ML20010H734

Catalytic Combustion Hydrogen in Presence of Methyl Iodide, Final Rept

ML20010H734
Person / Time
Site:	Sequoyah
Issue date:	08/31/1981
From:	Shaun Anderson, Pessagno S ACUREX CORP.
To:
Shared Package
ML20010H730	List: ML20010H729 ML20010H731 ML20010H734
References
FR-81-87-EE, NUDOCS 8109290243
Download: ML20010H734 (58)

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{{#Wiki_filter:. c APPENDIX B e ACUREX FINAL REPORT FR-81-87/EE CATALYTIC COMBUSTION OF HYDROGEN IN THE PRESENCE OF METHYL IODIDE r August 1981 Acurex Project 9302 For American Electric Power, New York, New York Duke Power Co., Charlotte, North Carolina Tennessee Valley Authority, Knoxville, Tennessee By S. J. Anderson and S. L. Pessagno ( Acurex Corporation Energy & Environmental Division 485 Clyde Avenue Mountain View, California 94042 ( l l t t 8109290243 810922 PDR ADOCK 05000327 R PDR

I TABLE OF CONTENTS ( Section P_a2' 1 INTRODUCTION........................ 1 3 2 TEST FACILITY....................... 3 EXPERIMENTAL RSULTS 11 11 3.1 Approach 3.2 Results 12 3.2.1 Catalyst Performance.............. 12 3.2.2 Catalyst Deactivation by CH I 13 3 30 3.3 Summary REFERENCES......................... 32 ( APPENDIX A -- COMBUSTION EFFICIENCY 33 APPENDIX B -- TIME / TEMPERATURE RELATIONSHIPS........ 36 APPENDIX C -- ADIABATIC FLAME TEMPERATURE 54 i { ( i iii +- --.,,n-... -, --r- .,e

LIST OF FIGURES Pai' Number 4 1 Experimental Test Facility Schematic............. 5 Mixing Pozzle/ Fuel Injector.................. 2 7 1 Catalyst Reactor Assembly with Refractory and Guard Heater.. 3 l 9 4 1/2-Inch Pitot Tube Design.................. 14 5 Fuel-Lean Catalyst Activity................. 15 6 Catalyst Combustion Efficiency.... '............ 7 Extrapolated Temperature / Time Relationship During CH I 3 17 Deactivation......................... 18 CH 1 Deactivation Phenomena................. 8 3 24 9 Catalyst Pr essure Drop.................... 25 10 Catalyst Pressure Drop............ 26 11 Catalyst Life Versus Surface Temperature........... 27 12 Catalyst Life Versus CH I Concentration 3 LIST OF TABLES 20 1 Test Summary......................... 22 2 Surface Area and Dispersion Results IV i i _,..-,e..

1 SECTION 1 INTRODUCTION Ihe accident at TMI-2 demonstrated that hydrogen generation rates greater than originally considered in nuclear power station designs can occur. j As a result, concerns over the impact of increased hydrogen generation rates on nuclear station safety have been raised. To address the issue of increased hydrogen generation, Acurex conceptualized a hydrogen mitigation system utiliz-ing a monolithic substrate catalyst to burn lean hydrogen mixtures in a con-trolled manner. Since monolithic catalysts have not been evaluated as hydrogen combustors American Electric Power, Duke Power, and TVA jointly funded a pro-gram to evaluate the operating characteristics of a catalytic combustor using various hydrogen mixtures. This report presents the results of this program. Monolithic substrate catalysts, as opposed to packed bed catalysts, can operate at very high mass throughputs and combustion efficiencies with low pressure drop. This high throughput capability, coupled with very broad flamability limits, makes monolithic catalysts attractive candidates for H2 combustors. Noble metal catalytic combustors can operate at temperatures up to 2300*F without loss of structural integrity or catalyst activity, i Although catalytic H combustion and poison deactivation have been 2 atudied by Southern Nuclear Engineering (References 1, 2) for pellet bed configurations, monolithic reactors have not been evaluated as H combustors 2 for the gaseous input conditions of 1cw temperature (ambient to 200*F), high water concentrations, and the possible presence of CH I Poison. This study 3 presents the performance characteristics of monolithic catalytic combustors using catalysts provided by UOP, Inc. and Acurex Corporation. Catalyst operation was investigated during two test series: --r w,- ,-r. ~ n..

e Catalyst performance Catalyst deactivation by CH I 3 o Catalyst performance tests investigated minimum lightoff temperature, mass throughput capability, and combustion efficiency over a broad range of H 2 compositions and at high water concentrations. Catalyst deactivation by gaseous CH I was investigated to determine catalyst life over a broad range 3 compositions. Procedures required to regen-of CH 1 concentrations and H2 3 erate deactivated catalytic reactors were also evaluated. l l l l I 2 1 l ~-

O e' g, SECTION 2 TEST FACILITY An experimental test facility was designed and fabricated to evaluate hydrogen combustion using monolithic catalysts. In an effort to simulate gas ( mixtures that could be present during a LOCA, the catalytic combustion chamber was fabricated to homogeneously mix air, H, steam, and gaseous poisons. The 2 system was capable of flowrates from 12 to 40 scfm and gas preheat temperatures t from ambient to 1000*F. The high flowrate capacity of the catalytic combustor was designed on the basis of a rapid post-LOCA clean-up. Figure 1 presents a schematic of the test facility including fuel injector, combustion chamber, steam generator, control console, and emissions monitoring instrinents. Each 'of these components is described below. ' Fuel Injector / Mixing Nozzle A gas mixing nozzle was designed to homogeneously mix a multiple compo'nent gas stream consistina of air, steam, H, and N /CH 1. De five-way 2 2 3 nozzle, pictured in Figure 2, was optimized for flows of 40 to 150 ft/sec (1-inch diameter catalyst) and constructed of black pipe fittings. The main body was ported in four places 90* apart around the periphery and at 45' apart while H and N /CH 1 entered through a 1/4-inch stainless steel pipe 2 2 3 located at the axial centerline with the tip positioned at the intersection of the air / steam jets. Combustion Chamber / Catalyst Reactor The combustion chamber, Figure 1, shows the five 1-inch by 1-inch catalyst segments mounted in a castable refractory housing. A guard heater, 3 I

4 4 i Flowmeter Flow control Hester/ controller Himing valve Regulator

"rggyvn]

Air TC >-' - < Steam TC "g Preheat ' A

Superheater/

i TC Pressure tap controller p, ( [ 1 Combustion

Guard f. eater cha h r Flow control t'h*"'t I

valves .i 4' Exhaust ik wpled Y Rotameters ..$*IYSE Y Y ~g p ) o Pmssum Steam ,l, ,p generator Pressurt 4 J regulators Heatedg i sample a n i Q 1) t) b fir-Hg Ol 1/N Quarts 3 g viewport TC input supply fuel 1 V -,.e l w m l Q tWata 9 { [gh Pay Tenen trap flowmeter CH 1 r 3 it Impingers Hl/12 H2 G.C. cond oner TC = thermocouple Figure 1. Experimental test facility schematic. l

.s t i TOP VIEW Air l l l l COWLETE IIDZZLE ASSEf8LY T---- r---- 7 0--- 1/4 6 lg l ____ g 4---- 1/4"to1/2"TT{c' -EE-I connector 'o Steet Steam I ~ l O: 'g g I j r I 1" to 1/2" I g, l SIDE VIEW "S l 43 -O-N (4)1/2" lept 1.2I=2-5/8" YQ::h,,re,' couple l 1/4" stainless 2 senzzle ) ( steel - adjust Weld around manifold to position 1 a. N 's e circumference below air / steam 1" seeT couple

'-Er=-

r = lb ~ b 1" mixing 6 I ~' ~ tube,, %= Injection 1 i 1" W T existing existing slots l l stxing tube , M# i l 4l Figure 2. Mixing nozzle / fuel injector. m + c m m

a controlled ' y a variable voltage source, held the com!Mtion chamber near the adiabatic condition during testing. A 24-inch long, 1-inch diameter mixing zone between the combustion chamber and the gas injector was used to insure Pressure ports complete fuel / air mixing prior to entering the catalyst. l located fore and aft of the combustion chamber measured the differential pres-sure drop across the catalyst reactor. The first catalyst screened, and subsequently used for all tests, was l a noble metal, UOP #4103 fine cell monolith. It was initially selected on activity at low preheat gas temperatures. Due to the basis of known high H2 activity, a graded cell monolith configuration was not the catalyst's high H2 (Graded cells are used to increase mass throughput for catalysts of needed. relatively 1cw activity or with hydrocarbon fuels ) The reactor assembly con-sisted of five 1-inch long by 1-inch diameter segments stacked on top of each other as seen in Figure 3. activity and low preheat temperature operation, In addition to high H2 facility and operating limitations were considered prior to catalyst selec-An existing combustion facility compatible with the 1-inch x 1-inch tion. UOP reactor was used to minimize facility capital costs and accelerate initial This facility was also used for the remaining catalyst pel-screening tests. soning test series. The dominant factor which detennined catalyst size was Increasing the diameter of the catalyst from 1 to 2 inches re-fuel costs. fl wrate. quires a fourfold increase in the H2 Catalyst temperature was measured by four Type K thermocouples that were potted in ceramic cement and attached directly to the catalyst cell wall. l Figure 3 shows the thermocouples positioned at the top, middle, and bottom segments of the reactor centerline. The middle catalyst segment had an extra side-mounted thermocouple to measure the radial temper m re pi ~ as. Thermo-l couples located 3 inches above the catalyst and 3 inches-below measured the An Acurex preheat and exhaust temperatures within the combustion facility. Autodata 9 data 1cgger automatically recorded the operating temperatures. 6

O + TC = thermocouple Figure 3. Catalyst reactor assembly with refractory and guard heater.

Steam Generation A Chromalcx CES-24 (72 lb/hr) steam generator was cperated in series A Jordan Mark 60 with Sylvania gas heaters to pro: luce superheated steam. pressure regulator regulated the steam to 10 psig and a Chromalox temperature Two co'ntroller maintained the steam at 300'F upon entry to the gas injector. pitot tubes,1/2-inch and 3/4-inch diameter, were used to measure steam flow-These were fabricated at Acurext off-the-shelf items were not capable rate. of measuring the low mass flowrates encountered daring testing. Figure 4 The shws a diagram of the 1/2-inch Acurex-built stainless steel pitot tube. end of er.ch pitnt tube (1-1/4-inch stainless steel plugs) was tapered from the existing 1-irch diameter supply steam line to their respective diameters in order to mininize pressure drop and turbulence. Also, to suppress turbu-lence, an L/d of 15 was maintained between the inlet convergence and the pitot tube probe. Contro: ConsoTe, and N /CH I flowrates were measured and metered at the control Air, E 2 3 2 console shown in Figure 1. All gaseous flows were measured by Fischer & Porter Both precalibrateo rotameters and subsequently delivered to the mixing r;zzle. and N /CH I gases were introduced to the fuel injector at ambient conditions. H 2 3 2 The air supply was preheated by Sylvania gas heaters and the temperature was regulated by a Chromalox controller to values dictated by the operating points of the test mai.rix. _CH31 Preparation Conventional low flowrate rotameters were ensatisfactory for measuring CH I as a liquid (liquid at room temperature, BP = 110'F) at the low concen-3 trations needed for testing. Even gasecus CH 1 (vaporized) could not be intro-3 duced at sufficiently low flowrates with rotameters. However, gas flowrates 8

( ( Static L/D = 15 e pressere g-tap ':,"::,' "lg ' N,, i If 1/2" i n ~ -,

]

Tap red exit Tapered entrance 1/16 diameter probe Stagnation t pressure tap l e l r Figure 4. 1/2-inch pitot tube design. 9 _~ ~ -.. _ -... -.. _ - _, _ - _. - _.. -. -. - _ -...... _

Gas could be raised to measurable levels by diluting the CH I with N. 3 2 at 150 psig were prepared cylinders containing 2.4.21ume percent CH I in N2 3 by AIRCO Gas Products Company. At this concentration, the partial pressure of CH I is well below its saturation vapor pressure, thereby insuring that the 3 does not CH 1 remained gaseous throughout testing. It should be noted that N2 3 affect catalyst activity or combustion. Lower CH I concentrations were achieved by expending the contents of 3 the original gas cylir. der to ambient pressure and refilling it back to 150 psig This dilution, approximately 121 to 1 (when done twice), yielded with N. 2 about 0.02 percent CH 1 by volume in N. Before and after each dilution, the. 3 2 bottle was rolled for about 30 minutes to insure good mixing. To verify the contents of the bottle, samples were per cdically analyzed by the Acurex Chem-istry Lab. Emissions Bench Combustion efficiency and catalyst performance was determined t,y emissions. A Carle Model 3500 gas chromatograph measured H2 measuring H2 in the exhaust that was dried by a TECO GC-1 gas conditioner. The fate of the CH I poison was evaluated by measuring CH I, HI, and 3 3 A Tenex trap was used to collect CH I samples while an acid / 1 emissions. 3 2base impinger train absorbed HI and I. HI and 1 absorbed in the impingers 2 2 were measured by ion electrodes. i e 10 1 ~. _,_ _.. - - - ~. _,.., _ _ _.. _... _ - -.. -. _ _. _ _. -. _. -.. -, _ _ -. ~

P SECTION 3 EXPERIMENTAL RESULTS 3.1 APPROACH I The program goal was to evaluate the performance of noble metal mono-lithic catalysts with H in the presence of CH 1. Catalytic combustion can 2 3 extend the lean flammability limits of H2 (<!;wn to 1 percent H ) and can 2 initiate combustion passively without external heating. A monolithic con-figuration was selected on the basis of its high combustion efficiency at high mass throughput and low pressure drop. Interest in conditions that might be expected in a LOCA focused catalyst testing to preheat temperatures between 72*F and 340*F, and steam concentrations from dry to saturated conditions. Methyl iodide (CH 1) was chosen as the test poison because it might be 3 prese;st during a LOCA and was shown by other investigators (Reference 2) to h2ve a pronounced effect on catalyst performance. Initially a 2 x 2 matrix of test conditions was conceini to examine the effect of CH I on catalyst perfonnance at two H e ncentiati o s (5 and 3 2 10 percent) and two steam concentrations (0 and 60 percent). However, initial testing showed rapid catalyst deactivation at CH I concentrations of about 3 20 ppm. As a result, the original test matrix was revised to determine which parameters, H or CH I concentrations, were more dominant on catalyst deactive-2 3 I tion. Four separate UGP #4103 fine cell segment catalysts were evaluated at a variety of air, steam H, and CH I flowrates and concentrations. The 2 3 11 . _ _,. _. _ _ _ _. _ _ ~.

total gas preheat temperature was held at ambiet conditions during testing As documented by Southern Nuclear Engineering (SNE) (Refer-anc lightoff. ences 1, 2) and substantiated by the results of our testing, increased gas preheat temperatures enhance the perfonnance and lightoff characteristics of noble metal catalysts. Therefore, the catalyst tests conducted at ambient conditions are considered conservative. Exceptions to these test points were those of high water concentration, where preheat determines the amount of water, as saturated vapor, allowed in the total mixture. For example,10 percent water by volume under saturated steam conditions corresponds to a gas temperature of about 170*F. For comparative purposes, an Ac' heavily loaded platinum cat 31yst was tested under similar conditions to s.iat of UOP's to determine loading effects on life and perfonnance. Due to UOP's proprietary policy, the amcunt of loading on their catalysts was not known. The Acurex catalyst was heavily loaded with platinum to 6 percent by weight. The culmination of all tests resulted in the following operating points, listed by their maximum and minimum values: e H concentrations, 5 to 10 volume percent 2 Steam concentrations, O to 40 volume percent e Preheat temperatures, 70'F to 340*F e CH I concentrations, 0.07 to 20 ppm e 3 e Total flowrates,12.5 to 40 edm 3.2 RESULTS 3.2.1 Catalyst Perfonnance Preliminary testing of the noble metal UOP #4103 catalyst demonstrated The low temperature lightoff and extremely high mass throughput capability. ~ 12

I catalyst reactor, as pictured in F.igure 3, achieved lightoff at H2 c(ncentra-tions as low as 1.5 percent by volume and face velocities (velocity of uncom-bustedgasstreamatcatalystentrance)upto140ft/sec. Figure 5 shows the results of these tests. Packed bed catalysts, though adequate H2 combustors, have very high pressuredropsathighvelocities(References 1,2). A packed bed catalyst-would required a much larger volume tnan the monolithic catalyst to maintain the high mass throughput used in these tests. For reference, a 24-inch diam-eter monolith resctor operating at 140 ft/sec can cor.;ume the contents of an 6 3 i ice condenser containment vessel (1.25 x 10 ft ) in less than 1 hour. l As shown in Figure 6 high combustion efficiency is maintained even though H2 concentrations are well below conventional lean flamability limit j operation. Note that combustion efficiency of 100 percent is achieved at H2 concentrations above 4 percent. Again, comparing the results of SNE's packed bed catalyst tests to the monolithic catalyst tests, we note marked diff ences in performance. The UOP #4103 catalysts maintain combustion efficitncies of 99 plus percent while packed bed combustion typica'ly operates around 90 per-cent. The efficiency values quoted for both systems, nonoliths and packed beds, are hased on the difference between the measured combusbon temperature and the-adiabatic flame temperature. As an alt, ative, combustion efficier.cy can be i determined by measuring uncombusted hydrogen in the catalyst exilaust (see Fig-ures 8, A-1, and A-2) using a gas chromatograph. Although calculating effi-l ciency based on emissions can be more accurate than using temperature,.the ' long sampling time of the gas analyzer significantly lengthens the test pro-I cedure. To expedite testing, the efficiency data shown in Figure 6 was calcu-lated based on temperature. 3.2.2 Catalyst Deactivation by CH3J, Deactivation Phenomena Deactivation of catalyst segments progressed from front to rear of the reactor assembly until combustion tenninated. 7eis type of progressive 13

160 g 1.30 'o l l x ~ ~~ 1.21 p x kz 140 'u 1.12 5 j b I 1.03 T, 120 l 3 l 0 0.94 c ^ x 8 0.85 ]o. y 100 I Apparent 3 cutoff 0.76 t line xU 80 - 8 "c 60 = Successful operation x Unsuccessful operation 40 20 - i I I i 1 e 0 1 2 3 4 5 ~6 H by y lume (percent) 2 Figure 5. Fuel-lean catalyst activity. 14

100 O ( 90 Ambient air No preheat 80 O 70 E O E

g. 60 O

36 scfm total flow (110 ft/sec) W3 50 3 O 45 sefm total flow (140 ft/sec) te g 40 z Ej 30 i Lean hmit 20 10 l 1 1 I I I I i 1 0 1 2 3 4 5 6 7 H byvolume(percent) 2 l Figure 6. Catalyst combustion efficiency. l 15 ~

( deactivation, as opposed to the slow overall decline in catalyst activity reported by SNE, was verified by monitoring the temperature of three of the five catalyst segments which sequentially declined from a temperature greater As the reaction than the flame temperature to the preheat gas temperature. fiont proceeded, temperature / time relationships such as those pictured in represent arbitrary time intervals at Figure 7 developed..t, t, and t3 j 2 which point the reaction front might be located. Figure 7 is an extrapola-This tion of what was typically seen as the reactor assembly deactivated. type of temperature / time relationship indicates that the combustion of H 2 with air is essentially complete within a narrow reaction zone and the re-mainder of the catalyst assembly is heated only by the exhaust gases. The temperature / time profiles show surface temperatures which exceed values predicted by adiabatic conditions. Due to the substantial difference in hydrogen and oxygen gas diffusivities, surface combustion actually occurs This observation at a richer fuel / air ratic than bulk gas concentrations. is consistent with temperature excursions identified by L. Louis Hegedus (Reference.3). Figure 8 shows an actual temperature versus time profile for 20 ppm CH I (a vulue 200 times greater than the concentrations recomended by Reg. 3 As shown, the bulk gas tm;.erature at time test. Guide 1.4), 10 percent H2 zero is at the adiabatic flame temperature (TAD). As time proceeds, seg-ment #1 slowly increases above TAD, then falls off rapidly to the preheat As the reaction front proceeds down the catalyst, the next l temperature. and similarly drops to ambient preheat segment (#2) slowly raises above TAD combustion is extinguished. i conditions as total deactivation occurs and H2 These results verify: (1) deactivation of catalysts due to CH 1 injection 3 occurs within a very is progressive, and (2) the complete oxidation of H2 Throughout testing, the deactivation rate for each narrow reaction front. This in-catalyst segment was consistent for the entire reactor assembly. formation is useful for detennining individual catalyst deactivation rates. I 16

e i l Thermocouple g placement g I g 4 l T i I s I 1 t t j 2 3 ^ TDIF I l. i e i l a 4 Bulk gas temperature i O yT AD D F l I l l i I l l I i i I i i I 3 2 3 4 5 Catalyst segment (flow direction to right) l l l Figure 7. Extrapolated temperature / time relationship during CH 1 deactivation. 3

I i 2500 Segment 1 20 ppm CH 1 N 3 M 77 ft/sec Segment 2 k 70"F preheat h i 1 0 % 11 \\ 2 2000 1 03 C 2 10 g = ----- L 1500 e el' e Miabatic ); flame - 7.5 5 E ~ 0 temperature +4* D l b c In 5 -f 5.0 2 50 T, E 1000 c j } t = c 1 -- 2.5 o 500 1 U I 4 Preheat temperature j j O _ 100 g l 0 0 10 20 30 40 50 60 70 80 Test time (minutes) 1 l j i' Figure 8. CH 1 deactivation phenomena. i 3 i 9 J ? i

Figure 8 also shows the concentration of H in the exhaust with the 2 corresponding combustion efficiency for the heavily doped CH I test. High 3 combustion efficiencies, much greater than 90 percent, were maintained through-ett testing until the catalyst was rendered completely inactive. This obser-vation is contrary to other invr:tigators (Reference 1) who report H2 conver-sion efficiencies of approximately 90 percent, prior to the introduction of CH I, and a steady decrease in efficiency down to 20 percent after poison 3 1 addition. Note that if no CH I is present (indicated by time = 0 on Figure 8), 3 the 99 percent plus efficiency enables monolithic catalysts to be a rapid cleanup device. An attempt was made to measure HI and I emissions from the catalyst 2 by absorbing each component in an acid / base impinger train and analyzing the resulting solution by ion electrodes. However, at the low CH 1 concentrations 3 encountered during testing, the selected measurement technique was not accurate enough to detect HI or I 2 below 150 ppmv. For future testing, alternate tech-niques must be devised to measure these species. i Two other tests were conducted measuring H in the exhaust: first, 2 where rapid deactivation occurred, and second, where, although the front seg-ment deactivated, no further catalyst deactivation cccurred in the remaining i segments. These results are presented in Appendix A. Test Results Table 1 shows the tabulated results of all the deactivation tests ( conducted during this program. Data are grouped generally on the basis of different reactors, 1 through 4, which, coincident.lly, corresponds to orders of magnitude changes in CH 1 concentrations. Catalysts 1 through 4 are UOP 3 l

1. 4103 reactors, while ACU represents the Acurex heavily loaded platinum reac-tor. During these tests. H2 concentrations were varied to investigate its affect on the deactivation phenomena. Percent H, preheat temperature, pres-i 2

sure drop, CH 1 concentration, and segment deactivation time are included 3 in the table. Based on this information, Individual segment deactivation 19 i \\

i TABLE 1. TEST

SUMMARY

i 1 Deactivation Face Pressure Bed Time Flowrate Test H Preheat CH I Velocity-Drop Point 2 3 Temperature per Segment

• i

(%) (*F) (ppm) (*F) (hrs) (acfm) (ft/sec) (psi) } 1. 5 70 9.8 750 0.02 25 77 1.05 1.A 7.6/6.9 340 9.8/9.7 1300 0.37 37.7 117 1.72 1.B 10 70 19.6 1510 0.20 25 77 1.0 l 2 2.A 5 70 0.37 750 0.13 25 77 2.8 8.16 70 0.8 1260 2.37 25 77 1.4 3.A 5 70 0.23 750 0.37 25 77 3.B 8 70 0.33 1250 7.0 25 77 1.3 E! 3.C 6.5 70 0.27 950 1.60 25 77 4.A 8 w/s** 168 0.33 950 1.22 25 77 1.0 ] 4.8 5 70 0.07 750 0.67 12.5 39 0.4 12.5 39 0.43 4 4.C 6.5 70 0.07 950 = 25 77 0.47 = 4.0 6.5 w/s** 162 0.025 1050 5 ACU S 70 0.09 750 0.01 25 77 1 i j

• Segment = 1-inch length of monolith I
  • w/s - with steam i

k

rates were calculated as a function of H and CH I concentrations. Appendix B 2 3 contains the temperature / time relationship curves that were used to generate Table 1. Inspection of Table 1 reveals that an individual segment deactivation 2 and 0.33 ppm CH I (tes.t point 3.8). time of 7 hours occurred at 8 percent H 3 j Under virtually the same H concentrations but over twice the CH 1 concentra-2 3 tion (test point 2.B). Table 1 shows a segment life of only 2.4 hours. Simi-larly, comparing test point 3.B to 3.C we can see that a slight reduction in 2 (to 6.5 percent) but identical CH I concentration reduces segment life H 3 from 7.0 to 1.6 hours. These results indicate that CH 1 deactivation is 3 l strongly affected by both CH 1 and H2 concentrations. Tests were conducted 3 at ambient preheat and 25 acfm (77 ft/sec). l Limited high preheat testing was conducted because increased tempera-l tures tend to reduce deactivation rates. This decrease in deactivation with increased temperature was seen in our regeneration procedure (explained in the following section) and also by SNE. Steam addition was examined for two separate cases: 162*F and 168'F preheat temperatures. Both points were at saturation conditions, correspond-ing to approximately 40 percent steam by volume. Surface area and dispersion measurements were performed pre-and post-test on the UOP catalysts. Due to similarities in the data, only catalysts 1, 2, and 3 were completely evaluated. Test results are shown in Table 2, In all cases, there was a significant reduction in both active surface area and t dispersion. As discussed earlier, catalyst surface temperatures as high as 2400*F were encountered -- 900*F higher than values predicted based on adia-batic conditions. At these temperatures, noble metal agglomeration can occur as indicated by low dispersion values. These results agree with the UOP surface analysis using a scanning electron microscope (SEM) which found sig-nificant metal agglomeration on catalyst rear segments, but only limited l i 21

i 1 TABLE 2. SURFACE AREA AND DISPERSION RESULTS i Pre-Test Post-Test Hours Dispersion Surf ce Area' Dispersion Tested i Catalyst. Weight SurJfceArea (pmol /g) { /ge) (pmol /g) N-(gm) ( /gm) i 1 38.53 21.75 11.59 0.11 0 5 l 2 38.18 20.38 12.93 4.37 0.42 10 3 39.45 19.07 10.35 7.00 0 18 i i i i i 1 i i s j t i

agglomeration on front segments. The high steam content of the bulk gas downstream of the main reaction zone will expedite the agglomeration process, and thus increased agglomeration at the rear units is expected. UOP also analyzed the catalyst suface for iodide using an EDX microprobe. Iodide was I no't found in any locat?on at the instrument's detectable limits (0.5 weight percent). During testing, pressure drop in the reactor never exceeded 1.5 psi for gas flows of 25 scfm (77 ft/sec). Values listed in Table 1 are the averaged pressure drops seen during testing. These results agree with cal-culated pressure drop. Catalyst pressure drop data as a function of test time during deactivation for two experiments can be seen in Figures 9 and 10. As shown, pressure drop was a maximum prior to CH I addition (at 3 stable combustion) and slowly decreased as deactivation of catalyst segments proceeded through the reactor. This is easily explained by fluid mechanics. Wha the reaction front is at the beginr.ing of the reactor assembly, hot ex-haust gases at correspondingly high velocities must traverse the remaining four segments before exiting. Since pressure drop is proportional to length, combustor pressure drop decreases as the reaction zone (high velocity gases) proceeds down the length of the reactor. Therefore, pressure drop is a func-tion of total reactor length and the position of the reaction front during the deactivation phenomena. Figures 11 and 12 show the results of eight tests conducted at 25 scfm (97 ft/sec) and 70*F preheat. Figure 11 shows individual segment (1 inch x 1 inch) life in r,ours versus ncminal surface temperature at constant CH I 3 concentration holding H concentration constant. Here again, catalyst life 2 was normalized to a 1-inch long segment. As shown, the number of test points was limited. Consequently, lines drawn through data taken at 10 and 20 ppm CH 1 assume trends similar to results obtained at 0.28 and 0.60 ppm CH 1. 3 3 concentration can be directly For these tests (70',F preheat and no steam), H2 23 i l _ _ _. ~, _. ~ _. _.,.. _ _ _ _, _.. _. _,. _.. __.

S J 4 3 2 1 0 0 0 0 4 4%AgT _= 3 I y eru t 3 I a C r T m e p p o m r e d t e s r a u g c ss k e l r u B s p r t 2 u I o s H y w 2 l C a T ta C 9 er ug i F 8 4 t a t e I 1 n h m emf io rpc p pps 2 aHF75 a700. 2 t D5701 \\- )C T k q 0 0 8 7 0 0 0 0 5 0 0 5 1 1 C* E32gEy m* i ; 'i! ,j .l i i I I a 1

T 4 Data point 4.A Q i 8% H2 4 40% steam h 0.33 ppm CH I k 3 1500 TC2 25 scfm ~ TC) i i I 5 1000 TC4 . Bulk gas temperature 1.0 5-

== e ~m f - 0.75 i B i = _. _ _ i o j 500 - 0.50 % i - 0.25 I I I 0 0 1 2 3 'f Test time (hours) 1 Figure 10. -Catalyst pressure drop. 'l e i

s, 10 9 4 8 ~ 7 1 6 5 e Dry s 0 40% H20 6 4 0.33 ppm CH 1 3 ? .$ 2 2: E I 1 x 0.9 N N 0.8 C. 0.7 6 dj {0.6 g gf 35 p .e/ 0 s 3 0.4 o' g hl 0.3 ) / Of ,1 0.2 1 I e I I I I 0.1 400 600 800 1000 1200 1400 16DO 1800 Surface temperature (*F) l t Figure 11. Catalyst life versus surface temperature. 26

I 100 80 T .J ( 60 Flow: 77 ft/sec h 40 - In et: 04 (M G Dry 7 20 E 40% H 0. 2 8% H2 j t ! 10 8 0 85 H ~ 2 4 O e g N 2 - y e 00 1 6.51 H 2 0.8 O.6 0.4 51 H 0.2 2 i i eil i i i l i i i 0*I 02 .04.06.0R.1 .2 4 .6.81 2 4 6 8 10 CH I concentration (ppm) 3 Figure 12. Catalyst life versus CH I concentration. i 3 27 l .. _. _. _..., _ = _ _.

l I estated :: react:r *.amce-sture. nese t=c ff;ures indf: ate catalys: itfe is '%s, an es:ccential fuccthe Of tctn H c:ncentn:1:n and G I ::ccen:nti:n. 3 c cercentratien is 'rcreased and/:r G I 3 1:nger catalys: If fe is acted as H2 t.1wited er a f ecicate tra if : e c ncentratf=n Of c ccen*rati:n is reduced. C4 I is vtey Icw 2ert :nay te 1 :netsecid limit wee-t ec icss cf activity 3 This a::arent trrest.cid is abcut C.I ;om CH I. Ex-3 cccurs in t e c:mcust:r. tra:clatha Of te data in Ff;ures 11 1-d 12 can te used t: ;redic* cauiys: Iffe. Aring steam : era:1:n, :ri:e :: C3 I additten, there was an ex:ected 3This d-:; w s ex:ected and A en-tre: fe tre ecmbal tulit gas ter:e-sture. dix C vtrifies 31s by c:7Jcaring dry :: satun*.ed adiata:1e fiame temceratures 00"C*HI"tt0"3" D' e#=* 1" ##"T ** 7 f:r varhus ;rt-eat temceratures and H2 temcerat:.rt nas the same affect On indivMr at caulyst Iffe as *:uld ne in-00"C'"I#3IIO"- II' tr:ductt:n =f an ice-t gas ce ccerating at a 1:wer F2 urts li and 12 shcw : at : e stemn ;cint (bcxed) agrees with amcient ;etaeat Ocints kdicating caulyst sur' ace temr in:u-t is : e dominant variatie tes: This ;cta: was cperated in caulyst life and nct tae ;rtsacce Of E d, ;e* se. g at I~3*F :rtheat and 25 ac#2. Tc dete-sine the influence f residence time (s:ece veiecity) en deactivathn rates, three Icw vel.3 city test ;cints (4.5 and 4.C) were c:n-1 ducted at 12.5 sc's (39 *:/sec). It was f:ced nat 1:=er flewra:es geaeraITy CC"C'"I#2*IO" II E'# '"II' ""IT* '"h'"CI"9 i fnniht: cautys life at 1:w H2 values (5.5 ;ercent). 5:ecific c nclusfens regarding ne life at higner M2 insufffcfen affect Of 1:w flewnte :n dear. fvati:n caract be dnwn cue :: T dau. The Acu*ex caulyst (AC) thcush heavily Iccded wita platinum ($ per-can: by set;nt), had ccr dis;ersi n due :: n;;laneratten af platican en the This resulted in :ccr caulytic activity durhg steady sta.e cos-substnte. bustian and ra:td deactivati:n with CH I additkn. Table I veriffes tese 3 resci:s. l l

Catalyst Regeneration After CHtt Deactivation Catalysts, deactivated after exposure to CH I, could be restored to 3 complete activiG ' regenerated) and used for further testing. Here regener-l ation refers to the process of restoring a partially or totally deactivated re' actor segment to its original combustion characteristics (i.e., combus-tion efficiency) achieved prior to CH I exposure. The reversibility of the 3 process indicates that CH 1 desctivation does not cause permanent loss of 3 catalyst activity. To quejitatively describe a typical regeneration process, the following three scenarios were observed. First, catalyst segments with low CH 1 exposure 3 time and segment temperature (downstream reactor segments which were the last to deactivate) were easily restored to full activity by simply stopping the CH I flow. Second, segments of longer exposure times (middle of catalyst 3 assembly) required only increased H2 concentration of typically 6 to 7 percent before restoring activity. Third, fronc segments exposed to CH I for sa m al 3 hours required H concentration greater than 10 percent and air preheat about 2 300'F.before regeneration occurred. concentration) The severity of conditions (elevated tempe 2ture and H2 required for regeneration refiects the degree of catalyst deactivation, Deactivation can be caused by two phenomena: (1)actuallossofactivecata-i lyst sites due to vaporization or agglomeration at high temperature, and (2) adsorption or chemical reaction of poison species with active sites. The former mechanism is irreversible and can occur at high temperature in the absence of a poison, while the latter is generally reversita, permitting catalyst regeneration. The maximum recommended operating temperature of the UOP #4103 catalyst is 1800*F. As discuesed earlier, catelyst surface temperature of the reaction front exceeds the expected adiabatic bulk gas teoperature due to the high diffusivity of hydrogen relative to oxygen. In several cases, segments o'. 1 l l l 29

i the catalyst reactor experienced temperatures exceeding 1800'F and a corre-sponding loss of catalyst activity was noted by difficulty in achieving cata-However, the severity of deactivation depended significcntly lyst lightoff. Front on the duration of catalyst exposure to CH I at low temperatures. 3 segments, which extinguished first, were exposed to CH ! for a longer period 3 As than the remainder of the reactor assembly which continued to operate. expected, regeneration of the front segments required higher preheat tempera-concentration. In addition, reactors exposed to CH I f0" 10"9 3 ture and H2 periods of time were more difficult to regenerate than those which deactivated rapidly at high concentrations of CH I. This implies that CH 1 exposure time, 3 3 not concentration, is more influential on the regeneration process. Cycile deactivation and regeneration was performed on several of the Regeneration, catalysts tested with no apparent change in performance. typically conducted at 300*F and about 7 percent H, will restore catalyst p Regeneration assemblies to their original pretest combustion efficiency. typically required.2 to 10 minutes, depending on the extent of deactivation Though regeneration data are somewhat limited, of each reactor segment. combustion efficiencies can be reliably restored to greater than 90 percent after CH 1 deactivation. 3 3.3

SUMMARY

The UOF #4103 catalyst is a proven combustor with excellent possibili-ties to burn hydrogen during and after a LOCA. It is capable of combusting below cencentional lean flamability limits, down to 1.0 percent, and at H2 Tests were conducted at flowrates frnm 12.5 to very high mass throughputs. These conditions corre-40 scfm and preheat temperatures from 70'F to 340*F. spond to face velocities of 39 to 117 ft/sec. occurred w'. thin a narrow reaction zone. batalytic combustion of H2 Due to high catalyst activity, combustion efficiency remains high until Combustion efficiency of the deactivatioa of the total catalyst odurs. 30

00P #4103 catalyst is very high, about 99 percent, compared to conventional packed bed noble metal catalysts which typically operate around 90 percent. The U0P #4103 catalyst deactivated in the presence of CH ! at low 3 H concentrations and in a predictable (repeatable) manner. Deactivation 2 pkceeded sequentially down the length of the catalyst reactor. Combustion activity was maintained greater than 90 percent until the final catalyst segment totally deactivated. Deactivation depends ~ exponentially on CH 1 and H concentrations while 3 2 velocity effects are not fully understood. For example, at 5 percent H C0"~ i 2 centration, catalyst (1 inch by 1 inch segment) life varied from 8 minutes at 0.37 ppm CH 1 to 40 minutes at 0.07 ppin CH 1. At a CH I concentration of 3 3 3 0.28 ppm, catalyst life varied from 22 minutes at 5 percent H to 7 hours 2 at 8 percent H

• 2 Although experimental data was limited above 6.5 percent H2 concentra-tion, a threshold limit is indicated at 0.1 ppm CH I dopant value where cata-3 lyst life appears infinite. Additional testing is required to further define r

this limit. Because surface temperature depends linearly on H concentration, 2 catalyst life also varies expt,aentially with surface temperature. Addition of steam to the H / air mixtures lowers catalyst surface temperature by depress-2 ing the adiabatic flame temperature. As a result,, team addition reduced catalyst life. For example, steam addition at 0.3;l ppm CH I and 8 percent H 3 2 reduced catalyst life from 7 hours to 1.2 hours. 5 H lar trends were noted for changes in the gas preheat temperature. Elevating the gas preheat tem-perature lengthened catalyst life by increasing catalyst surface temperature. ( 5 31

i REFERENCES " Joint Utility Catalytic Hydrogen Recombiner Development Program " 1. Southern Nuclear Engineering, Final Report, Dunedin, Florida /Bethesda, Maryland, July 1971. Brown, G. M., Turner, S. E., Sawyer, C. T., " Joint Utility Catalytic Hydrogen 2. Recombiner Development Program " BWR & PWR Offgas System and Miscellaneous Recombiner Tests, Southern Nuclear Engineering, Dunedin, Florida /Bethesda, Maryland December 1971. Hegedus, L. Louis, " Temperature Excursions in Catalytic Monoliths," AIChE 3. Journal, Volume 21, No. 5. September 1975. ) 32

O f' APPENDIX A COMBUSTION EFFICIENCY t e f I r l 33 l l .n

i i I i t i 1500 l ) Poison Data Point 2. A ( l introduced 0.37 ppm CH 1 n-3 h 5.0% H2 I f 70*F preheat Q i I TC) _ 1000 uL Adiabatic flame temperature Og 5.0 g e l 3e i e a E b w 3 M w 500 e i -,ma--- 2.5 g 50 3 TC3 ~ r e i c TC2 C O 4 B i g 1 N z Preheat "b j O 70 -temperature* I I I O '00 0 0 10 20 30 40 50 l 2 Test time (minutes) Figure A-1. Combustion efficiency. i l s ss

2000 Data point 2.B.1 0.8 Ppm CH 1 3 8.16% H2 g 70*F preheat Qg i T 1500 TC) _f 8 -O g TC3 E + Adiabatic U 3 1000 8 flame 2 C temperature Y b E E S e u O E D u .e m -50 "o 4 a E C f.< t I 500 E c B ~ m Preheat 5 + 8 temperatureI 70 i i 0 _io0 l 0 1 2 3 4 Test time (hours) I ( Figure A-2. Combustion efficiency. i t

O O ) APPENDIX B TIME / TEMPERATURE RELATIONSHIPS ) ) 36

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9 t e APPENDIX C 3 ADIABATIC FLAME TEMPERATURE ') ) ) \\ 54

f j 1800 Effects of steam on g the adiabatic flame [ temperature of H2 1600 at 150'F preheat 1400 r C 1200 L ky t ( 3 2 1000 Saturated, '25.3% H O 2 by volume ( 800 3 $ 600 ( 2 400 l i. l 200 I I I I I I I I I I I 0 O 1 2 3 4 5 6 7 8 9 10 11 12 Mp byvolume(percent) Figure C-1. Adiabatic fla e temperature (dry versus 25.3% H O saturated). 2 55 L

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