sample="quota" bates="512473163" isource="rjr" decade="1980" class="ni" date="19890614" GREAT LAKES RESEARCH a division of HORSEHEAD INDUSTRIES, INC. P. O. BOX 1021 ELIZABETHTON, TENNESSEE 31643 (615) 543-3111 TO: L. A. Joo' - GLR FROM: K. D. Church 542-1739 CC: Glenn Creamer - RJR Ron Darling - GLR DATE: 6/14/89 Subject: Plant Test Carbonization of Cotton Liners in the GLC Mini-Rebaker at Niagra Fall, NY Re. P.O. No. 89-21635 (RJR) The purpose of this trip was to investigate the feasibility of using the mini-rebake furnace to carbonize the first cut cotton linters using standard 36"0 x 144" L electrode double saggers fitted with a lid and a continuous nitrogen purge. The six saggers were charged with a total of 5,114 pounds of cotton linters (three half-bales per sagger) with thermocouple placement as shown in Figure 1. The lids were put in place and tack-welded for transport. Nitrogen purge tubes were installed at the bottom of each sagger. The saggers were transported to the Niagra Falls plant and returned to GLR via a flatbed truck. The mini-rebake furnace is a circular, gas fired, furnace 122"0 x 155" H fitted with a water seal and an internal fan to circulate the furnace atmosphere. The furnace is equipped with an incinerator and the furnace pressure is controlled by a valve in the exhaust duct to the incinerator. The three double saggers were placed in the furnace as shown in Figure 2. The thermocouples and nitrogen lines were passed through an opening adjacent to the sagger No. 4 position and connected to a strip chart recorder and individual flowmeters for nitrogen supply. The saggers were purged at 200 SCFH per sagger for 16 hours prior to startup at 0800 on 5/17/89 at which time the flow was reduced to 100 SCFH during the upbeat phase of the run. A daily record of temperature readings was kept, Table I, as well as a continuous strip chart recording of the entire run (E) Mini Rebake (NF) firing curve during 991# The cooling time cycle has allowed the annual estimate for the mini-rebake to 2X to 100,000#. 6-8 months needed to build and bring a new furnace line - 2-3X 1 mini-rebake to take care of annual supplies of in-market brands). trip to Morganton w/ Ron Darling - July? Composite of sagger 2-6 for C, H, N, O in 2 wks coke proposed from Mr. to ABN requirements fulfilled (if CHNO are ok) and of 1989. Wouldnt need Earliest test market could be 4Q'90. Further side-up operation; i.e., relocation of furnace from NF to E and design of new system E are tabled. FCC data appear to be good (need to get SA approval?) VM 2X9 Jet & make rods During the upheat phase of the run the furnace pressure was maintained at approximately 0.5" H20 and during the cooling phase from atmospheric to 0.2" H20. The firing curve for the run is shown in Figure 3 (plotted from sagger No. 1 temperatures). Comparing Figure 3 and Figure 4 (the firing curve for the GLR furnace) two major differences are observable; (1) The upheat rate between 500°C and 650°C for the mini-rebaker is much slower (20 hours vs. 6 hours), and (2) the cooling time is considerably reduced (24 hours vs. 80 hours). The upheat rate was slowed because the one burner is inadequate (the furnace originally had two burners) for the desired rate and the cooling efficiency is the result of the internal circulation fan. Note that the furnace and saggers were allowed to cool for an extended period (64 hours) before the saggers were removed. When the required 650°C was reached in all saggers the nitrogen purge was increased to 200 SCFH and maintained at that level until the saggers were below 175°C then reduced to 150 SCFH and reduced to 100 SCFH at 55°C and kept at this rate until removal from the furnace. The nitrogen purge was maintained while the saggers were sealed and then the supply tubes were disconnected and sealed. A comparison of sagger volumes and nitrogen flows for the GLR furnace and the Niagra Falls furnace is shown in Table II. Table III is a detailed account of the unloading of the saggers at GLR. As noted there was a considerable amount of oxidation in saggers 2 and 6 and only sagger 1 showed no evidence of oxidation. The oxidation is probably the result of air infiltration during cooling and transport. The pattern of oxidation is shown in Figure 5 and photos of the oxidized material from sagger 2 are shown in Figures 6 and 7. An unusual burning pattern is shown in these photos. The air apparently infiltrated into the bale at a crack and oxidation began inside the bale leaving about a 1" outer shell and progressing to either end and down the sides of the bale leaving an unoxidized outershell and inner core. The char yield for this run is shown in Table IV. Included in this list are the 1/2 bale raw weight and resulting char weight, drum number as shipped and the respective sagger number. The overall yield of 24.7% was calculated on the basis of unoxidized material (suspect material not included). Samples were taken from top, middle and bottom bales in sagger No. 1 and submitted for the standard analysis and the FCC III analysis. Samples for VM, ash and moisture were taken from middle bales in saggers 3, 4 and 5 and from the bottom bale in saggers 2 and 6. These data are shown in Tables V and VI along with the average data from twelve GLR runs for comparison. Keith D. Church 1c Attachments formulaname Table III Cotton Linters Carbonization Niagra Falls Plant Test Mini-Rebaker Run 5/15-22/89 Sagger Unloading and Inspection Sagger #1 No evidence of oxidation, all bales look excellent. Sagger #2 Top Bale - Severely oxidized with outer shell of unoxidized material and core of unoxidized material (pictures). Middle Bale- Top half of bale severely oxidized with outer shell. Bottom Bale - No oxidation, looks good. Sagger #3 Top Bale - Partially oxidized, saved center section. Middle, Bottom Bales - No oxidation, look good. Sagger #4 Top Bale - Severely oxidized, began at the middle of the bale and progressed toward either end with a shell of unoxidized material. Bale caught fire upon removal from the sagger. Middle Bale - No internal oxidation, slight amount of ash from top bale. Bottom Bale - No oxidation, looks good. Sagger #5 Top Bale - Severely oxidized, began at the middle of the bale progressing toward both ends and down the sides leaving a shell of unoxidized material which was thinner at the point of ignition. Middle Bale, Bottom Bale - No oxidation, look good. Sagger #6 To Bale - Severely oxidized with shell of unoxidized material. Middle Bale - Still burning when removed from the sagger. Same pattern as previously described. Bottom Bale - No oxidation, looks good. This bale was sampled at the edge and center for ignition-in-air test. 7-25 Keith Church SA # is out 33 m2/g Composite sample for C, H, N & O for saggers 2-6