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Recovery of Valuable Chlorosilane Intermediates by a Novel Waste Conversion Process

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Recovery of Valuable Chlorosilane Intermediates by a Novel Waste Conversion Process DOFJAW99566-1 (DE98 ) RECOVERY OF VALUABLE CHLOROSILANE INTERMEDIATES BY A NOVEL WASTE CONVERSION PROCESS Technical Report for Phase IIIA (Final) and Phase IIIB (Progress) BY Kurt E. Anderson October 1998 Work Performed Under Contract No. DE-FC04-94AL99566 For U.S. Department of Energy Office of Industrial Technologies Washington, DC BY Dow Corning Corporation Midland, Michigan DISCLAIMER This report was prepared as an account of work sponsored by an agency of ihe Unlted States Government. Neither the United States Government nor any agency thereof. nor any of their employees. makes any wamqty, express or implied. or assumes any legal liability or responsi- bility for the accuracy, completeness, or usefulness of any information. apparatus. product. or proccssdisc1ostd.orrepresents that its use wouldnot infringe privately ownednghis. 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DoUAU99566-1 (DE98 ) obbibutkn cdgory UC-1414 RECOVERY OF VALUABLE CHLOROSILANE MTERMEDIATES BY A NOVEL WASTE CONVERSION PROCESS Technical Report Phase IIIA (Final) and Phase IIIB (Progress) bY Kurt E. Anderson October 1998 Work Performed Under Contract No. DE-FC04-94AL99566 Prepared for US. Department of Energy Office of Industrial Technologies Washington, DC 20585 Prepared by Dow Coming Corporation P.Q. Box 994 Midfand, Michigan 48686-0994 ABSTUCT From July 1994 through May 1998, direct process residue (DPR)hydrogenalpis bas been studied in the laboratory, at a small Pilot Plant, and finaflyat a larger Pilot Plant within Dow Coming's Carrollton, Kentucky plant. The system reacts filtmd DPR with monomer at high temperaturr and pressure. The process demonstrates DPR conversion up to 86%. The reaction product contains high concentrations of valuable monomen such as dimethyldichiorosilane and methyldichlorosilane. A b*er DPR hydrogenolysis reactor based OR these mutts is being designed for operation in mpeat Dow Corning's Barry, Wales site. PREFACE The objective of this Dow coming Corporation and DOE cost-shared project is to develop a novel wasre conversion process for the recovery of valuable chlorosilane intermediates. The project started with Phase IIIA, Engineering development - Intermediate Scale, which consists of testing with two systems, termed the Pilot Plant and Pilot Plant 11, both atCarrollton ,KY. All of Phase IlIA is described in this report. Phase IIIB, Engineering Development - Full Scale, is the development of the commercial system at Bany, Wales. The first year of that development is described in this repon Fitlafly, Base IV, Demonsnation - Full Scale, which will not start until the development is completed., will complete the project. ACKNOWLEDGMENTS Brian Volintim is the Program Manager for the DOW Office of Industrial Technologies. Ken Lucien is the Technical Manager for the DOW Alwueque Operations Office. Frank Childs the Project Technical Monitor, is on the staff of Scientech, Inc. (Idaho Falls, Idaho). Steve Freebume is Manager of the Silicon Methyl Intermediates department for Dow Corning Corporation. Ben Franklin is a Contracts Specialin in the Federal Business and Contract Development Department of Dow Coming Corporation. Darrell Whiteley and J. Ashley Brinson were past Principal Investigators. Work slrpportcd by the U.S. lDepSltmnt of Energy, Assistant seuetsy for Energy Efficiencyand Renewable Ene%y,offictofIndustrialT~es,rmdaDoEAIbuquerqneoperatiollsOf6ceCooperative Agreemnt DE-FC04-94AL99566. 1 TABLE OF CONTENTS 1. INTRODUCTION .....- .__U......... ".- ......... .-... .....--. I 1.1 THE DPR PROBLEM ......................................................................................................................................... I 1. 2 PAST EFFORTS.................................................................................................................................................. I I .2 . I Literame Prior to 1990 ............................................................................................................................ i 1.2.2 Prior Dow Corning Eflwts with DPR Hya+ogenolysis .............................................................................. 2 1.3 DESCrUPliON OF PROCESSES ............................................................................................................................. 4 1.3. I Pilot Plant .................................................................................................................................................. 4 1.3.2 Md$ations to Pilot Plant Prior to St~t-up........................................................................................... 5 1.3.3 P~wessDescription Of Pilot Plant I1 ........................................................................................................ 6 I .3.4 Pilot Plant I1 DPR Filtration ..................................................................................................................... 7 I .3.5 Modifications To Pilot Plant I1 During Start.Up ....................................................................................... 9 I .4 FIRE AM) EXPLOSION SAFWST~DY ............................................................................................................. 11 1.41 Prmess Scenarios .................................................................................................................................... 11 I .4.2 Fire Scenarios.......................................................................................................................................... 1 1 1-43Explosion Scenarios ................................................................................................................................. 11 1.4.4 Conclusions From TkSt.. ................................................................................................................... 11 . 1.4-5 Recommendations .................................................................................................................................... 12 2. RESULTS AND DISCUSSION .... ...................................... ........ .................... ..--....................................... 13 _ 2 .1 CHRONOLOGY OF EXPERIMENTS..................................................................................................................... 13 2. I .1 I995 Experiments .Pilot Plant ................................................................................................................ 13 2.1.2 1996 Experiments .Pilot Plant ................................................................................................................ 14 2. I .3 I 997 Experiments .Pilot Plant I1 ............................................................................................................ 15 2.1.4 1998 fiperimen~~.Pilot Plant I1 ............................................................................................................ 17 2.2 MATERIAL BALANCES..................................................................................................................................... 17 2.2. I Pilot Plant Data handing........................................................................................................................ 17 2.2.2 Reactor Conversion ................................................................................................................................. 18 2.2.3 Eviknce of an inductionperiod .............................................................................................................. 20 2.2.4 Pilot P1an1 Filter ...................................................................................................................................... 22 2.2.5 Pilot Piant II Filter Lksigmd fiperiment ..............................................................................................
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