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Patented Apr. 23, 1963 3,086,932 ice Patented Apr. 23, 1963 2 and increases of the proportion of higher polyphenyls 3,086,932 PROCESS FOR PRODUtIiNG A RECOVERENG is an undesirable tendency. This is true as well for other ORGANIC NUCLEAR REACTOR COOLANT hydrocarbons, e.g., partially hydrogenated or alkylated MODERATGRS polyphenyls. Robert 0. Bolt, San Rafael, and William W. West, El The present invention is predicated on the discovery Cerrito, Cali?, assignors, by mesne assignments, to the that catalytic hydrogenolysis of ‘di?erent polyphenyls United States of America as represented by the United produces a marked reversion or conversion of higher States Atomic Energy Commission molecular weight constituents of aromatic and especially No Drawing. Filed Nov. 3%, 1959, Ser. No. 856,321 polyphenyl mixtures having undesirable characteristics 3 Claims. (Cl. Zita-493.2) 10 into lower molecular weight mixtures of more useful and The present invention relates, in general, to the pro desirable coolant-moderator types. Most unexpectedly duction and recovery of polyphenyl coolants from in hydrogenolysis, i.e., ring cleavage occurs with little ring tractable polyphenyl tars or residues and, more particu hydrogenation which might have been expected. Thus, larly, to the treatment of intractable, insoluble tarry resi highly damaged reactor coolant-moderator materials may dues obtained from coolants or moderators employed in 15 be reconditioned or various component fractions thereof nuclear reactors for conversion into useful moderator separated and treated to provide a material which is coolant products. highly satisfactory for reuse in the reactor. Varieties of aromatic hydrocarbons have been utilized Accordingly, it is an object of the present invention or have been proposed or investigated for use as coolants to provide a method for reconditioning coolant-moderator or moderators in nuclear reactors including polyphenyls, materials for use in a nuclear reactor. I aromatic condensed ring compounds, aromatic ethers and Another object of the invention is to employ a catalytic alkylated aromatic hydrocarbons. Polyphenyl hydro hydrogenolysis treatment for converting higher molecular carbons, especially biphenyl, the terphenyls and the qua weight reactor coolant-moderators into more desirable terphenyls are suitable for such use due to superior radio coolant~moderators. lytic and pyrolytic resistance and other requisite proper 25 Still another object of the invention is to provide a ties as disclosed in the ‘copending application of Rep method of converting high molecular weight intractable pino J. Fontana et al., S.N. 599,352, ?led July 23, 1956, tarry components of aromatic hydrocarbon coolant now abandoned. Ordinarily, mixtures of a ?uid nature moderators into coolant types suitable for use in a nuclear or low melting point solids corresponding to lower aver reactor. age molecular weights or eutectic mixtures are preferred. A further object of the invention is to employ a cat Upon long continued use in the high temperature intense alytic hydrogenolysis treatment for reconditioning poly radiation environment of the reactor the organic mixtures phenyl moderator-coolants for use in a nuclear reactor. show increases in viscosity with higher molecular weight Other objects and features of the invention will be materials being formed therein. Eventually, insoluble come apparent by consideration of the following de high molecular weight materials may form which ma- tailed description. terials precipitate to plug reactor passages and create a The present invention contemplates the treatment of hazard to further operation of the reactor. Accordingly, aromatic hydrocarbon mixtures employed as coolants and in conventional practice the mixture employed in the re moderators or higher molecular weight fractions obtained actor is periodically replaced or reconditioned by sep 40 therefrom by distillation, extraction, selective precipita arating the tarry constituents by distillation, precipitation, tion, etc. The process is especially applicable to the extraction, etc. The tarry residues obtained in such re treatment of polyphenyl mixtures such as the damaged conditioning operations represent an expensive loss of the biphenyl-terphenyl coolant-moderator employed, e.g., in coolant or moderator material and the indicated changes the OMRE and to other mixtures including, initially, bi of composition of the coolant lead to greater pumping 45 phenyl, terphenyls and quaterphenyls. Usually such in cost, lower heat transfer as well as other higher oper itial mixtures are ?uid or have a low melting point and ating costs for such a reactor. may comprise a considerable proportion of biphenyl with Nuclear reactors employing organic moderators and terphenyl and quaterphenyls or eutectic mixtures. Alkyl coolants are well known in the art. A reactor employing ated biphenyl, terphenyls and minor amounts of quater biphenyl as a moderator is disclosed in vU.S. Patent No. 50 phenyls may likewise be employed. For the purposes of 2,708,656, issued May 17, 1955, to E. Fermi et al. The the invention, a radiation ‘damaged mixture is one that use of organic liquids as coolants is also disclosed in has a higher average molecular Weight or undesirable Chapter 8 of “Principles of Nuclear Reactor Engineer- _ amounts of high molecular compounds and evidencing ing,” Glasstone, Van Nostrand Co., Inc., 1955. A bibli~ variously higher insoluble tar content, higher viscosity, ography of publications relating to such reactors is pre 55 melting point, etc. Certain polyphenyl synthesis meth sented in “Selected Abstracts on the Use of Organic Ma ods may produce mixtures of too high a molecular weight terials as Reactor Moderator-Coolants,” G. Naish and which mixture may likewise be treated. A damaged re— .R. W. Bowring, AERE Report inf/Bib 105. Moreover, actor or coolant material of the character described may biphenyl-terphenyl mixtures have successfully been uti comprise discarded material, a bypass stream obtained lized in the OMRE (organic moderated reactor experi 60 from a reactor coolant system, residues obtained by selec ment). C.f. “Details of OMRE” Nucleonics, vol. 14, tive separation from a reactor coolant circuit, or the like. No. 5, page 22, May 1956. In accordance with the invention such a material is The reactions which occur upon radiolytic pyrolysis of V subjected to a hydrogenolysis treatment wherein a sub the initial coolant-moderator mixtures are complex but stantial portion of the higher molecular weight compo generally tend to increase molecular weight, e.g., by con 65 nents are converted into lower molecular weight com verting lower polyphenyls to higher, polymerizing or com ponents such as biphenyl, terphenyl and alkylated deriva tives thereof which constitute superior reactor coolant bining unsaturated radiolysis products, etc., to progres moderator types. With source materials not originally sively produce a less desirable coolant and tinally a too severely damaged the reaction product, after ?ltering material which is not suitable for further use and which 70 and ‘being separated from gaseous or low-boiling compo must be replaced. Any substantial change such as re nents, is reintroduced into the operating reactor as recon duction of the proportion of lower molecular polyphenyls ditioned material. With highly damaged materials, such 3,086,982 xii as the insoluble, intractable tarry residues the reaction cate ring cleavage which eitectively divides high molecu product may be fractionated, e.g., in distillation or lar piolyphenyls to provide the desired lower molecular vacuum distillation apparatus and the recovered lower coolant-moderator compounds. It will be understood molecular weight, components may be used as makeup from the foregoing that if the original mixture includes moderator-coolant or otherwise admixed with other com- 5 polyphenyls of a higher molecular Weight than terphenyl, ponents to provide moderator-coolants as in conventional e.g., quaterphenyls, et seq., a general lowering of molecu practice. la-r weight will be obtained with substantial amounts of In the hydrogenolysis treatment the damaged coolant- biphenyl and ter-phenyl being produced. Such mixtures moderator mixture is contacted with hydrogen in the would correspond or could be easily blended to corre presence of a hydrogenolysis catalyst under high pres- 10 spond to the superior coolant-moderators disclosed in sure and at elevated temperatures in appropriate batch the aforesaid copending application of Fontana et a1. or continuous flow high pressure equipment of conven- and publications supra. Hydrogenated polyphenyls tional design. Generally speaking, it is contemplated that which are produced under indicated conditions are less so-ca,11ed “acid” cracking and mild hydnogenation cata- desirable compounds since radiation damage resistance is lysts are effective in producing hydrogenolysis of higher 15 lower. polyphenyls. More speci?cally A1203 (alumina) and Further details will be presented in the following certain mixtures of A1203 with CuO have been so em— speci?c example illustrating the manner of operating the ployed. Suitable operating conditions are presented in process ‘of the invention: Table I, infra. EXAMPLE TABLE I 20 Standardized amounts of terphenyl representative of higher molecular weight polyphenyls were reacted with Conditions Bmad range Preferred range hydrogen under high pressure ‘and at an elevated tem 0 perature with various combinations of cracking and hy Timerhmns-?o-------------- -- 01-8-0
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