U.S. patent number 3,876,533 [Application Number 05/440,286] was granted by the patent office on 1975-04-08 for guard bed system for removing contaminant from synthetic oil.
This patent grant is currently assigned to Atlantic Richfield Company. Invention is credited to Gary A. Myers.
United States Patent |
3,876,533 |
Myers |
April 8, 1975 |
Guard bed system for removing contaminant from synthetic oil
Abstract
A method for removing a contaminant comprising at least one of
arsenic and selenium from a synthetic crude oil or fraction thereof
characterized by a multi-step process as follows. First, a guard
bed is prepared from a plurality of particles of material that is
either iron, cobalt, nickel, oxides or sulfides of these metals, or
a mixture thereof. Next, the synthetic crude oil is admixed with
hydrogen and flowed past the particles of material at a temperature
and pressure great enough and with a residence time sufficient to
allow the contaminant to be removed from the synthetic crude and be
deposited on at least the surface layer of the particles of
material. As the surface layer of the particles becomes
substantially saturated with the contaminant, they are removed from
the surface of the particles as small fines, entrained in the fluid
stream and flowed from the guard bed. The small fines having the
contaminant thereon are separated from the synthetic crude from
which the contaminant has been removed. Thereafter, the synthetic
crude oil is treated as desired. Also disclosed are specific
methods of effecting the removal and separation of the contaminant
and the fines; including specific and preferred process
details.
Inventors: |
Myers; Gary A. (Plano, TX) |
Assignee: |
Atlantic Richfield Company (Los
Angeles, CA)
|
Family
ID: |
23748177 |
Appl.
No.: |
05/440,286 |
Filed: |
February 7, 1974 |
Current U.S.
Class: |
208/251H;
208/88 |
Current CPC
Class: |
C10G
25/00 (20130101); C10G 45/04 (20130101); C10G
49/22 (20130101); C10G 45/02 (20130101) |
Current International
Class: |
C10G
1/00 (20060101); C10G 1/04 (20060101); C10g
013/06 () |
Field of
Search: |
;208/251R,253,251H,88,89,295 |
References Cited
[Referenced By]
U.S. Patent Documents
Foreign Patent Documents
Primary Examiner: Gantz; Delbert E.
Assistant Examiner: Nelson; Juanita M.
Attorney, Agent or Firm: Wofford, Felsman, Fails &
Zobal
Claims
What is claimed is:
1. A method of removing a contaminant comprising one of arsenic and
selenium from a synthetic hydrocarbonaceous fluid obtained from
normally solid coal, oil shale or tar sand, comprising the steps
of:
a. preparing a guard bed consisting essentially of a plurality of
particles of a material selected from the group consisting of iron,
cobalt, nickel, at least one oxide of said metals, at least one
sulfide of said metals and a combination thereof; said particles
being of a size sufficiently large to allow attrition of a
plurality of surface layers up to at least 60 microns in thickness
for exposing new, more active material;
b. admixing said hydrocarbonaceous fluid with hydrogen to form an
admixture of fluid streams;
c. removing said contaminant from said synthetic hydrocarbonaceous
fluid by flowing said admixture past said particles in said guard
bed at a temperature and pressure and with a residence time
sufficient to effect removal of said contaminant from said
synthetic hydrocarbonaceous fluid and depositing said contaminant
on the surfaces of said particles of material; said pressure being
at least 500 pounds per square inch gauge (psig), and said
temperature being at least 300.degree.F.;
d. substantially saturating the surface of said particles with said
contaminant to cause flaking of small fines which are substantially
saturated with contaminant from the surface of said particles to
expose new and more active surface for removing said
contaminant;
e. entraining said substantially saturated small fines in said
admixture of fluid streams and flowing both from said guard bed;
and
f. separating said substantially saturated small fines containing
said contaminant from said admixture of said fluid streams and said
fines to leave said hydrocarbonaceous fluid substantially free of
said contaminant.
2. The method of claim 1 wherein said temperature is in the range
of from about 650.degree. to about 850.degree.F. and said pressure
is at least about 1,500 psig.
3. The method of claim 1 wherein said hydrocarbonaceous fluid
substantially freed of contaminant is hydrotreated.
4. The method of claim 1 wherein said fines are removed from the
combined stream of gas, liquid and fines by filtration.
5. The method of claim 1 wherein:
a. a gas stream comprising hydrogen and gaseous hydrocarbonaceous
fluid is separated to leave a slurry of hydrocarbonaceous liquid
and said fines; and
b. said fines are thereafter separated from said slurry to leave an
effluent liquid stream comprising said hydrocarbonaceous liquid
without said contaminant.
6. The method of claim 5 wherein said gas and liquid streams are
recombined after said fines have been removed; and before being
hydrotreated.
7. The method of claim 6 wherein said gas is separated by a
gas-liquid separator and said fines are separated from the slurry
by filtration.
8. The method of claim 7 wherein said gas includes entrained small
fines and said entrained small fines are separated from said gas
stream by a cyclone separator before said gas stream is recombined
with said hydrocarbonaceous liquid.
9. The method of claim 6 wherein a slurry of hydrocarbonaceous
liquid and fines is separated from a combined stream by a cyclone
separator to leave gas, and said fines are thereafter separated
from said slurry by filtration; and said gas and liquid streams are
recombined and hydrotreated.
Description
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to a method of removing catalyst-poisoning
impurities, or contaminants; such as, arsenic or selenium; from
hydrocarbonaceous fluids; such as, synthetic crude oil and
synthetic oil fractions.
2. Description of the Prior Art
There has been a resurgence of interest in sources of energy that
were formerly noncompetitive. These sources of energy include the
shale oil, or kerogen, such as derived from oil shale; the fluids,
such as methanol or coal gas, that are synthesized from coal; the
bitumen from the tar sands and the like. Many of these
hydrocarbonaceous fluids contain contaminants, or impurities, that
would poison expensive catalysts, such as platinum catalysts and
the like, that are used in hydrogenation and other processes to
which these hydrocarbonaceous fluids must be subjected before they
can be satisfactorily used as sources of energy. The best prior art
of which I am aware is disclosed in a co-pending application Ser.
No. 314,015, filed Dec. 11, 1972, now abandoned in favor of Ser.
No. 421,139, filed Dec. 3, 1973, with co-inventor Donald K.
Wunderlich and entitled "Synthetic Oil Treatment." That descriptive
matter will be briefly summarized hereinafter for the reader's
convenience. The prior art has included a method for removing
arsenic from hydrocarbon charge stocks, such as described in U.S.
Pat. No. 2,778,779. Such methods have included using the iron,
nickel and cobalt oxides to remove arsenic from streams of
naturally occurring crude, such as naptha or straight run gasoline.
By employing the oxides at low temperature, such as from room
temperature to about 200.degree.F, by disregarding the atmosphere
under which the reaction takes place, and by using substantial
amounts of water, the oxide acts as an oxidizing agent and oxidizes
the arsenic to a water soluble arsenic oxide. In this way the
arsenic oxide is dissolved in the water and removed from the
naturally occurring crude oil or oil fraction.
Also, arsenic has been removed from similar naturally occurring
crude oils by contacting them with a metallic salt of a strong acid
at low temperature, such as room temperature, without regard to the
atmosphere under which the contacting takes place. In this
particular process, it was taught that oxides do not work for
removing arsenic and this process is disclosed in U.S. Pat. No.
2,781,297.
Processes that work for removing other contaminants, or
catalyst-poisoning materials, such as organo-metallic compounds
like iron porphyrins, are frequently inoperable for removing
impurities like arsenic. For example, the catalytic hydrogenation
of hydrocarbons to effect the precipitation of an insoluble iron
salt of the iron porphyrin within a hydrogenating catalyst, as
described in U.S. Pat. No. 3,496,099, cannot be employed
satisfactorily in removing arsenic from synthetic crudes or the
like.
The invention described in Ser. No. 314,015 improved significantly
on the prior art, but had one drawback that prevented its being
totally satisfactory. The contaminant tended to be concentrated in
a surface layer from about 5 to about 60 microns thick, so the
center portion of the larger pellets and the like were not useful
and available for removing the contaminant.
In fact, none of the prior art processes have been completely
satisfactory in removing catalyst-poisoning impurities, such as
arsenic, from synthetic oil fractions.
SUMMARY OF THE INVENTION
Accordingly, it is an object of this invention to provide a method
of removing contaminants from a feed stream of synthetic crude or
the like that does not require the use of aqueous, or hydrophilic,
solutions, and alleviates the difficulties of the prior art.
More specifically, it is an object of this invention to provide a
method of removing a contaminant from a feed stream that
accomplishes the foregoing object and provides a stable guard bed
that maintains a continuous high level of activity at all times,
yet can be operated with economically feasible equipment, such as
pressure vessels, separators and filters.
These and other objects will become apparent from the descriptive
matter hereinafter.
The foregoing objects are achieved in accordance with this
invention by the following multi-step process. First, a guard bed
is prepared from a plurality of particles of material that is
either iron, cobalt, nickel, oxides or sulfides of these metals, or
a mixture thereof. Next, the hydrocarbonaceous fluid is admixed
with hydrogen and flowed past the particles of material at a
temperature and pressure great enough and with a residence time
sufficient to allow the contaminant to be removed from the
synthetic crude oil and be deposited on at least the surface layer
of the particles of material. As the surface layer of the particles
becomes substantially saturated with the contaminant, they are
removed from the surface of the particles as small fines, entrained
in the fluid stream and flowed from the guard bed. The small fines
having the contaminant thereon are separated from the
hydrocarbonaceous fluid from which the contaminant has been
removed. Thereafter, the hydrocarbonaceous fluid is treated as
desired.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a flow diagram of one embodiment of this invention
employing filtering.
FIG. 2 is a flow diagram of the embodiment of FIG. 1 in which a gas
stream is separated before the filtering.
FIG. 3 is a flow diagram of the embodiment of FIG. 2 in which fines
are separated from the gas stream by a cyclone separator.
FIG. 4 is a flow diagram of the embodiment of FIG. 2 in which a
cyclone separator is employed to separate the gas stream before
filtering.
DESCRIPTION OF PREFERRED EMBODIMENTS
To facilitate understanding, the treatment of a stream of a
synthetic crude, commonly referred to as syncrude, with the
particles of the material for removing the contaminant will be
described hereinafter.
In carrying out the invention as outlined above, the guard bed,
abbreviated GRD BED in the figures, is formed by depositing
pellets, or other particles, of the material into a pressure vessel
adapted to withstand the pressure and temperature to effect the
removal of the contaminant of arsenic or selenium, whether in
elemental or combined form. The pellets, or particles of material,
may have any shape. The particles of material preferably have a
size large enough to allow attrition of a surface layer of fines
repeatedly in order to expose new and active material for removal
of the contaminant. Ordinarily, the particles of material will
comprise pellets from 1/8 to 1/4 inch or more in diameter and 1/4
inch or more in length such as are conventionally extruded for
various catalysts such as iron oxide shift catalysts. The particles
of material preferably have a surface area of at least one square
meter per gram, still more preferably, having a surface area of at
least 50 square meters per gram. The particles of material may
comprise active ingredient alone; such as, the iron oxide or iron
sulfide; or may comprise the active ingredient in combination with
a conventional support (carrier). Such conventional support may
comprise silica, alumina, magnesia, zirconia, thoria, zinc oxide,
chromium oxide, silicon carbide, naturally occurring carriers like
clay, Kieselguhr, Fuller' s earth, pumice, bauxite and the like, or
any combination of two or more such carriers, whether naturally
occurring or prepared.
After the syncrude has been mixed with hydrogen, the resulting
admixture is flowed into contact with the guard bed of the
particles of material with sufficient heat, pressure and residence
time to effect removal of the contaminant from the syncrude and
deposition of the contaminant into the matrix of at least the
surface layer of the particles of material. This may be thought of
as a reaction, or adsorption of the contaminant onto the particles
of the material. In any event, the contacting of admixture and the
particles of material is at a temperature of at least about
300.degree.F. and preferably at least about 650.degree.F. Still
more preferably, the contacting is at a temperature in the range of
from about 650.degree. to about 850.degree.F. The temperature may
be effected by heating the constituents individually before
admixing them, supplying heat to the admixture directly, or
supplying heat to the guard bed. Ordinarily, it is advantageous to
heat the fluid streams. The guard bed pressure vessel is, of
course, suitably insulated to prevent infeasible heat losses. The
guard bed is maintained at a pressure of at least about 500 pounds
per square inch gauge (psig), preferably, at least about 1,500
psig. Depending upon the particular circumstances, which can vary
widely, the residence times vary widely, but generally will be at
least about ten seconds to afford the syncrude to contact the guard
bed particles of material. This may be effected by a single large
guard bed or a plurality of serially and/or parallel connected
smaller and less expensive guard beds. Thus, the delineated heat,
pressure and residence time allows sufficient time for the syncrude
to intimately contact the particles of material and to have the
contaminant removed from the syncrude. Specifically, the
contaminant, such as arsenic, is dispersed in a surface layer of up
to about 60 microns or more of the matrix of the material in a
manner analogous to adsorption phenomena, as indicated
hereinbefore, such that the contaminant is removed in non-water
soluble form.
The invention may be understood by referring to the flow diagram of
FIG. 1. Therein, the syncrude plus hydrogen comes in through
incoming conduit 11 into the guard bed 13. In the guard bed, the
contaminant is removed from the syncrude and disposed in at least
the surface layer of the matrix of the particles of the material by
the intimate contact at the delineated temperature and
pressure.
As the surface layer of material becomes saturated with the
contaminant; for example, at a concentration in the range of 15-20
percent by weight of active material; the surface layer begins to
flake off in small fines to expose new active material. The reason
for this automatic flaking off of the surface layers to afford a
pseudo automatic regulation of the activity in the system, is not
exactly understood. The following theory is given by way of
explanation, although this invention is not to be limited to the
consequences of any theory, since it is operable whether or not the
theory is accurate. It is theorized that the arsenic is large
enough that when it is substituted into the matrix of the material
for the sulfur or oxygen, the matrix is disrupted. Once the
disruption becomes severe enough, the macroscopic particles, or
fines, flake off. The fines are entrained in the fluid stream and
carried out the effluent conduit 15. Initially, of course, there
will be no flaking off of the fines as long as there is sufficient
activity in the system. Once the activity begins to be reduced, or
diminished, however, the flaking will begin to expose new and more
active material, and afford an automatic regulation of the
activity.
The fines are carried with the liquid stream into the filter 17
where the fines are removed from the fluid stream by filtration.
The filter 17 may comprise any of the conventional type filters
that have been employed in this type separation process. For
example, high pressure, high temperature filter cartridges that are
disposable may be employed. These high temperature, high pressure
cartridges; including both container and replacement cartridge, per
se; are available from a number of major filter suppliers or
manufacturers.
The fines that are collected on the filter may then be processed as
appropriate either to remove the contaminant, such as arsenic, for
commercial use or to regenerate the fines for reuse, or simply to
render the fines inert so that they may be discarded as any other
inert material. In my copending patent application Ser. No. 435,637
entitled SLURRY SYSTEM FOR REMOVAL OF CONTAMINANT FROM SYNTHETIC
OIL, filed Jan. 23, 1974, I described a system for employing small
particles similar to the small particles that would be effected by
the regenerated fines in this invention. That method was
characterized by injection of the small particles into an incoming
feed stream of syncrude or the like, removal of the contaminant and
separation of the small particles and contaminant from the
contaminant-free syncrude; and the descriptive matter of that
patent application is embodied herein by reference for details that
are necessary to a full understanding of that use of the
regenerated fines. A co-worker, Mr. Ralph Styring, has invented and
filed a patent application on a method of processing the solid
particles, such as the fines, for removing the contaminant. The
patent application is entitled METHOD OF REMOVING CONTAMINANT FROM
SPENT CONTAMINANT-REMOVING MATERIAL, filed Jan. 23, 1974, Ser. No.
435,760, and assigned to the assignee of this application. That
method is applicable for treating the filter cake (from filter 17,
FIG. 1) comprising the fines of the material that contain the
contaminant, such as arsenic, in accordance with this invention;
and the descriptive matter of that application is incorporated
herein by reference for the details of that method.
Any amount of the particles of material can be employed in the
guard bed. A given volume of fluid, or predetermined volume of
fluid based on contaminant concentration therein and bed capacity,
can be flowed through the guard bed before switching if desired.
The predetermined volume can be determined theoretically or
empirically. On the other hand, the effluent stream from the guard
bed can be monitored for the contaminant and if detected in a small
concentration near zero, the particular guard bed can be "switched
out" and the admixture of hydrogen and syncrude routed through
another guard bed. The particles of material in the spent guard bed
are thereafter changed out and replaced by new and active
material.
Referring again to FIG. 1, the effluent stream of the syncrude
without the contaminant therein and the hydrogen are then
transported via conduit 19 to the hydrogenation reactor (HDN REAC)
21. In the hydrogenation reactor 21, hydrogenation conditions are
employed in accordance with conventional practice such that the
hydrogenated stream will effluent via conduit 23. This conventional
hydrogenation need not be described in detail herein, since a
plurality of references disclose the details and their disclosure
is embodied herein by reference.
A flow diagram of another embodiment of the invention is
illustrated in FIG. 2. Therein, a gaseous stream is separated from
the admixture of the syncrude, hydrogen and fines saturated with
the contaminant before the fines are filtered from the slurry left
after the gas stream has been separated. Specifically, the incoming
stream of syncrude and hydrogen passes through conduit 11 and into
contact with the guard bed 13 containing the particles of material
at the requisite temperature and pressure for removing the
contaminant from the syncrude, similarly as described with respect
to FIG. 1. The admixture of hydrogen and syncrude without the
contaminant pass on through. Ultimately, the admixture will entrain
the fines that are substantially saturated with contaminant to form
a dilute slurry. Thereafter, the dilute slurry will pass through
conduit 15 to a separator 25. The separator 25 comprises a
conventional gas-liquid separator with conventional liquid level
controls. The gas passes overhead through conduit 27 to join the
effluent stream from the filter 17 that is being flowed through
conduit 19 to the hydrogenation reactor 21, similarly as described
with respect to FIG. 1. After the gas stream is separated in the
separator 25, there remains a slurry comprising the fines of the
particles of material containing the contaminant and the liquid
portion of the syncrude. The gaseous portion of the syncrude
comprises hydrogen and any gaseous hydrocarbons formed, ordinarily
a minor amount in the absence of a hydrogenation catalyst. The
slurry of liquid syncrude and the fines pass through conduit 29 to
the filter 17. The filter 17 in FIG. 2 effects a more nearly
uniform filtration of the fines from the liquid phase, since there
is less turbulence effected by an intermixed gas phase. The filter
17 may comprise any conventional filter, such as the high
temperature, high pressure cartridge filter, or filter bank
described hereinbefore with respect to FIG. 1. The liquid syncrude
without the contaminant and with the fines filtered therefrom,
passes out conduit 19, as indicated immediately hereinbefore.
The gas and liquid streams are recombined upstream of the
hydrogenation reactor 21. In the hydrogenation reactor 21, the
hydrogenation reaction is carried out, as described with respect to
FIG. 1 and as is conventional.
Still another embodiment of the invention is illustrated in the
flow diagram of FIG. 3. Therein, the incoming syncrude and hydrogen
pass through the guard bed where the contaminant is removed from
the syncrude and dispersed in the particles of guard bed. As
described hereinbefore, the surface layers that become
substantially saturated with contaminant ultimately flake off as
the fines. The fines are entrained in the syncrude and hydrogen and
pass with them through conduit 15 to the separator 25. When small
separators are employed as the separator 25, the gaseous component
that is separated may contain fines that are entrained therewithin,
particularly at relatively higher velocities. Consequently, the gas
stream effluents through the conduit 27 to a cyclone separator (CYC
SEP) 31. The cyclone separator 31 may comprise any of the
conventional pressurized cyclone separators for separating small
particles such as dust particles or the like from gaseous fluid
streams at an elevated pressure. The fines are thrown toward the
wall by centrifugal force of the cyclonic effect and fall
downwardly into the funnel-shaped portion and outwardly through
conduit 33. The fines flowing out conduit 33 may be so small as to
create dusting problems or the like and may be uneconomically
feasible to be regenerated for reuse. If such is the case, the
arsenic will be removed and these fines disposed of as a
conventional inert material. On the other hand, the fines can be
agglomerated in conventional sols for regenerating the particles of
material originally employed. The fines from conduit 33 may or may
not be combined with the filter cake from the filter 17 before the
arsenic is removed from the collected fines, both in the filter
cake and from the conduit 33.
The slurry left after the gas stream is separated passes out the
bottom of the separator 25 through conduit 29 to filter 17. The
fines are separated as filter cake by the filter 17, similarly as
described with respect to FIG. 2. The liquid syncrude, without the
contaminant, passing through conduit 19 upstream of the
hydrogenation reactor 21 is recombined with the gas stream passing
from the cyclone separator 31 through conduit 35. As described
hereinbefore, the hydrogenation reaction is carried out in the
hydrogenation reactor 21 in accordance with conventional
practice.
A flow diagram of still another embodiment of this invention is
illustrated in FIG. 4. The incoming feed stream of syncrude and
hydrogen passes through conduit 11 and into contact with the
particles of material in the guard bed 13. The contaminant is
transferred from the syncrude onto the surface of the particles of
material in the guard bed 13. Ultimately, the surface layers of the
particles of material becomes substantially saturated with the
contaminant and begin to flake off and be entrained with the
syncrude and hydrogen. The admixture of the syncrude, hydrogen and
fines flow through conduit 15 to the cyclone separator 37.
The cyclone separator 37 is somewhat larger than the cyclone
separator 31, FIG. 3. In the cyclone separator 37, both the liquid
and the fines are thrown toward the walls by the centrifugal force
developed by the cyclonic motion of the fluids. The slurry of
liquid and fines fall into the funnel-shaped portion and out
through conduit 39 to the filter 17. The gas stream passes
outwardly through the conduit 35 to be combined with the liquid
syncrude in conduit 19.
The slurry from conduit 39 passes into the filter 17 and the fines
are removed from the liquid by the filters as described
hereinbefore with respect to the other embodiments. The liquid
syncrude without the contaminant passes outwardly through the
conduit 19. The gaseous and liquid streams comprising the hydrogen,
any gaseous hydrocarbons, and the liquid syncrude are recombined
upstream of the hydrogenation reactor 21.
The usual hydrogenation reaction is carried out in accordance with
conventional practice and as described hereinbefore in the
hydrogenation reactor 21.
The fines collected by the filters 17 in the respective embodiments
are all treated as described hereinbefore with respect to FIG.
1.
Cyclone separators are conventionally available for separation of
fines, such as dust particles from gas streams, as well as
separating both liquid and solid particles, such as the slurry of
the liquid syncrude and the fines, from the gas stream.
Accordingly, there is no need to embellish the already lengthy
descriptive matter herein by the inclusion of such well known and
conventional apparatus.
While cartridge type filters, or filter banks, have been described
hereinbefore with respect to the filter 17, any other suitable
filters or method of filtration that will withstand the high
temperature and pressure can be employed. For example, rotary self
cleaning filters may be employed, as well as other metallic or high
temperature filters. If desired, the high temperature bag filters
can be employed to facilitate removal of the filter cake.
While the oxides and sulfides of iron have been described
specifically hereinbefore, the particles of material that are
useful in this invention as active materials may comprise nickelic,
ferric, cobaltic, ferrous, nickelous, and cobaltous forms. For
example, ferric oxide, both Fe.sub.2 O.sub.3 and Fe.sub.3 O.sub.4,
nickelic oxide Ni.sub.2 O.sub.3 and Ni.sub.3 O.sub.4 and cobaltic
oxide Co.sub.2 O.sub.3 and Co.sub.3 O.sub.4 can be employed.
Similar reasoning is applicable to the comparable sulfides of the
metals and to the ferrous, cobaltous and nickelous forms of the
oxides and sulfides.
EXAMPLE
A fixed bed containing Fe.sub.2 O.sub.3 particles in the form of
right cylinders 1/4 inch in diameter and 1/4 inch in length is
exposed to a molecular hydrogen-shale oil (containing about 80 ppm
arsenic) stream prepared by mixing about 4,000 standard cubic feet
of hydrogen per barrel (42 U.S. gallons) of shale oil. Said stream
is passed through said bed at a rate of about 5 weight hourly space
velocity and at a temperature of about 700.degree.F. and a hydrogen
partial pressure of about 1,500 psig.
The thus treated stream is recovered from said fixed bed and passed
through a 7 micron SWAGELOK stainless steel filter to remove solid
fines which are saturated with arsenic thereby leaving a shale oil
stream containing less than 10 ppm arsenic. This shale oil stream
is now in a condition to be passed through a conventional
hydrogenation system.
From the foregoing, it can be seen that this invention effects the
objects set out hereinbefore and alleviates the difficulties of the
prior art processes.
Having thus described the invention, it will be understood that
such description has been given by way of illustration and example
and not by way of limitation, reference for the latter purpose
being had to the appended claims.
* * * * *