ML19323B680

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Advances in Fluorocarbon Process for Decontamination of Nuclear Facility Off-Gas, Presented at 1979 Annual MRS Meeting
ML19323B680
Person / Time
Site: Crane 
Issue date: 11/27/1979
From: Kanak B
UNION CARBIDE CORP.
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ML19323B642 List:
References
RTR-NUREG-0662, RTR-NUREG-662 NUDOCS 8005140066
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.. t,., ;g. u a ADVANCES IN 'IEE F11KROCARBON PROCESS FOR DECNTAMINATION OF NUCLEAR FACILITY OFF-GAS I.'. B. E. Kanak To Be Presented At The 1979 Annual M.R.S. Meeting i Session F2 f November 27-30, 1979 g Boston, Massachusetts {- 6 l By acceptance of this article, the publisher and/or recipient acknowledges l the U. S. Government's right to retain a nonexclusive royalty license in { and to any copyright covering this paper. Oak Ridge Gaseous Diffusion Plant

  • Union Carbide Corporation, Nuclear Division l

Oak Ridge, Tennessee

  • Cperated for the U. S. Department of Energy by Union Carbide Corporation,.

Nuclear Division, under contract W-7405 eng 26. e i - ~., -

1 4 1 ADVANCES IN THE FLUOR 0 CARBON PROCESS FOR DECONTAMINATION OF IL" LEAR EACILITY OFF-GASES

  • l B. E. Kanak Union Carbide - Nuclear Division Oak Ridge, Tennessee INTRODUCTION The Nuclear Division of Union Carbide is responsible for the development of the fluorocarbon-based selective absorption process for removing noble gas fission products, carbon-14, and other radio-active contaminants f' ram the gaseous vastes of nuclear facilities.

3 In order to accomplish the duel objectives of component removal and subsequent concentration, the process utilizes three operations: absorption, fractional stripping, and final stripping. Each of these performs a separation by exploiting the solubility differences be-tween the various off-gas components in the process solvent, di-chlorodifluoromethane (R-12). The performance and reliability of the process have been demonstrated on an engineering scale with 10 years l of pilot plant operation at the Oak Ridge Gaseous Diffusion Plant 85 133

1317, (ORGDP) which included extended testing with Kr, Xe, and I, and Removal efficiencies of greater than 99.99% for Xe, CO.

2 2 CH 1, greater than 99.9% for Kr and H O and greater than 99% for NO 3 2 2 and N 0 have been experimentally obtained. With a feed stream con-2 taining 150 ppm of noble gas, a 97% noble gas product has been achieved. In addition to demonstrating the required removal effi-ciencies, the process has shown a remarkable tolerance for many of the normally troublesome off-gas components and does not rely upon elaborate feed pre-treatment steps. Recent work has led to a major flow scheme simplification, reducing the three-colu=n process to a single patented column. A third generation pilot plant facility c= ploying this new concept has successfully undergone initial testing

  • This document is based on work performed at the Oak Ridge Gaseous Diffusion Plant operated by Union Carbide Corporation under contract W-705 eng 26 with the U. S. Department of Energy.

3 ' yy9 ' ~, 2 this last year at ORGDP. s BACKGROUND Throughout its history, the fluorocarbon development effort has i. addressed of f-gas applications in almost every aspect of the nuclear l ). fuel cycle. Steinberg originally suggested using R-12 as a solvent in a three-column process to selectively absorb Kr and Xe from the g gaseous wastes of a reprocessing plant in 1959. In 1966, a pilot y plant was constructed and a development effort was initiated at ORGDP U to establish the general feasibility of the fluorocarbon process. At that time, the work was aimed at the development of a mobile proces-l sing system which could be transported to the site of a hypothetical reactor within 24 hours of a fuel failure accident and recover the noble gases and other volatile radionuclides released to the contain-ment vessel. As envisioned, all of the recovery equipment was to be 2 5 situated in a series of trailer trucks. Unfortunately, with res- "f pect to the Three Mile Island incident, this work did not proceed ) past the conceptual design stage. O In J 970 the program emphasis shif ted to the routine cleanup of LWR off-gases, and the fluorocarbon process was subsequently offered 3 i commercially for LWR application'. Based on the demonstrated operability and performance of the ORGDP pilot plant, process safety considerations, and in particular, the lack of any required feed pre-treatment, the fluorocarbon process was adapted for reprocessirs plant applications in 1971. A second generation pilot plant f acility was built at ORGDP in 1972 which off ered greater flexibility and the more sophisticated analytical 5 equipment necessary for detailed component analysis. This facility demonstrated that in addition to providing Kr and Xe removal, the fluorocarbon process could effectively be utilized to contain carbon-14 as CO, various nitrogen oxides, elemental and organic iodine, and 2 water. Rigorous process models and scale-up studies 6,7,8 were com-pleted to allow the confident design and optimization of a full-scale facility. These works laid the groundwork for the construction of the single column process in 1978. The concept of the fluorocarbon process as a mobile emergency reactor off-gas decontamination system has recently been revived in the wake of the Three Mile Island incident and is undergoing review by responsible persons in the industry. It would be possible to have a' mobile unit ready for deployment within three to four years. h

- - ~s v ,, $, c w. 4 M u ^n ' OQi%N fy .' ~ %\\ 4 c'o f-l' t; s , i 3' 1 PROCESS BASIS .o Fluorocarbon solvents have been identified as a valuable and somewhat unique group of solvents unusually suited for separating a number of industrially important components from various gas mix-tures9.lD. Steinberg selected R-12 for noble gas removal primarily because of its capacity, separation factor, and thermal and radi-l ation stability, as well as process safety and economic features. The physical properties of R-12 are well known. The basic thermo- ,i dynamic properties are detailed by Mr. Harness, et al.ll Distribution coefficients for several of the off-gas components of interest are shown in Figure 1. A substantial amount of equili-brium data now exists for krypton and xenon in R-12 solution. The initial work was performed by Steinberg at Brookhaven National Laboratory. Later work was reported from the University of Tokyo by Yamamoto and Takeda12 The most recent data are given by Shaffer at l3 Merriman utilized several techniques based on Hildebrand's ORNL regular solution theory to estimate krypton and xenon equilibrium I4 coefficients All investigators show good agreement. i 1 Toth, et al.,15 recently completed a laboratory study to define the behavior of other nuclear fuel reprocessing plant off-gar com-ponents such as CO, NO 1, and CH I. While 12 was found to be 2 2 2 3 fairly soluble in R-12, CH 1, NO2, and CO2 were found to be totally 3 t miscible in the temperature range of interest. Distribution coeffi-cients were also determined for these species. Beyond this work, l4 some estimated solubility relationships have also been given 1 ~ PROCESS DESCRIPTION I l Figure 2 is a schematic of the selective absorption process as it was originally conceived. The main separation of radioactive con-taminants from the bulk gas is eff ected in the absorber. The inter-mediate or fractional stripper serves to remove the coabsorbed car-rier gas f rom the solvent, thereby enriching the remaining dissolved gas in the more soluble components. The final stripper removes all the remaining gas from the process solvent for collection and regenerates the solvent for recycle back to the absorber. The ab-sorption step is carried out in a packed column only, while both stripping operations are performed in packed columns with reboilers and overhead condensers. In addition, the intermediate stripper e iH"cludes a flash drum. Typically, the absorber is operated at 100 psig, the intermediate stripper at 50 psig, and the final stripper at about 18 psig. Support equipment items for the basic process include a feed gas heat exchanger, process gas compressor, solvent cooler, storage tanks, and several refrigeration compressors. If the feed gas contains significant quantities of high boiling r _a _ _n:

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I *f - y ; - s, ; 1. m.*:. ,.J7Afy >:.. L' .,,, ; " M '. l ,5 3 .r-j DECONTAMINATED VENT GAS fy A VOLATILE SOLUSLE T CowoN ENTs xi. Co. x.. r.a r s b SOLVENT l j RECOVERY a 3 cAS 4 RECYCLE e E J E 5 C iE e e r SOLVENT g RECYCLE y y U as z 8 ~~ E %d HIGH BOILING M + CONTAMINATED COMPONE NTS* FEED GAS 1.CH 1,NO2 2 3 2 ________r { HO y i - - - - - g -~ Figure 2 SCHEMATIC OF THREE-COLUMN SELECTIVE ABSORPTION PROCESS 1 s 1.- I. fDe W -- -= Q g ... ? n p - 4.,e ~ ...~ e ?. .a 3, ga.

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w.- - , ?.yg p[,, jg,; q '., .^ s f f p7 e 6 components such ss H 0, I, CH 1, or NO, a solvent purification 2 2 3 2 still is available as an in-line option to prevent these materials from accumulating in the recirculating solvent. A solvent recovery system is necessary to remove solvent vapor from the process off-gas. Figure 3 is a photograph of the second generation ORGDP pilot plant. Detailed engineering drawings and descriptions of this facility are available elsewhere16, g Nj In the course of operation and analysis of this facility, a $l soluble gas peak was observed in the fractional stripper. It was j: found that this phenomenon, caused by gross internal condensation of the upflowing stripping vapor 6, could be controlled and the mag- ? nitude of the peak could be increased dramatically. It became appar-l' ent that if sufficient etripping stages were provided below the con-densation zone, the final stripper could be eliminated with the pro-duct being collected as a side-stream. Furthermore, it also seemed i feasible to place the intermediate stripper directly below the absor-ber and operate the entire assembly at a common pressure. Subse-quently, a column was designed that combined the three functional steps of absorption, fractional stripping, and final stripping into l7 one continuous contactor Figure 4 is a schematic of this piece of equipment. Decontaminated off-gas flows from the top of the combi-nation column and regenerated solvent is pulled from the bottom. The a I fission product gases are collected as a side-stream. The combina-tion column requires substantially less equipment and control instru-l mentation than the conventional flow sheet, and because of its sim- ) plicity, it offers numerous operational, reliability, and economic advantages. Due to the great potential and design uncertainties, a combination column was built and installed at ORGDP for evaluation. Figure 5 is a photograph of the column taken during construction. I The column is approximately 24 feet tall and has the same flow ca-l pacity as the three-column development facility. The absorption and j intermediate sections are 3 inches in diameter, while the final j stripper section has a diameter of 6 inches. High efficiency wire j mesh packing is used throughout. Pilot plant tests have shown that l scale-up on the column area is direct with this packing if well 7 designed gas and liquid distributors are employed. Hence, larger equipment utilizing the same packing material can be designed with confidence. The combination column has aeen undergoing performance evalu-ation for almost 1 year. These tests not only established the over-all feasibility of the concept, but showed conclusively that the combination colu=n can perform essentially as well as the three-column process. On the basis of a one-to-one comparison of the two options, the combination column has recently been selected as the preferred version for future applications. --im,-- ____m__ N e

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e. 8 REFERENCES 1. Steinberg, M., The Recovery of Fission Product Xe and Kr by Absorption Processes, USDOE Report BNL-542, Brookhaven National Laboratory, Long Island, New York (1959). 2. Merrtman, J. R., A A'cbile Processing Unit for Erypton-Xenon Absorption, USDOE Report K-L-2397, Oak Ridge, Tennessee (1967). 3. Stephenson, M. J., Merrican, J. R., and Dunthorn, D. I., Appli-cation of the Selective Absorption Process to the Removal of Kr and Xe from Reactor Off-Gas, USDOE Report K-L-6288, Oak Ridge, Tennessee (1972). 4. Griffith, G., "92% Cleanup of Nuclear Gaseous Wastes", Power Engineering A':rch, 62 (1973). 5. S tephenson, M. J., and Eby, R. S., Development of the FASTER Pro-cess for Removir.; Erypton-95, Carbon-14, and Other Contaminants from the Off-G:s of Fuel Reprocessing Plants, USDOE Report K-GD-1398, Oak Ridge, Tennessee (197 6). 6. Stephenson, M. J., Av. clysis of a Fractional Gas Stripper, USDOE Report K-1895, Oak Ridge, Tennessee (1978). 7. Kanak, B. E., Analycis of a Gas Absorption Column with Soluble Carrier Gas and 7:22:ile Solvent, USDOE Report K-2007, Oak Ridge, Tennessee (1979). 8. Vood, D. E., A"'*;~'iity Analysis of the Freon Absorption System for Cycat ng t.;;sents fr m Reprocessors, USDOE Report ORNL-TN-5797, Oak Ridge, Tennessee (1977). 9. Merrican, J. R., Pashley, J. H., Stephenson, M. J., and Dunthorn, D. I., Process for the Separation of Components from Gas Mia-tures, U. S. Fatent 3,762,133 (1973). 10. Merriman, J. R., Pashley, J. H., Stephenson, M. J., and Dunthorn, D. T., Removal of ?wified Helium or Hydrogen from Gas Niatures, U. S. Patent 3,735,120 (I L ). 11. McHarness, R. C., Eiseman, B. J., and Martin, J. J., " Freon-12", Refrigeration En;ineering, 32 (September 1955).85Kr in Some Or-12.

Yamamoto, Y.,

and Takeda, H., " Solubility of ganic Solvents", . ?::. Eng. U. Tokyo, A-7, 44 (1970). 13. Shaf f er, J. H., S'..ockley, W. E., and Green, C. E., The Solubility of Erypton and Xen:v. at Infinite Dilution in Dichlorodifluorome-th2ne, USDOE Report ORNL-TM-6652, Oak Ridge, Tennessee (1978). 14. Merrt:an, J. R., ~he Solubility of Gases in CC2 F : A Critical 12 Revdeu, USDOE Rep:ot KY.-G-400, Paducah, Kentucky (1977). 15. Toth, L. M., Bell, J. T., and Fuller, D. W., Chemical and ?hyeical Reh: ice af Some Contaminants in the R-12 Off-Gas Process: An In er~ - Report, USDOE Report ORNL-TM-6484, Oak Ridge, Tenneseee (1978). 16. Stephenson, M. J., Eby, R. S., and Muffstetler, V. C., ORGDP Selsative Ahz:ry:icn Pilo: Plant for Decontadnation of Puel Repr;;cssing Ftr.:.~.ff-hs, USDOE Report K-1876, Oak Ridge, Tennessee (1977). 17. Stephenson, M. J., and Eby, R. S., Cas Absorption Process, U. S. Patent 4,129,425 (1978). . - = - - yp y, ., y _., _ : m

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