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DOE INDIRECT COAL LIQUEFACTION PROGRAM —ANOVERVIEWJohn Shen a , Gary Stiegel b & Arun C. Bose ba U.S. Department of Energy , Washington, DC, 20585b U.S. Department of Energy , Pittsburgh Energy Technology Center , P.O. Box 10940,Pittsburgh, PA, 15236-0940Published online: 25 Apr 2007.

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FUEL SCIENCE & TECHNOLOGY INT'L., 14(4),559-576 (1996)

DOE INDIRECT COAL LIQUEFACTION PROGRAM-- AN OVERVIEW

John Shen

U.S. Department of Energy, Washington, D.C 20585

Gary Stiegel and Arun C. Bose

U.S. Department of Energy, Pittsburgh Energy Technology CenterP.O. Box 10940, Pittsburgh, PA 15236-0940

ABSTRACT

U.S. Department of Energy (DOE) has been supporting an indirect coalliquefaction program aimed at developing improved technologies to convertcoal based synthesis gas into economically competitive and environmentallyclean hydrocarbon and oxygenate transportation fuels. A key element of thisprogram is the development of a liquid phase reactor technology which couldoffer improved economics and operational flexibility over the conventional gasphase reactors. This paper will review the accomplishments of liquid phasemethanol technology development at the proof-of-concept (POC) scale unit inLaPorte, Texas and the advancement of this technology to commercialdemonstration which has been underway since 1993 under the support of DOEClean Coal Technology program. The POC facility has recently been upgradedto allow for developing liquid phase reactor technologies for Fischer-Tropschsynthesis and the production of other oxygenate fuels and chemicals fromsynthesis gas. The upgraded POC unit, now known as the Alternative FuelsDevelopment Unit (AFDU), as well as the results of new campaigns that havebeen conducted at this unit will also be reviewed.

559

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INTRODUCTION

SHEN, STIEGEL, AND BOSE

Coal is the most abundant domestic energy resource in the United States.

The Fossil Energy organization within the U.S. Department of Energy (DOE)

'has been supporting a coal liquefaction program to develop improved

technologies for converting coal to clean and cost-effective liquid fuels to

complement the dwindling supply of domestic petroleum crude. The goal of

this program is to produce coal liquids that are competitive with crude at $25

to $30 per barrel Indirect and direct liquefaction routes are the two

technologies being pursued under the DOE coal liquefaction program.

In indirect liquefaction, coal is gasified in the presence of steam and

oxygen to produce a synthesis gas containing mostly carbon monoxide and

hydrogen. This synthesis gas (syngas), after being cleaned of impurities and

adjusted to the desired H,ICO ratio (if required), is converted to liquid fuels in

the presence of catalysts. A unique feature of the indirect liquefaction is its

ability to produce a broad array of sulfur and nitrogen free products including

motor fuels, methanol, oxygenates (octane enhancers), and chemicals with the

use of different combinations of catalysts and process conditions. The

conversion of syngas to motor fuels is known as Fischer-Tropsch (F- T)

synthesis.

Commercial indirect liquefaction plants in operation since 1955 have

included coal based plants in South Africa and US., and natural gas based

plants in South Africa. New Zealand. and Malaysia. In all these plants, the

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DOE COAL LIQUEFACTION PROGRAM 561

syngas is converted in gas phase reactors Because of the high exotherm

associated with the reactions, it has long been known that a liquid phase reactor

could offer cost and operability advantages over gas phase reactors due to its

superior heat transfer capabilities. Earlier efforts in developing a liquid phase

r-T reactor after World War II were suspended in the late 1950s because of

the availability of cheap petroleum crude (Poutsma, 1980). Interests in this area

were revived in 'late 1970s with the rise in petroleum crude price. Scoping

economics studies supported by DOE and Electric Power Research Institute

(EPRl) indicated that the capability of a liquid phase reactor to process a low

H,ICO ratio syngas from advanced coal gasifiers could offer significant cost

advantages over gas phase reactors (Gray et aI., 1980; Brown et aI., 1982). In

cooperation with industrial organizations, DOE in 1981 began to support a

R&D program to advance the liquid phase reactor technology for coal based

syngas conversion beyond that of the late 1950s. Initial focus of this program

has been on the liquid phase reactor technology development for methanol and

F·T synthesis. Recent publications indicate that other industrial companies also

have been active in similar technology development (Chemical Week, 1994;

Chemical Marketing Reporter, J993) .

LIQUID PHASE METHANOL TECHNOLOGY

A schematic diagram of both liquid and gas phase reactors is shown in

Figure I. In the liquid phase reactor, finely divided catalysts are suspended in

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562 SHEN, STIEGEL, AND BOSE

TO HEAT& PRODUCTRECOVERY - I

SYNGASFEED

TO HEAT&PROOUCTRECOVERY

BFW

LIQUID PHASE REACTOR

lei GAS PHASE

FIG. 1 Gas and liquid phase reactors

an inert liquid medium by a syngas stream bubbled through the catalyst slurry.

Reaction exotherm is removed through the use of an internal heat exchanger.

This type of reactor is also known as slurry bubble column reactor.

Bench scale development of liquid phase methanol was conducted in the

mid-1970s by Chern Systems with support from EPRI. Proof-of-concept (PaC)

scale development began in 1981 with the construction of a 5-ton per day

methanol plant located in LaPorte, Texas, under a DOE contract cost-shared

by Air Products and Chemicals, Inc. (APCI) and EPRI. Other participants in

this contract included Fluor and Chern Systems. The pac scale work was

completed in 1989 following a successful 120-day sustained campaign.

Highlights from this campaign are summarized below.

• The operation was carried out to simulate the liquid phase methanol operation

in a once-through mode using a simulated Texaco gasifier syngas (067

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DOE COAL LIQUEFACTION PROGRAM 563

H/CO ratio) over a commercial methanol catalyst. Key operating conditions

were: 15 ern/sec superficial inlet gas velocity and 35% by weight catalyst

loading. The temperature profile in the reactor was essentially isothermal.

DRAKEOL 10, which is a food grade mineral oil consisting of primarily

C18-CJl paraftins, was used as the liquid medium

• An initial reactor productivity of I gram of methanol per gram of catalyst

per hour was achieved, exceeding the POC design capacity by a factor of 2.

The productivity loss was o. 16%/day during the extended operation period.

• Load following operation was successfully simulated for power and methanol

co-production in Integrated Gasification Combined Cycle (IGCC) systems.

Reductions of syngas rate up to 80% were accommodated easily. Also, the

catalysts could be re-suspended and its performance restored after a cold

reactor shutdown. Finally catalyst addition to and withdrawal from the

reactor were demonstrated.

• Results from the POC scale reactor compared favorably with those predicted

from the bench unit results.

• Methanol products contained 0.3-1 % water and call be marketed as fuel grade

methanol without further processing. A typical analysis of the liquid phase

methanol composition is given in Figure 2.

A summary of the development history and more detailed discussions for

this technology can be found elsewhere (Brown, 1994; Studer, et aI., 1989).

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COMPONENT PERCENT

WATER 0.68

METHANOL 97.34

ETHANOL 0.47

PROPANOLS 0.18

BUfANOLS 0.14

PENTANOLS 0.09

ESTERS 0.98

DlMETHYLETHER 0.02

OIL 0.10

100.00

FIG. 2 Liquid phase methanol composition

COMMERCIAL DEMONSTRATION OF LlOUID PHASE METHANOLTECHNOLOGY

Commercial demonstration of liquid phase methanol technology has been

underway since 1993 through a cost-shared cooperative agreement with APCl

and Eastman Chemicals awarded under the DOE Clean Coal III solicitation.

Highlights of this activity are summarized below.

• Site: Eastman Chemical's Coal to Chemicals Plant in Kingsport, Tennessee.

• Capacity: 250 tons per day (TPD) of methanol (a scale-up from 10 TPD at

the LaPorte scale).

• Start-up date: 1996; Test operation period: 4 years.'

• Fuel-grade methanol product tests duration: 2 years.

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DOE COAL LIQUEFACTION PROGRAM 565

At present the syngas from the Texaco gasifier at the Kingsport plant is

shifted to a nominal Hz/CO ratio of 2.0 before feeding to a fixed-bed gas phase

Lurgi methanol reactor. During the liquid phase methanol demonstration, this

shifted syngas will be the primary feed being used. Limited operations will be

conducted with a 0.67 II/CO ratio syngas to provide direct reactor scale-up

data from the LaPorte unit. The product test program will include testing of

liquid phase methanol as a fuel for both stationary and mobile applications. The

Kingsport project also includes a "provisional dimethyl ether (DME)

implementation" phase to demonstrate the liquid phase methanollDME co­

production technology. More discussions on this technology will be provided

later.

LAPORTE AFDU FACILITY

Construction of the LaPorte POC unit for the liquid phase methanol work

was completed in 1984. The reactor has a pressure rating of 900 psia (6.2

MPa). Syngas feed to the POC unit is supplied across the fence by an APCI

owned natural gas reformer unit. Following the completion of the liquid phase

methanol work, the LaPorte facility was upgraded to permit the development of

liquid phase technologies for F-T, oxygenates, and chemicals synthesis. The

upgraded facility, now called the Alternative Fuels Development Unit (AFDU),

has two parallel reactor trains: one (low pressure) for F-T synthesis and the

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other (high pressure) for oxygenates and chemicals synthesis. A description of

the two reactors is given below:

LaPorte LaPorteLow Pressure High PressureReactor Reactor

Inside Diameter, em. 57.2 45.7

Height, m- Total 8.8 16.5- Normal Liquid Level 6.1 12.2

Pressure(maximum), MPa 6.2 12.4

Superficial Inlet GasVelocity(maximum), ern/sec 22 30

Internal Heat ExchangerDuty, GJlhr 3.5 3.0

L10UID PHASE REACTOR CAMPAIGNS AT LAPORTE AFDU FOROTHER APPLICATIONS

Additional liquid phase reactor campaigns conducted at LaPorte AFDU

since 1989 have included syngas to methanol and DME (1991) (Bhatt et al.,

1991), water gas shift (1992) (Hsiung et al., 1992), isobutanol dehydration to

isobutylene (1993) (Armstrong et al., 1993), syngas to methanol and isobutanol

(1994) (Heydorn et aI., (994), and F-T-I (1992) (Bhatt et aI., 1992) and F-T

II (1994). Highlights of the first four campaigns are discussed below. The two

F-T campaigns will be discussed later.

• In the methanollDME co-production campaign, a physical mixture of

methanol and dehydration catalysts was employed. Syngas conversion to

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DOECOAL LIQUEFACTION PROGRAM 567

DME was effected through a sequential reactions of methanol synthesis

followed by methanol dehydration. The use of a second dehydration catalyst,

which led to a syngas conversion beyond the thermodynamic equilibrium

limit, resulted in a 50% improvement in equivalent methanol productivity

(2'DME + methanol) over the liquid phase methanol process. The reactor

operated well with the binary catalyst system over a wide range of catalyst

compositions.

• In the water gas shift campaign, the system for co-feeding steam to the

syngas feed stream was successfully employed. This mode of operation is

anticipated in F-T synthesis when the H,ICO ratio in syngas feed is below

0.67.

• In the isobutanol dehydration campaign, the reactor worked well for an

endothermic reaction with expanding gas flow. This is an intermediate step

in converting coal based syngas to precursors for octane enhancing ethers.

• In the methanollisobutanol co-production campaign, syngas was converted to

both products over a modified methanol catalyst. This campaign, carried out

in the new high pressure reactor, achieved a superficial inlet gas velocity of

1ft/sec (30 ern/sec).

LlOUID PHASE FISCHER-TROPSCH TECHNOLOGY: REVIEW ANDFUTURE GOAL

The liquid phase F-T reactor system differs from that for liquid phase

methanol in two key aspects:

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568 SHEN, STIEGEL, AND BOSE

• F-T synthesis produces a wide spectrum of products through a chain

propagation mechanism. The heavy fraction of the product, called wax,

remains in the reactor and serves as the liquid medium. Thus, a wax/catalyst

separation step is needed to remove the wax from the reactor.

• F-T synthesis permits a higher per pass syngas conversion because of

the absence of the thermodynamic equilibrium limitations. This leads to a

much greater contracting gas flow in the reactor.

As a result, both the hydrodynamics and operability are much more complex in

a liquid phase F-T reactor system.

Bench Scale Work Bench scale work for liquid phase F-T technology was

conducted by Mobil under two cost-shared DOE contracts in 1982-85. The first

contract focused on a low wax mode operation (Kuo, 1983) and the second on

a high wax mode operation (Kuo, 1985). Highlights from this work are

summarized below.

• The studies were performed using a Mobil proprietary precipitated iron

catalysts with a 0.67 H!eO ratio syngas. An 80% per pass syngas

conversion was achieved during the two extended runs. The temperature

profile in the reactor was essentially isothermal.

• A reactor productiviry of 0.5 gram of hydrocarbons per gram of catalyst per

hour was achieved.

• In the high wax mode operation, reactor wax was separated from the

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DOE COAL LIQUEFACTION PROGRAM 569

catalyst in a gravity settler located outside the reactor. The catalyst

concentration in the wax product was around 300 ppm.

LaPorte Scale Work F-T I and II campaigns at LaPorte were carried out with a

067 H,ICO ratio syngas over iron catalysts prepared by United Catalysts, Inc.

(UCI), co-funded by an industrial consortium headed by APCI. Highlights of

the two campaigns are summarized below.

• In the F-T I campaign, a hydrocarbon productivity of 0.7 tons per day

was achieved with a silica binder added high wax iron catalyst. The initial

catalyst loading was 35% by weight. Catalyst loss was a problem through

this 19-day campaign because of the absence of a workable wax/catalyst

separation system. The catalyst activity appeared to be stable during the

entire campaign.

• In the F-T II campaign, a hydrocarbon productivity of 3.5 tons per day

was achieved with an unsupponed low wax iron catalyst. The new internal

heat exchanger in the low pressure reactor performed well to remove the

reaction heat generated. Data analyses for this campaign are underway.

The above results suggest that two key issues need to be addressed in

planning future operations:

• A workable wax/catalyst separation system is needed to enhance the

flexibility of LaPone unit operations.

• A physically stronger iron catalyst is needed to ease the demand on the

wax/catalyst separation system. An alternative to the iron catalyst system

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will be the use of a supported cobalt catalyst combined with a stoichiometric

H,ICO ratio syngas. Recent results of DOE supported work at Energy

International (EI) indicate that a cobalt/promoters on alumina catalyst has

achieved a productivity of 1.6 gram hydrocarbons per gram catalyst per hour

(Singleton, 1994).

F.ulure Work atJillLh-aP()rte Unit Future work at the LaPorte AFDU will be

directed at establishing the operability envelope for superficial inlet gas

velocity and catalyst loading in a liquid phase F-T reactor, with the goal to

match or exceed the 15 ern/sec superficial inlet velocity and 35% by weight

catalyst loading demonstrated under the liquid methanol work. In a DOE

supported study by Bechtel, the number of liquid phase reactors in a 20,000

barrels per day F-T plant would decrease from 11 to 6 if the 7.5 ern/sec gas

velocity and 20% by weight catalyst loading were replaced by a more

aggressive choice of 14 ern/sec and 35% (Fox, 1990). In addition this study

recommends work on exploring the use of internal baffles to reduce

backmixing effects in a liquid phase F-T reactor. This could lead to an

increase in per pass syngas conversion from 80% to 95.5% and thus allowing

the reactor to operate in a once-through mode.

Environmental Premiums of F-T Liquids

Diesel fuel from F-T synthesis is high in cetane number and free of sulfur,

nitrogen, and aromatics. It could be an attractive blending feedstock to help

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DOE COAL LIQUEFACTION PROGRAM 571

refiners meet the mandated stringent diesel fuel specifications in place or

pending. In a reformulated diesel fuel study by Southwest Research Institute

funded by DOE (Erwin et al., 1994), the cetane numbers and engine emission

data of different reformulated diesel fuel blends were obtained. Results indicate

that a F-T diesel from wax hydrocracking is effective as a cetane improver, as

shown in Figure 3. Engine emission test data show that F-T diesel fuels rank

high for clean burning among the reformulated diesel fuels tested. In addition

to diesel fuel, a DOE supported study at Amoco indicated that F-T wax shows

good promise as a fluid catalytic cracking feedstock to produce iso-olefins as

precursors for octane enhancing ethers (Reagan, 1993). Efforts to quantify the

F-T liquids premium are part of the DOE supported ongoing coal liquids

upgrading and end use study by an industrial team headed by Bechtel (Lowe et

aI., 1994).

Prospect for Liquid Phase Reactor Commercialization

Power and Liquid Fuels Co-Production An early introduction of the liquid

phase reactor technology to the commercial market could be its inclusion

within an IGCC power plant for co-production of power and liquid fuels. The

feedstocks for the gasifiers could be coal, petroleum coke/resid, or biomass.

The feasibility of including a liquid phase methanol plant in a coal-based

baseload IGCC plant was conducted by Bechtel for the Florida Power Light

Company and EPRI (Walters et al., 1990). In this study a spare gasifier is

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100-,------------------------,

FIG. 3 Cetane numbers of blends of F-T diesel with diesel components

added to fully load the power block and to produce methanol. Results show

that the IGCC/methanol case could have cost advantages over the IGCC power

only case through higher component availability and higher plant capacity

factor. A separate scoping study was also conducted by Bechtel for the F-T

case (Tam, 1993). In this study the plant configuration in the DOE supported

indirect liquefaction baseline design for all-liquid production was modified by

using once-through liquid phase F-T reactors and feeding the unconverted

syngas to a combined cycle block for power production. Results show that the

cost of electricity in the IGCCfF-T case is sensitive to the F-T liquid selling

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DOE COAL LIQUEFACTION PROGRAM 573

price and could be lower than the IGeC power only case if the F-T liquids can

be sold at a favorable premium.

Liquid Phase Reacto!...AQclications Beyond Coal Another early commercial

application of liquid phase reactor technology could be its use in the natural

gas based indirect liquefaction plants dedicated to liquid fuels production.

Natural gas feed has the advantage over coal feed in these plants because of

nearly a 50% reduction in capital costs. Industrial organizations with large

remote natural gas reserves have been active in R&D on converting natural gas

to liquids. Successful development of liquid phase reactors with high

productivity could offer an attractive alternative to the gas phase reactors now

in commercial use.

CONCLUSIONS

Development of a liquid phase reactor to replace the commercial gas phase

reactors for syngas conversion has made substantial progress since its inception

in 1981 as a part of the DOE indirect liquefaction program. Liquid phase

methanol development was successfully completed at the POC scale in 1989,

and advanced to commercial demonstration in 1993 under the support of DOE

Clean Coal Technology program. Development of liquid phase reactor

technologies for F-T synthesis and for syngas conversion to oxygenates and

chemicals have been underway at the POC unit. The goal of these efforts is to

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achieve high reactor productivity under aggressive operating conditions equal to

or exceeding those demonstrated in the liquid phase methanol technology.

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Studer, D.W., 1. L. Henderson, T. H. Hsiung, and D. M. Brown. 1989."Status Report on.the Liquid Phase Methanol Project", EPRI 14th AnnualConference on Fuel Science and Conversion, Palo Alto, CA, May 18-19, 1989.

Tam, S. S. 1993. "Indirect Coal Liquefaction Via Fischer-Tropsch Technologyfor the Baseload IGCe Plant", lEA Second International Conference on TheClean and Efficient Use of Coal and Lignite: Its Role in energy, Environmentand Life", November 30 - December 3, 1993.

Walters, A.B. and S. S. Tam 1990. "Methanol Coproduction with a Base LoadIGCC Plant", Ninth EPRI Conference of Coal Gasification Power Plants, PaloAlto, CA, October 17-19, 1990.

RECEIVED: August 24, 1995

ACCEPTED: September 9, 1995

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