Bench Top Reaction System



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Parker Autoclave Engineers Bench Top Reaction System General Description Parker Autoclave Engineers BTRS - Jr is a complete reaction system for vapor phase catalyst evaluation and continuous flow process analysis. The reactant preparation portion is capable of handling up to four inputs. Two inputs can be high pressure liquid pumps. The reactants are passed through an optional mixer/vaporizer assembly for blending and creating a single homogeneous, non-pulsating stream to be fed to the reactor. Summary Reactor Temperature up to 1832º F (1000º C) System Pressure up to 4350 psi (300 bar) Reactor sizes of 5, 10, 20, 40, and 100 ml Oven Temperature of 482º F (250º C) Components located in Oven: mixer/vaporizer, reactor, sample valve, status valve, back pressure regulator body, pressure transducer isolator. Feed Lines: 1/8 bulkhead, 7 micron filter, metering valve, 3-way valve for vent or online porting, and reverse flow check valve. Compression fittings for stainless steel tubing with 1/8 OD and 1/16 ID 200-240 VAC, 50/60 Hz, single phase, 20 Amp service required Contact factory for custom configurations Applications Parker Autoclave Engineers BTRS - Jr is utilized in the Chemical, Petrochemical, Environmental, and Pharmaceutical Industries for: Hydrogenation, Liquid Waste Disposal, Fischer-Tropsch, Fermentation Environments, etc. Mixer Vaporizer Assembly System Controls Parker Autoclave Engineers BTRS - Jr facilitates tomorrows requirements for University and Research facilities the world over. Manual Back Pressure Regulator Optional Status Valve Instrumentation Products Division Autoclave Engineers Operation 8325 Hessinger Drive Erie, Pennsylvania 16509-4679 USA PH: 814-860-5700 FAX: 814-860-5811 www.autoclaveengineers.com 06-1121CE-1112 Fixed-Bed Tubular Reactor Optional Sampling Valve Reactor Oven Heater Bulk Head Connectors Mechanical Feed Controls The World Leading Provider of High Pressure Equipment for Research and Industry since 1945!

ISO-9001 Certified Parker Autoclave Engineers Bench Top Reaction Systems -Micro -BTRS Model BTRS - Jr Micro-Scale Bench Top Reaction Systems for Catalyst Research and Development Reaction Systems

Reaction Systems BTRS - Jr System Description The BTRS - Jr is a complete reaction system for vapor phase catalyst evaluation and continuous flow process analysis. The reactant preparation portion is capable of handling up to four inputs. Two inputs can be high pressure liquid pumps. The reactants are passed through an optional MIXER/VAPORIZER ASSEMBLY for blending and creation of a single homogeneous, non-pulsating stream to be fed to the reactor. The MANUAL FEED CONTROLS include high pressure metering valves, in-line filters, reverse-flow check valves, and a 3-way diverter valve. These valves permit on/off control and flow measurement of fluids prior to being directed into the system. These controls are mounted on the front panel of the reactor module. One thermostated, FIXED-BED TUBULAR REACTOR is provided with a single-zone heater controlled from the catalyst bed (process) thermocouple. The reactor and heater are mounted within an isothermal oven. A forced convection blower assembly provides heating for the oven. This totally heated environment ensures that undesirable condensation is minimized. This adds significantly to the performance and reproducibility achievable in a BTRS. The optional multi-port REACTOR STATUS VALVE can permit reactant bypass. This valve provides a convenient means of performing analytical sampling of the feed material. When the reactor is placed in the by-pass position, a high pressure, inert gas stream is activated to purge the reactor contents to a safe vent. Pressure measurement at the inlet of the reactor is performed via a MECHANICAL GAUGE ASSEMBLY. The gauge is isolated from the hostile reacting environment by a high pressure, silicone-filled isolator with a welded stainless steel diaphragm. Pressure is maintained by a manually-controlled, spring-loaded, BACK PRESSURE REGULATOR. Digital indication of pressure and closed-loop pressure control are also available as options. A heated multi-port, near zero dead-volume, SAMPLING VALVE can be provided for transfer of the vapor phase effluent from the system to a customer-supplied gas chromatograph. This valve is also located in the isothermal oven. An optional heated transfer line and carrier gas controls are provided for sample transfer to a customer supplied gas chromatograph. System control consists of three tunable PID controllers for temperature control of the reactor, oven, and transfer line. Also included are push-button switches to permit rotation of the multi-port reactor status and sampling valves. A rupture disc assembly is included as a standard feature to eliminate the risk of dangerous over pressurization. A multi-port reactor status valve allows purging of the reactor during a shutdown. Power is terminated to any heater station with a burned-out or open sensor via the individual temperature controller. BTRS - Jr Applications Chemical Hydrogenation Functional Group Modification Selective Oxidation Ammoxidation Isomerization Environmental Liquid Waste Disposal Total Oxidation Effluent Treatment Resource Conservation 2 Petrochemical Cracking Reforming Isomerization Fisher-Tropsch Food & Pharmaceutical Fermentation Supported-Enzyme Catalysis Hydrogenation

BTRS - Jr Product Specifications General SYSTEM RATINGS: System Pressure: 450 psi / 1450 psi / 2900 psi (31 Bar / 100 Bar / 200 Bar) (Recommended Maximum) Reactor Temperature: 650 C (1,202 F) Oven Temperature: 250 C (482 F) DIMENSIONS: Cabinet: 41 (105cm) Wide x 33 (82cm) Tall x 14 (35cm) Deep Oven: 12 (30cm) Wide x 24 (61cm) Tall x 8 (20cm) Deep POWER SUPPLY: 220 VAC, 50/60 Hz, 20 Amp service, single phase WETTED MATERIALS: 300 Series Stainless Steel, Teflon (PTFE), Kalrez, Nitronic 60, Vespel (polyimide), [Nickel alloy A-286] (A-286 is on the 20 & 40 ml 2,900 psi (200 Bar) models only) BULKHEAD CONNECTIONS: Compression fittings for stainless steel tubing with nominal 1/8 OD and 1/16 ID FILTER RATING: 7 Micron CHECK VALVES: O-ring seal design, 20 psi (1.4 Bar) cracking pressure METERING VALVES: 18 turn, 0.047 (1.19 mm) orifice, 1 stem,.010 Cv, micrometer handle BALL VALVES: 3-way, 180 actuation for directional flow switching and shut-off THERMOCOUPLES: Type K (Nickel-Chromium & Nickel - Aluminum) TUBING 1/8 OD x 1/16 ID 316 Stainless steel seamless tubing Teflon and Vespel are registered trademarks of Dupont Co., Wilmington DE Kalrez is a registered trademark of Dupont Dow Elastomer, Wilmington, DE Nitronic is a registered trademark of AK Steel Corporation, Middletown OH produced under license by Electralloy Div. of G.O. Carlson Inc., Oil City, PA Note: Parker Autoclave Engineers reserves the right to substitute an equivalent material for trademarked material. Parker Autoclave Engineers purchases substitute materials based on specification conformance, typically a widely accepted specification created by an industry standards organization. Feed Preparation Feed streams are provided for four (4) reactants, the purge gas, and the GC carrier gas. The purge gas feed controls are only supplied if the reactor status valve option is selected. The GC carrier gas feed controls are supplied only if the sample valve option is selected. Reactant Feed Lines: Includes bulk-head connectors, inlet filters, metering valve, 3-way ball valve, and a check valve. Purge / Feed Control: Includes bulk-head connectors, inlet filter, metering valve, 3-way ball valve, and a check valve. GC Carrier Control: Includes bulk-head connectors, inlet filter, and a 3-way ball valve. Oven Components Mixer/Vaporizer: Optional unit includes four (4) inlet filters, and four (4) 54 (137 cm) coils for pre-heating gas and vaporizing liquids. Pressure Gauge and Optional Transducer: Gauge: 2-1/2 diameter face, dual scale, psi and Bar. Pressure Transducer: Accuracy of +/-0.13% of full scale at constant temperature. Isolator: 316 SS, silicone oil filled Reactors: Select from 5, 10, 20, and 40-ml standard volumes. Includes inlet and outlet filters and full length internal thermowell. Volume Inner Diameter Outer Diameter Heated Length Heater 5 0.31 / 7.9mm 0.56 /14.3mm 6 /152.4mm 674 W 10 0.31 / 7.9mm 0.56 /14.3mm 12 /304.8mm 1,348 W 20 0.52 /13.1mm 0.75 /19.1mm 6 /152.4mm 674 W 40 0.52 /13.1mm 0.75 /19.1mm 12 /304.8mm 1,348 W Reactor Flow Direction: The standard tubing configuration creates downward flow, i.e. in the top and out the bottom, unless otherwise specified on the purchase order. Pre-bent tubing to produce the reverse reactor flow direction is included as loose parts with the unit. Trickle Feed Connection: The standard end fitting of the tube reactor is equipped with an unused (plugged) connection. It can be used for feeding ingredients directly to the reactor through a dedicated line (which creates the possibility of independent temperature control) and bypasses the mixer vaporizer assembly. Reactor Status Valve: Optional valve with 1/8 tube connections, 8 port, 2 position, air operated, push button activated, permits sampling of reactant feeds when used in combination with optional sampling valve. The reactor status valve is not available on 2,900 psi (200 Bar) models. Sample Valve: Optional Valve with 1/8 tube connections, 8 port, 2 position, air operated, push-button activated. Captures a 1 ml sample (standard) of product and sends it to a customer supplied Gas Chromatograph. Autoclave Engineers can easily fabricate sample loops between 0.75 and 3.0 ml if capturing an alternate sample size is desired. Back Pressure Regulator: Manually operated (standard) with optional automatic control. See table for control ranges. The customer is responsible to confirm the compatibility of process fluids (at operating temperatures) with the wetted components of the reactor. The polyimide (used in the multi-port valves and the back-pressure regulator) has good resistance to most hydrocarbons and chemicals at 250 C (482 F). Polyimide has limited resistance to primary amines, ammonia and live steam. Contact the factory to discuss materials and process alternatives for solving compatibility problems. 3

BTRS - Jr Product Specifications Product Handling Gas/Liquid Separator: The gas/liquid separator is located after the reactor and before the back pressure regulator. It includes a ball valve and metering valve for draining into a customer supplied collection tank. Volume: Cooling Coil: Manual Drain: 150 ml 1/4 Copper Tube Metering Valve and 1/4 Turn Ball Valve Heated Transfer Line: The heated transfer line connects the sample valve to a customer-supplied gas chromatograph (GC). It ensures a complete sample arrives at the GC by delivering it at elevated temperature to prevent any condensate formation. Length: 6 feet (1.83m) Inner Diameter: 0.027 (0.69mm) Max Temp: 300 C GC Adapter: Universal needle nut assembly including needles, septa, nut and ferrule to adapt to most GC s Control System Reactor Temperature: Reactor Wall Temperature: Optional Pressure Indicator/Controller: Optional GC Transfer Line: System Failsafe Alarms: Data Acquisition: Closed Loop Digital Controller with 8-segment ramp-soak. Over-Temperature Monitoring Digital Pressure Indication or Pressure Indicating Controller Closed Loop Digital Temperature Controller Over-temperature alarm to shut down all system heaters. Consult Factory for additional control options. Operating Pressure Ranges and Component Ratings Maximum Recommended Operating Pressure Gauge Range/ Transducer Range Maximum Allowable Working Pressure Back Pressure Regulator Range Rupture Disk Rating 450 psi (31 Bar) 600 psi / 42 Bar 500 psi / 35 Bar 500 psi @ 1,202 F (35 Bar @ 650 C) 5-500 psi (0.3-35 Bar) 500 psi (35 Bar) 1,450 psi (100 Bar) 2,000 psi / 138 Bar 3,000 psi / 207 Bar 1,600 psi @ 1,202 F (110 Bar @ 650 C) 10-1,500 psi (0.7-103 Bar) 1,600 psi (110 Bar) 2,900 psi (200 Bar) 5,000 psi / 345 Bar 3,000 psi / 207 Bar 3,200 psi @ 1,202 F (220 Bar @ 650 C) 25-4,000 psi (1.7-276 Bar) 3,144 psi (216 Bar) Parker Autoclave Engineers assembles the 1,450 psi (100 Bar) model from stock components for rapid delivery Nickel alloy A-286 is substituted for 316 Stainless Steel for the 20 ml or 40 ml reactors used in 2,900 psi (200 Bar) models. This change increases strength at high temperature. Also, the optional reactor status valve is not available on 2,900 psi (200 Bar) models. All other specifications remain unchanged. The listed rupture disk rating is nominal. The specification range is +6% and -3%. The listed rupture disk rating is nominal. The specification range is +1.5% and -0.75%. 4

BTRS - Jr General Arrangement BTRS - Jr Flow Schematic PRESSURE SENSOR RUPTURE DISK BACK PRESSURE REGULATOR FEED SYSTEM MIXER/VAPORIZER TE GAS/LIQUID SEPARATOR REACTOR STATUS VALVE TC TAHH TAD 1 2 3 8 4 7 6 5 1 2 SAMPLE VALVE 3 TE TY TC TAHH TAD HEATED TRANSFER LINE 8 4 7 6 5 TE TY TC TAHH TAD HEATED OVEN VENT 5

BTRS - Jr Product Ordering Information MODEL CODE: A Base BTRS - Jr 045 = 450 psi (31 Bar) 145 = 1,450 psi (100 Bar) 290 = 2,900 psi (200 Bar)+ BTRS-JR A - B - C - D - E - F - G - H - J BTRS-JR - - - - - - - - B Reactor Volumes 005 = 5 ml 010 = 10 ml 020 = 20 ml 040 = 40 ml C Mixer Vaporizer D Reactor Status Valve + E Pressure Monitoring and Control 0 = Analog Gauge / Manual Regulator 1 = Analog Gauge with Transducer and Digital Indicator / Manual Regulator 2 = Analog Gauge with Transducer / Automatic Regulator / Closed Loop Pressure Controller F Sample Valve G Heated Transfer Line H Gas/Liquid Separator (Manual) +Reactor Status Valve NOT Available for 2,900 psi (200 Bar) unit. For other pressure/temperature ranges, consult factory. Supporting Information J Control Options 1 = Discrete Controls Please refer to the following sections of the catalog for complimentary products and additional technical details. If your catalog is incomplete or out-of-date, feel free to register your name and download literature from Parker Autoclave Engineers website. A good starting point is http://www.autoclaveengineers.com to reach the main page of Parker Autoclave Engineers reactor products. High Pressure Micro-Metering Pumps - Ideal liquid metering pumps for low viscosity feeds to the BTRS Family. Customer Support Services - Details Parker Autoclave Engineers capabilities for start-up, training, and turnkey installation. The following Engineering Drawings are available upon request from Parker Autoclave Engineers for more detailed technical information. Drawing Number 40A-9009 BTRS-Jr Reactor Oven General Arrangement (illustrates 5 ml reactor and includes separator assembly) Drawing Number 40A-9010 BTRS-Jr Reactor Oven Process and Instrumentation Diagram Drawing Number 20C-0241 Reactor Assembly (5cc, 316 SS) Drawing Number 20C-2854 Reactor Assembly (10cc, 316 SS) Drawing Number 20C-2855 Reactor Assembly (20cc, 316 SS) Drawing Number 20C-2834 Reactor Assembly (40cc, 316 SS) Drawing Number 20C-2760 Reactor Assembly (20cc, A-286/316 SS) Drawing Number 20C-2856 Reactor Assembly (40cc, A-286/316 SS) WARNING FAILURE, IMPROPER SELECTION OR IMPROPER USE OF THE PRODUCTS AND/OR SYSTEMS DESCRIBED HEREIN OR RELATED ITEMS CAN CAUSE DEATH, PERSONAL INJURY AND PROPERTY DAMAGE. This document and other information from Parker Hannifin Corporation, its subsidiaries and authorized distributors provide product and/or system options for further investigation by users having technical expertise. It is important that you analyze all aspects of your application and review the information concerning the product or system in the current product catalog. Due to the variety of operating conditions and applications for these products or systems, the user, through its own analysis and testing, is solely responsible for making the final selection of the products and systems and assuring that all performance, safety and warning requirements of the application are met. The products described herein, including without limitation, product features, specifications, designs, availability and pricing, are subject to change by Parker Hannifin Corporation and its subsidiaries at any time without notice. Offer of Sale The items described in this document are available for sale by Parker Hannifin Corporation, its subsidiaries or its authorized distributors. Any sale contract entered by Parker will be governed by the provisions stated in Parker's standard terms and conditions of sale (copy available upon request). 2012 Parker Hannifin Corporation Autoclave Engineers is a registered trademark of the Parker Hannifin Corporation 06-0006BE October2012 Instrumentation Products Division Autoclave Engineers Operation 8325 Hessinger Drive Erie, Pennsylvania 16509-4679 USA PH: 814-860-5700 FAX: 814-860-5811 www.autoclaveengineers.com Parker Hannifin Manufacturing Ltd. Instrumentation Products Division, Europe Industrial Estate Whitemill Wexford, Republic of Ireland PH: 353 53 914 1566 FAX: 353 53 914 1582 ISO-9001 Certified Bulletin RS-BTRS-Jr