acti gasification to liquid fuel system

Renewable Energy Testing Center

5301 Price AvenueMcClellan, CA 95652916-929-8001 (p)916-929-8020 (f)www.technikon.us

TECHNIKON

Accelerating the Marketplace for Renewable Technologies

Operated by Funded through the Department of Defensertment of De

US Army Armament Research Development and Engineering Center

Demil and Environmental Technology DivisionEnvironmental Sustainment and Energy Branch

ACTI Biomass Gasifi cation to Liquid Fuel System Assessment

1602-113 NA

October 2009

US Army Contract W15QKN-05-D-0030US Army Contract W15QKN-05-D-0030Task 5 RETC, WBS # 1.1.3Task 5 RETC, WBS # 1.1.3

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TECHNIKON REPORT # 1602-113 NAOCTOBER 2009

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ACTI Biomass Gasifi cation to Liquid Fuel System

Assessment

Technikon Report # 1602-113 NA

This report has been reviewed for completeness and accuracy and approved for release by the following:

Director of Measurement Technologies //Original Signed//

Kim Hunter, PE Date

Vice President //Original Signed//George Crandell Date

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Table of Contents

Executive Summary .......................................................................................................1

1.0 Introduction ........................................................................................................3

1.1. Organizational Background ..................................................................31.2. Report Organization ...............................................................................41.3. Test/Study Objectives ............................................................................5

2.0 Scope of Test/Study ............................................................................................7

2.1. Major Pyrolysis Gas Constituents ..........................................................72.2. Major Synthesis Gas Constituents .......................................................72.3. Major Liquid Hydrocarbon Constituents .............................................82.4. Test Plan and Goals ...............................................................................92.5 Report Preparation, Review and Quality Assurance and Quality Control (QA/

QC) Procedures/Protocols ......................................................................92.6 Testing Protocol ...................................................................................10

3.0 Process Description ..........................................................................................11

4.0 Process Discussion ...........................................................................................19

5.0 Conclusions .....................................................................................................21

Appendix A Sampling Test Plan Details and Protocol .......................................... 23

Appendix B Sampling Details ............................................................................... 31

Appendix C Process Data Details & Flow Charts ................................................. 35

Appendix D Analytical Methodology And Results Details ................................... 51

Appendix E Reactor Assessment and Calculations ............................................... 61

Appendix F Acronyms and Abbreviations ........................................................... 75

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List of Figures and Tables

Table 2-1 Measurement of Major Pyrolysis Gas Constituents .........................7

Table 2-2 Measurement of Synthesis Gas Constituents ...................................8

Table 2-3 Liquid Components ..........................................................................8

Figure 3-1 ACTI Pyrolysis Gasifi er .................................................................12

Figure 3-2 Gasifi er Details ...............................................................................12

Figure 3-3 Venturi Scrubber ............................................................................13

Figure 3-4 Pyrolysis Gas Holding Tanks .........................................................14

Figure 3-5 Catalytic Steam Reformer ..............................................................15

Figure 3-6 Reformer Shell ...............................................................................15

Figure 3-7 Fischer-Tropsch Slurry Reactor .....................................................16

Figure 3-8 Liquid Hydrocarbon Recovery System ..........................................17

Figure A-1 Theoretical Flory FT Product Distribution ....................................67

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EXECUTIVE SUMMARY

This report summarizes a test program to assess the performance of a biomass-to-liquid-fuel technology designed to thermally convert biomass to a hydrocarbon fuel suitable for use in DOD multi-fuel power plants. Technikon, operators of the Renewable Energy Testing Center (RETC) for the Department of Defense (DOD), and American Combustion Technologies Incorporated (ACTI) conducted the test during the week of May 11, 2009 at ACTI’s demonstration facility in Paramount, California.

The results of multiple test runs show that the ACTI pyrolysis gasifi cation unit and steam reforming unit can convert biomass into a gas that can be theoretically upgraded to a hy-drocarbon liquid through the catalytic Fischer-Tropsch (FT) synthesis process. The FT synthesis could not be demonstrated due to mechanical and processing diffi culties. Hence, the operation of the liquid conversion steps is discussed in general terms only.

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1.0 INTRODUCTION

Technikon, LLC is a privately held contract research organization located in McClellan, California, a suburb of Sacramento. Technikon offers research services to industrial and government clients specializing in advanced technologies in the areas of metal casting, point source emissions and renewable energy.

1.1. Organizational Background

The Renewable Energy Testing Center (RETC) program is based on the concept of testing and validation of renewable energy technologies related to biomass feedstock with a par-ticular focus on biofuels for transportation. Technikon has a world-class research, demon-stration and deployment facility located in the greater Sacramento, California region that is being utilized for this initiative. The Renewable Energy Testing Center program focuses on support of relevant and emerging renewable energy technologies in the area of cellulosic waste and biomass to energy and fuel conversion technologies that would support DOD needs for compliance to Executive Order 13423 that sets goals for the DOD to increase alternative fuel consumption at least 10% annually.

The development of renewable energy technologies presents a major opportunity for re-ducing US dependence on foreign oil. The DOD, the Department of Energy (DOE) and industry share the goals of reducing energy and fuel costs needed to support transportation, manufacturing and production of electricity. The RETC program assists energy technol-ogy companies during the technology development phase by providing engineering and facilities support at RETC’s renewable energy testing and validation center with a focus on systems meeting DOD renewable fuel requirements.

The objective of RETC is to provide industry with an independent facility for developing and evaluating renewable energy and renewable fuels technologies with respect to robust-ness, safety, energy effi ciency, environmental effectiveness and other key performance

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specifi cations. The RETC, and the oversight of the RETC staff, brings together technology developers, government entities and universities in a facility that allows the kind of testing needed to bring renewable energy systems to the commercialization phase. It also allows developers to integrate technologies that are needed to supply a complete waste to energy system at an accelerated pace and at a signifi cant cost reduction. Present state and federal grant structures are less fl exible and almost exclude the smaller developers from making applications since they do not have the data needed to get awarded. The RETC fi lls this gap in funding and accelerates renewable energy commercialization.

1.2. Report Organization

This report has been designed to document the methodology and results of a specifi c test plan that was used to evaluate the performance of a system employing thermochemical conversion (pyrolysis) and catalytic steam reforming to convert redwood chips to synthesis gas followed by catalytic (FT) hydrogenation/polymerization of the synthesis gas to yield a liquid hydrocarbon fuel. The test plan was designed to determine if the technology dem-onstrated by ACTI could produce synthesis gas that could be used for the production of liquid fuels and to assess the performance of the subsequent liquid fuel conversion steps. Section 2.0 of this report includes a summary of the methodologies used for data collection and analysis. Specifi c data collected during this test and a discussion of the results are sum-marized in Section 3.0 of this report.

Appendix A summarizes the (solid, liquid and gas) measurement and sampling protocols for the ACTI test. The complete sampling logs for each day of testing are contained in Appendix B. The location of each sample point is identifi ed on the process fl ow sketches in Appendix C. The processing of samples, analytical methodology and analytical results are detailed in Appendix D. A modeling study and theoretical performance evaluation of the ACTI Slurry Reactor is given in Appendix E. Appendix F contains a list of the Acronyms and abbreviations used in this report.

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1.3. Test/Study Objectives

The primary goal of this RETC Subtask effort is to determine the rate and composition of pyrolysis gas generated in the ACTI gasifi er and of the synthesis gas produced in the catalytic reformer. A secondary goal is to determine the composition and production rate of any hydrocarbon fuel fraction suitable for use in military multi-fuel (internal combustion and gas turbine) power plants.

The test program was carried out at ACTI’s 22 dry pound per hour (DPPH) development/demonstration facility in Paramount, California, over a period of four (4) consecutive days.

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2.0 SCOPE OF TEST/STUDY

The scope of this test is to collect and characterize pyrolysis gas, synthesis gas and liquid fuel samples from the ACTI system to determine the primary gas constituents and liquid components using appropriate sampling equipment, analytical instruments and procedures. The primary feedstock used during these tests was redwood chips.

2.1. Major Pyrolysis Gas Constituents

The major pyrolysis gas constituents that were measured are summarized in Table 2-1.

Table 2-1 Measurement of Major Pyrolysis Gas ConstituentsComponent Average Concentration (vol %) Concentration Range

H2 22.9 22.1 - 23.8

CO 29.4 27.6 - 30.9

CO2 17.5 17.2 – 18.0

CH4 12.4 12.1 - 12.8

C2H6 1.6 1.5 - 1.6

C2H4 4.1 3.8 – 4.4

C2+ 3.5 3.2 - 3.9

N2 8.0 4.8 - 10.1

Ar/O2 0.7 0.7 - 0.7

2.2. Major Synthesis Gas Constituents

Table 2-2 summarizes the synthesis gas constituents that were measured. This data was obtained from gas analysis using bag samples sent to an outside lab. The original test plan called for gas sampling, and analysis, in real time using a Nova Analytical Systems Multi-Gas Analyzer. However, the Nova analyzer experienced calibration and stability problems

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that could not be solved in a timely fashion. The analyzer was subsequently returned to the manufacturer (see Technikon Report 1602-211a).

Table 2-2 Measurement of Synthesis Gas ConstituentsComponent Average Concentration (vol %) Concentration Range

H2 47.4 39.2 - 55.5

CO 35.6 24.3 - 46.9

CO2 9.0 3.9 - 14.1

CH4 1.6 0.6 - 2.5

C2H6 0.1 0.0 - 0.1

C2H4 0 0

C2+ 0 0

N2 6.2 5.2 - 7.1

Ar/O2 0.2 0.0 - 0.3

2.3. Major Liquid Hydrocarbon Constituents

Table 2-3 summarizes the liquid hydrocarbon components to be measured. Note that due to inability to stabilize the system, no liquid fuel was produced during the test period.

Table 2-3 Liquid ComponentsComponent Concentration

Iso-Butane Not available

n-Butane Not availableButene Not available

Iso-Pentane Not available

n-Pentane Not available

C6 –C8 + Hydrocarbon Not available

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2.4. Test Plan and Goals

In addition to the primary goal of determining stream compositions, the ultimate goal of testing would be to quantify the conversion effi ciency of:

• Dry wood chips to pyrolysis gas • Pyrolysis gas to synthesis gas • Synthesis gas to liquid hydrocarbons and • To assess the suitability of the hydrocarbon liquid for use in DOD powerplants.

Additional tests can be structured to meet these objectives. Appendix A contains the de-tailed Technikon test plan.

2.5. Report Preparation, Review and Quality Assurance and Quality Control (QA/QC) Procedures/Protocols

The preliminary test samples that were collected by the test team, transferred by chain of custody and analyzed at approved outside labs. The resulting data were reviewed by Technikon team members to ensure completeness, consistency with the test plan, and ad-herence to the prescribed quality analysis/quality control (QA/QC) procedures. Appropriate observations, conclusions and recommendations were added to the report to produce a draft report. The draft report was then reviewed by senior management and comments in-corporated into a draft fi nal report prior to fi nal signature approval and distribution.

Appendix A summarizes the (solid, liquid and gas ) measurement and sampling protocols for the ACTI test. The complete sampling logs for each day of testing are contained in Appendix B. The location of each sample point is identifi ed on the process fl ow sketched in Appendix C. The processing of samples analytical methodology and analytical results are detailed in Appendix D. A modeling study and theoretical performance evaluation of the ACTI slurry reactor is given in Appendix E. Appendix F contains a list of the acronyms and abbreviations used in this report.

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2.6. Testing Protocol

The ACTI system was run at a feedstock rate of about 22 dry pounds per hour (DPPH). Redwood chips were used as a feedstock. Gas samples were collected when it had been de-termined that the sampled system was operating at stable, steady-state conditions. Liquid samples were taken from the venturi scrubber at the end of each test day but were not ana-lyzed due to contamination of the scrubber liquid from a previous test. The solid residue from the gasifi er (char) was collected and sampled at the end of each test day. The liquid hydrocarbon system did not reach steady state operation during the test program hence no liquid samples were collected.

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3.0 PROCESS DESCRIPTION

The ACTI process is schematically described in the process fl ow sketches in Appendix C. These comprise eight sketches covering the following operational areas:

1. SK1 – Gasifi er2. SK2 – Venturi Scrubber3. SK3 – Condenser / Demister4. SK4 – Gas Transfer System5. SK5 – Amine Absorber / CO2 Regenerator6. SK6 – Deleted7. SK7 – Steam Reformer8. SK8 – FT Slurry Reactor9. SK9 – Hydrocarbon Recovery (general representation only)

SK1 – The Gasifi er Unit (Figures 3-1 & 3-2) operates on the principle of pyrolysis where the biomass feed is not combusted directly but, rather, is heated externally, in the absence of oxygen, to a temperature where volatile organics, proteins and carbohydrates decom-pose. The energy for pyrolysis is supplied by externally-fi red gas burners surrounding the gasifi er in a retort arrangement. Biomass is introduced into the retort through a dual knife-gate air lock and conveyed within the retort by screw conveyors. The resulting “pyrolysis gas” is conveyed to an intermediate storage tank through a compressor. The residual solid “char” is deposited in an external receptacle. Typical retort temperatures for the test were 750-880 °F. The retort was operated at a slight vacuum of ½ inch water column.

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Figure 3-1 ACTI Pyrolysis Gasifi er

Figure 3-2 Gasifi er Details

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SK2 – Th e Venturi Scrubber (Figure 3-3) - Pyrolysis gas leaving the gasifi er is brought into intimate contact with a turbulent water stream in the venture scrubber. As the hot gas is cooled, moisture and volatile components condense into the scrubber stream. Particulate matter is also entrained and removed. The sensible heat absorbed from the pyrolysis gas is transferred to heat exchanger HE-1 in the water recirculation loop and ultimately rejected at the cooling tower.

Figure 3-3 Venturi Scrubber

SK3 – The Condenser / Demister (Figure 3-3) passes the cooled gas through a shell and tube condenser to remove additional moisture and then through a demister to remove any entrained water droplets.

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SK4 – Gas Transfer System (Figure 3-4). The scrubbed pyrolysis gas is conducted to a gas transfer tank (V-1) via a vacuum blower (B-1). This tank serves as an accumulator for gas compressor CP-1 which pressurizes the gas into a fi nal holding tank V-1a/b at approxi-mately 100 psig. Pyrolysis gas was sampled for analysis at this point.

Figure 3-4 Pyrolysis Gas Holding Tanks

SK5 – Amine Adsorber / CO2 Regenerator. Clean pyrolysis gas from the holding tanks is pressurized to approximately 200 psig in compressor CP-2 and passed to an absorbing column where CO2 is absorbed into an amine solution. The amine solution is subsequently depressurized releasing CO2 to the atmosphere. The lean amine solution is returned to the adsorber via a high-pressure pump.

SK7 – The Steam Reformer (Figures 3-5 & 3-6) catalytically reacts to carbon monoxide, CO, in the gas stream with water to increase its hydrogen content via the reaction: CO + H2O => H2 + CO2. Prior to its introduction into the reformer, the gas is passed through a zinc oxide adsorption bed to remove any hydrogen sulfi de, a potent catalyst poison. Steam for the reformer is supplied by a dedicated electric steam generator. Since the reaction is highly endothermic, the reactor is heated by a gas-fi red burner. The hydrogen-enriched stream leaving the reformer is “synthesis gas” or syngas. Gas samples are taken at this point for analysis.

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Figure 3-5 Catalytic Steam Reformer

Figure 3-6 Reformer Shell

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SK9 – Fischer-Tropsch Slurry Reactor (Figure 3-7) – Synthesis gas from the reformer is combined with H2, CO and light hydrocarbons recycled from the product recovery stage then compressed to approximately 450 psig by CP-3 and introduced to the bottom of the slurry reactor. The ascending gas bubbles commingle with solid catalyst pellets suspended in a high-molecular weight reaction fl uid at approximately 475 °F. Liquid dispersion and gas contacting are enhanced by mechanical agitation. The Fischer-Tropsch reaction can be generally characterized: CO + catalyst => -CO*; -CO* + 2H2 => -CH2- + H2O. Carbons continue to add to the growing -CH2- chain until the molecule desorbs from the catalyst surface. The distribution of molecular weights in the hydrocarbon product is strongly de-pendent on the properties of the catalyst. Hydrocarbon vapors leaving the slurry reactor are separated in the hydrocarbon recovery section and higher molecular weight wax products are recovered from the reaction medium through a sintered metal fi lter.

Figure 3-7 Fischer-Tropsch Slurry Reactor

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SK8 – Hydrocarbon Product Recovery (Figure 3-8). The vapor effl uent from the slurry reactor is expanded into a distillate (diesel) recovery vessel at 150 psig and 100 °F where the distillate fraction condenses. The uncondensed vapor undergoes a further expansion into a light ends separation vessel, at approximately 50 psig and 75 °F, where lighter liquid fractions (naphtha and gasoline) are separated from the non-condensable light ends. The light ends are then passed through an additional liquid knock out step before being recom-pressed and recycled to the slurry reactor. The light ends gas is sampled at this point. Molten paraffi n wax from the slurry reactor is fi ltered into a heated paraffi n holding vessel at 400 °F.

Figure 3-8 Liquid Hydrocarbon Recovery System

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4.0 PROCESS DISCUSSION

Gasifi er – The ACTI pyrolysis gasifi er appears to be well designed and its operation straightforward. The capability exists to evacuate the feed airlock or to purge it with nitro-gen. This was not done during the test but would be advantageous for reducing the oxygen coming into the system.

Amine Absorber – The CO2 absorber system is an extremely simple design featuring ab-sorbtion into a sprayed lean amine solution at high gas pressure and desorbtion from the rich sprayed solution at low pressure. The system is robust and mechanically simple but suffers from low mass transfer effi ciency probably yielding only one or two theoretical stages of ab-sorbtion and less than one stage on the desorbtion side. Liquid entrainment in the gas stream is an inherent problem in spray absorbers. This was reported to be the cause of repeated fail-ures of the catalytic reformer during the ACTI test. The details of the absorber design were not provided. However, if it does not include a mist eliminator, one could be added internally as a woven mesh pad or externally as an entrainment separator pot.

Slurry Reactor Adva ntages – Slurry reactor technology for FT synthesis has continu-ously evolved since the 1980s until it has become the reactor of choice for low-temperature (450 °F) conversion of syngas to distillate (diesel). Slurry FT reactors’ advantages over equivalent fi xed-bed plug fl ow reactor (PFR) designs are high turn down, isothermal opera-tion, improved temperature control and ease of catalyst replacement. Slurry reactors also enjoy greater fl exibility over their PFR counterparts with respect to feed composition in terms of the H2:CO ratio.

Slurry Reactor Concerns – To maximize slurry reactors’ catalytic surface area, the cata-lyst particles are usually in the 20-50 micron range. One area of great concern to slurry reactor designers is separating the catalyst from the high molecular weight wax product withdrawn from the slurry reaction medium. In the ACTI unit, wax is withdrawn through a sintered metal fi lter suspended in the reaction medium. Variations of this method have been employed in other pilot and commercial slurry reactors and are generally problematic due

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to blinding of the fi lter pores by the catalyst (Air Products and Chemicals Inc., “Catalyst and Reactor Development for a Liquid Phase Fischer-Tropsch Process”, DOE Report no. DOE/PC/30021-T22, 1989). Back pressure and hydraulic shock are common techniques used to clear these fi lters but frequent removal is still required. During the ACTI test no ready means to clear or remove the fi lter was observed. This ceases to be a problem when the catalyst diameter is much larger than the pore diameter – say, millimeters rather than microns. But the area available for reaction is reduced correspondingly resulting in low conversion of reactants. ACTI did not provide details on the design of the reactor or the catalyst so we do not know how these issues are addressed.

The Fischer-Tropsch reac tion is highly exothermic and normally requires some mode of active heat removal for temperature control in both slurry and fi xed bed reactors. This is true even for pilot scale units (Lampert, Erickson, “Fischer-Tropsch Synthesis of Hydrocarbons”, DE84017841, MIT/BNL-83-4, Sept. 1983). While the ACTI reactor em-ploys electrical heating to bring it up to operating temperature, no active mechanism was observed at the reactor for removing the heat of reaction. This was not an issue during the current test because the reactor was operated at very low space velocity compared to typi-cal FT slurry reactors. But the design will impose limitations on product throughput and reactor productivity when operating rates increase. Refer to Appendix E for details.

Hydrocarbon Product Recovery – The hydrocarbon recovery train consists of a series of pressurized condensation vessels with diesel being condensed at the highest pressure and the gasoline/naphtha fraction at a lower pressure. The ACTI design places signifi cant reliance on ambient heat transfer which limits the “sharpness” of the separation. Refer to Appendix E for further discussion.

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5.0 CONCLUSIONS

• The ACTI pyrolysis gasifi er is well designed and is fully serviceable for the proposed mission. The performance of ACTI’s follow-on gas-to-liquid conversion unit could not be assessed directly due to operational problems experienced during the test. Refer to Appendix E for a theoretical discussion of the gas-to-liquid system’s capability.

• ACTI’s approach to the gas-to-liquids conversion process emphasizes simplicity above effi ciency and operability. This is not unusual in demonstration facilities. However, po-tential customers need to ensure that philosophy is not carried over into units de-signed and constructed for operation in the fi eld.

• The selection of slurry reactor technology offers the best FT synthesis option for the ACTI target market. It accepts a wider range of H2 to CO feed mixtures, offers better temperature control and allows simpler catalyst maintenance than does the alternative fi xed bed reactor technology.

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APPENDIX A SAMPLING TE ST PLAN DETAILS AND PROTOCOL

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ACTi WOOD CHIPS to LIQUID FUEL TEST PLANCompany: ACTiDate: 4/27/2009Contract: 1602-110

Test Description and Objectives:1. Observe operation of ACTi's gasifier/F-T Diesel fuel conversion process.2. Collect steady state operating data for the overall process and individual unit operations.3. Quantify, insofar as practical, overall mass and component material balances on the gasification,

Process Datasheetreforming and F-T conversion steps.Process data from transmitters and direct-reading instruments is recorded on this page.The instruments are identified by the Process Flow Diagram (PFD) theyappear on using conventional ISA nomenclature. E.g.. SK5-PI-2 corresponds to pressure gauge number 2 on PFD sketch 5 (SK5).

Material Balance DatasheetSolid inputs and outputs (wood chips and char) will be weighed throughout the processing run. Liquid water accumulated in the venturi scrubber during the run will be weighed at the end of a run. This should correspond to the moisture in the wood chips.Liquid condensate from the reformer gas cooler and the light ends cooler will be weighed at the end of a run.

Composition DatasheetThe dry producer gas will be analyzed for CO, CO2, CH4 and H2 during a run:- downstream of the gas transfer compressor- downstream of the zinc oxide adsorber- at the reformer gas cooler- at the light ends gas separatorGas samples will be collected in Tedlar® bags at the CO2 regenerator and the light ends recycle loop for remote composition analysis.

Sample datasheetSolid samples will be taken from the gasifier inlet and outlet for remote analysis.Liquid samples for remote analysis will be taken from the:- venturi scrubber and scrubber condenser reservoirs- reformer condenser- paraffin tanks Note: allow paraffin tank to cool 8hr before sampling- diesel distillate tanklight ends separator- light ends knock out pot- light ends gas cooler

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TEST PROTOCOL

The following paragraphs describe the tools and methods used to collect materialbalance and chemical composition data from the ACTi gasification/liquid fuelproduction unit. The operation of the unit itself is not addressed by Technikonand is the responsibility of ACTi.

Feed Preparation

Wood chips have been shipped to the test site in (approximately. 600 lb) super sacks.The chips contain about 60% moisture by weight. To ensure feed uniformity the chipsat the surface of the sacks should not be used since these have dried considerably.Wood chips will be filled into tarred 5 gal. buckets then dispensed into the gasifierair lock at a rate of about 2 pounds per 2 minute interval.

Process Data

Process data is collected at 30 minute intervals and recorded on the Process DataWorksheet. Full-length sleeves, trousers and eye protection should be worn in theprocessing area.

Most of the instruments have identifying tags. Instrument tag numbers includethe PFD sketch on which the instrument appears, the ISA abbreviation for the instrumenttype and the number assigned to the instrument. For example, SK9-PI-2 would be thesecond pressure indicator appearing on PFD sketch 9. Some instruments shown on the PFDs and listed on the process data worksheet have not been tagged. The locationof these untagged instruments will be evident from the PFD.

Material Balance Data

Solid Weigh Points:SK1-WP-1 is the feed to the gasifier. Five gallon pails are filled with approximately 15 poundsof chips (about 7 minutes run time). The time at which the bucket is emptied is recorded on the Material Bal. Datasheet along with the weight of the chips added. This weightis recorded in the incremental column. The incremental weight is then added to the previous value in the total weight column to update the running total. Feed totals will be maintained separately for the startup, run and shutdown phases of operation.

SK1-WP-2 is the char discharged from the gasifier. This weight will be recorded similarly to SK-WP-1 above. The time interval for char removal will be dictated by the process.Before starting the gasifier, any char in the discharge will be weighed and added to the total for preceding shutdown. When startup is complete, before starting a run, the char in the dischargewill be weighed and added to the startup total.

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Non-Product Liquid Weigh Points:Weights will be taken for all process and product liquids that accumulate in the system during a run.Typically, weight is measured by draining the entire quantity of liquid into one or more 5 gallon buckets.The buckets are then weighed and the tare subtracted. The weight is then recorded on the MaterialBalance Datasheet.

SK2-WP1 measures the water accumulated in the venturi scrubber system. This is primarily condensed moisture contained in the input wood chips. At the beginning of a run the liquid level in thescrubber reservoir is measured through sight glass SK1-LI-1. At the end of the run the reservoir is drained down to the beginning level into 5 gallon buckets.

The buckets are then weighed, the tare subtracted and the weight recorded.

If the moisture content of the feed is high enough, an intermediate weight may need to be taken.SK7-WP1 measures the liquid accumulated in the reformer syngas cooler SK7-HE-3. The totalaccumulation over a run will be less than 5 gallons.

SK8-WP-1 measures the liquid accumulated in the light ends cooler SK8-HE-4. The accumulationover the run will be less than 5 gallons.

Product Liquid Weigh Points:SK9-WP-1(1a) These 2 weigh points measure the high MW paraffins produced during a run. Because

the liquid paraffin is at 400°F, it must be allowed to cool overnight before it is drained and weighed.SK9-WP-2 measures the hydrocarbon fuel fraction produced during the run. It will be drained from thediesel storage tank.

SK9-WP-3 measures residual liquid condensed in the light ends stream from the hydrocarbon tank.

SK9-WP-4 measures liquid entrained in the gas stream from the light ends separator.

Composition Data

The composition of the process gas will be monitored at four points in the system:1) Producer Gas - downstream of the producer gas transfer compressor SK4-CP-12) CO2 free Producer Gas - downstream of the CO2 scrubber and H2S adsorber SK73) Reformed Synthesis Gas - downstream of the steam reformer SK74) Liquid Fuel Light Ends Gas - at the light ends separator SK9-V-13

During steady state operation, gas samples are collected at 30 minute intervals, sequentially, from each of the gas sampling points. The gas samples are processed in a NOVA flow-through gas analyzer which reports values in the gas stream for CO, C02, CH4 and H2 as voltages.These voltages are converted to volume% values and recorded by a Qtech® data acquisition system running DakView® software. The component volume %values are also manually recorded on the Composition Datasheet.

Gas from the four process sampling ports is carried through heated gas lines (200 °F) to a sampling manifold ahead of the NOVA analyzer. The manifold is connected to the NOVA sample port via a length of unheated tubing to allow the gas to cool to 150 °F (NOVA limit).During a typical gas sampling operation a toggle valve is opened at the desired sample port.A needle valve (provided by ACTi) at the port is cracked open allowing gas to flow through thesample line and manifold to a pressure regulator at the NOVA. The needle valveis slowly opened until 30 psig is read on a pressure gauge at the analyzer(the NOVA manual recommends 5 psig but the factory assures us 30 psig is acceptable).

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Additional samples will be captured in Tedlar® bags for remote analysis from:1) Scrubbed Gasifier gas at the gas transfer tank SK4-V-12) Flashed CO2 Gas - at the CO2 regenerator SK5-V-33) Liquid Fuel Light Ends Gas - at the light ends separator SK9-V-13Gas samples will be obtained once per run during steady state operation.

During the process startup phase a continuous analysis of the producer gas leaving the gasifier can be recorded at the sample port on PFD SK4.

Sample Data

Representative liquid samples will be taken from all locations where process liquids accumulate (except the amine CO2 absorber and the reformer steam saturator). Liquid samples will be takenin the morning for the previous day's run to allow hot process liquids to cool. Both solid and liquid samples will be collected in 40ml bottles and labeled with the run number, time, date and sample location e.g. SK9-LSP-2. The collection of these samples will be logged on the Sample Datasheet.

Numbering Conventions

Run number = ACTI - run # - mm/dd e.g. ACTI-3-4/24

Sample Label = ACTI - run # - mm/dd <next line> sample point e,g, ACTI-2-4/22 <next line> SK9-LSP-4

in the case of multiple samples taken from the same sample point for differentanalyses, the sample label will be appended with a letter e.g. SK4-BSP-1(a) or -1(b)

………………………………………………………………………………………………………………………….

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Test Checklists

Run No. __________________

Run Date __________________

Run Description

Pre-start Checklist

___ add char from previous shutdown to total lb___ scrubber liquid level recorded - SK2-LI-1 mm___ gasifier propane starting weight lb___ reformer propane starting weight lb___ gas transfer totalizer - SK4-FQI-1 ft3___ weigh reformer syngas cooler - HE-3 lb___ sample reformer syngas cooler___ drain/weigh light ends cooler - HE-4 lb___ sample light ends cooler___ drain/weigh paraffin tank - # 11 lb___ sample paraffin tank___ drain/weigh paraffin tank - # 11a lb___ sample paraffin tank___ drain/weigh HC condensate tank - # 10 lb___ sample condensate tank___ drain/weigh light ends separator - # 12 lb___ sample light ends cooler___ drain/weigh knock out pot - # 8 lb___ sample knock out pot___ buckets filled with chips

Start of Run Checklist

___ calculate startup net wood chip weight lb___ collect chip sample for run - SK1-SSP-1___ begin with full bucket of chips___ scrubber liquid level recorded - SK2-LI-1 mm___ gas transfer totalizer - SK4-FQI-1 ft3___ gasifier propane tank weight lb___ reformer propane tank weight lb___ record run start time hh:mm

End of run Checklist

___ record run end time hh:mm___ scrubber liquid level recorded - SK2-LI-1 mm___ gasifier propane tank weight lb___ reformer propane tank weight lb___ gas transfer totalizer - SK4-FQI-1 ft3___ calculate run net wood chip wt. lb___ return unused chips to super sack___ calculate net run char weight lb___ collect char sample for run - SK1-SSP-2

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APPENDIX B SAMPLING DET AILS

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SAMPLING DATASHEETRun No.Run Date:Run Description:

Gasification Scrubbing ReformingSlurryReactor

HCRecovery

Time SK1-SSP-1 SK1-SSP-2 SK2-LSP-1 SK3-LSP-1 SK7-LSP-1 SK8-LSP-1 SK9-LSP-1 SK9-LSP-1a SK9-LSP-2 SK9-LSP-3 SK9-LSP-4

Page 1 of 1

GAS ANALYSIS DATA SHEETRun No.Run Date:Run Description:

Gas Transfer CO2 RemovaReformer HC Recovery

Time

SK4-GSP-1volume% volume% volume% volume% SK4-BSP-1 SK5-BSP-1 SK7-GSP-1

volume% volume% volume% volume% SK7-GSP-2volume% volume% volume% volume% SK9-GSP-1

volume% volume% volume% volume% SK9-BSP-1

C0 C02 CH4 H2 C0 C02 CH4 H2 C0 C02 CH4 H2 C0 C02 CH4 H2

Note:

Nova instrument would not calibtate and was not usable during test.

34



35


APPENDIX C PROCESS DATA D ETAILS & FLOW CHARTS

36



37


PROCESS DATASHEETRun No.: ACTI-1-5/12Run Date: 5/12/2009Run Description: Initial startup and system gas purge (purge xfer tanks)

Gasification Scrubbing Gas Transfer CO2 Removal

TimeSK1-PI-1mm wc

SK1-TI-1°F

SK1-TI-2°C

SK2-TI-1°F

SK2-LI-1inches

SK2-PI-1in H2O

SK3-PI-1in H2O

SK4-FQI-1ft3

SK4-PI-1psig

SK5-PI-1psig

SK5-PI-2psig

Gasifier Fire Box RetortVenturi

ReservoirVenturi

ReservoirVenturi

DemisterGas Cooler Demister

Prod. Gas Flow

PressurizedHold Tanks

CO2Absorber

AbsorberRegen.

12:00 6.2 1478 370 73 0 0 0

12:30 9.2 1606 557 87 0.6875 0 0

13:00 10.5 1631 475 98 1.625 0 0 54000 39 0 0

13:30 5.6 1556 450 98 0 0 54700

14:00 11.8 1635 431 92 3.1875 0 0 55400

16:00 10.5 1624 451 92 5.25 0 0 57000 30

16:30 6.43 1594 444 91 6.5 0 0 57800 60

17:00 5.04 1555 430 89 8.1875 0 0 58300 83

17:30 8.3 1585 437 82 8.75 0 0 59250 118

SHUT DOWN 59500 FINAL GAS TOTAL

Reformer Slurry Reactor HC Recovery

TimeSK7-PI-1

psigSK7-PI-2

psigSK7-TI-1

°FSK7-TI-2

°FSK8-PI-1

psigSK8-TI-2

°FSK8-TI-3

°FSK9-PI-1

psigSK9-PI-2

psigSK9-PI-3

psigSK9-TI-1

°FSK9-TI-2

°FSK9-TI-3

°FZnO

AdsorberReformer

Cooler ReformerReformer

Cooler ReactorReactorLiquid

ReactorVapor Paraffin Tank

CondensateTank

Light Ends Separator Paraffin Tank

CondensateTank

Light Ends Separator

12:00

12:30

13:00 0 0 --- --- 30 473

13:30

14:00

16:00

16:30

17:00

17:30

SHUT DOWN

BEGIN FEEDING F/T UNIT

SUSPEND FEEDING - TAKE F/T UNIT OFF LINE

STARTUP - OUTPUT GAS BURNED WHILE XFER TANKS PURGED

BEGIN FEEDING F/T UNIT

SUSPEND FEEDING - TAKE F/T UNIT OFF LINE

STARTUP - OUTPUT GAS BURNED WHILE XFER TANKS PURGED

38


PROCESS DATASHEETRun No.: ACTI-1-5/13Run Date: 5/13/2009Run Description: Gasifier and reformer operating. Slurry reactor flange leaking.


TimeSK1-PI-1mm wc

SK1-TI-1°F

SK1-TI-2°C

SK2-TI-1°F

SK2-LI-1inches

SK2-PI-1in H2O

SK3-PI-1in H2O

SK4-FQI-1ft3

SK4-PI-1psig

SK5-PI-1psig

SK5-PI-2psig


ReservoirVenturi

ReservoirVenturi


Prod. Gas Flow

PressurizedHold Tanks

CO2Absorber

AbsorberRegen.

14:30

15:00

15:30 8.72 1644 383 89 0.625 0 0 59500 63 192 0

16:00 4.3 1606 429 100 1.25 0 0 60200 84 150 0

16:30 5.15 1572 477 99 1.75 0 0 61800 92

SHUT DOWN - SLURRY REACTOR TOO LOW FOR FUEL GENERATION 61800 FINAL GAS TOTAL


TimeSK7-PI-1

psigSK7-PI-2

psigSK7-TI-1

°FSK7-TI-2

°FSK8-PI-1

psigSK8-TI-2

°FSK8-TI-3

°FSK9-PI-1

psigSK9-PI-2

psigSK9-PI-3

psigSK9-TI-1

°FSK9-TI-2

°FSK9-TI-3

°FZnO

AdsorberReformer


CoolerZnO

Adsorber ReactorReactorLiquid

ReactorVapor

ParaffinTank

CondensateTank


ParaffinTank

CondensateTank


14:30

15:00

15:30 175 0 1817 --- 605 200 40 55 55 110

16:00 145 0 1848 576 200 50 25 25 110

16:30

SHUT DOWN - SLURRY REACTOR TOO LOW FOR FUEL GENERATION

STARTUP

BEGIN FEEDING GASIFIER

STARTUP


39


PROCESS DATASHEETRun No.: ACTI-1-5/14Run Date: 5/14/2009Run Description: Attempt simultaneous operation of gasifier, reformer and slurry reactor.


TimeSK1-PI-1mm wc

SK1-TI-1°F

SK1-TI-2°C

SK2-TI-1°F

SK2-LI-1inches

SK2-PI-1in H2O

SK3-PI-1in H2O

SK4-FQI-1ft3

SK4-PI-1psig

SK5-PI-1psig

SK5-PI-2psig


ReservoirVenturi

ReservoirVenturi


Prod. Gas Flow

PressurizedHold Tanks CO2 Absorber

AbsorberRegen.

10:30

12:15

12:30 7.49 968 359 75 0 0 0 61800 77 92 0

13:00 4.4 814 224 82 0.25 0 0 61900 82 70 0

13:30 10.83 1582 245 95 0.75 0 0 62200 80 110 0

14:00 14.24 1595 342 103 1.1875 0 0 63100 95

14:30 8.56 1329 389 93 2.5 0 0 63620 108

14:45 63800 FINAL GAS TOTAL


TimeSK7-PI-1

psigSK7-PI-2

psigSK7-TI-1

°FSK7-TI-2

°FSK8-PI-1

psigSK8-TI-2

°FSK8-TI-3

°FSK9-PI-1

psigSK9-PI-2

psigSK9-PI-3

psigSK9-TI-1

°FSK9-TI-2

°FSK9-TI-3

°F

ZnO AdsorberReformer


Cooler ZnO Adsorber Reactor Reactor Liquid Reactor Vapor Paraffin TankCondensate

TankLight Ends Separator Paraffin Tank

CondensateTank


10:30

12:15

12:30 95 20 1783 --- 606 480 489 540 30 45 110 amb. amb. amb.

13:00 67 0 1850 535 520 498 530 30 45 80 amb. amb. amb.

13:30 105 380 550 510 501 460 >300 390 80 134

14:00

14:30

STARTUP


REFORMER OFFLINE

SHUT DOWN

STARTUP


REFORMER OFFLINE

SHUT DOWN

40


MATERIAL BALANCE DATASHEETRun No. ACTI-1-5/13Run Date: 5/13/2009Run Description: Gasifier only run.

Gasification Scrubbing Reforming Slurry ReactHC Recovery

TimeSK1-WP-1

lbSK1-WP-2

lbSK2-WP-1

lbSK7-WP-1

lbSK8-WP-1

lbSK9-WP-1

lbSK9-WP-

1a lbSK9-WP-2

lbSK9-WP-3

lbSK9-WP-4

lbincremental total incremental total as reqd. end of run end of run end of run end of run end of run end of run end of run

15:00 0 015:10 10 1015:20 10 2015:30 10 3015:40 10 4015:50 10 5015:57 10 6016:07 10 7016:25 10 80

SHUT DOWN7.1 7.1 48.7 RESERVOIR DRAINED AND LIQUID WEIGHED AT END OF RUN

80 total input48.7 total water31.3 total solids

60.875 water as % of feed39.125 solids as % of feed

22.68371 char as % of solids77.31629 gas as % of solids

MATERIAL BALANCE DATASHEETRun No. ACTI-1-5/12Run Date: 5/12/2009Run Description: Initial startup and system gas purge (purge xfer tanks).

Gasification Scrubbing ReformingSlurryReactor

HCRecovery

Time SK1-WP-1 lbSK1-WP-2

lbSK2-WP-1

lbSK7-WP-1

lbSK8-WP-1

lbSK9-WP-1

lbSK9-WP-

1a lbSK9-WP-2

lbSK9-WP-

3 lbSK9-WP-4


12:00 0 012:41 50 5013:00 20 7013:30 30 100

15:0016:00 100 20016:30 20 22017:00 10 23017:30 10 240

SHUT DOWN19.65 19.65 CHAR 182.1 RESERVOIR DRAINED AND LIQUID WEIGHED AT END OF RUN




SUSPEND FEEDINGRESUME FEEDING

41


MATERIAL BALANCE DATASHEETRun No. ACTI-1-5/14Run Date: 5/14/2009Run Description: Attempt simultaneous operation of gasifier, reformer and slurry reactor.

Gasification ScrubbingReforming Slurry Reactor HC Recovery

TimeSK1-WP-1

lbSK1-WP-2

lbSK2-WP-1

lbSK7-WP-1

lbSK8-WP-1

lbSK9-WP-1

lbSK9-WP-

1a lbSK9-WP-2

lbSK9-WP-3

lbSK9-WP-4


12:15 0 0 BEGIN FEEDING12:26 10 1012:36 10 2012:43 10 3012:58 10 4013:07 10 5013:26 10 6013:46 10 7013:55 10 80

SHUT DOWN7.65 7.65 CHAR 49.1 RESERVOIR DRAINED AND LIQUID WEIGHED AT END OF RUN




42


PRO

CES

S FL

OW

DIA

GR

AM

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AC

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ifier

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LE

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CH

EC

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D:

xxx

xxx

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d C

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to L

iqui

d Fu

el

Gas

ifier

4/3/

09

SK1

M-1

F-1

Air

Prop

ane

M-2

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Ash

Woo

d C

hips

Ele

ctric

Pw

r

Elec

tric

Pw

r

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t Tra

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To V

entu

ri S

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ME

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PO

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12

34

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TEM

PP

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SR

ATE

N2

O2

CO

CO

2H

2H

2OH

2SC

1C

2C

3C

4C

5-C

11C

12-C

20S

olid

s

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TI-2

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lysi

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m A

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aula

te m

ass

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is

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er

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rt

cold

di

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/hr60

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r han

d fe

d th

ru a

ir lo

ck o

n 2

min

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le (2

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y 2

min

.)

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co

ntro

l loo

p

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s sa

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solid

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PLC

PLC

PLC

43


PRO

CES

S FL

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DIA

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AM

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AC

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ifier

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tric

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CO

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1C

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3C

4C

5-C

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s

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1

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ge

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ple

at e

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of s

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m g

as

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estim

ate

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44


PRO

CES

S FL

OW

DIA

GR

AM

S FO

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AC

Ti D

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ter

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E:

PR

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BY:

KH

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: x

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to L

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r

4/3/

09

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er1

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12

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TEM

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erS

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int L

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ple

at e

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45


PRO

CES

S FL

OW

DIA

GR

AM

S FO

R T

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AC

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RA

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YS

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nsfe

r

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STR

EA

ME

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PO

WE

RH

EA

T TR

AN

SFE

R1

23

45

67

89

12

34

12

TEM

PP

RE

SR

ATE

N2

O2

CO

CO

2H

2H

2OH

2SC

1C

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3C

4C

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s

46


PRO

CES

S FL

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AM

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PO

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23

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67

89

12

34

12

TEM

PP

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SR

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CO

2H

2H

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1C

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s

47


PRO

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AC

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fur P

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pita

tion

Not

use

d in

this

test

.

48


SK

7 S

ynga

s R

efor

mer

PRO

CES

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OW

DIA

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AM

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67

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12

34

12

TEM

PP

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SR

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CO

CO

2H

2H

2OH

2SC

1C

2C

3C

4C

5-C

11C

12-C

20S

olid

s

49


PRO

CES

S FL

OW

DIA

GR

AM

S FO

R T

HE

AC

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AC

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ctor

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ED

: x

xxxx

x

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d C

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to L

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d Fu

el

3/12

/09

SK

8

MA

TER

IAL

STR

EA

ME

LEC

TRIC

PO

WE

RH

EA

T TR

AN

SFE

R1

23

45

67

89

12

34

12

TEM

PP

RE

SR

ATE

N2

O2

CO

CO

2H

2H

2OH

2SC

1C

2C

3C

4C

5-C

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s

Syn

gas

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-10

From

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orm

er C

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ctor

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450

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0 ps

ig

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er

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orTo

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te C

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nkS

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om D

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late

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-hh

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ple

at

end

of s

hift

liqui

d sa

mpl

e LS

P-1

wei

gh p

oint

W

P-1

Sie

men

s R

W 4

0

gray

con

trol b

ox

CV

-9a

50


PRO

CES

S FL

OW

DIA

GR

AM

S FO

R T

HE

AC

Ti D

EMO

NST

RA

TIO

N F

AC

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9 Pr

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t Rec

over

y

MA

TER

IAL

STR

EA

ME

LEC

TRIC

PO

WE

RH

EA

T TR

AN

SF

ER

12

34

56

78

91

23

41

2TE

MP

PR

ES

RA

TEN

2O

2C

OC

O2

H2

H2O

H2S

C1

C2

C3

C4

C5-

C11

C12

-C20

Sol

ids

51


APPENDIX D ANALYTICAL MET HODOLOGY AND RESULTS DETAILS

52



53


Bag Sampling Results

54



55



56



57


Run

Sam

ple

O2/

Ar

N2

CO

CH

4C

O2

H2

C2H

6C

2H4

C2+

Sum

AC

TI-1

-5/1

2S

K4-

GS

P-1

a/b

0.7

4.8

30.9

12.8

1822

.91.

64.

363.

8799

.93

AC

TI-1

-5/1

3S

K4-

GS

P-1

a/b

0.7

929

.612

.317

.422

.11.

494.

193.

310

0.08

AC

TI-1

-5/1

4 S

K4-

GS

P-1

c/d

0.7

10.1

27.6

12.1

17.2

23.8

1.6

3.84

3.22

100.

16av

erag

e0.

78.

029

.412

.417

.522

.91.

64.

13.

5

AC

TI-1

-5/1

3S

K7-

GS

P-2

a0.

37.

146

.92.

53.

939

.20.

09N

DN

D99

.99

AC

TI-1

-5/1

4S

K7-

GS

P-2

c/d

0.03

5.2

24.3

0.6

14.1

55.5

ND

ND

ND

99.7

3av

erag

e0.

26.

235

.61.

69.

047

.40.

1

Gas

ifier

Com

paris

on

Gas

ifier

Pyr

loys

is G

as A

ssay

s

Gas

ifier

Ref

orm

er G

as A

ssay

s

58


Analyst: Floyd R. Girocco

Sample #Sample

Date Date TestedDish wt.

(gms)

Dish & Sample

wt.(gms)

Sample wt. (gms) Time in Time out

Dry Wt. (gms)

Weightchange

%Moisture

Wood #1 3/27/2009 3/27/2009 173.53 223.99 50.46 13:02 13:17 198.61 25.38 50.30Wood #1 3/27/2009 3/27/2009 173.53 223.99 50.46 13:23 13:38 193.06 30.93 61.30Wood #1 3/27/2009 3/27/2009 173.53 223.99 50.46 13:45 14:00 192.36 31.63 62.68Wood #1 3/27/2009 3/27/2009 173.53 223.99 50.46 14:21 14:36 192.27 31.72 62.86

Sample ran using the moisture teller.

Sample #Sample

Date Date TestedDish wt.

(gms)

Dish & Sample

wt.(gms)


Dry Wt. (gms)

Weightchange

%Moisture

Wood #2 3/27/2009 3/27/2009 168.45 219.54 51.09 13:03 9:43 186.37 33.17 64.92Sample ran using the drying oven in the sand lab.Sample taken out on 03/30/09.

Moisture Sampling-Wood-ACTISAND LAB DATA SHEET

Wood Chip Moisture Content for American Combustion Test

Analyst: Floyd R. Girocco

Sample #Sample

DateDate

TestedDish wt.

(gms)

Dish & Sample

wt.(gms)


Dry Wt. (gms)

Weightchange

%Moisture

ACTI Ash #1 5/12/2009 6/25/2009 173.48 175.79 2.31 9:01 9:16 175.76 0.03 1.30

Sample #Sample

DateDate

TestedDish wt.

(gms)

Dish & Sample

wt.(gms)


Dry Wt. (gms)

Weightchange

% 1800*Lost on Ignition

ACTI Ash #1 5/12/2009 6/25/2009 67.1357 69.4351 2.2994 9:33 Program 67.1669 2.2682 98.6431NOTE: Muffle furnace has a program to ramp up to 1800oF, hold for 2 hours and then reduce the temperature to 400oF.

ACTI Ash Moisture and LOI Tests

SAND LAB DATA SHEET

59


60


61


APPENDIX E REACTOR ASSESSMENT AND CALCULATIONS

62



63


ACTI Slurry Reactor Modeling and Process Assessment

Background: Operational diffi culties prevented us from obtaining steady state perfor-mance data from the ACTI slurry reactor. That precludes a direct assessment of the reac-tor’s performance and limitations. However, there is suffi cient data available on Fischer-Tropsch reactor design and reactor operations to make a preliminary assessment of the ACTI slurry reactor design. To that end, design and operating data was analyzed from three operating programs and one design study (Reichspressen laboratory unit, Reichspressen demonstration unit, Mobil pilot plant and a DOE production-scale design study). The physical properties of the reaction media and the documented performance of the catalysts were input to a simplifi ed model of the ACTI reactor.

Reactor Model: The ACTI slurry reactor is modeled as an adiabatic reactor supporting a plug fl ow gas phase dispersed in a fully mixed liquid phase. While not entirely consistent with adiabatic operation, the FT reaction is modeled as isothermal for rate calculations. The accepted mechanism for the catalyzed Fischer-Tropsch reaction has CO adsorbing onto catalytic sites where the carbon-carbon bond is formed, then reacting with H2 from the gas phase. Because CO is strongly adsorbed, the reaction follows zero-order kinetics with respect to CO and fi rst-order kinetics for H2. Hence, the reaction rate constant “k_rxn_H”, and net conversion “X_H” are usually calculated with respect to Hydrogen. Although the actual dimensions of the ACTI reactor were not provided, they are estimated, for this evaluation, to be: reactor height = 12 ft; slurry height = 8 ft; reactor inside diameter = 0.6 ft. The synthesis gas feed rate is 2000 scfh at a composition of: 55 Vol% hydrogen; 25 Vol% carbon monoxide; and 20 Vol% inert materials. These were values obtained at the gasifi er and the reformer during periods of stable unit operation.

Ideal Single Pass Reactor Performance: The simplest scheme to analyze is once-through processing of the reactant gases in a single pass. For this scheme a reaction rate constant of ≅0.10 sec-1 has been reported for a range of operating plants. This is an “intrinsic” rate constant which is determined in the absence of mass transfer limitations and it assumes a level of catalytic activity consistent with established Fischer-Tropsch process technology.

At these conditions the model calculates a CO conversion of 0.99 and a syngas (H2 + CO) conversion of 0.62. About 27 lb/hr of hydrocarbon product would be produced. The rate constant needed to achieve this conversion is 0.03 sec-1, about 1/3 the activity of existing catalytic technology. Assuming the process is rate limited, not mass transfer or heat trans-fer limited, substantially higher feed rates could be accommodated if the ACTI catalyst performs to industrial standards.

Mass Transfer Limitation: The mass transfer coeffi cient for hydrogen at the gas-liquid interface (kla)H was estimated at 0.54 sec-1. That value was corrected for the presence of entrained gas and solid (catalyst) phases. It is over fi ve times greater than the highest ex-

64


pected reaction rate constant and, therefore, should not impose a signifi cant resistance to the overall reaction.

The resistance to mass transfer presented by ACTI’s catalyst is not known. The Thiele modulus plot (on the mass transfer calculations page) indicates that resistance to mass transfer – primarily catalyst pore diffusion - would become important for catalyst pellets over 0.3 centimeters in diameter at the model slurry conditions. Note: the Fischer-Tropsch process data used to develop the model calculations was obtained using catalyst particles in the 25-50 micron range.

Heat Transfer Limitation: A great deal of heat is generated by the Fischer-Tropsch re-action (129,000 Btu/hr in the single pass model). The ACTI design makes no provision for active heat removal from the reactor. The heat of reaction must be removed from the reactor effl uent stream by the downstream product recovery train. The cooled, light gases would then need to be recycled to the reactor for temperature control. Using a practical low temperature limit of 100 °F for cooled gas gives a cooling gas rate of 33,000 scfh. This translates to a reactor gas recycle ratio of 15 (moles at reactor entrance / mole fresh feed). About 70 ft2 of active heat transfer area (e.g. HE-4) would be needed to achieve this gas cooling.

Ideal Recycle Reactor Performance: The once-through slurry reactor model was re-evaluated employing a recycle ratio of 15. In addition to its cooling function, this scheme allows unreacted hydrogen to be returned to the reactor at a higher concentration than for the once-through case. Specifi cally, at a recycle ratio of 15, there is a 30% increase in the hydrogen mole fraction in the reactor gas and a similar increase in the liquid hydrogen con-centration in the slurry. The hydrocarbon production rate and the reactor heat output both see corresponding increases of 14-15%.

Product Distribution: The product distribution for Fischer-Tropsch synthesis can be rep-resented by a Flory polymerization model where products are formed by the addition of one carbon unit at a time to a growing chain. If the probability of carbon addition “α” is independent of the chain length, then MN = (1- α) α(Ν−1) where N is the number of carbon atoms and MN is the mole fraction of molecules with N carbons. A typical Flory distri-bution of Fischer-Tropsch products is given in Figure A-1. The optimum value of α for Diesel production is near 0.85. The Diesel cut of this product distribution is about 40% by weight. About 26% goes to gasoline, 12% to liquid petroleum gas (LPG), 2% to methane and 20% to wax. The preceding model analyses assume the entire hydrocarbon product is Diesel (C15H32), but less than half of the product distribution would yield Diesel in a true Flory process. Since the catalyst will only utilize carbon in the form of CO, the hydro-carbon byproducts cannot participate in the Fischer-Tropsch reaction and must be purged from any recycle stream. This can be done by fl aring a portion of the recycle stream or by incorporating additional steps in the recovery process to separate and store the byproducts.

65


Figure A-1 Theoretical Flory FT Product Distribution

Discussion: The design of the ACTI demonstration plant is necessarily an exercise in compromise. The ACTI design promotes mechanical simplicity over process effi ciency. This is apparent in the selection of operating rates that are low enough to negate the need for internal heat transfer from the slurry reactor. It is also evident in design of the catalyst which does not require an external system to separate catalyst from the slurry. And in the hydrocarbon recovery train which relies substantially on ambient cooling to affect the separation of Diesel distillate from the lighter product fractions. There are, however, two areas where the ACTI system is more complex than preceding Fischer-Tropsch slurry reac-tor plants; 1) the use of mechanical agitation in the slurry and 2) the installation of a steam reformer upstream of the reactor.

The reason for incorporating mechanical agitation was not discussed with ACTI. It would be expected to increase gas dispersion and mass transfer at very low gas fl ow rates. It would also ensure the uniform distribution of catalyst in the slurry over a wider range of gas velocities and catalyst densities and diameters. Hence, it would allow the reactor to achieve reasonable conversions at very low throughputs.

A key advantage of slurry reactors is their ability to process syngas feeds with low H2/CO ratios – typically 0.5 to 0.75. This is particularly true where an iron-based catalyst is used for hydrocarbon synthesis because iron catalysts possess an inherent water-shift capability

66


that generates additional hydrogen as the reaction progresses. Since ACTI indicated they use an iron-based catalyst, their use of a steam reformer to boost the H2/CO ratio of their syngas is puzzling. This could be a strategy to compensate for low catalyst loading in the reactor, high mass transfer resistance in the catalyst, or low catalyst activity. If the catalyst is susceptible to coke formation, an increase in hydrogen concentration would suppress this. There may be other factors to justify the reforming step which are not apparent.

By designing their reactor to operate at rates below the region of heat transfer limitation ACTI has placed some constraints on their process. The productivity, or space-time yield (lb product/hr-ft3), of the reactor cannot be signifi cantly increased without incorporating an active heat removal step. This limits, for example, the ability to increase rates or take advantage of improvements in catalyst performance. Physical scale-up of the process will be complicated since changes in the reactor’s surface-to-volume relationship will aggra-vate the heat removal problem. Cooling and recycling unreacted syngas (and light reaction products) can effectively remove heat from the slurry. But the recycle rate cannot exceed the superfi cial gas velocity that induces “slug fl ow” in the slurry - less than 1 ft/sec in conventional Fischer-Tropsch slurry reactors. The ACTI reactor might support higher gas velocities depending on the physical characteristics of the catalyst/slurry system. Note: the recycle model’s superfi cial velocity is 1.1 ft/sec at the recycle ratio of 15.

Finally, the simplicity of the hydrocarbon recovery system makes it diffi cult to control the quality of the Diesel product. The extent of reliance on ambient heat transfer is expected to be problematic at locations where there is large climatic variability. Under the best cir-cumstances precise control of product separation will be labor intensive without the aid of active cooling systems supported by some level of automation. The ACTI demonstration plant did not have provisions to recover the lighter hydrocarbon fractions, or their energy value. Light ends were periodically purged from the recycle line along with the accompa-nying H2 and CO and burned.

Sources of Error: The physical dimensions of the ACTI slurry reactor are estimates based on observation of the unit in the fi eld. The ratio of slurry volume to reactor volume will vary with operating conditions. The quiescent slurry volume is used in the model calcula-tions and is an educated guess.

The physical properties of the slurry liquid are based on the molten high molecular weight wax that normally accumulates in the reactor as a byproduct of the Fisher-Tropsch reac-tion. This is the usual reaction medium for hydrocarbon production. However, the ACTI process employs a “synthetic” reaction medium with molten wax accumulating at the sur-face. Other operators have used halocarbon-based media when the Fischer-Tropsch reac-tion is used in the production of alcohols but we have no information about ACTI’s reac-tion medium. Our assessment assumes the physical properties of the medium are similar to those in conventional processes.

67


The water gas shift reaction is known to occur on iron-based Fischer-Tropsch catalysts but this reaction is not taken into account in the model calculations.

The molar volume occupied by the hydrocarbon product (C15H32) is ignored in the recycle model calculations. Also, the latent heat of vaporization of the hydrocarbon product is not taken into account in the heat transfer calculations. This could result in an approximate 20% increase or decrease in heat duty depending on how the standard state was defi ned for the enthalpy of reaction.

68


Page 1 of 4

Sources:

DH2_slurry 0.00054 cm2/s H2 eff. Diffusivity in slurryPLS 0.1666667 (Pore Length Scalar) estimate catalyst

pore length as fraction of catalyst bead diameter

T_factor 2.2900527 factor to calculate Thiele modulus

k_rxn_H2 0.0941 s-1 Reichprssen Labk_rxn_H2 0.1289 s-1 Reichprssen Demok_rxn_H2 0.0779 s-1 Mobil Pilotk_rxn_H2 0.1069 s-1 DOE Designk_rxn_H2 0.10195 s-1 Estimated FT 1st order intrinsic rate const.

for H2. This rate constant reflects the average catalyst and slurry properties of the above reaction systems.

Z_reactor 12 ft Slurry reactor heightZ_slurry 8 ft Slurry heightD_reactor 0.6 ft Slurry reactor diameterV_slurry 2.261952 ft3 Slurry volume

dp 0.0098425 ft catalyst diameter - assume 0.3 cmrho_s 187.28388 lb/ft3 typical catalyst densityepsilon_s 0.1 estimated volume fraction catalyst pellets

in slurry - commercial model data

epsilon_g 0.25 estimated gas volume fraction in slurry - commercial model data

epsilon_l 0.65 liquid volume fraction by difference

Rg 10.73 ft3 psi R-1 lbmole-1

Ideal Gas Constant

T_abs 960 °R Absolute temperature of reaction medium

P 515 psia Absolute reactor pressureH_rxn_H2 85985 Btu/lbmole Heat of FT reaction (-CH2- uint basis)Cp_H2 6.85 Btu/lbmole F Heat capacity H2Cp_CO 7.29 Btu/lbmole F Heat capacity COCp_N2 7.22 Btu/lbmole F Heat capacity inerts (as N2)Cp_gas 6.77 Btu/lbmole °F Approximate reaction gas heat capacity

Thermodynamic Variables

REACTOR PERFORMANCE MODELING

Reaction Variables

Topical Report Slurry Reactor Design Studies DOE Project No. DE-A C22-89PC89867Fischer-Tropsch Synthesis of Hydrocarbons, NTIS DE84017841, BNL 51799 UC-90d (Coal Conversion and Utilization-Liquifaction - TIC-4500), MIT/BNL-83-4Catalyst and Reactor Development for a Liquid Phase Fischer-Tropsch Process,DOE Report No. DOE/PC/30021-T20 (NTIS DE90002792), 1985

69


Page 2 of 4REACTOR PERFORMANCE MODELING

y_0H 0.55 mole fraction H2 iny_zH 0.5800575 mole fraction H2 outp_0H 283.25 psia pressure H2 in p_zH 298.72963 psia pressure H2 out y_0Co 0.25 mole fraction CO iny_zCo 0.0047939 mole fraction CO outp_0Co 128.75 psia pressure CO in p_zCo 2.4688399 psia pressure CO out Henry_H2 46466 psi ft3/lbmole Henry law constant for H2 in reaction

slurryC_0H 0.0060959 lbmole/ft3 inlet conc. H2 in slurryC_zH 0.006429 lbmole/ft3 outlet conc. H2 in slurry

X_H 0.45 Conversion of H2X_CO 0.99 Conversion of CO

Hmole_rate_in 3.3429231 lbmole/hr

Hmole_rate_out

1.8386077 lbmole/hr

Cmole_rate_in 1.5195105 lbmole/hr

Cmole_rate_out

0.0151951 lbmole/hr

HCmole_rate_ 0.1002877 lbmole/hrnet_mole_in 6.0780421 lbmole/hrnet_mole_out 3.1696989 lbmole/hrinert_mole_rate

1.22 lbmole/hr Note: gas phase FT hydrocarbon component neglected

Uco 1 usage ratio, change in moles CO/change in moles H2

Ico 0.4545455 inlet ratio of CO to H2X_H_CO 0.61875 net syngas conversion X (H+CO)

(1+Uco)/(1+Ico)*X_HQz_x_0 121.57028 ft3/hr gas volume rate at zero conversion (X=0)

Qz_x_1 62.811313 ft3/hr gas volume rate at total conversion (X=1)

contrac_factor -0.483333 gas contraction factor from reaction (varies with H2/CO ratio)(Qz_x_1-Qz_x_0)/Qz_x_0

Ideal Single Pass Reactor Performance

70



k_rxn_calc 0.0287347 s-1 Adjust the conversion (X_H) until rate constant (k_rxn_calc) matches the intrinsic rate constant given by (k_rxn_H2). This represents the maximum conversion with no heat or mass transfer limitations.

Hydro_out 0.1253596 lbmole/hr Hydrocarbon product (C-15 basis)26.576239 lb/hr Total mass rate of hydrocarbon product

Q_rxn 129348 Btu/hr heat of reaction accompanying this D_T_cooling 400.00 °F Reactor effluent cooled from 500 to 100

°F for hydrocarbon recoverycooling_flow 48 lbmole/hr The cold effluent return flow required to

dissipate the heat of 546 scfm reaction under the above operating

conditions.33.210445 acfm

Rec_reqired 15.06 Recycle ratio required to carry away heat of reaction volume returned to reactor/volume leaving system

Rec 15.060 Recycle ratiorec_X_H 0.033 conversion of H2 at this recycle ratiorec_X_CO 0.982rec_X_in 0.938H_recycle 48.684 lbmole/hr in recycle streamCO_recycle 0.229 lbmole/hr in recycle streaminert_recycle 18.307 lbmole/hr in recycle streamH_feed 52.027 lbmole/hr in reactor inlet streamH_exit 50.309755 lbmole/hr in reactor exit streamCO_feed 1.748 lbmole/hr in reactor inlet streamCO_exit 0.031473 lbmole/hr in reactor exit streamInert_feed 19.523 lbmole/hr in reactor inlet streamnet_feed 73.298 lbmole/hr in reactor inlet streamnet_exit 69.864145 lbmole/hr in reactor exit streamy_H_feed 0.710 mole fraction CO at reactor inlety_H_exit 0.720 mole fraction CO at reactor exity_Co_feed 0.024 mole fraction H2 at reactor inlety_Co_exit 0.000 mole fraction CO at reactor exitrec_p_zH 370.85581 psia H2 partial pressure in reactor gas stream

rec_C_zH 0.0079813 lbmole/ft3 H2 concentration in reactor in slurry

rec_k_rxn_calc

0.0264168 s-1 Adjust the conversion (X_H) until this rate constant matches the intrinsic rate constant given by (k_rxn_H2). This represents the maximum conversion with no heat or mass transfer limitations.

rec_Hydro_out 0.1430732 lbmole/hr Hydrocarbon product (C-15 basis)

30.331528 lb/hr Total mass rate of hydrocarbon product

Ideal Recycle Reactor Performance

71



rec_Q_rxn 147625 Btu/hr heat of reaction accompanying this Note: the heat of reaction has increased from the "single pass" case because the average H2 concentration hence rxn rate is higher.

rec_Ico 0.03 inlet ratio of CO to H2rec_X_H_CO 0.0638542 net syngas conversion X (H+CO)

rec_Qz_x_0 1466.0719 ft3/hr gas volume rate at zero conversion (X=0)

rec_Qz_x_1 1396.1324 ft3/hr gas volume rate at total conversion (X=1)

rec_contrac_fact

-0.047705 gas contraction factor from reaction (varies with H2/CO ratio)(Qz_x_1-Qz_x_0)/Qz_x_0to bring the effluent stream down to 100 °F for hydrocarbon recovery.

rec_cooling_flow

54 lbmole/hr The molar rate of reactor effluent required to dissipate the heat of

624 scfm reaction under the above operating conditions.

37.903164 acfm

3.53147E-05 ft3/cm30.002204623 lbmol/gmol0.145037738 psia/kPa0.94781712 Btu/kJ

0.032808399 ft/cm0.067196898 lb/ft-

s/Poise5.71015E-06 lb-

force/in/(dyne/cm)

0.7268813 s

rate 0.0004431 lbmole/s1.5043154 lbmole/hr1.50431545.2351884 lbmole/hr677160.33 Btu/hr

Conversion Factors

72


Transport Variables (Single Pass Case)gasifier_ra 2000 scfh typical syngas feed rate - from ACTI test dataSV 884.19206 hr-1 space velocity (based on syngas @ S.T.P.)Q0 121.57028 ft3 hr-1 initial gas volumetric rate at 500 psig and 500 °Fug0 0.119435 ft s-1 initial gas superficial velocity @ 500 psig and 500 °FQz 63.398902 ft3/hr final gas volumetric rate - corrected for gas contraction ugz 0.0622853 ft s-1 final gas superficial velocity - corrected for gas contractionug_ave 0.0908602 ft/s average gas superficial velocity with gas contraction

mu_L 0.022 g/cm-s estimated liquid viscosity - uncorrected for catalyst solidsrho_L 0.77 g/cm3 estimated liquid density - uncorrected for catalyst solidsnu_L 0.0285714 ft2/s estimated kinematic viscosity mu_L/rho_LDiffH_L 0.00054 cm2/s hydrogen liquid diffusivitysigma_L 0.0168253 gram-forcestimated gas-liquid surface tensiong_accel 980 cm/s accelleration of gravity/gravitational constantd_reac 18.288 cm reactor diameter in centimeterskla_H 0.7169656 s-1 mass transfer coefficient = 2.01*(d_reactor)^0.17*(epsilon_g)^1.1

uncorrected for catalyst solidssolids_corr 0.75 typical FT slurry mass transfer coef. correction for catalyst solidskla_H_corr 0.5377242 s-1 corrected slurry mass transfer coefficient for H2

Transport Variables (Recycle Case)

rec_Q0 855.20862 ft3/hr initial gas volumetric rate at 500 psig and 100 °Frec_ug0 0.8401874 ft s-1 initial gas superficial velocity @ 500 psig and 100 °Frec_Qz 1397.3914 ft3/hr final gas volumetric rate - corrected for temp rise and gas contraction rec_ugz 1.3728471 ft s-1

rec_ug_av 1.1065173 ft/s average gas superficial velocity

GAS-LIQUID MASS TRANSPORT

final gas superficial velocity - corrected for temp rise and gas contraction

73


GAS-LIQUID MASS TRANSPORT

LIQUID-SOLID MASS TRANSPORT

CatDiameter

cm

Thielemodulus

0.05 0.11450260.1 0.2290053

0.15 0.34350790.2 0.4580105

0.25 0.57251320.3 0.6870158

0.35 0.80151850.4 0.9160211

0.45 1.0305237

Thiele Modulus vs. FT Catalyst Diameter

0

0.2

0.4

0.6

0.8

1

1.2

1.4

0 0.1 0.2 0.3 0.4 0.5

Catalyst Diameter (cm)

Thie

le M

odul

us

reaction controlling

reaction + pore diffusion controlling

74


Heat Transfer Surface Required to Remove Heat of Reaction from Recycle Stream

CW_T_in 80 °F Cooling water temperatureCW_DT 12 °F Allowable water temp riseeffluent_in 500 °F Hot reactor gas into exchangereffluent_out 100 °F Cooled gas leaving exchangerDT_hot 432 °F exchanger "hot side" delta TDT_cold 20 °F exchanger "cold side" delta TLMTD 134.0843 °F exchanger log mean temp diff

U_overall 15 Btu/hr-ft2-F Overall HT coef for cooling gasHT_area 73.39909 ft2 required surface area for exchanger

assume HE-4 is primarily responsible for this load

HEAT TRANSFER

75


APPENDIX F AC RONYMS AND ABBREVIATIONS

76



77


Acronyms and AbbreviationsACTI American Combustion Technologies IncorporatedDOD Department of DefenseDOE Department of EnergyDPPH Dry Pound per HourDTPD Dry Ton Per DayFT Fischer-Tropsch Synthesis ProcessHE-X Heat ExchangerPSIA Pounds per Square Inch AbsolutePSIG Pounds per Square Inch GaugeQA/QC Quality Assurance and Quality ControlREII Renewable Energy Institute International RETC Renewable Energy Testing CenterSOP Standard Operating ProcedureSRM Standard Reference MaterialWBS Work Breakdown Structure

Acronyms for Process Flow DiagramsB-X BlowerCP-X CompressorCV-X Control ValveE-X Fabricated EquipmentHV-X Hand ValveH-X Fired HeaterM-X Electric MotorP-X PumpV-X Process Vessel

acti gasification to liquid fuel system

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