Document Dvrm9zm6rwbN4xZOmM19z9j44

1*2.* RCV. 1*1*82 INTEROFFICE COMMUNICATION Ponca City, Oklahoma February 12, 1971 to: Mr. R. H. Gerlach, Westlake, Louisiana subject: PRELIMINARY DATA ON THE MASS SPEC-DISCLOSED R304 CATALYST SPECIES To confirm our telecon of February 8 on the R304 catalyst species, I am attaching herewith some of Mr. Mynard Hamming's preliminary mass spec data which are to be completed and presented later in a formal research report, as per his report No. 839-0-3-71 on oxychlorination catalyst species. These data are taken from the R304 catalyst samples obtained by Dr. Martin C. Hawley and myself, and will be a part of our turnaround analysis report as per the last two turnaround studies. We have never analyzed for these R304 catalyst species before, as this is the first time (November 6, 1970 turnaround) that we have had access to a sampling of R304. You may wish to consider the several process implications of these data prior to seeing Mynard's final report and our new turnaround study report. We have not tried to analyze these data, but plan to do so when all the present on-going R304 studies are complete. Also, by this preliminary data copy, we will ask Petrochemical Research for their mechanism interpre tations of these anhydride structure formations and chemistry. FJR-NP Attachments CC: CVF(2), FKte^MCH, KRG, HDB, LNV,<3WHTF, MCHam, GP, EAS F. J. Radd Senior Research Associate Central Research Division CC* 00008139 From Table 1 it can be noted that in going from succinic anhydride to phthalic anhydride (increasing number of double bonds in the hydrocarbon moiety) the concentration of anhydrides increases toward the bottom of the towe 1. (Not all samples have been examined.) It is also of interest to note that with the increase in concentration of anhydrides there is evidence of the anhydrides being converted to acids. The spectral evidence for acids is the appearance of the characteristic rearrangement peak of acids at m/e 88. The reaction of anhydrides with various hydrocarbons to form acids is a character istic reaction of anhydrides (acidolysis of anhydrides). Additional proof of these components is being obtained by accurate mass measure ments of several of the peaks on the mass spectra. Several chloroparaffin components have been detected. These are shown in Table 2. The concentration of the chloroparaffins decreased in going toward the bottom of the reactor. ecu O08l90 TABLE 1 TYPES OF ANHYDRIDES DETECTED General Formula and Structure Type CnH2n-23 R-C=0 ^ / R-C=0 Molecular Ion Peak m/e 130 Appearance Sample 54 (top of reactor) (low concentration) Type CnH2, n-4.03. R. -C\=0 I? R-C=0 Succinic anhydride -m--/-e-- 128 Sample 54 (low concentration) Type C nH2,, n-6,03, m/e 154 Sample 55 (low concentration) Ty"e CnH2,,-83 m/e 152 Samples 56 and 57 (increasing concentration) Type cnH2n_ 103 ^ C,,U2n-123 o-o /_ m/e 150 Sample 58 - r (increasing concentration) m/e 148 Sample 59 (increasing concentration) Phthalic anhydride ecu oooai9l TABLE 2 CHLOROPARAFFINS DETECTED IN SAMPLES Structure Molecular Ion Cl Cl \/ C=C / Cl \ Cl 164 Tetrachloroethylene H Cl N. / C=C / Cl \ Cl Trichloroethylene HH \/ C=C /\ Cl Cl Dichloroe thylene 96 HH \/ ,C=C /\ H Cl (?) These components are being checked by making accurate mass measurements. 000008192 CCR