System for producing a powdery composition comprising coal products in a coal deashing process

An improved system for deashing coal liquefaction products wherein a feed mixture (including a deashing solvent, soluble coal products and insoluble coal products) is separated in a first separation zone into a first light fraction and a first heavy fraction (including insoluble coal products and some deashing solvent). The first heavy fraction is withdrawn from the first separation zone and the pressure level of the first heavy fraction is reduced at least 100 psig for vaporizing the deashing solvent and for yielding a composition substantially comprising coal products. The composition is essentially a powdery, solid material and is capable of being transferred via a slurry or mechanical means.

BACKGROUND OF THE INVENTION 
1. Field of the Invention 
The present invention relates generally to coal deashing processes and, 
more particularly, but not by way of limitation, to systems for producing 
a powdery composition comprising coal products in coal deashing processes. 
2. Description of the Prior Art 
Various coal deashing processes have been developed in the past wherein 
coal has been treated with one or more solvents and processed to separate 
the resulting insoluble coal products from the soluble coal products. 
U.S. Pat. Nos. 3,607,716 and 3,607,717, issued to Roach and assigned to the 
same assignee as the present invention, disclose processes wherein coal is 
contacted with a solvent and the resulting mixture then is separated into 
a heavy phase containing the insoluble coal products and a light phase 
containing the soluble coal products. In such processes, the light phase 
is withdrawn and passed to downstream fractionating vessels wherein the 
soluble coal product can be separated into multiple fractions. Other 
processes for separating the soluble coal products from the insoluble coal 
products utilizing one or more solvents are disclosed in U.S. Pat. Nos. 
3,607,718, and 3,642,708, both issued to Roach et al, and assigned to the 
same assignee as the present invention.

DESCRIPTION OF THE PREFERRED EMBODIMENTS 
Referring now to FIG. 1, general reference numeral 10 designates a system 
for deashing coal liquefaction products arranged in accordance with the 
present invention, which includes a mixing zone 12, a first separation 
zone 14 and a second separation zone 16. 
In general, a feed mixture (comprising soluble coal products, insoluble 
coal products and deashing solvent) is passed from the mixing zone 12 
through a conduit 18 into the first separation zone 14 wherein the feed 
mixture is separated into a first heavy fraction and a first light 
fraction. The first light fraction is passed through a conduit 20 into the 
second separation zone 16 wherein it is separated into a second light 
fraction and a second heavy fraction. 
In accordance with the present invention, the first heavy fraction is 
withdrawn from the first separation zone 14 and passed through a conduit 
22 into a flash zone 24 where the pressure on the first heavy fraction is 
reduced by an amount sufficient to vaporize the deashing solvent from the 
first heavy fraction and to yield a composition substantially comprising 
coal products. The composition is powdery in form, and thus is capable of 
being transferred by mechanical means, in a slurry form or other 
convenient means. 
In one particular process, pulverized raw coal is contacted with a 
liquefaction solvent and liquefied to produce a mixture comprising the 
liquefaction solvent, the soluble coal products and the insoluble coal 
products. In this process, substantially all of the liquefaction solvent 
is removed by flashing, or some similar means, from the soluble and the 
insoluble coal products to produce a prepared mixture (coal liquefaction 
products) and then the prepared mixture is contacted with a deashing 
solvent in the mixing zone 12. The resulting mixture (comprising the 
soluble coal products, the insoluble coal products and the deashing 
solvent) comprises the feed mixture passed through the conduit 18 into the 
first separation zone 14. 
Although the particular process generally described above for producing the 
feed mixture contemplates the utilization of different liquefaction and 
deashing solvents, the present invention also contemplates systems wherein 
the coal is contacted by a single liquefaction-deashing solvent or systems 
wherein the coal is contacted by more than two liquefaction-deashing 
solvents. Therefore, the feed mixture passing through the conduit 18 and 
introduced into the first separation zone 14 is referred to therein as 
including a "deashing solvent", which may be the deashing solvent or the 
liquefaction solvent or a combination of the liquefaction and deashing 
solvents or some other solvent or solvents utilized for producing the feed 
mixture comprising the soluble coal products, the insoluble coal products 
and the deashing solvent. 
In the particular process generally described above, the "liquefaction 
solvent" preferably is an organic solvent suitable for liquefying coal, 
and various solvents suitable for liquefying coal are disclosed in the 
U.S. Pat. Nos. 3,607,716; 3,607,717; 3,607,718 and 3,642,608, the 
disclosures of which are incorporated herein by reference. The "deashing 
solvent" is of the type sometimes described as a "light organic solvent" 
in the just-mentioned U.S. patents and consists essentially of at least 
one substance having a critical temperature below 800 degrees F. selected 
from the group consisting of aromatic hydrocarbons having a single benzene 
nucleus and normal boiling points below about 310 degrees F., 
cycloparaffin hydrocarbons having normal boiling points below about 310 
degrees F., open chain mono-olefin hydrocarbons having normal boiling 
points below about 310 degrees F., open chain saturated hydrocarbons 
having normal boiling points below about 310 degrees F., mono-, di, and 
tri-open chain amines containing from about 2-8 carbon atoms, carbocyclic 
amines having a monocyclic structure containing from about 6-9 carbon 
atoms, heterocyclic amines containing from about 5-9 carbon atoms, and 
phenols containing from about 6-9 carbon atoms and their homologs. Also, 
the details of particular processes for liquefying coal and subsequently 
separating the soluble coal products from the insoluble coal products are 
disclosed in the just-mentioned U.S. patents. 
The term "insoluble coal products" as used herein refers to the undissolved 
coal, ash, other solid inorganic particulate matter and other such matter 
which is insoluble in the deashing solvent solution under the conditions 
of the instant process. The insoluble inorganic material in coal which is 
sometimes assumed to be about equal to the ash remaining after igniting 
the coal under controlled conditions is sometimes referred to in the art 
as "mineral matter." With respect to coal and related minerals, typical 
mineral matter components include kaolinite, calcite, gypsum and pyrite. 
In thermally treated or hydrogenated materials, pyrite usually has been 
changed to pyrrhotite. Mineral matter analyses are reported frequently as 
oxide contents, that is, SiO.sub.2, Al.sub.2 O.sub.3, CaO and the like. 
The term "soluble coal products" as used herein refers to the constituents 
in the feed mixture which are soluble in the deashing solvent. 
The term "ash-free coal" as used herein refers to the soluble coal products 
and the insoluble coal products less the ash remaining after igniting the 
coal or coal products under controlled conditions. 
Referring to the coal deashing process 10 of the present invention as 
depicted in FIG. 1, the mixture consisting essentially of the soluble coal 
products, the insoluble coal products and any liquefaction solvent 
(referred to herein as the "prepared mixture"), is passed through a 
conduit 26 into the mixing zone 12 and the deashing solvent is passed into 
the mixing zone 12 via a conduit 28. The deashing solvent may be contained 
in a solvent surge vessel or the like (not shown) and, in this embodiment, 
the deashing solvent is withdrawn from such vessel and pumped through the 
conduit 28 into the mixing zone 12. The prepared mixture is contacted by 
and mixed with the deashing solvent and the resulting mixture is 
discharged from the mixing zone 12 into and through the conduit 18, the 
mixture discharged from the mixing zone 12 comprising and being referred 
to herein as the "feed mixture." 
In the first separation zone 14, the feed mixture is separated into a first 
light fraction and first heavy fraction. The first light fraction 
comprises most of the soluble coal products and most of the deashing 
solvent. The first separation zone 14 is maintained at a temperature level 
below about 700 degrees F. and at a pressure level in the range of from 
about the critical pressure of the deashing solvent to about 1000 psig to 
effect the separation. Preferably the first separation zone 14 is 
maintained at a temperature level in the range of from about 400 degrees 
F. to below about 700.degree. F. and at a pressure level in the range of 
from about 700 psig to about 1000 psig. Most preferably the first 
separation zone 14 is maintained at a temperature level in the range of 
from about 400 degrees F. to about 650 degrees F. and the pressure level 
is maintained in the range of from about 800 psig to about 950 psig. The 
first light fraction is withdrawn from the first separation zone 14 and 
passed through a heater 30 and the conduit 20 into the second separation 
zone 16. The heater 30 serves to heat the first light fraction passing 
therethrough to an elevated temperature level, for example, to a range 
from about 630 degrees F. to about 900 degrees F. The pressure level in 
the second separation zone 16 is in the range of from about the critical 
pressure of the deashing solvent to about 1000 psig and preferably in the 
range of from about 650 psig to about 1000 psig. In the second separation 
zone 16, the first light fraction separates into a second light fraction 
comprising most of the deashing solvent and a second heavy fraction 
comprising the substantially ash-free soluble coal products and some of 
the deashing solvent. The second light fraction is withdrawn from the 
second separation zone 16 and passed through a conduit 32 for re-use in 
the system, and the second heavy fraction is withdrawn from the second 
separation zone 16 and passed through a conduit 34 for solvent removal and 
recovery of a deashed coal product suitable for use in combustion 
processes. 
The first heavy fraction is withdrawn from the first separation zone 14 
through the conduit 22 and passed into the flash zone 24 wherein the 
pressure level on the first heavy fraction is reduced to a level in the 
range of from about 0 psig to about 50 psig, to flash the first heavy 
fraction and form one stream comprising the deashing solvent and one 
stream comprising the insoluble coal products. The insoluble coal products 
are withdrawn from the flash zone 24 through a conduit 36. The deashing 
solvent is withdrawn from the flash zone 24 and passed through a conduit 
38 for reuse. 
In this process, it is important that the first heavy fraction within the 
first separation zone 14 be maintained in a flowable condition so the 
first heavy fraction, which includes the insoluble coal products and some 
of the deashing solvent, can be withdrawn from the first separation zone 
14 in a convenient and efficient manner and in a manner having a minimum 
of fouling or clogging problems. Further, it is desirable that the first 
heavy fraction be of a nature that it can be passed through a pressure 
reducing device (the flash zone 24), such as a restricted orifice, for 
example, with minimal erosion thereto. The present invention results in a 
first heavy fraction which is flowable from the first separation zone 14 
and through the conduit 22 into the flash zone 24. Further, the first 
heavy fraction produced in accordance with the present invention is 
suitable for passing through a restricted orifice wherein the pressure 
level of the first heavy fraction is reduced by at least 100 psig with 
minimal erosion to such restricted orifice, the pressure differential 
generally being at least 500 psig. Also, it has been discovered that, when 
the first heavy fraction produced in accordance with the present invention 
is flashed via a restricted orifice or the like to vaporize the deashing 
solvent, the remaining coal product composition withdrawn from the flash 
zone 24 is in a relatively dry, powdery, solid material form and this 
composition is capable of being transferred via a slurry or mechanical 
means. 
In accordance with the present invention, the first heavy fraction in the 
first separation zone 14 and in the conduit 22 comprises deashing solvent 
in a range from about 10 percent by weight to about 35 percent by weight. 
A more complete understanding of the composition of the first heavy 
fraction in the first separation zone 14 can be obtained by reference to 
TABLE I wherein a characterization of the first heavy fraction, for 
various coal liquefaction products derived from different feed coals and 
various operating conditions of the first separation zone 14, in terms of 
the percentages of deashing solvent, ash and ash-free coal present in the 
first heavy fraction, by weight, is set forth: 
TABLE I 
__________________________________________________________________________ 
Characterization Of The First Heavy Fraction 
Ratio of 
Deashing 
Solvent to 
Temperature 
Pressure 
Prepared 
Level (.degree.F.) 
Level (psig) 
Mixture in 
in the First 
in the First 
First Heavy Fraction 
Sample.sup.1 
Deashing 
the Mixing 
Separation 
Separation 
% Deashing % Ash-free 
No. Solvent Zone 12 
Zone 14 
Zone 14 
Solvent 
% Ash 
Coal 
__________________________________________________________________________ 
1 Benzene 1.76 470 800 17.32 22.68 
60.00 
2 Benzene 1.78 445 800 20.52 23.09 
56.39 
3 Benzene 1.69 470 800 21.11 21.11 
56.78 
4 Toluene 1.76 505 800 23.15 22.24 
54.61 
5 Toluene 1.68 538 800 20.51 23.10 
56.39 
6 Toluene 1.79 565 800 20.73 22.79 
56.48 
7 Xylenes.sup.2 
2.0 565 800 16.83 23.92 
59.25 
8 Mixed Solvent.sup.3 
3.0 565 800 18.59 23.17 
58.24 
9 Xylenes.sup.2 
2.4 595 800 21.19 33.69 
45.12 
10 Toluene 2.05 503 810 20.22 24.47 
55.31 
11 Toluene 2.56 532 700 10.20 30.40 
55.80 
12 Toluene 3.8 617 800 25.40 36.30 
38.30 
__________________________________________________________________________ 
.sup.1 Samples 1-8 coal liquefaction product feed derived from Pittsburgh 
#8 coal, Samples 9-11 derived from Kentucky #9 and #14 coal and Sample 12 
derived from Illinois #6 coal by catalytic liquefaction process. 
.sup.2 75.5% meta and para xylenes, 18% ortho xylene, 1.7% ethylbenzene 
and 4.8% other higher boiling components (percentages being by weight). 
.sup.3 20.1% toluene, 54.0% xylenes (mixture of ortho, meta and para) and 
25.9% ethylbenzene (percentages being by weight). 
The composition characterized within TABLE I is also set forth in FIG. 2 
wherein a triangular composition diagram is illustrated. The composition 
of the first heavy fraction in the first separation zone 14 is defined as 
the region within the trapezoid shown in the triangular composition 
diagram of FIG. 2. This composition has desirable fluid properties at 
temperature levels in a range from about 460 degrees F. to about 650 
degrees F., depending upon the composition of the prepared mixture, choice 
of deashing solvent and the like. The relatively high viscosity of this 
flowable first heavy fraction also permits the discharge of the first 
heavy fraction from a relatively high pressure zone, having a pressure 
level in a range from about 700 psig to about 1000 psig, to a relatively 
low pressure zone, having a pressure level in a range from about 0 psig to 
about 50 psig. Thus, this unique composition comprising the first heavy 
fraction is flowable through an ordinary, commercially available valve and 
the pressure level of such composition (the first heavy fraction) can be 
reduced by up to about 1000 psig in a single step or stage (across a 
single valve) with minimal erosive wear of the valve seat or the valve 
stem, in lieu of utilizing a plurality of valves in series to effect the 
necessary pressure reduction, with a relatively small pressure drop being 
effected across each individual valve. In contrast with the first heavy 
fraction produced in accordance with the present invention, other 
materials having a relatively high solids content (such as slurries of 
coal liquefaction products from a coal hydrogenation process) will cause 
serious erosion of valve parts when expanded through a single pressure 
reducing valve in a manner just described in connection with the present 
invention. 
The chemical analysis of the first heavy fraction in the first separation 
zone 14 indicates that there is a substantial variation in the chemical 
composition obtained from different feed coals and yet, it has been found 
that the first heavy fractions so produced in accordance with the present 
invention have essentially the same physical properties (flowable, viscous 
fluid), notwithstanding the different chemical compositions. A summary of 
the chemical composition of the first heavy fraction (solvent free basis) 
produced in the first separation zone 14 and in the conduit 22 connecting 
the first separation zone 14 with the flash zone 24 for five different 
feed mixtures derived from different feed coals is summarized in TABLE II, 
below (the oxygen content being determined by disregarding the oxygen 
chemically associated with the mineral matter or ash): 
TABLE II 
______________________________________ 
Ultimate Analysis of Coal Product Composition 
Chemical 
Sample .sup.1 
Sample.sup.2 
Sample.sup.3 
Sample.sup.4 
Sample.sup.5 
Constit- 
No. 1 No. 2 No. 3 No. 4 No. 5 
uents Wt. % Wt. % Wt. % Wt. % Wt. % 
______________________________________ 
Carbon 57.4 50.2 46.9 59.4 63.6 
Hydrogen 
3.0 3.0 2.7 3.3 3.3 
Nitrogen 
1.0 1.0 1.2 1.0 1.3 
Sulfur 0.8 4.05 6.9 3.6 2.5 
Oxygen 
(By Dif- 
ference) 
3.3 1.75 -- -- 2.6 
Ash 34.5 40.4 43.6 32.7 26.7 
______________________________________ 
.sup.1 Wyodak feed coal to coal deashing 
.sup.2 Illinois #6 feed coal to coal deashing 
.sup.3 Kentucky #9 and #14 feed coal to coal deashing 
.sup.4 Kentucky #9 and #14 feed coal to coal deashing 
.sup.5 Pittsburgh #8 feed coal to coal deashing process 
Further, the "coal product composition" withdrawn from the flash zone 24 
via the conduit 36 is essentially free of the deashing solvent. The coal 
product normally has the following composition: coal mineral matter in a 
range from about 20 percent to about 50 percent as indicated by ashing; 
and the remaining portion of such composition is predominantly carbon with 
relatively minor amounts of hydrogen, nitrogen, sulfur and oxygen. The 
hydrogen to carbon atomic ratio of such composition is in a range from 
about 0.60 to about 0.80, with the ratio typically being about 0.66, for 
example. The carbon content of such composition is generally in a range 
from about 45 percent by weight to about 70 percent by weight. 
The composition withdrawn from the flash zone 24 via the conduit 36 
(sometimes referred to herein as the "flashed first heavy fraction") is a 
light, powdery, black solid material and typical physical properties of 
this material are summarized in TABLE III, below: 
TABLE III 
______________________________________ 
Physical Properties Of Coal Product Composition 
______________________________________ 
Bulk Density - 31 lb/ft.sup.3 
Particle Density - 97 lb/ft.sup.3 
Angle of Repose - 40-45.degree. 
Size Distribution 
Tyler Screen 
Mesh Size Weight % Weight % Ash 
______________________________________ 
+28 9.0 37.1 
-28 +48 13.6 37.4 
-48 +65 8.2 37.7 
-65 +100 8.4 38.1 
-100 +150 8.5 37.6 
-150 +200 9.6 37.3 
-200 +270 7.3 37.7 
-270 +400 8.1 37.7 
-400 27.3 38.0 
______________________________________ 
With respect to the Angle of Repose listed in TABLE III, above, it should 
be noted that the material withdrawn from the flash zone 24 may be readily 
fluidized. Further, with respect to the Size Distribution listed in TABLE 
III, above, it should be noted that the ash concentration in the flashed 
heavy fraction withdrawn through the conduit 36 was uniform throughout the 
various size fractions. 
A more complete understanding of the chemical nature of the coal product 
composition of the present invention can be had by reference to a method 
of chemical fractionation utilizing highly selective solvents as described 
by D. D. Whitehurst et al in "The Nature And Origin of Asphaltenes In 
Processed Coals", the annual report of RP 410-1 produced under sponsorship 
of Electric Power Research Institute, and published February, 1976 
(Government doc. no. PB 257569), the disclosure of which is incorporated 
herein by reference. 
Chemical fractionation using Sequential Elution with Specific Solvents 
Chromatography (hereinafter referred to as SESC) provides a novel means 
for the separation of the coal product composition into discrete chemical 
classes which then can be used to characterize the composition. 
In a variation of the above identified SESC procedure, a sample of coal 
derived material is eluted successively with the following solvents to 
form nine distinct fractions: 
1. Hexanes (mixed isomers) 
2. Hexanes/15% toluene 
3. Chloroform 
4. Chloroform/10% Diethyl Ether 
5. Diethyl Ether/3% Ethanol 
6. Methanol 
7. Chloroform/3% Ethanol 
8. Tetrahydrofuran/3% Ethanol 
9. Pyridine/3% Ethanol 
and a tenth fraction comprising the residual insoluble coal products not 
eluted by the selective solvents. The ash-free coal content of the tenth 
fraction then is calculated by difference using the ash analysis of the 
original SESC sample. A SESC Analysis on an ash-free basis then is 
prepared. The results of several SESC Analyses of various coal derived 
materials are set forth in TABLE IV, below: 
TABLE IV 
__________________________________________________________________________ 
SESC Analysis On Ash-free Basis 
Sample 
Fractions, Wt. % 
No. 1 2 3 4 5 6 7 8 9 10 
__________________________________________________________________________ 
1.sup.1 
0.23 
4.74 
0.68 
0.90 
0.90 
2.14 
1.69 
0.90 
6.31 
81.51 
2.sup.2 
0.47 
5.10 
20.60 
19.1 
14.6 
6.4 
9.9 
11.0 
7.1 
5.7 
3.sup.3 
0.22 
4.11 
17.86 
15.04 
12.23 
5.63 
12.55 
10.06 
11.69 
10.61 
4.sup.4 
0.14 
0.54 
2.30 
2.03 
2.17 
2.17 
4.19 
6.22 
18.94 
61.30 
5 0.00 
0.14 
0.28 
1.00 
1.00 
15.93 
1.28 
6.97 
22.05 
51.35 
6.sup.5 
0.35 
0.17 
0.69 
1.03 
1.38 
1.38 
2.76 
12.59 
15.00 
64.66 
7 0.18 
2.15 
3.58 
3.94 
4.84 
2.87 
1.97 
6.63 
16.13 
57.71 
8 0.35 
0.00 
1.06 
1.76 
1.41 
1.23 
3.70 
24.82 
21.13 
44.54 
9 0.00 
0.69 
5.03 
4.51 
5.03 
3.64 
6.76 
7.63 
19.76 
46.97 
10 0.00 
0.47 
2.04 
2.51 
2.35 
2.82 
5.17 
10.82 
25.71 
48.12 
11 0.00 
0.00 
0.72 
1.45 
2.17 
1.45 
11.16 
12.57 
19.71 
50.58 
__________________________________________________________________________ 
.sup.1 Kentucky #9 and #14 raw coal 
.sup.2 Kentucky #9 and #14 ashcontaining solvent refined 
.sup.3 Pittsburgh #8 ashcontaining solvent refined coal 
.sup.4 Samples 4 and 5, coal product composition of the present invention 
derived from Pittsburgh #8 feed coal 
.sup.5 Samples 6-11, coal product composition of the present invention 
derived from Kentucky #9 and #14 feed coal 
Thus, as can readily be seen in TABLE IV, the various fractions produced as 
a result of the selective elution provide a means by which the coal 
product composition can be characterized through reference to the discrete 
chemical classes contained therein such that it can be easily 
distinguished from other coal derived materials. 
The characterization is best achieved by reference to the SESC fractions 8, 
9, and 10. It has been found that SESC fraction 10, on an ash-free basis, 
amounts to from about 40 percent to about 65 percent by weight of the coal 
product composition. Further, SESC fraction 9 amounts to from about 15 
percent to about 30 percent by weight of the coal product composition and 
SESC fraction 8 amounts to from about 5 percent to about 25 percent by 
weight of the coal product composition. The balance of the coal product 
composition is the SESC fractions 1-7, on an ash-free basis. 
Clearly, the ranges of these fractions differs greatly from the same 
fractions for other coal derived materials. Therefore, since these 
fractions represent the presence of certain discrete chemical classes 
possessing different chemical functionalities, the coal product 
composition is distinctly different from other coal derived materials. 
The operating conditions (temperature level, pressure level and ratio of 
deashing solvent to feed) in the first separation zone 14 are influential 
in producing the powdery flashed first heavy fraction. The powdery 
composition is produced when the first separation zone is operated at 
certain temperature levels, certain pressure levels and ratios of deashing 
solvent to feed, while at certain other temperature levels, pressure 
levels and ratios of deashing solvent to feed, the composition (the 
powdery, flashed first heavy fraction) is not produced. Various conditions 
are itemized in TABLE V which have been found satisfactory to produce the 
composition (the powdery, flashed first heavy fraction) of the present 
invention. 
In particular, it has been found that when the deashing solvent is toluene 
the temperature level in the first separation zone 14 should be maintained 
below about 640 degrees F. and preferably the temperature level in the 
first separation zone 14 is maintained in a range of from about 450 
degrees F. to about 555 degrees F. 
Further, when the deashing solvent is benzene, the temperature level in the 
first separation zone 14 should be maintained below about 620 degrees F. 
and preferably the temperature level in the first separation zone 14 is 
maintained in the range of from about 500 degrees F. to about 530 degrees 
F. 
Still further, when the deashing solvent is a mixture of xylenes, the 
temperature level in the first separation zone 14 should be maintained in 
a range of from about 450 degrees F. to below about 650 degrees F. 
Also, when the deashing solvent is a mixture comprising at least two 
members selected from the group consisting of toluene, benzene, xylene 
(ortho, meta, para or mixtures thereof), and the like, the temperature 
level in the first separation zone 14 should be maintained in a range of 
from about 450 degrees F. to about 650 degrees F. 
TABLE V 
______________________________________ 
Ratio of 
Deashing Deashing Temperature Pressure 
Solvent Solvent Level Level (psig) 
Introduced into 
to Prepared (.degree.F.) in the 
in the First 
mixing Zone 12 
Mixture in the 
First Separation 
Separation 
Via Conduit 28 
Mixing Zone 12 
Zone 14 Zone 14 
______________________________________ 
Toluene 3.8.sup.1 617 800 
Toluene 1.7.sup.2 520 800 
Benzene 6.0.sup.2 500 960 
Benzene 5.0.sup.2 500 950 
Xylenes.sup.3 
2.0.sup.2 565 800 
Mixed Solvent.sup.4 
3.0.sup.2 565 800 
______________________________________ 
.sup.1 Prepared mixture comprises ashcontaining catalytically hydrogenate 
coal. 
.sup.2 Prepared mixture comprises ashcontaining solvent refined coal. 
.sup.3 75.5% meta and para xylenes, 18% ortho xylene, 1.7% ethylbenzene 
and 4.8% other higher boiling components (percentages being by weight). 
.sup.4 20.1% toluene, 54.0% xylenes (mixture of ortho, meta and para) and 
25.9% ethylbenzene (percentages being by weight). 
It should be noted that each of the conditions listed in TABLE V were 
determined utilizing different coal feed materials and such differences in 
operating conditions utilizing the same deashing solvent may be 
attributed, in part, to the difference in coal liquefaction feed materials 
in the prepared mixture. 
Various conditions are itemized in TABLE VI which are believed to produce a 
non-powdered, flashed first heavy fraction withdrawn from the flash zone 
24 via the conduit 36: 
TABLE VI 
______________________________________ 
Ratio of 
Deashing Deashing Temperature Pressure 
Solvent Solvent Level Level (psig) 
Introduced into 
to Prepared (.degree.F.) in the 
in the First 
Mixing Zone 12 
Mixture in the 
First Separation 
Separation 
Via Conduit 28 
Mixing Zone 12 
Zone 14 Zone 14 
______________________________________ 
Toluene 3.1.sup.1 674 800 
Toluene 2.1.sup.2 630 800 
Toluene 1.7.sup.2 555 800 
Benzene 6.0.sup.2 620 960 
Benzene 5.0.sup.2 590 950 
______________________________________ 
.sup.1 Prepared mixture comprises ashcontaining Catalytically hydrogenate 
coal. 
.sup.2 Prepared mixture comprises ashcontaining solvent refined coal. 
The carbon content of the coal product composition produced by flashing the 
first heavy fraction in accordance with the present invention is useful as 
a fuel for generation of hydrogen, carbon monoxide or other fuel gases by 
various gasification techniques well known in the art. The physical nature 
of the powdery composition produced in accordance with the present 
invention is such that it is well suited to solids handling by fluidizing 
methods, for handling in screw feeders or other solids handling equipment. 
Referring more particularly to FIG. 3, shown therein is one particular 
embodiment of the flash zone 24. An opening (orifice) 40 is formed through 
a plate 42 which is disposed and secured within the conduit 22. A valve 
member 44, having a seating surface 46 formed on one end thereof, is 
disposed within the opening through the conduit 22. More particularly, the 
valve member 44 is slidingly disposed through an opening 48 formed through 
a packing (not shown) in plate 50 which is disposed and secured within the 
opening in the conduit 22, the plate 50 being spaced a distance from the 
plate 42. 
The valve member 44 is positioned with respect to the orifice 40 and the 
seating surface 46 is shaped to seatingly engage the plate 42, in one 
position, closing the orifice 40. As the valve member 44 is moved away 
from the plate 42, flow is permitted through the orifice 40, the position 
of the valve member 44 seating surface 46 with respect to the orifice 40 
controlling the rate of flow through the orifice 40. Thus, the valve 
member 44 is movable in directions 52 for controlling the rate of flow 
through the orifice 48. The valve member 44 is connected to a control 56 
(such as a control valve, for example) via a mechanical connection 
designated via the general reference 58 in FIG. 3, for moving the valve 
member 44 in directions 52. 
One end portion of a connecting tube 60 is inserted through the conduit 36, 
the other end being disposed in the space within the conduit 22, generally 
between the plates 42 and 50. The connecting tube 60 is connected to and 
oriented within the conduit 36 in such manner that fluid is discharged 
from the connecting tube 60 into the conduit 36 at an angle to cause the 
discharging fluid to enter the conduit 36 tangentially with respect to its 
wall, thereby creating a cyclone type of flow pattern as generally 
indicated via the direction arrow 62. As shown in FIG. 3, one end of a 
conduit 38 is disposed through one end of the conduit 36 and this end of 
the conduit 38 spaced a distance above the end of the connecting tube 60, 
which is disposed in the conduit 36. 
During operations, the first heavy fraction is withdrawn from the first 
separation zone 14 and passed through the conduit 22 into the flash zone 
24. In the flash zone 24, the first heavy fraction is passed through the 
restricted orifice 40 wherein the pressure level of the first heavy 
fraction is reduced by at least 100 psig. The first heavy fraction then 
passes through the connecting tube 60 and into the conduit 36. The flashed 
first heavy fraction enters the conduit 36 and the light vapor phase 
(essentially the deashing solvent) rises upwardly through the conduit 36. 
The light vapor phase is discharged through the conduit 38 and the 
insoluble coal products pass downwardly through conduit 36. 
Various other specific embodiments of the flash zone 24 are possible and 
the specific embodiment shown in FIG. 3 has been provided only for the 
purpose of illustrating the present invention. 
Changes may be made in the process apparatus or in the steps of the process 
or in the sequence of the steps of the process or in the compositions of 
the present invention without departing from the spirit and scope of the 
invention as defined in the following claims.