containing mineral acid, for ‘example, cobalt
nitrate, as the starting material. When thus
utilizing the nitrates it is ‘preferred-to intro-
In accordance with the invention an inorganic
duce the salt in the form of a solution, for ~ex=-’
porous material is subjected to subatmospheric
pressure in a closed vessel. While maintaining
ample, an aqueoussolution, though solvents'othe'r
than water vmay be used.
The amount of salt
introduced into‘ the'vessel is dependent upon the
nature of the particular catalyst‘ to beprepared;
reductionby application of heat is deposited upon 50 In'the preparation of catalysts comprising cobalt
in combination with carbon, particularly effec
the supported material. The pressure is then
tive for the conversion of ole?ns, it is preferred‘
raised ‘to atmospheric or higherand vthereafter
again reduced to subatmospheric. pressure, pref- .
to add a su?icient amount of’ the cobalt 'saltto
erably not substantially in excess of about 150
the'carbon to, obtain a ?nished catalyst contain:
mm. of‘merc'ury. While maintaining the reduced 55 ing from about 3% to about "35%, and preferably
the 'reducedpressure, a compound of an element
of group VIII of the periodic table capable of
pressure, heat is applied to effect a gradual in_
crease in the temperature of the‘ mixture until
a temperature of about 400° C. and preferably
not substantially in excess of about 300° C. is
attained; volatilized materials as well as gaseous
. from about'5% to about 25% of cobalt.
Catalytic
materials comprising higher or lower concentra
tions of cobalt depending upon the particular
characteristics of the catalyst obtained may, how
ever, be prepared in accordance with» the process
decomposition products being meanwhile continu
of the invention.
ously removed from the vessel. When genera
The "concentration of the cobaltnitrate in“ the
tion of decomposition products to any substantial
solution used as the starting material may vary
degree has ceased the heating is discontinued.
within the scope of the invention. In general,
Thereupon the resulting catalyst is cooled while 65 it is preferred to employ a su?icient amount of
maintaining the subatmospheric pressure‘ condi
solvent for the cobalt nitrate to immerse the
greater part of the mass of ‘charcoal. The mix
tions.
’
ture is then agitated, for example, by rotation.
In apreferred method of ‘executing the inven
tion’the catalyst is prepared in a sealed rotating
of ‘the drum, until intimate‘ contact between the‘
drum provided with means for heating and cool 70 solution and charcoal'has been established. The
pressure'in the drum is then increased to at
ing its contents, removing volatilized materials
least atmospheric pressure.
.
'
therefrom and for varying the pressure therein.
Although this'type of apparatus is preferred, the
use of others comprisingstati-onary vessels is,
however, comprised within the scope of the‘ inven
By this‘procedure impregnation of the ‘cobalt
nitrate‘ into the inorganic porous'material is ob
tained to the 'degree'essential to the attainment‘
2,407,813.
5
of a catalyst possessing su?iciently high activity
ditions. The exact composition of the catalysts
as Well as the characteristics essential for its
use in such processes as the conversion of ole
comprising the elements of group VIII in- com
bination with carbon prepared in this manner
and which are particularly effective for the con
version or treatment of ole?nic hydrocarbons is
not readily determined. The element of group
?nic hydrocarbons to the lower boiling of the
linear polymers thereof. It has been found that
such a method resulting in deep impregnation is
particularly important when utilizing as the in
organic porous material, materials of such a
highly hydrophobic nature as charcoal, where
impregnation would not be attained to a suffi
VIII maybe present therein in elementary form,
in combination with oxygen or even in combina
tion with carbon, or may comprise a mixture of
these various forms. The carbon in the particu
lar catalysts comprising this material in com.
cient extent by merely ‘wetting it with the solu
bination with an element of group VIII prepared
tion of the element of group VIII at atmospheric
in accordance with the method of the invention
pressure. The invention is, however, not neces
is not merely a diluent or support material but
sarily limited to this particular method of impreg
nating the porous support material and at times, 15 an active component of the catalyst, in the ab
sence of which the catalytic effect upon such
depending upon the use to which the ?nished
reactions as the conversion of normally gaseous
catalyst is to be put, it may be desirable to ob
ole?nic hydrocarbons, particularly ethylene, to
tain the less active catalysts resulting from the
the lower boiling of the linear polymers thereof
mere impregnation of the porous materia1 at‘ at
is only negligible, if not completely absent.
mospheric pressure before proceeding with the
Materials capable of promoting or otherwise ‘
preparation in accordance with the invention.
modifying the activity of the ?nished catalyst
may be added thereto. Such materials compris
ing, for example, elements other than t'hoseo’f
group VIII or compounds thereof, may be added
in relatively small amounts to the materials in
.- After impregnation of the support material
with the cobalt nitrate solution suction is again
applied to the drum to reduce the pressure therein
below atmospheric, and preferably below about
150 mm. of mercury.
While maintaining the
to attain a gradual rise in the temperature of
the ‘contents without, however, occasioning any 0
the drum during the course of manufacture. The
porous material need not consist of a material
of but one type and may comprise a mixture of
two or more inorganic materials of porous struc
sudden substantial increase in temperature.
During the heating the volatilized solvent will
prising one or more elements of group ‘VIII in
reduced pressure heat is applied to the vessel,
which is preferably rotated during the process,
ture. Thus, in the preparation of catalysts com
combination with carbon, inorganic material‘
be constantly removed from the vessel as well
as decomposition products comprising oxides of
nitrogen resulting ‘from the decomposition of the
cobalt nitrate. It has been found that under
these conditions gradual decomposition of a con
siderable portion of the cobaltm'trate will take
place even before complete removal of the solvent
has been accomplished. The heating is continued
until a temperature not substantially in excess
of about 400‘? C. and preferably about 300° C. is
attained. Acriterion ‘of the rate of temperature
increase is the volume of decomposition products
eliminated from the vessel. Increments in heat
input are applied when generation. in any sub
inert with respect to behavior of the catalyst
such as for example pumice,‘ crushed‘ ‘brick,
bauxite, clays, etc., may be admixed with ‘the
charcoal prior to preparation of the catalyst or
even during the course of its preparation‘.
Catalysts prepared in accordance with the
40 above method possess appreciable activity and
are ready to be utilized as such. If desired, how
ever, the catalyst may be subjected to additional
'
treatments culminating in still greater activity
of the catalysts thus produced. Suchadditional
treatments may comprise subjectionof the cata
lyst to higher temperatures in the order of for
example about 500° C. while sweeping with a gas
consisting of or comprising hydrogen, nitrogen,
ceased, or, preferably, the rate of heating is so
normally gaseous paraf?nic hydrocarbons, such
regulated to maintain a constant rate of evolu
tion of the decomposition products. When the 5,0 as methane, ethane, propane, or mixtures thereof.
A method particularly effective for further in
prescribed maximum temperature range is at
creasing the activity of the catalysts of the inven
tained the heating is continued until generation
tion comprises their subjection toan elevated
of decomposition products is no longer ascertain
temperature up to, for'example, about 500° C‘.,
able to any substantial extent.
stantial amount of decomposition products has
while maintaining them at a subatmospheric
pressure, preferably about 10 mm. mercury.
While maintaining the subatmospheric pres- '
sure in the drum the contents are cooled, for
example, to below about 50° C. and preferably
Example I
to about room temperature, before raising the
pressure therein by admission of air or other
1300 grams of cocoanut charcoal was charged
means. The catalyst may then be removed from 60 to a rotating drum and subjected to a subatmos
the drum Without any substantial deterioration
pheric pressure of 5 mm. mercury. While main
of the catalyst upon contact with air or during
taining this subatmospheric pressure, 12% grams
storage.
of Co (N03)2-6I-I2O dissolved in 1229 grams of
Under these conditions of preparing the cata
water was introduced into the drum. ‘The drum .
lyst it has been found that spontaneous ignition 65 was rotated to assure intimate mixing after
to any substantial degree of even such compounds
which the pressure was raised ‘to atmospheric.
as cobalt nitrate, so deleterious to the activity
After a period of about 10 minutes suction was
of the ?nished catalyst, and which effect is in
again applied to the vessel to reduce the pressure
herent to a degree often preventing economical
therein to 26 mm. mercury. Then while main
production of such catalysts by methods avail 70 taining this subatmospheric pressure and rotat
able heretofore, is completely avoided. The re
ing the drum heat was applied in such manner
sulting catalysts are furthermore not only ex
as to slowly raise the temperature of the contents
to 300° C. This total heating period was eleven
ceedingly uniform with respect to composition
hours.’ The contents of the drum were then
and activity but are unusually stable upon con
tact with the atmosphere and under‘ storage con
7.5.
cooled to 40° C. while maintaining the subatmos
7
25407313"
ph‘eric pressure. Air was then allowed to enter
the‘ drum‘ to attain atmospheric pressure and the
catalyst was removed therefrom. During this
method‘ of preparation sudden rises in tempera
ture indicative of spontaneous ignition of the
cobalt nitrate were absent andv a catalyst of ex
ceptional uniformity of composition was attained.
’s
atilize‘d materials and‘ decomposition products?
from the vessel substantially as rapidly as formed:
therein, continuing the heating until evolutionlo'f‘
any substantial amount of‘ decomposition prod‘
ucts has ceased, thereafter maintaining the con
tents of the vessel at a higher temperature not
substantially in eXcessVof about 500° C., cooling
140 cc. of the catalyst thus produced was placed
the contents of the vessel, and maintaininga
in a tubular stainless steel reactor and flushed
subatmospheric pressure below about‘ .150‘ mm.
with nitrogen for a period of 3vhours at a tem 10 of mercury in said vessel during said admixing,
perature of 300° C. Ethylene was then passed
heating and cooling steps.
over the catalyst at a temperature of 100° C.
3. In the preparation of catalysts comprising
and ata pressure of 800 pounds at the rate of 942
cobalt and activated carbon particularly effective.
grams of ethylene per liter of catalyst per hour.
in. the conversion of ole?nic hydrocarbons to the.
The operation was continued for a period of 16
lower boiling of the linear polymers thereof,_the
hours. A conversion of ethylene to normally liq
uid polymers of 57% was still obtained during
the.last 4 hours of the total operating period.
56% of the polymer produced consisted of butyl
method of obtaining catalysts of substantially im
proved uniformity with respect to composition
and catalytic activity which comprises admixing -
an aqueous oxygen containing mineral acid salt
ene.
20 of cobalt capable of undergoing substantial .de
'
EatamLpZe II
composition when subjected to heating attem
peratures below about 400° C. with activated car
A catalyst comprising cobalt in combination
with activated carbon was prepared from cocoa
bon in a closed vessel, applying heatto the ves
nut charcoal and cobalt nitrate under the condi
tions of Example I with the exception that the
sel under controlled conditions effecting a grad
ual increase in the temperature of the’contents
heating period was reduced to 101/2 hours. No
evidence of sudden temperature rise was noted
materials and decomposition products fromthe
during the’ production. of the catalyst and a cat
alyst of exceptional uniformity of composition
vessel substantially as rapidly as formed therein,
continuing the heating until evolution of any‘
thereof up to about 400° C., removingtvolatilized
30 substantial amount of decomposition products
was obtained.
has ceased, cooling the ‘contents of the vessel,
.140 cc. of the catalyst thus produced was
and maintaining a subatmospheric pressurebe~
Vplaced in a- stainless steel tubular reactor and
low about 150 mm. of mercury in said vessel dur
subjected to subatmospheric pressure of 1 mm.
ing said admixing, heating and cooling steps;
mercury for a period of 5 hours at a temperature
4. In the preparation of catalysts comprising
of 500° C; The catalyst was cooled and ethylene 35
cobalt‘ and activated carbon particularly e?ective'
passed through the reactor at. a temperature of
in the conversion of-ole?nic hydrocarbons to the
100° C., under atmospheric pressure and at a
lower boiling of the linear polymers thereof, the
?ow rate of 500 grams of ethylene per liter of
method of obtaining catalysts of substantially
catalyst per hour. During a 2.8-hour period of
improved uniformity with respect to composition
operation .280 grams of liquid polymer was pro
and catalytic activity which comprises admix
duced per liter of catalyst, 95% of which polymer
> -Was butylene.
I claim as my invention:
1. In ‘the preparation of catalysts comprising
ing an aqueous oxygen-containing mineral acid
salt'of cobalt capable of undergoing substantial
decomposition when subjected to" heating attem
' cobalt and activated carbon particularly effective 45 peratures below about 400° C. with activated car‘
in‘ the conversion of ole?nic hydrocarbons to the
bon in a close'dlvessel, applying heat to. the ves
sel' under controlled conditions effecting a grad
lower boiling of the linear polymers thereof, the
ual increase in the temperature of the contents
method of obtaining catalysts of substantially
thereof up to about 400° C., removing’ volatilized
improved uniformity with respect to composition
and catalytic activity which comprises admixing 50 materials and decomposition products from the
vesselsubstantially as rapidly as formed-therein,
aqueous cobalt. nitrate with activated carbon in
continuing the heating .until evolution of any
a closed vessel, applying heatto the vessel under
controlled conditions effecting a gradual increase
in the temperature of the contentsthereof up. to
substantial amount of decomposition products
has ceased, thereafter maintaining the contents
about 400° C., removing volatilized‘ materials and 55. of the vessel at a higher temperature not‘sub
stantially' inexcess of about 500° C., cooling the
decomposition products from the vessel substan
contents of the vessel and maintaining a sub
tially as rapidly as formed therein, continuing
atmospheric pressure below about 150 mm. of‘
the heating until evolution of any substantial
mercury in ‘said vessel vduring said admixing,
amount of decomposition products ‘has ceased,
cooling the contents of the vessel, and maintain 60 heatingiand cooling steps.
51 In the preparation of catalysts comprisingv
ing a subatmosph'eric pressure below about 150‘
a metal selected from the group consisting of
mm. of mercury in said vessel during said ad
cobalt and nickel and activated carbon particu
mixing, heating and coolinglsteps'
larly ‘effective in the conversion’ of ole?nic hydro
2. In the preparation of catalysts comprising
cobalt and activated carbon particularly effective 65 carbons to the lower boiling of the linear poly
mers thereof, the methodof ‘obtaining catalysts.
in the conversion of ole?nic hydrocarbons to
of substantially improved. uniformity with ‘re
the lower boiling of the linear polymersthereof,
spect tocomposition and catalytic activity which
the method of obtaining catalysts of substan
tially improved uniformity with respect to com
comprises admixing an aqueous solution of a ni
position and catalytic activitywhich comprises 70 trate of a metal selected from the group consist
admixing aqueous cobalt nitrate with activated
ing of cobalt and ‘nickel with activated carbon in
carbon in a closed vessel, applying heat to‘the
a closed vessel, applying heat to the vessel under
vessel under controlled conditions e?ecting a
controlled conditions effecting a gradual increase
gradual increase in the temperature of ‘the con
in the‘ temperature of the contents thereof up to
tents‘thereoi up to- about 400° C., removing vol-‘
about 400° vC., removing volatilized materialsand
2,407,813
decomposition products from the vessel substan
tially as rapidly as formed therein, continuing
the heating until evolution of any substantial
amount of decomposition products has ceased,
cooling the contents of the vessel, and maintain
ing a subatmospheric pressure below about 150
mm. of mercuiy in said vessel during said admix
ing, heating and cooling steps.
6. In the preparation of catalysts comprising
10
from the group consisting of cobalt and nickel
capable of undergoing decomposition at a tem
perature below about 400° C. with activated car
bon in a closed vessel, applying heat to the vessel
under controlled conditions effecting a gradual
increase in the temperature of the contents
thereof up to about 400° C., removing volatilized
materials and decomposition products from the
vessel substantially as rapidly as formed therein,
a metal selected from the group consisting of 10 continuing the heating until evolution of any
cobalt and nickel and activated carbon particu
substantial amount of decomposition products
larly effective in the conversion of ole?nic hydro
has ceased, cooling the contents of the vessel,
carbons to the lower boiling of the linear poly
and maintaining a subatmospheric pressure be
mers thereof, the method of obtaining catalysts
low about 150 mm. of mercury in said vessel dur
of substantially improved uniformity with re 15 ing said admixing, heating and cooling steps.
spect to composition and catalytic activity which
8. In the preparation of catalysts comprising
comprises admixing an aqueous solution of a
nitrate of a metal selected from the group con
a metal selected from the group consisting of
cobalt and nickel and activated carbon particu
sisting of cobalt and nickel with activated car
larly effective in the conversion of ole?nic hydro- _
bon in a closed vessel, applying heat to the vessel 20 carbons to the lower boiling of the linear poly
under controlled conditions effecting a gradual
mers thereof, the method of obtaining catalysts
increase in the temperature of the contents
of substantially improved uniformity with re
thereof up to about 400° C., removing volatilized
spect to composition and catalytic activity which
materials and decomposition products from the
comprises admixing an aqueous oxygen-contain
vessel substantially as rapidly as formed therein, 25 ing mineral acid salt of a metal selected from
continuing the heating until evolution of any
the group consisting of cobalt and nickel capable
substantial amount of decomposition products
of undergoing decomposition at a temperature
has ceased, thereafter maintaining the contents
below about 400° C. with‘ activated carbon in a
of the vessel at a higher temperature not sub
closed vessel, applying heat to the vessel under
stantially in excess of about 500° C., cooling the 30 controlled conditions effecting a gradual increase
contents of the vessel and maintaining a sub
in the temperature of the contents thereof up
atmospheric pressure below about 150 mm. of
to about 400° 0., removing volatilized materials
mercury in said vessel during said admixing,
and decomposition products from the vessel sub
heating and cooling steps.
stantially as rapidly as formed therein, continu
7. In the preparation of catalysts ‘comprising 35 ing the heating until evolution of any substan
a metal selected from the group consisting of
tial amount of decomposition products has
cobalt and nickel and activated carbon particu
ceased, thereafter maintaining the contents of
larly e?ective in the conversion of ole?nic hy
drocarbons to the lower boiling of the linear
polymers thereof, the method of obtaining cat
alysts of substantially improved uniformity with
respect to composition and catalytic activity
which comprises admixing an aqueous oxygen
containing mineral acid salt of a metal selected
the vessel at a higher temperature not substan
tially in excess of about 500° C., cooling the con
tents of the vessel and maintaining a subatmos
pheric pressure below about 150 mm. of mercury
in said vessel during said admixing, heating and
cooling steps.
'
HARRY A. CHENEY.
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