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Патент USA US2404474

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Juìy 23, 1946.
R. B. coLLlNs
Filed Nov. 29, 1944
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Zizer‘moco egale `
Patented July 23, 1946
Robert B. Collins, Downers Grove, Ill., assignor to
Universal Oil Products Company, Chicago, Ill.,
a corporation of Delaware
Application November 29, 1944, Serial No. 565,769
4 Claims.
(Cl. ’Z3-15)
This invention relates to an improved type of
apparatus for the continuous determination of
tion concerns an apparatus for the continuous
determination of the chemical, composition of
flowing materials which comprises in combina
the chemical composition of various materials
tion an insulating conduit, means for passing a
and more particularly, an apparatus for the con
tinuous determination of carbonaceous deposit on Ca stream of material therethrough at a substan
tially constant rate, means for imposing a field
catalytic materials.
of high frequency >alternating electric current
During the treatment of hydrocarbons in
across a section of said conduit, and means
various processes, such as cracking, reforming,
measuring the temperature of said stream before
dehydrogenation, and the like, some of the charg
ing material is converted to a high molecular lll and after it passes through said ñeld of high
frequency alternating electric current.
weight carbonaceous deposit which accumulates
The method of analysis'which forms the basis
on the catalyst particles and is generally removed
for the apparatus of the present invention is de
by _combustion in order to render the catalyst suit
scribed in more detail and is claimed in copend
able for continued use. It is desirable during the
ing application Serial No. 565,694, filed November
operation of such processes to at all times know
29, 1944, by Herbert A. Hulsberg.
the amount of deposit on the catalyst in order
In general, the present apparatus depends
that the quantity of combustion air may be ac
curately controlled. This is especially true in
the so-called fluid catalyst cracking process be
cause unless the combustion air is accurately con
upon the heating eiîected by the radio frequency
field through which the material being analyzed is
20 passed. With a given frequency and current in
put, when the character of the material is such
as to absorb more heat energy, the heating effect
present in the eiiluent gas from the regenerator
will be greater and the temperature rise corre
and when such is the case a phenomenon known
spondingly higher. With the present apparatus,
as afterburning often takes place. The conven
tional method for the determination of carbona 25 as the stream of material is continuously passed
therethrough, the inlet and outlet temperatures
ceous deposit on the catalyst is by means of com
are measured and by use of a predetermined heat
bustion. This analytical method is slow and
ing curve the _analysis is made. This curve may
tedious and generally takes from 1 to 2 hours for
be drawn by calibrating the apparatus with
completion. In this length of time conditions in
the plant can deviate considerably from those de 30 known materials.
trolled there are times when excess oxygen is
The present invention, therefore, provides an
apparatus useful for the rapid measurement of
the carbonaceous deposit on the catalyst.
The present invention also provides a system
for the continuous determination of changes in
chemical composition of other materials as Well
as the amount of carbonaceous deposit on various
solid catalysts.
In making carbonaceous deposit determinations
with the apparatus of the present invention it is
essential that the moisture content of the catalyst
be maintained at a practical minimum in order
that the effect of water in the sample does not
offset the effect of the carbonaceous deposit on
the radio frequency loss. The radio frequency
employed is not particularly critical although
with higher frequencies it will be generally found
By means of the present invention a continuous 40 that the rate of heating is higher for a given cur
check may be had on the catalyst in the plant
at all times.
In prior methods and apparatus useful for the
determination of carbonaceous deposit on
catalyst, the general procedure is to withdraw a 45
sample from the plant and then analyze it batch
rent. In general, frequencies of about 15 mega
cycles or thereabouts are recommended, although
it is well within the scope of the invention to use
higher or lower frequencies. The current input
to the electrodes which should be employed is
dependent upon the speed at which it is desired
to pass the material through the apparatus.
Wise in combustion type apparatus. The com
The accompanying diagrammatic drawing and
bustion products are then collected and the
following description thereof are included in this
analysis determined from the quantities of the
various combustion products. The present inven 50 specification to more clearly point out the fea
tures and advantages of the present invention.
tion eliminates a considerable time lapse between
Figure 1 illustrates one form of the invention.
the taking of the sample and the i'lnal determina
Figure 2 shows a cross-sectional view taken as
tion and makes it possible to obtain the analysis
indicated by line 2-2 in Figure 1.
almost immediately after a sample is taken.
In one specific embodiment the present inven 55 Figure 3 illustrates a form of the invention
or similar material which has a very low radio
this particular form of the invention the passage
of material between the electrodes is regulated
by valve I9 in conduit I8 and valve 25 in conduit
26. Also in this form of the invention thermo
couples I3 and I5 are connected to a differential
type of instrument 21 which will give >a direct
frequency loss. This tube is connected by means
of flanges to conduit 2 which in turn is connected
the inlet and outlet of the'apparatus.
adapted for use in the determination of car
bonaceous deposit in a ñuid catalytic cracking
Referring now to Figures 1 and 2, I denotes an
insulating tube comprised of quartz, Pyrex glass,
reading of the temperature difference between
to a suitable source of supply of the material to
In operation, valves I9 and 25 are opened to
be analyzed. At its opposite end insulating tube
I is connected by means of suita-ble iianges or
other connecting means to conduit 3 in which is
disposed rotary valve 4. The purpose of valve 4
is to maintain a uniform rate of flow of material
the desired degree whereby the pressure Within
through the apparatus and in order to do this it '
is only necessary to rotate the valve at a sub
stantially constant speed by means of -a syn
chronous motor or the like.
Disposed along opposite sides of insulating
tube I are electrodes 5 and 6 which are respec
tively connected to radio frequency oscillator 'I
conduit 29 will act to force material through the
apparatus. yOscillator 'I is regulated to give the
desired frequency and current and the carbona
ceou's deposit analysis is continually made by
reference to the temperature differential indi
cated by instrument 21 as compared to that given
for known samples.
I claim as my invention:
l. An apparatus of the class described which «
20 comprises in combination an insulating conduit,
means for passing a stream of material there
through at a substantially constant rate, means
by means 'of 'conductors 8 and 9. The electrodes
may be secured to insulating tube I by means
for imposing a field of high frequency alternat
ing electric current across a section of said con
of cement, clamps or other suitable means. Pre
cautions must be taken to `prevent unnecessary 25 duit, and means for measuring the temperature
losses between the electrodes other than through
of said stream before and after it passes through
the material being tested. The current supplied
said field of high frequency alternating electric
to the electrodes is measured by means of radio
frequency ammeter I'il. Oscillator 'I may be any
2. An apparatus of the class described Which
of a ‘number of conventional oscillators ‘designed 30 comprises in combination a radio frequency insu
to give the necessary current and is supplied with
lating conduit, means for passing a stream of
power from a suitable source by means of con
material therethrough at a substantially constant
ductors II and I2. A thermocouple I3 is placed
rate, a _pair of electrodes disposed along opposite
in 'insulating tube I to measure 'the temperature
sides of a portion of said conduit and connected
of material 'entering the apparatus. It is well 35 to a radio frequency oscillator, and means for
within the scope of the 'invention to place this
measuring the temperature of said stream before
thermocouple in conduit 2. Suitable temperature
and after rit passes through said conduit between
indicating or recording means >le is 'connected
said electrodes.
to 'th'erm'ocouple I3. 'Temperature indicator or
3. An apparatus of the class described com
recorder 'M may be any standard potentiometer 40 prising in combination an insulating conduit
type instrument. At the loutlet end of the appa
connected at one end to a supply conduit con
ratu's, thermo’couple i5 is disposed within -insu
taining flow regulating means and at its op
lating tube I as shown or in conduit v3. This
posite end to a discharge conduit containing now
thermocouple ‘is connected to a suitable tempera
45 regulating’ means, means for imposing a ñeld of
ture indicating 'instrument I6.
high frequency alternating electric current across
Referring now to Figure 3, Vconduit -2 is shown
a ksection of said insulating conduit, a thermo
connected to cooler I'I which in turn is vconnected
couple in the inlet end of said insulating conduit,
by means ‘of conduit I8 ‘and valve I9 to conduit
anda ‘thermocouple in the` outlet end 'of said
2d. Cooler 'il is provided with inlet and ’outlet
insulating conduit.
connections 2| and 22 provided respectively with 50
4. The apparatus of `claim 3 further charac
valves 213 and 24 by means of which a `suitable
terized in that said thermocouples are connected
cooling medium may vbe passed ‘in 'indirect heat
to a differential temperature indicator.
exchange with the material to be analyzed. In
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