3 CONTRACT TITLE AND NUMBER: Bench-Scal e Co-Processi ng

CONTRACTOR NAME: UOP John G. Gatsis 25 E. Algonquin Road Des Plaines, Illinois 60017-5017 Hark A. Miller

DE -AC22 - 87 PC 798 18

Carl Lea

COKTRACT PERIOD: April 1, 1988 to March 31, 1991

QUARTERLY REPORT

This quarterly report i s the fifth for Contract DE-AC22-87PC79818.

The objective of this contract is to extend and optimize UOP's single-

stage sl urry-catalyzed co-processing scheme, which was devel oped under

previous Contract DE-AC22-84PC70002. Particular emphasis is given to

defining and improving catalyst utilization and c o s t s , evaluating

alternative and disposable slurry-catalyst systems, and improving cat-

alyst recycle and recovery techniques. The work during this quarter has

concentrated on Tasks 3.1.1 (Pilot Plant Modification), 3.1.2 (Plant

Recertification), and 3.1.3 (Reactor Back-Mixing Study). The results

of these tasks are discussed in this report.

PILOT PLANT ~ODIFICATIONS

A number of parallel tests were completed in both the bench-scale

unit and a rocking autoclave under UOP's previous contract. The auto-

clave test was developed as a quick and inexpensive means o f screening

. new feedstocks and catalysts t o reduce the work load on the bench-scale

u n i t . Operating conditions for the autoclave and bench-scale u n i t were

set t o make the autoclave resu l t s as useful as possible fo r predicting

continuous-run performance. Reasonable correspondence between the tests

was observed f o r t h e re ference c a t a l y s t and feedstocks, bu t when a

slurry iron catalyst was tried i n Run 17, the performance of the bench-

s c a l e u n i t f e l l f a r short o f the results predicted on the basis of the

autoclave resul ts . Th i s r u n was also plagued w i t h operating problems.

The low-pressure ( f r ac t iona t ion ) side of the plant kept plugging and

had t o be bypassed. Conversions were observed t o be l i t t l e be t te r t h a n

those obtained using no catalyst a t a l l . The resul ts were disappointing

because catalyst costs for the reference vanadium-based slurry catalyst

a r e h i g h , and t h e use o f an inexpensive throwaway iron ca ta lys t would

have made the process economics more at t ract ive.

Differences i n the performance o f t he autoclave and bench-scale

uni ts w i t h t h e i ron catalyst were d i f f i cu l t t o reconcile. Either the

autoclave resu l t s were no t r e p r e s e n t a t i v e o f t r u e c o n t i n u o u s

performance, o r t he bench-scale u n i t was somehow mechanically limited

and w a s not performing up t o pred ic t ions . I t was suggested t h a t

p e r h a p s t h e bench- sca l e u n i t was not completely back-mixed. To

minimize coking, any coke precursors that are formed must have intimate

contac t w i t h the c a t a l y t i c metal and hydrogen. Improved mixing also

minimizes the contact o f reactants w i t h the hot reactor walls and helps

t o maintain a more uni form temperature profile. To test whether the

bench-scale reactor was t ru ly back-mixed, a 1 iquid-recycle system was

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added t o the p l an t t o return a por t ion of the l i q u i d product from the

bottom of the high-pressure sepa ra to r t o the inlet of the r e a c t o r .

G i l l e sp ie and Carberry (1) have shown that the addition of a recycle

stream t o an unmixed r e a c t o r can be used t o simulate a continuous

s t i r r e d tank reactor (CSTR). As the r a t io o f recycle t o fresh feed i s

increased, conversion approaches t h e conversion f o r an idea l CSTR.

W i t h a recycle r a t io of 20, for example, the conversion i n a plug-flow

reactor becomes indistinguishable from t h a t of the idea l CSTR. For a

partly-mixed r eac to r , a lower recycle r a t io o f about 3: l t o S:1 would

be suff ic ient t o achieve near-perfect mixing.

Prior t o Run 20, the bench-scale u n i t was modified, a s shown i n

Figure 1, t o incorporate the liquid-recycle system. A recycle pump and

high-pressure mass f l o w meter were added, and several o t h e r p l an t

changes were made t o accomodate the larger flows associated w i t h l i q u i d

recycle. The volume of the high-pressure separator (HPS) was doubled,

and a longer r eac to r preheat zone and new prehea ter were added t o

increase the heater duty.

PI LOT PLANT RECERTIFICATION

Puns 20 and 21

The first run w i t h the modified p l a n t was a shakedown r u n t o refer-

ence p l a n t performance t o t h a t o f the long-term o p e r a b i l i t y study

-3 - UOP

conducted i n Run 19. In add i t ion t o the p l a n t changes, new batches of

the reference vanadium catalyst (K1.2) and feedstocks (I1 1 inoi s Coal

No. 6 batch C1.4 and Lloydminster Vacuum Resid batch R10) were used.

T h e bench-scale u n i t was s tar ted up with the system fu l l of flush

o i l . Slurry feed was cu t i n t o the r eac to r a t 0900 hrs on 1/24/89.

During the s t a r t - u p , a number of problems were encountered. A t 60

hours on stream (HOS), loss of t h e f r a c t i o n a t o r bottoms pump as a

r e s u l t of e lectr ical problems caused level fluctuations throughout the

plant. The r u n eventually h a d t o be s h u t down a t 65 HOS because o f

plugging. After the r u n , the reactor system was disassembled and three

inches o f s o l i d s were found in t h e r e a c t o r p r e h e a t e r . S e v e r a l

addi t iona l attempts t o r e s t a r t the p l a n t also led t o p lugging of the

feed l ine . The problem was traced t o the design o f the new prehea ter ,

w h i c h d i f fe red in t h e dispersing section from the o r ig ina l design used

during ea r l i e r runs. The preheater was remachined t o conform w i t h t h e

o ld design, and the p l a n t cer t i f icat ion r u n was restarted on 2/17/89 as

Run 21.

The f i r s t portion of Run 21 was conducted without r ecyc le t o com-

pare the new reference feedstocks with those used previously i n Run 19.

The average resu l t s from four t e s t periods (8, 10, 11, and 12) are sum-

marized i n Tables 1 A and lB, and are compared t o the Run 19 averages.

The coal, 510+'C nondisti l lable (ND), and 371t'C conversions were a l l

equal t o previous reference performance. However, the heptane insol - uble (HI) conversion was about 4% higher than in R u n 19. This t rend

was a l s o observed in autoclave t e s t s using the Run 19 and 21 feeds

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I

(Table 2 ) . Detailed analyses of the new reference feedstocks used i n

Run 21 (R10 and C1.4) and the prior reference feeds (R8 and C1.3) have

been reported previously (2). The compositions of the feedstocks are

so similar t ha t any d i f f e rences i n Runs 19 and 21 a r e probably not

feedstock related. More l ikely, the new reference catalyst (K1.2) is a

l i t t l e b i t more active or bet ter dispersed than the original r e fe rence

catalyst (K1.0).

REACTOR BACK-NIXING STUDIES

Fol lowing t e s t period 12 o f Run 21 (181 HOS), t h e new l i q u i d

recycle system was brought on stream. P l a n t operation was lined out a t

a recyc le r a t i o of 5:l ( recyc le t o f r e sh feed). Three t e s t periods

(17-19) were worked up a t the 5: l r a t i o . Then t h e recyc le r a t i o was

dropped t o 2.5:1, and three more good t e s t periods (21, 22 and 25) were

obtained. The plant was shut down (as scheduled) on 3/3/89 t o conserve

feed.

Average results f o r the various recyc le r a t i o s a r e compared i n

Tables 3A and 38, and d e t a i l e d information on t h e ind iv idua l t e s t

per iods i s given i n t h e Appendix. Coal conversion i s e s s e n t i a l l y

constant a t about 89 wt-% fo r a l l the recycle r a t io s tested. However,

t he presence o f l i q u i d recyc le does appear t o improve asphal tene

conversion (as measured by t h e disappearance o f H I ’ S ) and 510+’C ND

conversion. A t a 2.5:1 recycle t o feed r a t i o , H I conversion increased

-5- uop

. .

from 83.2 t o 88.1 w t - % and t h e ND conversion increased from 57.7 t o

63.3%. Further increases i n t h e recyc le r a t i o ( t o 5:l) d i d n o t ,

however, improve c o n v e r s i o n any more. In f a c t , t h e average HI

conversion dropped t o 85.7%, and the ND conversion t o 56.4%. Whether

these differences are ent i re ly due t o increased back-mixing o r t o other

effects tha t accompany the change i n recycle r a t e i s not c lear .

Although every attempt was made t o hold operating condi t ions con-

s t a n t f o r the three se t s of t e s t s , some differences d id occur. As the

recycle r a t i o was increased, the superficial velocity through the reac-

t o r a l s o increased. Block temperatures on the preheater and reactor

had t o be h o t t e r f o r t he higher recycle cases t o achieve t h e same

a v e r a g e r e a c t o r temperatures . For example, t h e prehea ter block

temperature was 314'C w i t h no recyc le , 450'C f o r 2.5:l r ecyc le , and

460'C f o r 5 : l recycle. The bottom and t o p block temperatures were 400

and 440'C w i t h no recycle, 450 and 437'C a t 2.5:1, and 452 and 450'C a t

5:l. In t e rna l reac tor profiles are compared i n Figure 2. The "best"

(i.e., f l a t t e s t ) prof i le was achieved a t the 2.5: l r ecyc le r a t i o . A t

5: 1, a1 though t h e average reactor temperature was the same, the i n l e t

temperature was low and the o u t l e t temperature was h i g h due t o heat

t r a n s f e r l i m i t a t i o n s . lower conversions a t 5:l were possibly due t o

insuff ic ient temperature i n t h e f r o n t end of t h e r e a c t o r and/or t o

r e t rog rade r eac t ions a t the higher temperature a t the back end of the

reactor.

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Improved back-mixing i s probably a t l eas t par t ly responsible fo r

the improved HI and ND conversions t h a t were observed. Further d a t a

are needed before any quantitative conclusions can be reached. Regard-

l e s s o f whether or not there was any r ea l improvement i n conversion,

t h e r e was a c l e a r improvement i n t h e operabi l i ty of the bench-scale

u n i t w i t h added l iquid recycle. The recyc le stream had a "flywheel"

e f f e c t t h a t he lped t o keep t h e p lan t r u n n i n g s t a b l y , even a f t e r

re la t ively major upsets i n t he feed r a t e o r HPS l e v e l . The higher

velocit ies through the reactor reduced the formation o f coke on the hot

reactor walls. The in te r ior o f the reactor was v i s i b l y c l e a n e r a f t e r

Run 21 than i t had been a f t e r similar runs w i t h no recycle. Thus, i t

may be possible t o operate the plant a t higher temperatures than were

p o s s i b l e w j t h o u t t he recycle . Because o f these b e n e f i t s and t h e

possibi l i ty t h a t improved back-mixing makes bench-scal e r e s u l t s more

representative of the conversions expected from a completely back-mixed

commercial u n i t , l i q u i d recycle was continued i n subsequent runs. The

recyc le r a t i o was s e t a t t h e maximum level for which a f l a t reactor

temperature prof i le could be maintained.

Runs 22 and 23

Runs 22 and 23 were made i n the bench-scale u n i t us ing 2 u t - % i ron

c a t a l y s t (Kerr-McGee porous iron oxide similar t o tha t used a t Wilson-

v i l l e ) w i t h reference feedstocks and operat ing condi t fons. The same

i ron c a t a l y s t was used unsuccessfully i n Runs 15 t o 17 of the previous

contract. The major difference between Runs 22 and 23 and t h e e a r l i e r

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runs was the use of l iquid recycle t o improve reactor back-mixing.

Run 22 was plagued w i t h operational problems. The f i r s t s tar t -up

attempt was made on 4/19/89. The reactor and HPS r e c y c l e system were

s ta r ted up us ing FCC c la r i f i ed o i l , l i q u i d recycle was established, and

temperatures were brought u p t o 400'C before c u t t i n g i n the s l u r r y

feed. Then block temperatures were r a i s e d t o g i v e a 425'C average

reactor temperature (ART). By 52 HOS, the l ine from the low-pressure

separator (LPS) t o the vacuum column had plugged, the vacuum column had

t o be bypassed, and the separator product had t o be r u n d i r ec t ly in to a

c o l l e c t i o n pot. A t 55 HOS, the lines t o the collection pots were a l so

plugged and the plant had t o be shut down. After c l ean ing o u t a l l of

t h e l i n e s , a second a t t e m p t was made on 4/26/89 using t h e same

procedure. This time the block temperatures were ad jus t ed t o g i v e an

ART o f 435'C. The p l a n t again had t o be s h u t down a f t e r 48 hours o f

operation, this time because o f plugging a t the reactor inlet . For the

t h i r d s t a r t - u p a t tempt on 5/3/89, t h e IPS and vacuum column were

bypassed, and the products went d i rec t ly t o a c o l l e c t i o n po t . An ART

o f 425'C was used, s imilar t o the first t ry . A t 24 HOS, the feed pump

gearbox broke. A plug formed i n the suction line t o both HPS r e c y c l e

pumps. l e v e l problems i n t he HPS caused heavy hydrocarbon t o carry

over in to the two recycle gas compressors, shutting them down, and t h e

run was abor ted once more. A t t h a t po in t , t h e whole r e a c t o r and

separator section was d i sassembl ed and cleaned . The reactor 5 tsel f was

f a i r l y clean. The HPS vessel, the hot knock out pot downstream of i t ,

and various plugged l i nes were replaced.

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Run 23 was a repeat of the unsuccessful Run 22. Feed was cut i n on

5/16/89, and t h e block temperatures were lined out t o give an ART of

425.C. The plant ran f a i r l y well f o r 96 hours. The LPS and vacuum

column were again bypassed t o eliminate possible plugging there. Seven

t e s t periods were conducted. Yields and conversions f o r periods 2 , 6 ,

and 7 a r e summarized i n Tables 4A and 48. Compared w i t h the average

values for Run 27 ( w i t h 2% iron ca ta lys t and no l i q u i d r ecyc le ) , t h e

average conversions f o r Run 23 were 2 t o 3% lower. Increasing the

recycle r a t i o and degree o f back-mixing apparent ly had no e f f e c t on e i ther conversion or plant operability for the iron system.

In an attempt t o improve the conversions, the ART was increased t o

about 440'C a f t e r 96 HOS. W i t h i n 4 hours, the HPS l i q u i d level control

s t a r t e d t o become e r r a t i c . Two more t e s t periods were conducted, bu t

the plant was not well lined out, and the resulting mass balances a r e

high. These d a t a for period 9 a r e summarized i n Tables 5A and 5B.

Conversions did improve re la t ive t o the 425'C case, but s t i l l f e l l f a r

short of levels tha t have been achieved using other catalysts , such as

vanadium o r molybdenum, t h a t have a strong hydrogenation funct ion. A t

123 HOS, the plugging became so severe into and out of the collection

pots t h a t a steady level could n o t be maintained. Maintaining a steady

HPS l i q u i d r ecyc le a l s o became d i f f i cu l t , and the r u n was aborted on 5/20/09.

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T h e absence of a strong hydrogenation func t ion for t h e i ron

catalyst system has consistently resulted i n excessive c o k i n g during

bench-scale t r i a l s . T h i s problem has n o t occurred i n the autoclave

because the analytical workup of the products i s done manually. How-

ever, because o f the r e l a t i v e l y small l i n e s izes i n the bench-scale

u n i t , the u n i t i s e spec ia l ly susceptible t o plugging problems. In

numerous at tempts (Runs 15, 16, 17, 22 and 23), the low-pressure side

of the plant has never successfully been operated. The main problem

has been i n the bottoms outlet l ine from the LPS, where after the l i gh t

ends are flashed of f , the solids (unconverted coal and c a t a l y s t ) t e n d

t o come o u t of so lu t ion and plug the in l e t l i ne t o the vacuum column.

T h i s phenomenon has n o t been observed w i t h vanadium o r molybdenum

catalysts and may have to do w i t h the properties o f the l i q u i d product.

The more highly hydrogenated and paraffinic product produced by the V

and Mo c a t a l y s t s appears t o have a g rea t e r a f f in i ty for keeping the

solids i n solut ion. In t h e case of t he i ron c a t a l y s t , many o f t h e

p a r a f f i n s may be cracked out , leaving a more r e f r a c t o r y aromatic

ma te r i a l . The l iqu id-product p rope r t i e s f o r R u n s 23 a n d 2 1 a r e

compared i n Tables 6A and 68. The product from the iron run has a much

lower A P I gravity, a lower hydrogen content, higher sulfur content, and

much greater I eve1 s of heptane insol ubl es and mi cro-carbon (MCRT) .

Going t o higher pressures , l a rge r l ine s izes , o r incorporating a

bottoms recycle loop on the LPS t o increase the l i q u i d veloci ty i n the

LPS o u t l e t l ine may a l l improve the operabili ty of the LPS system w i t h

the iron catalyst . However, the iron catalyst simply does n o t make as

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f

h i g h l y hydrogenated a product as other a v a i l a b l e s l u r r y c a t a l y s t

systems. Even i f a l l o f t he o p e r a b i l i t y problems can be so lved , a

ques t ion s t i l l exis ts as t o whether or not the iron system is r ea l ly

any less expensive t h a n competing vanadium or molybdenum catalysts . A t

current raw material p r i c e s (3) , Fe203 goes for $0.205/lb (S0.293/lb

Fe), V205 for $6.65/1b (S11.88/lb V) , and Moo3 for $3.60/lb ($5.42/1b

Mo) . Prel iminary work w i t h a new molybdenum ca ta lys t ( t o be reported

i n greater de ta i l i n the next quarterly report) , has shown t h a t with as

l i t t l e a s 0.13 wt-% molybdenum, bench-scale u n i t y ie lds and conversions

can be achieved t h a t a r e supe r io r t o those f o r t he 2.0 w t - X i r o n

c a t a l y s t whi le s t i l l maintaining excellent p l a n t operabi l i ty . The

15-times lower catalyst concentration for t h e molybdenum re1 a t i v e t o

the iron nearly of fse t s the 18.5-times greater catalyst cost. When the

yield and product quali ty advantages o f the molybdenum system are taken

i n t o account, the economics f o r the molybdenum ca ta lys t become superior

t o those f o r iron, even on a throwaway c a t a l y s t b a s i s . W i t h ongoing

opt imiza t ion of the molybdeum system and the development o f a ca t a lys t

recovery process t o fur ther reduce catalyst costs, the advantage o f the

molybdenum system over iron i n s lurry catalyst applications can only be

expected t o intensify. For this reason and because of the poor p l a n t

o p e r a b i l i t y when using the i ron c a t a l y s t , t he decis ion was made t o

discontinue a l l further work w i t h i r o n c a t a l y s t s and concen t r a t e on

development o f a molybdenum-based s lur ry ca ta lys t system.

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CONCLUSIONS

The continuous bench-scale u n i t was successfully rereferenced a f t e r

the addition of a HPS liquid-recycle system. T h i s recyc le system was

added t o s imulate improved reactor back-mixing. A t a 2.5:l r a t i o of recyc le t o f r e s h feed , asphal tene and n o n d i s t i l l a b l e conve r s ions

increased by about 5 w t - X over reference performance with no recycle.

Coal conversion was unchanged. The recycle system a l s o improved t h e

o p e r a b i l i t y of t h e bench-scale u n i t by g iv ing i t more iner t ia against

feed upsets. Higher superficial ve loc i t i e s i n t he r e a c t o r helped t o

decrease coking a t the reactor walls.

Test ing of a s l u r r y i ron c a t a l y s t i n Runs 22 and 23 resulted i n

coking and p l u g g i n g o f t he low-pressure s i d e o f t h e p l a n t . The

addition of the recycle system d id not improve conversions over Runs 15

t o 17 with the same iron catalyst but no recycle. The development o f a I

Mo slurry catalyst system t h a t is less expensive than the iron, even on

a throwaway basis, has cdused further work w i t h i ron c a t a l y s t s t o be

discontinued.

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REFERENCES

1. B. G i l l e s p i e and 3. Carberry, " I n f l u e n c e of Mixing on I s o t h e r m a l

R e a c t o r Y i e l d a n d A d i a b a t i c Reactor C o n v e r s i o n " , J & EC

Fundamentals 5 (May 1966):164-171.

2. D. A. Nafis, e t a l , "Bench-Scale Co-Process ing : Q u a r t e r l y R e p o r t

No. 2 , " p r e p a r e d for the United S t a t e s Department o f Energy under

Contract No. DE-AC22-87PC79818, Feb. 15, 1989.

3. Chemical MarketinP ReDorter, Vol. 236, No. 4, July 24, 1989.

DISCLAIMER

This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsi- bility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Refer- ence herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recom- mendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof.

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Table 1A- Plant Recertification

19 Ave. 21 Ave. Run LTOS 8,lO-12 Test Perfod

Run Test Period

Ave Rx Int 1, DegC Rx Outlet 9, psig WSV/Base YHSV Rec. H2 Pty., mol% HPS Rec/feed Ratio

Feed Code Grams NAF feed Resid Code Grams Resid Coal Code Grams Wf Coal Catalyst Code wt% c a t . met./RAFF

feed Distribution: ut% C5-177C W t X 177-343C W t X 343-Slot ut% SIO+C w t X c19F Coal ut% H2 Consump. ut% t o t a l feed

rd Analysis: 'I gravity 5 carbon :% hydrogen :% sulfur ;% nitrogen :% hept. insol. ;% HCRT ;% dist . (371C-)

425.5 3058 1 .o 86.1 0.0

f 08 5285.8

R08 3475.6 c1.2

1810.1 Kl .O 1 .oo

0.0 0.6 13.0 62.2 34.2 2.4

102.4

425.8 3022 1.2 86.1 0.0

f 09 2485.5

R10 1657.0 c1.4 820.5 K1.2 0.99

-6.8 76.65 7.90 4.38 0.80 8.49 10.55 0.96

0.0 0.5 11.4 54.8 33.3 2.2

102.2

Products : Grams 6as COX Grams 6as C1 Grams 6as C2 Grams 6as C3 Grams 6as C4 6ratns 6as CS+ Grams 6as NH3 Grams 6as H2S Grams Net H20 Grams S w/Net H20 Grams OH Product Grams TSB Product Grams Unconv .coal 6rrms HZ Consump.

Total (UAF) ut bal Total C balance Total H balance Total f balance Total N balance* Total ash balance Total Cat. balance

19 Ave. LTOS

2.7 45.7 .36.6 38.3 22.9 26.9 NA 35.4 282.8

)IA 2308.7 2439.6 194.3 124

100.8 101.5 106.6 66.9 100.0 101 .o 90.4

Noma1 ited Conversions: -7.2 Coal 89.3 75.72 C7 Insoluble 79.3 8.03 Wondist. (SlOC+) 56.2 3.99 Dist. (371C+) 34.9 0.94 8.34 10.70 wtx H20tCOx 5.3 0.66 wtX H2S 0.6

wt% NH3 0.4 WtX C144 2.7 wt% CS-177C 5.9 W t X 177-343C 18.2 WtX 343-51OC 31.5 Wt% SSWC 34.2 wt% Unc )(AF Coal 3.7 ut% t o t a l prod 102.4

Product D i ttri but ion:

21 Ave. 8,lO-12

0.4 17.3 14.1 13.4 0.1 7.5 8.3 30.8 124.8

NA 1182.5 1027.5 87.4 55.5

99.7 99.1 101 .o 79.5 100.0 87.2

NA

89.5 83.2 57.5 34.1

5.2 1.3 0.3 2.2 5.5 17.5 32.9 33.9 3.5

102.2

*loo% Nitrogen Balance assumed t o calculate NH3 by disappearance of N from 1 Squid streams.

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Table 18- Plant R e c e r t i f i c a t i o n

Run Test Per iod

To1 uene So1 ubl e Bot t TSB A P l TSB wtX C TSB w t % H TSB ut% S TSB w t X N TSB ut% HI TSB w t X WCRT TSB ut% ash TSB ppm C a t . TSB 01160, volX

IBP, Deg C 5% 10% 20% 30% 40% 50% 60% EP x @EP W t X 01160 OH

TSB OH A P I TSB OH G L C , wt%

IBP, Deg C 5% 10% 20% 30% 40% 50% 60% 70% 80% 90% 95% EP X @EP

ut% 01160 Btms TSB Btms API

19 Ave. 21 Ave. LTOS 8.10-12

oms Product Proper t ies : 3.3 4.4

85.98 86.48 10.18 9.95 2.27 2.21 NA 1.33

11.65 9.14 NA 19.95 0.01 0.00 38 32

398.3 457.3 473.3 493.0 512.8

NA NA NA

542.0 NA

42.42 10.9

340.3 412.0 434.5 459.0 474.8 488.8 500.3 511.8 523.5 536.5 554.5 568.5 577.5 100.0 57.6 -4.0

410.5 477.3 496.5

NA I A NA NA NA

537.8 28.1 28.30 12.9

327.0 402.8 427.8 456.0 473.8 487 .O 498.5 509.8 520.8 532.3 548.0 562.5 572.8 97.0 71.7 -3.5

Run Test Per iod

19 Ave. 21 Ave. LTOS 8,lO-12

Overhead Product Proper t ies : OH A P I 24.4 OH wt% c NA OH w t X H NA OH wtX s 1.44 OH wtx N 0.33 OH GLC, w t X

5% 120.0 10% 163.3 204: 219.8 30% 261 .O 40% 298.0 50% 332.0 60% 361 .O 70% 388.3 80% 415.0 90% 442.8 95% 460.5 EP 488.5 x @ f P 100.0

AP I 13.6 wtx c NA wtx N NA wtx s 1.9 W t X N EJA W t X HI 6.0 w t X WCRT NA W t X diSt. (37lC-) 31.9

IBP, Deg C. 38.0

Tota l Liquid Proper t iesf

Unconverted Coal Sol ids Prope ucc wtx c HA UCC w t X H HA UCC wtx s NA UCC wt% N HA

% Desutf."* 64.6 X Denitrif .- NA

23.9 84.99 11.60 1.29 0.31

0.3 101 .o 160.0 244.8

322.8 352.3 380.0 406.3 431.3 457.5 474.5 514 .O 100.0

288.3

14.9 85.6 10.8 1.7 0.8 4.0 9.0 30.8

!rt ies** 82.1

5.6 10.7 1.6

77.4 32.9

Weigh ted average o f overhead and toluene soluble bottoms products. **Calculated as (gTIBx)/(gTIBC t gTIBH + gTIBS - gCatS t gTIBN)*lOO% ***Calculated as (Feed S or 1 - Liquid Prod. S or N)/(Feed S or N)*100To

-15-

Table 2 - Comparison o f Autoclave Results f o r Run 19 and Run 21 Feeds

Feed from: Run 19 Run 21 Autoclave Test: 5392-**** 6431-009 Coal Type Resid Type Catalyst Type Resid/Coal , w t / w t Catalyst, ut% MAFF

Temp., Deg C. Pressure, atm. Res. Time, hrs.

Weight Recovery, X MAF U t . Rec., X Ash Balance, %

Conversions, ut% * HAF Coal Heptane Ins. S l O C + 373C+

Prod. D i s t . , ut% NH3 HZO HZS c02 C1 -C4 C5-37 1 C** 371-51oc 510C+ RAF Coal* H2 Consumption***

Total

MF C1.2 R8

K1 .O 1.92 1.01

420 200

2

96.44 96.18 99.76

90.52 80.40 70.16 49.03

0.2 0.0 2.8 0.2 2.7

45.7 24.6 22.5 3.3

-2.18 100.0

MF C1.4 R10

K1.2 2.00 1 .oo 420 200

2

94.67 89.50

93.01 03.72 68.92 47 * 55

0.2 2.9 3.2 0.3 4.9

38.6 24.7 25.1 2.5

-2.21 100.0

94.48

Total Llquid Product Properties 15.4 15.9 AP I

wtx wt% ut% wtx wtx ut%

* ** *** ****

carbon 85.04 85.33 hydrogen 10.98 10.51 sulfur 2.00 1.55 nitrogen 0.67 1.01 heptane ins. 5.945 5.483 HCRT NA 10.9

Adjusted f o r Ash Balance, i f Ash Balance < 100%. Adjusted f o r 100% MAF Recovery. Adjusted f o r ca ta lys t reduction. Average of tests 5392-031, 5392-041, 5392-059 8. 5392-101.

-16-

Table 3A- Comparison o f Recycle R a t i o s Run Test PerZods Recycle Ratio Ave Rx Int T, DegC Ux Outlet P, psig WSVIBase UHSV Rec. tl2 Pty., nol%

Feed Code 6rms WAF feed Resid Code Grams Resid Coal Code Grams WF Coal Catalyst Code Wt% cat. aet./WAfF Feed D i str I but ion : wt% CS-l7tC WX 177-343C WtX 343-510C wtx 5104 ut% CltAf Coal ut% H2 Consump. ut% total feed

21 Ave. 21 Ave. 21 Ave. 17-19

5.0

125.8 3005

1.1 07.1

F09 2348.4

R10 1565.6

C1.4 782.8

K I .2 0.99

Run Test Periods Recycle Ratio

21 Ave. 21 Ave.

0.0 2.5 8,lO-12 22,23,25

21 Aye. 37-19

5.0

~- ..

&lo-12 22,23,25 2.5 0.0

425.8 3022 1.2 86.1

f09 2485.5

R10 1657.0 C1.4

828.5 Kf .2 0.99

Products: 6rams Gas COX Grams Bas C1 Grams 6as C2 Grams 6as C3 Grams Gas C4 Grams 6as C5+ Grams Gas NH3 Grams Gas H2S Grams Net H2O 6rams S u/Net H2O 6rams OH Product Grams TSB Product 6rams Unconv. coal Grams H2 Consump.

425.4 3006 1.07 85.87

F03 2270 2

R10 1513.5

C 1 .4 756.7 K1.2 0.99

0.4 17.3 24.1 13.4 8.1 7.5 8.3 30.8

124.8 MA

1182.5 1027.3 87.4 55.5

0.0 17.5 13.3 14.3 8. 1 6.4

12.5 31.9 246.3

NA 1299,5 743.1 84.3 69.3

101.6 101.4 101.7 71.2

100.0 74.1 NA

0.0 17.2 13.9 14.3 7.7 6.5 4.3

36.1 137.7

I A 1011.3 1043.2 91 .o 48.2

0.0 0.5

l t .4 54.8 33.3 2.2

102.2

0.0 0.5

11.4 54.8 33.3 3.0

103.0

0.0 0.s

11 .I 54.8 33.3 2.1

102.1

Total (WF) ut bal 99.7 Tota l C balance 99.1 Total H balance 101 .o Total S balance 79.5 Total N balance* 100.0

'Total Cat . balance NA Total ash balance 87.2

99.4 99.0 106.2 74.2 100.0 86.8 NA Feed Anatys i s :

A P I grrvdty ut% crrbon ut% hydrogen r t X sulfur ut% nftrogen w t X hept. fnsol . Wt% HCRT w t X dist. (37lC-)

-7.2 75.72 8.03 3.99 0.94 8.34 10.70 0.66

-7.2 t 5 . 7 2 8.03 3.99

Normal ired Convert f oris : Coal 89.5 C? Insoluble 03.2 Nondist. (510Ci) 57.5 Dirt. (37lCt) 34.1

-7.2 75.72 8.03 3.99 0.94 0.34

10.70 0.66

89.0 88.1 63.3 38.4

88.3 85.7 56.4 35.5 0.94

8.34 10.70 0.66

Dduct D i strt but i on : t% HZO+tOx 5.2 tX H2S 1.3

0.3 LX NH3 tX Cl44 2.2 :% CS-17tC 5.5 ;X 177-343C 17.5 :X 343-5lOC 32.9 :% 510tC 33.9

3.5 .% Unc WAF Coal ,% total prod 102.2

6.3 1.4 0.5 2.3 6.3

19.8 34.1 28.6 3.7

103.0

5.9 1.5 0.2 2.3 517 17.7 30.2 34.6 3.9

102.1

*IO& Nitrogen Balance assumed to calculate NH3 by disappearance of N from 1 iquid streams.

-17-

i

Table 36- Comparison o f Recycle Ratios

Run 21 Ave. 21 Ave. 21 Ave. res t Periods 8,lO-12 22,23,25 17-19 Recycle Ratio 0.0 2.5 5.0

Toluene Soluble Bottoms Product Prooerties: 756 A P I 758 ut% C TSB ut% H TSB ut% S TSB ut% N TSB wt% HI TSB wt% HCRT TSB ut% ash 758 ppm Cat. TSB 01160, vo\%

IBP, Deg C 5% 10% 20% 30% 40% SOX 60% EP X @EP ut% 01160 OH 1SB OH API 7SB OH GLC, W t X

I%P, Deg c 5% 10% 20% 30% 40% 50% 60% 70% 80% 90% 95% EP X QEP

ut% 01160 Btms TSB Btms A P I

4.4 86.48 9.95 2.21 1.33 9.14 19.95 0.00 32

410.5 477.3 496.5

NA NA t lA NA NA

537.8 28.1 28.30 12.9

327.0 402.8 427.8 456.0 473.8 487 .O 498.5 509.8 520.8 532.3 548.0 562.5 572.8 97.0 71.7 -3.5

1 1' # . f

87.8 10.6 1 .5 1.2 4.4

16.77 0.0 NA

290.3 470.7 493.0 518.7

NA NA NA NA

544 .O 32.7 32.8 14.8

236.7 389.7 424.3 456.0 475.3 488.7 501 .o 512.7 524.0 536.0 553.0

NA 571.3 95.3 67.2 5.8

7.4 88.3 11 .o 1.6 1.6 4.9 16.4 0.0

11.6

210.3 467 .O 481.3 504.0 527.3

NA NA NA

539.7 36.3 36.3 14.5

252.7 403.3 431.7 459.0 475.0 487.0 497.7 508.0 519.3 531 .O 545.3 559.7 572.0 97.3 63.7 5.7

Run Test Periods Recycl e Rat i o

21 Ave. 21 Ave.

0.0 2.5 8,lO- 12 22,23,25

Overhead Product Properties : OH API OH wt% c OH ut% ti OH wtx s OH w t X N OH 6LC, w t X

fBP, Deg C. 5% 10% 20% 30% 40% 50% 60% 70% 80% 90% 95% EP x Q f P

23.9 84.99 11.60 1.29 0.31

0.3 101 .o 168.8 244.8 288.3 322.8 352.3 380.0 406.3 431.3 457.5 474.5 514.0 100.0

lo t AC wt wt wt ut wt wt wt

.a1 Liquid Properties* 'I 14.9 .% c 85.6 ,% H 10.8 .% s 1.7 .% N 0.8 :% HI 4.0 ,% RCRT 9.0 ,X d is t . (37lC-) 30.8

22.2 85.7 11.9 0.8 0.2

1.7 100.7 174.0 247.3 290.0 325.3 356.3 385.7 414.0 440.7 473.0 500.0 561.7 98.7

16.8 86.4 11.4 I .o 0.5 1.6 6.1 35.1

Unconverted Coal Sol ids Properties+* ucc ut% c 82.1 81 .O UCC w t K H 5.6 5.6 ucc ut% s 10.7 11.2 UCC wtx N 1.6 2.2

x Desulf.-+ X D e n i t r i f ..r**

77.4 .86.4 32.9 53.0

21 Ave. 17-19 5.0

26.4 84.8 11.8 0.7 0.2

-3.3 89.3 157.3 233.3 273.0 306.0 335.3 362.7 388.7 414.0 440.0 455.0 480 a 7 100.0

16.8 86.6 11 .4 1.2 0.9 2.5 8.3 31.6

82.2 5.7 10.2 1.8

85.2 22.3

Weighted average o f overhead and toluene soluble bottoms products. *Calculated as (gTIBx)/(gTIBC + gTI8H + gTIEJS - $Cat$ + gTIBN)*lOO% **Calculated as (Feed S or N - Liquid Prod. S or N)/(Feed S or N)*lOO%

-18-

Table 4A- Comparison o f Iron Cata lys t Runs

Run 17 Ave. Test Period 4,5,12,13

Ave Rx Int 1, OegC 425.7 Rx Outlet P, psig 3000 WSV/Base YHSV 0.5 Rec. H2 Pty., mol% 90.1 HPS Rec/Feed Rat io 0.0

Feed Code F06 Grams WF feed 1017.0 Resid Code R08 Grams Resid 678 0 Coal Code c1.2 Grams WF Coal 339.0 Cata lys t Code K3.0 ut% c a t . net./WFF 2.95

Feed Dis t r ibu t ion : W t X C5-177C 0.0 ut% 377-34313 0.6 W t X 343-510C 13.2 W t X 5lOtC 52.9 wtX 13AF Coal 33.3 w t X H2 Consump. 2.0 W t X t o t a l feed 102.0

Feed Analysis: API g r a v i t y -6.8 ut% carbon 76.91 wt% hydrogen 7.96 ut% sulfur 4.40 ut% ni t rogen 0.80 ut% hept. fn so l . 8.63 ut% WCRT 10.73 ut% d i s t . (371C-) 0.97

23 Ave.

126.2 3012 1.07 87.01 5.4

F10 2260.5

R10 1529.5 C1.4 731. I K3.1 2.19

0.0 0.5 11.6 55.6 32.3

I .6 101.6

2.6~

-7.8 76.29 8.13 4.03 0.94 8.53 10.94 0.67

Run 17 Ave. Test Period 4,5,12.13

Products: Grams 6as COX Grams 6as C l Grams 6as C2 Grams 6as C3 Grams Gas C4 Grams 6as C5+ Grams 6as NH3 Grams 6as H25 Grams Net H20 Grams S w/Net H2O Grams OH Product Grams TSB Product Grams Unconv .coal Grams H2 Consump.

0.7 5.9 4.6 4.2 1.5 1.6 NA 6.6 29.5

NA 14.9 808.7 94.7 20

Total (WF) u t bal 93.9 Total C balance NA Total H balance NA Total S balance 99.3 Total N balance* NA Total 8th balance 98.6 Total Cat. balance 87.3

Normal ired Conversions: Coal 70.3 C7 Insoluble 52.2

Dist. (371C+) 25.3 Nondist. (510C+) 47.5

Q t c wl wl wl wl wl wl wl wl wi wl

rduct Di s t r ibu t ion : :% H2O+COx 3.2 ;X H2S 0.7 :% NH3 HA :% C1-C4 1.7 :% c5-177c 1.7 :% 277-34313 16 .4 ;% 343-51063 33.0 ;% SlO+C 35.4 :% Unc ClAF Coal 9.9 :% t o t a l prod 102.0

23 Ave. 2,697

4.2 18.8 13.7 12.4 4.3 10.4 4.8 8.3

170.8 NA 0.0

1922.2 251.3 36.6

105.6 102.2 100.0 128.6 108.7 112.3 105.0

67.4 50.0 41.6 25.6

7.5 0.4 0.2 2.1 1.5 12.2 26.5 10.8 10.6 101.6

*lo& Nitrogen Balance assumed t o c a l c u l a t e NH3 by disappearance o f N from l i q u i d streams.

-19-

.

Run T e s t Period

Table 46- Comparison of Iron Cata lys t Runs 17 Ave. 23 Ave.

4,5,12,13 2,6,7 Run T e s t Period

17 Ave. 23 Ave. 4,5,12,13 2,6,7

TSB w t X N TSB w t X H I TSB w t X MCRT TSB ut% ash TSB ppm Cat. TSB 01160, vol%

IBP, Deg C 5% 10% 20% 30% 40% 50% 60% EP x CEP w t X 01160 OH

TSB OH A P I 758 OH GLC, w t X

fW, Oeg C 5% 10% 20% 30% 4m 50% 60% 70% 80% 90% 95% EP X 8EP

ut% Of160 Btms TSB Btms API

NA 12.35 NA

0.00 0

121 .5 232.8 281.8 344.8 394.5 435.0

NA NA

521 . S NA

64.76 15.2

185.5 231.3 257.3 305.8 343.8 375 3 403.3 431.3 455.5 479.0 510.0 531.3 596.3 100.0 35.2 -7.3

9.63 3.5 0.8

12.7 16.05

0.0 0.0

159.0 282.3 335.0 398.0 440.0 480.0 514.0

NA 335.0

55.0 53.5 15.1

Toluene Soluble Bottoms Product Propert ies : Overhead Product Proper t ies : TSB A P I 10.2 5.9 OH API 0.00 TSB w t X C 84.81 84.74 OH ut% c 0.00 TSB w t X H 9.95 TSB ut% S 2.71

188.2 247.2 284.7 323.7 356.2 385.0 411.3 435.5 459.3 406.2 512.2 543.7 99.0 46.5 -4.5

OH ut% H OH w t X S OH w t X N OH GLC, wtX

IBP, Oeg C. 5% 10% 2VL 30% 40% 50% 60% 7ox 80% 90% 95% E? x e w

0.00 0.00 0.00

0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0

Total l i q u i d Propert ies* AP I 10.0 wtx c 83.3 W t X H 9.8 W t X s 2.7 W t X N NA W t X HI 12.1 ut% MCRT HA W t X d i s t . (371C-) 25.8

0.0 0.0 0.0 0.0 0.0

0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0

5.9 84.7

9.6 3.5 0.8

12.7 16.1 21 .4

Unconverted Coal Sol i d s Properties** ucc wtx c HA 84.9 UCC W t X H HA 6.2 ucc wtx s NA 6.5 UCC W t X N NA 2.3

X Desulf .*+* X Deni trif .++*

54 .4 MA

31.3 33.4

q e i g h t e d average of overhead and to luene s o l u b l e bottoms products . ++Calculated as (gTIBx)/(gTIBC + gTIBH i gTIBS - gta tS + gTIBN)*100% *++Calculated as (Feed S or N - l i q u i d Prod. S or N)/(Feed S or N)*100%

-20-

Run 7est Period

Table 54- Severity Comparison for Zron Catalyst

23 Ave. 2,697

Ave Rx Int 1, DegC 426.2 Rx Outlet P, psig 3012 WSV/Base YHSV I .07 Rec. H2 Pty., mol% 87.01 HPS Rec/Feed Ratio 5.4

Feed Code Grams )IAF feed Resid Code Grams Resid Coal Code Grams CIAF Coal Catalyst Code w t X cat. net./WFF

F10 2260.5

R10 1529.5

C1.4 731.1 K3.1 2.49

23 Ave. 9

441 .O 3019 0.78

82.78 7.2

F10 1649.9

R10 1116.3

C1 .4 533.6 K3.1 2.19

feed Distribution: W t X C5-177C 0.0 0.0 Wtx 177-343c 0.5 0.5 W t X 343-51OC 11.6 11.6 ut% SlO+C 55.6 55.6 wtX MF Coal 32.3 32.3 wtX H2 Consump. 1.6 3.0 w t X to ta l feed 101.6 103.0

Fec AI ul wl wl wt wt wt wt

td Analysis: ?I gravity t% carbon 1% hydrogen :% sulfur :% nitrogen ;% hept. insol . ;% MCRT rX d i s t . (371C-)

-7.8 -7.8 76.29 76.29 8.13 8.13 4.03 4.03 0.94 0.94 8.53 8.53

10.94 10.94 0.67 0.67

Run lest Period

Products : Grams 6as COX Grams 6as C 1 Grams 6as C2 Grams 6as C3 Grams 6as C4 Grams 6as C5+ Grams 6as NH3 Grams Gas H2S Grams Net H20 Grams S w/Net HZO Grams OH Product Grams TSB Product Grams Unconv. coal Grams H2 Consump.

4.2 18.8 13.7 12.4 4.3

10.4 4.8 8.3

170.8 NA 0.0

1922.2 251.3 36.6

Total ( U T ) wt bat 105.6 Total C balance 102.2 Total H balance 100.0 Total S balance 128.6 Total N balance+ loa. 7 Total rsh balance 112.3 Total Cat. balance 105.0

Noma1 ired Converstons: Coal 67.4 C7 Insoluble 50.0 Uondist. (SlOC+) 41.6 O M . (371Ct) 25.6

Product D i stri but ion: ut% H2OtCOx 7.5 wt% H2S 0.4 Wt% NH3 0.2 Wt% CI-C4 2.1 Wt% C5-177C 1.5 W t X 177-34313 12.2 Wtx 343-51OC 26.5 ut% 51otc 40.8 ut% Unc CIAF Coal 10.6 ut% to ta l prod 101.6

23 Ave. 9

*100% Nitrogen Balance assumed t o calculate NH3 by disappearance o f N from 1 iqu id streams.

4.6 24.9 20.9 17.3 5.3 3.2 3.6

16.0 120.1

I A 0.0

1606.4 164.3 50.3

116.9 117.3 100.0 i46.2 114.0 142.9 126.8

73.6 57.5 53.7 34.4

6.5 0.8 0.2 3.5 2.9

10.8 29.5 32.2 8.5

103.0

c

Run Test Period

Table 58- Severity Comparison for Iron Catalyst

23 Ave. 23 Ave. Run 2,697 9 Test Period

23 h e . 23 Ave. 9 2 ~ 7

Toluene Soluble Bottoms Product Properties: Overhead Product Properties: 0.0 0.0 OH API 7.6 TSB API

TSB ut% C TSB ut% H TSB ut% S TSB ut% N TSB ut% HI TSB ut% W R Y TSB wt% ash TSB ppm Cat. TSB D1160, vo lX IBP, Deg C 5% 1oX 20% 30% IC% SOX 60% EP x 8EP ut% Dl160 OH

TSB OH API 756 OH GLC, w t X IBP, Oeg C 5% lox 20% 30% 4m 50% 60% 70% 80% 90% 95% EP X 8EP

ut% 01160 Btms TSB Btms A P I

5.9 84.74 9.63 3.5 0.8 12.7 16.05 0.0 0.0

159.0 282.3 335.0 398.0 440.0 480.0 514.0

NA 535.0 55.0 53.5 15. 1

NA 188.2 247.2 284.7 323.7 356.2 385.0 411.3 435.5 459.3 486.2 512.2 543.7 99.0 46.5 -4.5

86:32 9.63 3.0 0.7 10.9 IS. 16

0.0 0.0

115.5 191.5 282.5 342.0 382.5 419.0 449.0 496.5 532.5 66.5 65.3 15.1

110.0 162.5 237 .O 278.5 312.5 344 .O 374.0 402 5 430.0 458.5 491.5 516.5 569.0 100.0 34.7 -9.2

OH ut% C OH wt% H OH ut% S OH ut% N OH GLC, ut%

IBP, Deg c. 5% 10% 20% 30% 40% 50% 60% 70% 80% 90% 95% EP X CEP

0.0 0.0 0.0 0.0

0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0

Total Liquid Properties* API 5.9 ut% c 84.7 ut% H 9.6 wtx s 3.5 ut% N 0.8 w t X H I 12.7 ut% MCRT 16.1 ut% dist. (37lC-) 21.4

0.0 0.0 0.0 0.0

0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0

7.6 86.3 9.6 3.0 0.7 10.9 15.2 32.0

Unconverted Coal Sol ids Propertfes+* ucc wtx c 84.9 84.5 UCC wt% H 6.2 5.9 ucc ut% s 6.5 II .3 UCC ut% N 2.3 2.8

x Desul f .*+* % Denitrif.-*

31.3 33.4

33.9 30.8

+Yeighted average o f overhead and toluene soluble bottoms products. **Calculated as (gTIBx)/(gTIBC + gTIBH + gTIBS - gCatS + gTIBN)*100% ***Calculated as (feed S or N - l i q u i d Prod. S or N)/(Feed S or N)*lOO%

-22-

i

Table 6A- Comparison o f V and Fe Catalysts

Run 21 Ave. Test Period 22,23,25

Ave Rx Int 1, OegC Rx Outlet P, psig YHSV/%ase UHSV Rec. H2 Pty. mol% )IPS Rec/feed Rat io

Feed Code Grams WAF feed Resid Code Grams Resid Coal Code Grams M A F Coal Catalyst Code wtX ca t . met./MfF

Feed Distribution: wt% c5-177c wtx 177-343c WtX 343-51OC wtx 51o+c w t X K4F Coal ut% H2 Consump. w t X t o t a l feed

Feed Analysis: A P I gravfty wt% carbon wt% hydrogen ut% su l fur wtX nitrogen wt% hept. insol. w t X HCRT ut% d i s t . (371C-)

425.4 3006 1.07

85.87 2.5

F09 2270.2

R I O 1513.5

c1.4 756.7

K1.2 0.99

0.0 0.5

11.4 54.8 33.3 3.0

103.0

-7.2 75.72 8.03 3.99 0.94 8.34 IO. 70 0.66

23 Ave.

426.2 3012 1.07

87.01 5.4

F10 2260.5

R10 1529.5

C1.4 731.1 K3.1 2.49

0.0 0.5

11.6 55.6 32.3

I .6 101.6

-7.0 76.29 8.13 4.03 0.94 8.53

10.94 0.67

2,6,7 Run 21 Ave. Test Period 22,23,25

Products : Grams Gas COX Grams Gas C1 Grams 6as C2 Grams Gas C3 Grams 6as C4 Grams 6as CS+ Grams Gas NH3 6rams 6as H2S 6tams Net H2O brims S w/Net H20 Crams OH Product Grams TSB Product Grams Unconv. coal Grams HZ Consump.

0.0 17.5 13.3 14.3 8.1 6.4

12.5 31.9

146.3 NA

1299.5 743.1 84.3 69.3

Total (WF) ut bal 101.6 Total C balance 101.4 Total H balance 101.7 Total S balance 71.2 Tota l N balance* 100.0 Total ash balance 74.1 Total Cat. balance NA

Normal 5 zed Convers 3 ons : Coal 89.0 C7 Insoluble 88.1 Nondirt . (510Ct) 63.3 Dist. (371Ct) 38.4

Product Di str i but i on : ut% HZOtCOx 6.3 ut% H2S 1 .4 nt% NH3 0.5 wt% C l - C I 2.3 W t X C5-l77C 6.3 wt% 177-343C 19.0 W t X 343-51OC 34.1 wtx 51otc 28.6 ut% Unc CtAF Coal 3.7 ut% total prod 103.0

23 Ave. 2 A 7

4.2 18.8 13.7 12.4 4.3

10.4 4.8 8.3

170.8 NA 0.0

1922.2 251.3 36.6

105.6 102.2 100.0 128.6 108.7 112.3 105.0

67.4 so.0 41.6 25.6

7.5 0.4 0.2 2.1 1.5

12.2 26.5 40.8 10.6

101.6

*1OoX Nitrogen Balance assumed t o calculate NH3 by disappearance o f N from l iquid streams.

-23-

I

Table 6B- Comparison o f V and Fe Catalysts

Run Test Period

21 Ave. 23 Ave. 22,23,25 2.6.7

Run Test Period

21 h e . 23 Aye. 22,23,25 2,6,7

TSB A P I TSB W t X C TSB w t X H . 758 W t X S TSB w t X N IS6 W t X HI TSB w t X MCRT TSB wtX ash TSB ppm C a t . TSB D1160, volX

IBP, Deg C 5% 10% 20%

*30% 4ox 50% 60% EP X @EP W t X 01160 OH

TSB OH API TSB OH GLC, w t X

IBP, Deg C 5% 10% 20% 30% 40% SOX 60% 70% 8oX 90% 95% EP X CEP

ut% 01160 Btms TSB Btrns API

7.7 87.8 10.6

1.5 1 .2 4 .4

16.77 0.0 NA

290.3 470.7 493 .O 518.7

HA NA HA NA

544.0 32.7 32.8 14.8

236.7 389.7 424.3 456.0 475 ' 3

501 .O 512.7 524 .O 536.0 553.0

NA 571.3 95.3 67 .2

5.8

488.7

5.9. 84.74

9.63 3 .5 0.8

12.7 16.05

0.0 0.0

159.0 282.3 335.0 398.0 440.0 480.0 514.0

NA 535.0 55 .0 53.5 IS. 1

NA 188.2 247.2 284.7 323.7 356.2 385.0 411.3 435.5 459.3 106.2 512.2 543.7 99.0 46.5 -4.5

OH wtx c OH wt% H OH w t X S OH ut% N OH GLC, ut% IBP, Deg C. 5% 10% 20% 30% 40% 50% 60% 70% 80% 90% 95% LP x QEP

85.7 11.9 0.8 0.2

1.7 100.7 174.0 247.3 290.0 325.3 356.3 385.7 414.0 440.7 473.0 500.0 561.7 98.7

Total l i q u i d Properties' AP I 16.8 wtx c 86.4 wtx H 11.4

1 .o wtx s w t X N 0 . 5 wtx HI 1.6 w t X MCRT 6.1 ut% dis t . (37lC-) 35.1

0.0 0.0 0.0 0.0 0.0

0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0.0

5.9 84.7

9 .6 3 .5 0.8

12.7 16.1 21.4

Unconverted Coal Sol ids Properties+* ucc wtx c 81 .O 84.9 UCC ut% H 5.6 6.2 occ wt% s 11.2 6.5 UCC ut% N. 2.2 2.3

x Desulf.** 86.4 31.3 X Denitr4f.- 53.0 33.4

+Weighted average of overhead and toluene soluble bottoms products. -Calculated as (gTIBx)/(gTIBC i gTIBH + gTIBS - gCatS + gTfBN)*IOO% *+*CalcuTated as (Feed S or N Liquid Prod. S or N)/(Feed S or N)*100%

-24-

w

It

Y c c

ILI

z 0

a

---I-

?

L 0, c, Q, L aJ L Q

a

N v) 0

0 v) t

E 0 e, e, 0 m

a X

N v) t

h (3 t

t t *

Q,

U

= X Q:

c

z .

Q 2: " 8 '3 S33Y030

-26-

APPENDIX

Oetai 1 ed lest Results

Run No. 21 - 2:l Iloydnins!er Rend:I lhnois Coal No. 6

Run 19 Awe. 21 21 21 l e s t Ptriod LTOS 8 10 11 Per. length, hrs 30 12 12 12 I n i t i a l H9j 109 133 145 Bvt Ex Int I , Ocgt 425.5 421.5 424 428 Rx Outlet P, psig 3058 3015 3020 3051 UHSL/Base UHSU 1.0 1.12 1.13 1.12 Rcc, H2 Pty., ~ 0 1 % 86.1 86.65 86.33 65.00

1 utX U Catalyst

HPS Rc~lTted Rat10 0.0 0.0 0.0 0.0

21 12 12

157 126.6 3000 1.04 66.53 0.0

21 17 12 229 425 3008 1.16 87.65 4.7

21 18 12 241

425.5 3000 1.13 67. MI 5.0

21 19 12 253 427 3006 1.D5 66.76 5.3

21 22 12 289

126.4 3000 1.11 86.11 2.6

21 23 12

301 42% 1 3007 1.12

85, 64 2.1

21 25 12 325

125.7 301 0 1.00 85.87 2.7

fwd todc fD8 109 104 fO9 fD9 fO9 fo3 fO9 fO9 f W fO9 6rms RRf feed 985.8 2369.62 3020.38 2356.67 2195.13 2117.14 2382.52 2215.44 2336.37 2369.60 2104.67 Resid Code ROB R10 R10 R10 R10 R10 R10 R10 R10 RlO R10

Cos1 Code E1.2 tl.1 f1.4 Cl.4 t1.4 tl.1 t1.4 t1.4 (1.4 Cl.1 C1.1 6rms MF Coal 1810.1 789.81 1006.79 785.56 731.71 815.71 744.17 738.48 778.79 789.87 101.56 b t a l y s t Code K1.O K1.2 K1.2 K1.2 (1.2 K1.2 K1.2 K1.2 K1.2 K1.2 K1.2 utX cat. nct.MAff 1.00 0.99 0.99 0.99 0.93 0.99 0.99 0.99 0.99 0.99 0.99

Crms Resid 3175.6 rn9.n 2~13.59 157t.i~ 1463.12 1631.13 tsee.35 ~ 6 . 9 6 t557.5e 1 ~ 9 . 7 3 1103.11

feed Distri butlon: ut2 C5-I??C 0.0 O.OG 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 utX 373-343: 0.6 0.17 0.47 0.47 O.q? 0.47 0.17 0.47 0.47 0.17 0.17 utX 343-510C 13.0 11.42 11.4; 11.12 11.42 11.12 11.12 11.42 11,42 11.12 11.12 utx 51b.C 52.2 51.78 54.78 51.78 51.76 51.73 5'1.78 54.78 51.78 51.78 54.78 utX RAT teal 31.2 33.33 33.33 33.33 33.33 33,33 33.33 33.33 33.33 33.33 33.33 ut% 112 tonsmp. 2.5 2.38 2.01 2.39 2.26 1.77 2.11 2.27 2.30 3.73 2.45 ut1 tota l fed 102.4 102.38 102.01 102.34 102.28 101.77 102.11 102.27 102.90 103,73 102.45

feed Rnalysis: RPI grauity -6.8 -7.2 -7.2 -7.2 -7.2 -7.2 -7.2 -7.2 -7.2 -7.2 -7.2 utX carbon 76.65 75.72 15.72 75.72 75.12 75.72 75.72 75.72 75.72 15.72 75.12 utX hydrogen 7.90 8.03 8,03 8.03 6.03 8.03 8.03 8.03 8.03 8.03 6.03 ut% sulfur 1.38 3.99 3,99 3.99 3.99 3.99 3.99 3.99 3.99 3.99 3.99 utX nitrogen 0.80 0.94 0.99 0.91 0.91 0.91 0.91 0.94 0.91 0.94 0.94 utX hept. insol. 8.19 8.34 8.31 8.31 8.31 8.31 8.34 8.W 8.34 8.34 8.34 utX RCRl t0,55 10,7R 10.70 10.70 10.70 10.10 10.70 10.70 10.70 10.70 10.70 utX dlst. (371C-) 0.96 0,66 0.66 0.66 0.66 0.66 0.66 0.66 0.66 0.66 0.66

A- 1

Run Wo. 21 - 2:l Lloydrinstcr Rtsid:Illirtois Coal Ho. 6

Pun 19 he. 21 21 21 21 21 21 21 21 21 21 lest Ptriod LlOS 8 10 11 12 17 18 19 22 23 25

1 ut1 U Catalyst

Products: Crms Qs COX bas 6as tl h s 6as c2 bas 6as c3 Srms 635 t4 6rms bas (54 bas ~ D S WH3 6ras bas H25 6ras kt H20 6rms S ulnet H20 6rms OH Product &as IS8 Product 6rm5 Unconu.ura1 bas HZ consnp.

2.7 0,15 0.f6 0.13 0.46 0.00 0.00 15.7 16.36 16.59 18.33 17.99 15'67 17.93 36.6 12.91 12,70 15.77 11.96 13.36 11.52 38.3 12.44 12.10 15.29 13.73 13.71 14.93 22.9 7.73 7.52 9.08 8.02 8.02 ?.?E 26.9 6.21 6.27 9.41 7.92 6.61 7.70 I1R 5.28 8.89 12.74 6.47 3.92 2.45 35.4 29.86 27.41 31.71 31.31 31,90 12.78 282.8 119.0 69.0 151.0 100.0 127.0 151.0

IIR WA HA M M HR HA 2308.7 1027.00 1152.00 1325.00 1226.00 lMI2.00 1057.00 2439.6 1063.83 1433.89 862.19 750.29 1101.15 1103.92 194.3 82.59 115.14 79.37 12.37 104.11 90.98 121 55.32 60.70 55.06 49.98 13.27 51.01

0.00 0.00 0.00 0.00 17.92 19.52 16.51 16.36 13.97 11.88 12.17 12.84 14.76 16.11 12.97 13.83 ?,13 1D.M 7.69 6.48 5.07 7.13 5.16 6.67 6.47 11.08 16.12 10,41 30.51 37.31 26.89 31.49 132.0 161.0 159.0 116.0

HA Mi HA HA 975.00 1509.00 1338.36 1051.00 912.59 612.50 798.87 818.01 77.68 66.57 1W.51 83.15 50.38 67.83 (16.15 51.51

lob1 (W) ut bal 100,8 100.73 92.89 105.M 100.20 97.85 103.55 %.BO 102.67 101.17 100.60 lotal C balance 101.5 98.23 94.4i 103.15 106.15 98.15 102.20 96.57 101.12 102.12 100.62 lob1 H balance 106.6 100.49 93.72 106.23 10Lf9 106.22 109.31 103.17 105.11 3.09 105.95 ictal S ba!ance 66.9 79.0[! ??.1? 79.79 81.65 73.44 79.05 69.56 69.72 71.99 71.74 Total N balancr 100.0 100.00 100.OC 1OO.M lo(i.00 100.00 100.00 100.00 100.00 1OO.OL1 100.00 lotal ash balance 101.0 89.09 B3.01 85.60 90.91 95.17 84.16 10.77 51.33 83.28 81.6f

Womlized tmrs ims: Coal 89,3 89.62 87.69 90.38 90.13 86.91 88.91 89.13 91.67 81.46 87.85 C7 Insoluble 79.3 85.22 81.61 81.91 83.97 85.05 84.95 87.01 90.50 86.89 86-77 Hodst. (51DCO 56.2 57.97 19.24 59.82 62.96 53.60 56.13 59.03 67.82 60.50 61.70 hst. (371Ct) 34.9 31.63 28.25 35,15 38.32 33.26 35.60 37.57 40.88 36.99 37.41

Product Distribution: utX H20+EOx 5.3 7.52 2.48 6.12 1.57 5.30 6.24 6.15 6.81 6.61 5.48 ut% H2S 0.6 1.25 0.98 1.40 1.42 1.46 1.73 1.12 1.56 1.12 1.19 utX HH3 0.1 0.22 0.32 0.51 0.29 0.16 0.10 0.30 O,% 0.67 0.19 dr ti -tt 2.7 2,07 1.74 2.36 2.19 2.12 2.21 2.52 2.52 2.05 2.35 ut1 C5-177C 5.9 4.71 6.15 5.27 5.93 1.11 6.26 6.57 5.95 7.19 5.12 ut% 177-313c 18.2 17.07 14.73 11.42 20.67 17.55 17.07 18.62 3.28 18.32 19.86 utg 343-5101: 3.5 32.17 30.90 33.85 31.26 29.87 M.iO 30.58 35.95 32.67 33.61 ut% 5104 31.2 33.58 40.62 32.20 29.35 36.53 31.71 32.18 25.58 30.62 29.70 dl h n f f COal 3.7 3.46 1.10 3.21 3.29 1.36 3.69 3.62 2.78 4.18 4.05 ut1 total prod 102.4 102.38 102.01 102.31 102.28 tOl.77 102.11 102.27 102.90 103.73 102.15 '

*1002 Nitrogen Balance sssrncd to calculate HH3 disappearance of N f r a liquid streas.

A-2

Run Ha. 21 - 2:l Llovhinstcr Res1d:Iliinois Cos1 Ho. 6 I ut% u Cataivst

Run I9 But. 21 21 lest Pert od I T O S 8 IO

lolutnc soluble Bottms Product Properties: ise RPI IS6 ut% t TS8 utX H ISB utX 5 1st ut1 N TSB ut% HI IS8 utX KRT 1% ut1 ash TSB ppn Cat. 158 D1160, UOIX IBP, Dcg c 5x 1 ox 20% 30X 10% 50X 601 EP

utX 01160 OH 1% 0)i RPI 156 OH M, ut1

5% 101 201 301 to1 50% 601 701 801 9% 951 IP x tEP

x crp

rep, oeg c

utX D1 I6D Btns TSB ab$ RPI

3.3 as. 93 io.ia 2.27 NR

11.65 WR 0.01

38

398.3 151.3 473.3 493.0 51 2.8

HR HR Hfi

542.8 NR

12. (i 10.9

310.3 412.0 134.5 459.0 47’1.8 488. e 500.3 511.8 523. s 536,s 554.5 568.5 577.5 100.0 57.6

4.1 85.54 10.1 t

2.4 1.4 b. 29 19.4

0 27

400 46f 486 51 t 536 w R HA 540

31.5 31-5

13

309 385 11 0 138 158 472 483 494 505 51 9 531 HS 511 100

65.50

4. S BS, 21 9,63 2.6 1.23 7.19 16.55

0 12

398 46f 461 505 530 WA Rfl HI1 536 33

33.1 13

321 391 423 452 470 183 493 500 521 535 556 574 514 95

66.90

21 11

4.4

9.64 2.01 1.M 12.8 22.2

0 30

~ 6 . 6 1

433 197 51 8 HR NR HR HR HR 53E I9

13.5 12.6

36 41 3 436 463 181 496 509 521 531 510 551 568 5’12 96

80.50

21 12

1,4 80 I 47 10.11 1.81 1.61

10.27 21.65

0 29

41 1

I99 522 NR HR ufl Ni! 529 26

26.1 13.1

335 416 442 t7 1 186 491 507 51 6 526 535 54% 563 574 31

73.91

2t 17

7.6 B,25

I1 1.68 1.6 4.27 16.6

0 12

131 f12 168 507 528 nfi HA #I1 5 3

35 35.0 Ik3

330 11 7 tJ2 166 179 490 500 51 0 521 532 St7 561 571 97

65.00

21 21 18 19

1.3 1.3

11.01 11.1 1.61 1.38 1.67 1.54 5.98 4.42

36.95 15.75 0 0 13 9.9

87.~9 8 . 6 7

113 387 61 471 178 178 499 506 526 528 M WR W A M W HR 538 514 36 36

35.7 38.2 14.5 14.6

I14 311 392 401 425 128 451 457 172 +?4 481 487 195 I 9 8 506 508 518 519 530 531 545 544 550 558 570 575

97 98 61,29 61,82

21 22

6.9 88.18 10.91 1.12 1-62 1.89

17.72 0

6.4

377 477 498 525 !I8 1IR WA HA 539

21 21. I 14.3

297 307 11 7 w %a 182 t95 507 519 531 5% 559 568 97

72.91

21 23

7.5 87.19 10.17 1.7

0.73 1.M 17.44

0 ItR

1 l? 470 499

514 WR WR ufl 511 30 30

528

14.8

110 380 126 463 481 499 51 2 524 534 546 567 11R 513 92

?0. OD

21 25

8.7 81.1 10.8 1.27 1.12 4. 03

15.15 0

10.2

317 165 482 503 523 514 HR Hfl 519 41

41.1 15.4

303 to2 130 151 474

496 507 SI 9 531 517 562 513

91 58.60

185

4.0 -4 -5.1 -8 3.3 4.3 e 1.8 6.7 3.2 s.1

A-3

tun no. 21 - 2:l Llovdrrinster Resid:Illinois Coal No. 6 1 utX U Catalyst

Run 19 flue, 21 21 i t s t Period LTOS 6 10

M e a d Product Properties: BH PI OH utx t Mi ut r u BH utx 5 OH utX H OH at, utx fBP, ocg t. 5 1 lox 20x 3 O X t o 2 50% 60X ?OX BOX 902 9 5 X fP J K P

24.4 M HA

1-44 0.33

34.0 120.0 1 6 1 3 219.8 261.0 29e.o 332.0 361.0 386.3 415.0 142.8 $668.5 48E. 5 1uG.o

lob1 Liquid Propertier API 13.6 ut% t WR utX H WA Mix s 1.9 utX H HA MiX HI 6.0 utX MCRT WR utX dist, (371C-) 31.9

23.5 25.2 65.65 81.65 11.45 11.65 1.31 1,29

0.3% 0.337

0 0 102 66 171 134 245 231 285 27B 317 314 345 3* 372 372 397 399 122 425 419 152 $67 $69 514 502 IHJ 109

13.8 13.7 65.6 65.0 10.8 10.5 1.9 2.0 0.9 0.8 3.2 1.0 9.9 9,2

29.9 27.2

Unconverted Coal Solids PropertitsH: ucc utx c WR 86.2 81,6 ucc ut1 ti ilfl 5.1 5.3 ucc utx 5 Hfl 6.7 11.1 KC utr w HA 1.7 1.7

x I k S U l f . ~ 61.6 61.96 60.08 1 D t n i t r i f . w WA 2 3 . ~ 30.30

21 11

23.6 64.86 11.73 1.21

0.253

1 115

2% 302 338 368 397 423 $46 470 4BC 536 100

i m

16.0 855 10.9 1.5 0.6 5.0 6.6 30.7

80.9 5. 8

11.9 1.5

67.26 18.96

21 12

23.4 W,79 11.55 1.35

0.301

0 101 177 2% ZBE 322 352 379 IO6 432 459 476 504 100

16.2 66.2 11.1

1.5 0.8 3.9 8.2

35.5

79.9 5.7

12.6 1.6

MI. 26 26.55

21 11

25.7 61.65 11.13 0.76

0.191

-6 97

179 242 279 310 339 365 390 414 439 I 5 4 4li IN

16.2 96,6 11.3 1.2 0.9 2.2 8.7

29.7

64.3 5.6 6.2 1.9

75.23 21.53

21 21 16 19

26.4 27 H,27 85.27 11.8 11.9 0.14 0.69

0.191 0.189

0 -4 69 82

149 lll 230 228 272 268 306 302 336 331 364 359 390 386 I16 112 411 I 40 $55 456 487 493 1 1 100

16.6 17.5 6 . 1 66.9 11.4 11.5

1.2 1.0 0.9 0.8 3,l 2.1 8.1 7.6

31.4 33.7

81.9 80.1 5.9 5.7

10,1 12.2 1,8 1.7

3.06 19.83 15.60 29.80

* h g h t t d weragc of outrhtad and toluene soluble bottons products. wCalculattd as (g 118 x M g 116 C + g TI8 H + g TI8 S - g tat S + g TIB H)*lOO1 WCalculated as ’(Teed S or H - Liquid Prod. S or W)/(Feed S or N)*lDO%”

21 22

18.4 85.47 11.91 0.85

0.21 5

4 112 1% E7 299 335 361 397 127 $55 492 521 559 98

15.1 96.3 11.6 1.0 0.6 1.4 5.1

36.8

81.8 5. 8

10.1 2.3

78.10 14.86

21 23

23.3 1.13 11.51 0.77

0.195

0 92 19 241

325 358 389 11 8 I% 477 502 573 99

2na

17.4 86.5 11.0 1.1 0.4 1.5 6.5

34.3

79. I 5.3

13.0 2.2

76.69 65.15

21 25

24.9 85.51 12.27

0.7 0,11t

1 96

115 244 283 316 349 371 391 422 450 411 553 99

17.6 66.5 11.6 0.9 0.6 1.8 6.6

34.2

81.8 5.5

10.6 2.1

eo, 50 48.91

A-4

i

Run no. 23 - 21 Uoyhinster Resid:Illinois Ewl No. 6

Run 23 23 23 23 23 lest Period 2 6 7 9c 90 Per. Length, hrs 12 12 12 12 12 Initial HOS 24 n 84 la8 toe Aut Rx Int 1, Oegt 424 427 qZ1.5 411 111 Rx Outlet P, psig 3025 30DO 3012 3019 3019 uHsu/Base UHSU 1.16 1.15 0.91 0.78 0.78 Rec. H2 Pty. . moll 88.12 8 t 6 3 87.99 83.55 82.00 HPS Rcclfnd Ratio 5.2 1.8 6,l 7.2 7.2

2 ut1 fr Estalyst

fed Code n o r10 r10 6ras MF feed 2416.41 2418.56 1916.63 Resid Code R10 RlO RlO Grms Resid 1655.26 1636.10 12%.79 CWl CDdt c1.1 Cl.4 tl.4 6rms Mf Ewl 791.18 782.16 619.84 btalyst Code K3.1 K3.1 K3.1 ut1 eat. mt.MRFf 2.19 2.49 2.19

f10 no 1649.6 16+9.86

R10 R l D 1116.30 1116.30

E1.4 t1.4 533.56 533.56 K3.1 K3.1 2.49 2.43

f red Distribution: ut% C5-177C 0.00 0.00 0.00 0.00 0.00 u t X 177-343 0.48 0.18 0.18 0.48 0.48 ut1 313-510C 11.59 11.59 11.59 11.59 11.59 uti 5101~ 55.60 55.60 55.60 55.60 55.60 Ut1 nRf CMl 32.31 32.31 32.34 32.34 32.34 uti H2 Consvrp, 1.70 1.58 1.51 3.03 3.06 utX total feed 101.70 101.58 101.57 103.03 103.06

fed Rnslysis: UP1 gravity -7.6 -7.8 -7.8 -7.8 -7.8 ut% arbon 76.29 76.29 76.29 76.29 76.29 utX hydrogen 8.13 8.13 8.13 8.13 8,13 utY sulfur 1.03 4.03 1.03 4.03 1.03 ut% nitrogen 0.94 0.94 0.91 0.94 0.94 utX hept. insol. 8.53 8.53 8.53 8.53 8.53 utf HCRl 10.94 10.94 10.94 10.94 10.94 utX dlst. (371C-1 0.61 0.67 0.67 0.61 0.67

A-5

i

Run Roo 23 - 2:l lloydninster Resid:Illinois Coal NO. 6

Run 23 23 23 23 23 Test Period 2 6 1 9t 90

z ut i re Catalyst

Products: bras 6as (Ox 2.86 3.12 6rms 68s t l 14.02 17.39 6rms 6ar t 2 t0.07 13.58 Qms 68s c3 9.57 12.39 6ras 63s c4 3.92 4.00 6rms 63s cs+ 25.57 2.30 firms bw HH3 0.00 14.51 Srms 6as H25 7.89 8.17 Crms kt H20 139.3 199.1 bas S ulHct H20 WR HR &as Wi Product 0.00 0.00 Qms 156 Product 2111.58 1958.75 6rms Unconu,coal 263.24 270.41 6ms HZ CDnsvlp. 41. 54 38.25

6.01 4.60 4.52 25.10 25.17 24.70 17.11 20.87 20.87 15.34 17.32 11.30 5.06 5.33 5.33 3.40 3.26 3.24 D.00 0.00 1.22 8.18 16.05 16.05

113.8 116.0 124.3 NR HA WR

0.00 0.00 0.00 1633.21 1635.22 1577.52 220.12 141.15 18?,19 30.05 9 . 0 4 50.49

Total Mir) ut ba1 106.55 t01.97 108.27 tlb.?? 116.95 lot81 t balance 104.94 97.70 103.65 117.64 116.93 lotal H balance 100.00 100.00 10G.00 100.00 106.00 Total. S balance 125.05 l25.?3 135.56 137.31 155.01 lotal H balancr 107.12 100.00 119.03 128.0i 1 0 0 . O G Total ash balance 110.63 109.11 116.99 138.50 147.33 lob1 tat. balance 105.43 114.14 95.20 123.0f 130.57

Homalized Conversions: ccal 68.71 66.10 67.20 71.34 69.95 C? Insoluble 53.21 48.09 48.83 59.10 55.97 Hondist. (Slot*) 38.28 42.05 4t.tt 54.81 52.55 Dut. (311C+) 22.15 25.56 28.72 35.46 33.25

Product h s t n bot1 on: utx H2o+cox 5.45 8.24 8.67 6.26 6.68 utr HZS 0.30 0.36 0.39 0.63 0.83 u t 1 HH3 0.00. 0.59 0.00 0.00 0.37 utx Cl-Cl 1.44 1.92 3.03 3.51 3.53 utX t5-177t 0.98 1.63 1.15 3.76 2.14 u t r i n - 3 4 3 ~ 12.29 11.23 12.94 19.22 18.41 utX 343-51OC 26.95 26.66 25.91 29.69 29.36 utx 51o*t 44.18 40.00 38.25 32.39 32.01 utXUnc MIT Coal 10.10 10.96 10.61 7.33 9.12 utX total prod 101.10 1M.58 101.57 103.03 103.06

*10OI Hydrogen and Hitrogen b l a m e s assued t o calculate H2O and HH3 based only on liquid strew analyses.

A-6

a

Run No. 23 - 2:l Lloydninster Rcwd:Ilfinols Ewl HD. 6 2 u t i Fe Catalyst

Run 23 23 23 ICs t Pen od 2 6 7

Toluene Soluble Bottms Product Properties: 19 IIPI 158 ut% 5 I S B ut% H TSR ut% 5 I58 ut% n 1% ut% HI 19 ut1 ntRT TSB ut1 ash TSB pplr fe TSB 01160, wolx IBP, Beg C 5% 1 ox 20X 30% l o x 501 6 o X EP

utX 01160 OH TSB 011 API 1% OH Rf, utK

IBP, Deg t SX 1 OK zox 301 40% sox 60X 70X 8DX 901 95% tP I[ CfP

x ew

ut1 0116D Btns

5.1 84.24

9.68 3.40 0.92

11.18 16.37

0 0

211 302 312 406 452 191 526 WA 531

53 50.8 14.8

21 1 252 275 31 4 346 374 100 424 146 471 199 523 569

99 49.2

TSB Btns MI -4.4

6.4 W.89 10.03 3.60 0.13

13.33 15.79

0 0

120 2Ba 311 391 425 166 502 WR 530

56 55

14.6

112 225 261 306 316 378 to7 133 156 480 509 531 569 99 43 1.5

5.1 85,OE

9.19 3.33 1.01

13.51 16.00

0 0

116 257 322 397 143 483 51 4 WR 540

56 54.8 15.8

112 21 7 253 297 331 362 399 41 5 439 464 194 51 7 558 99

15.2 -4,s

23 9C

8.1 86.20 9.6t 2.12 1.05

11.37 14.92

0 0

116 125 271 340 391 41 9 Ml 199 524

66 65

15.7

111 115 229 272 397 338 368 396 421 tu 485 509 563 1 00 35

23 9D

1 86.44 9,66 3.18 0.38

10.47 15.10

0 0

115 258 294 344 381 41 9 451 SO! 541 67

65.6 14.1

109 21 0 245 285 31 8 350 390 109 136 165 498 524 575 100

31.4 -9.3 -9.1

A- 7

Run No. 23 - 2:l Lloyhinster Resid:Illinois Coal Ho. 6

Run 23 23 23 23 23 lest Period 2 6 7 9c 90

2 ut1 fc Catalyst

Ovtrhcad Product Proper t i es : OH API 0 B 0 0 0 OH ut% C 0 0 0 0 0 OH ut% H 0 0 0 0 0 OH V t X S 0 0 0 0 0 OH ut1 N 0 0 0 0 0 OH 6Lt, ut% IBP, &g t. 0 0 0 0 0 5% 0 0 0 0 0 1 Of! 0 0 0 0 0 ?OK 0 0 0 0 0 30% 0 0 0 0 0 40% 0 0 0 0 0 50% 0 0 0 0 0 601 0 0 0 0 0 70% 0 0 0 0 0 BO% 0 0 0 0 0 90X 0 0 0 0 0 951 0 0 0 0 0 f P 0 0 0 0 0 I w 0 0 0 0 D

Total l iquid Properties. I(pr 5.7 6.1 5.7 8.1 7.0 ut% c 84.2 8t.9 85.1 86.2 86.4 ut% H 9.1 10.0 9.2 9.6 9.7 ut% s 3.f 3.6 3.5 2.7 3.2 ut% H 0.9 0.4 1.0 1.1 0.4 ut% HI 11.2 13.3 13.5 11.1 10.5 ut% HCRT 16.f 15.8 16.0 14.9 15.4 ut% did. (371C-) 19.8 20.8 23.6 33.1 3.8

Llnconucrtcd Coal Solids Prupcrtiew

UtC ut% H 6.4 6.5 5.9 5.9 6.0 ucc ut% s 5.6 4.8 9.2 10.7 11.8 NE ut% n 2.5 1.5 2.9 3.0 2.6

ucc utx t 85.5 17.2 82.1 84.9 e4.0

I D c w l t , ~ 30,33 32.79 30.65 31.85 29.90 1 Den1trif.m 19.33 65.65 15.10 -2.65 64.16

Neighfed auerege of w c r k a d and toluene soluble bottms products. wtalculatcd as (g 1IE x M g TI8 t * p 118 H * g TI9 S - Q Cat S W a l c u l a t c d as ‘ ( f e d S or H - Liquid Prod. S or HMftrd S or Il)*lW%”

g 118 W)*lOOX

A-8