A schematic diagram of the fully automated fluid catalytic cracking (FCC) pilot plant is shown in figure 1. Preheated gas oil feed flows in the bottom of a riser, where it is mixed with hot regenerated catalyst. In the riser (9 meters long) the reactions take place and at the riser exit the mixture flows into the stripper vessel where the separation of gases from the solid catalysts occurs. The solids flow through the spent catalyst lift line and they return to the reactor bottom following regeneration.

The reaction products, from the stripper exit, flow through a heat exchanger and then after their temperature is reduced to 20°C in order to condense the heavier products. Then the mixture is led to a stabilizer column for better separation of liquid and gaseous products. The specifications of CPERI pilot plant are: max feed rate=40 g/min, C/O range=3-30, riser temperature=till 650°C, regenerator temperature=till 730°C, catalyst inventory=4 kg.

The unit process specifications are reported in table 1. The unit consists of the following modules:

i) Reactor module: The unit includes of two reactors operating in series and heated with a radiation split-type furnace. Both reactors can be used in series for up and down flow. Reactor volume is 265 cc and they can operate till temperature of 550°C and pressure of 150 bar.

ii) Gas delivery modules: This part of the system contains three (3) independent gas feed modules (H2, N2, H2/H2S) with all necessary equipment.

iii) Liquid delivery module: Oil is contained in a nitrogen-blanketed vessel, which is situated on a weigh scale. This feed vessel is provided with electrical heating that is under automatic temperature control by the computer. A sample of the product at the separator outlet can be taken via a pneumatic actuated three-way valve.

iv) Gas outlet module:  Initial part of this module is the pressure control section, which maintains the required reactor pressure. Pressure control section, are heat traced and insulated. The outlet vent is connected to a wet test meter to measure the outlet flow of the system. 

v) Separation and liquid outlet module: A pipe in pipe cooler cools the reactor outlet product. The separator has a narrow electrically heated liquid-part and wide water cooled gas-part. Product is collected in a heated vessel, which is located on a weigh scale.

The HyDis is a vacuum distillation unit with 40 L capacity operating at 10mbar pressure. The unit operation is a fully-automated batch unit that is employed for but not limited to:

• Separation of petroleum fractions
• Separation of bio-components
• Pilot production/separation demonstration of final products of other processes (hydrotreatment, cracking etc.)

The SCT-MAT reactor is made by Pyrex glass and it is heated by a three-zone furnace. The unit operates typically at 560°C with a run time of 12s. Preheated feed at 60°C is injected into the reactor through an oil capillary heated only by the oven. For this injection a special motor pump is used. The reactor consists of an annular bed where the catalyst is diluted with inert glass beads. The vapor products of the cracking are cooled to 0°C at the reactor exit where part of them are condensed and collected in a specially designed high volume liquid receiver. The remaining not condensed gaseous products are led to gas collection system and are collected by water displacement. Following the oil injection, N₂ flows into the reactor in order to drive the products along the reactor. The conversion of the liquid products is determined by a Simulated Distillation Analyzer. The gaseous products are analyzed at a Refinery Gas Analyzer.The gasoline produced is analyzed by a DHA analyzer. The weight of coke, deposited on the catalyst, is measured by an Elemental Analyzer.

The ACE Model R+ unit is available in LEFH. The unit is capable of using various feedstocks with a wide range of properties and different catalyst types to perform cracking reactions at various experimental conditions (injector lengths, cracking and regeneration temperatures, stripping conditions).

The ACE-Model R+ uses a catalyst addition and withdrawal system which moves catalyst into and out of the ACE reactor automatically. Dry catalyst samples of known mass are placed into the six (6) catalyst feed hoppers. The reactor is placed into a three zone furnace and heated to the desired cracking temperature. Injectors of different lengths can be adapted into the metal reactor in proportion to the case study. Cracking feedstock, nitrogen and air are each fed to the unit from independent systems. The feedstock is drawn from a heated oil vessel and supplied by a syringe pump which is calibrated to supply the oil at the desirable volumetric or mass rate. The liquid products of the reaction are collected in six (6) receivers placed in a bath. After the experiment is completed the liquid crackates are collected and weighed. Their composition is determined offline by a Simulated Distillation Analyzer. The gaseous hydrocarbons are collected through water displacement in a gas collector vessel and their concentration is measured on line through a Refinery Gas Analyzer. The gasoline produced is analysed by a DHA Analyzer. During in situ regeneration of the catalyst, reactor effluent gases pass through a catalytic converter which oxidizes any CO and hydrocarbons to CO₂ and H₂O. The CO₂ containing gases are diverted through a mass flow meter and Infrared CO₂ Analyzer, which is used to calculate the amount of carbon deposited on the catalyst.

The CPERI Cyclic Deactivation unit (CDU), designed by Xytel, is fully computerized (automated) and simulates satisfactory the E-cats by depositing metals on FCC catalysts, while performing an accelerated deactivation method. The unit utilizes a metallic reactor with fluid bed configuration and capacity of 150- 200 g of catalyst. The CDU mimics the FCC catalyst deactivation via repeated cycles consisting of: cracking of VGO spiked with the appropriate amount of contaminant metals, stripping and regeneration in the presence of 50% steam. The steam is generated in a heated line prior to entering the reactor. LEFH follows a flexible protocol where the complete CDU run consists of 54 or 51 cycles, of which each cycle follows a cracking, a stripping and a regeneration step.

The VB01 unit is a small-pilot scale hydroprocessing unit with capacity 10-180ml/hr. This fully-automatic continuous-flow unit allows testing at a wide range of operating parameters (max 150bar and max 450οC), corresponding to the operating window of most industrial-sale hydroprocessing units. VB01 consists of three main systems; a) a dual liquid- and dual gas-feed system (allowing single feed hydroprocessing or dual feed co-hydroprocessing tests), b) an reaction system with six independent heating zones and c) a separator system. The liquid product can be sampled at multiple intervals while the gaseous product is analyzed off-line, allowing accurate mass balance and H2 consumption calculations.

The VB01 hydroprocessing pilot plant has several applications including:

• Evaluation of hydrotreating/ hydrocracking/ hydroisomerization catalyst activity/aging
• Determination of HDS, HDN, HDO and HDC kinetics and activity
• Assessment of new/alternative feedstocks (oils, biomass / elastic / plastic / pyrolysis bio-oils, oils derived from microalgae, Fischer-Tropsch waxes etc)
• Upgrading liquid biomass (lipids, pyrolysis biooil, plastics pyrolysis oils, microalgal oil etc)
• Co-hydroprocessing fossil- & bio-based feedstocks (hybrid fuels)

This high pressure bench scale unit of LEFH is a versatile unit for the evaluation of the activity and selectivity of solid catalytic materials in different high pressure reactions. The unit is equipped with a feed inflow system able to supply both gases and liquid feeds. The unit operates with a stainless steel fixed bed reactor, externally heated with a three-zone furnace. The exit stream of the reactor can be either cooled via a heat exchanger and directed to a system of vessels for the separation and collection of the liquid and gaseous products or directed via a heated line to an online GC with both an FID and TCD detector able to analyze hydrocarbons and alcohols. The test facility can operate to a temperature range up to 600°C and pressures up to 100 atm.

The small scale of the unit renders it ideal for the development and investigation of heterogeneous catalysts for high pressure reactions, as well as the performance of kinetic measurements. It can be used for the determination of different variables for research on catalyst improvement, such as reaction temperature, pressure, feed flow etc., catalyst screening, activity and selectivity testing, testing of catalyst lifetime etc. Typical reactions that can be performed in the high pressure test facility are hydrogenation, oxidation and hydrotreating reactions.

LEFH has a series of high pressure medium temperature autoclave reactors of different sizes. More specifically, there are two autoclave reactors of 450 and 975 ml made from Hastelloy C-276. Maximum pressures and temperatures are 200 bar and 350^oC respectively. Each reactor has a stirrer, a cooling coil, a catalyst basket and a catalyst addition device and they both have the capability of receiving a sample from the gas or liquid phase during reaction. Each reactor has a dedicated reactor controller that allows for accurate control and monitoring of all process parameters. The autoclave reactors have the capability of investigating different types of processes such as: i) liquids biofuels upgrading via HDO reactions, ii) liquid phase reactions involving heterogeneous catalytic conversion of sugars dissolved in aqueous and organic solvent systems towards value added chemicals and fuels, iii) biomass fractionation reactions for complete separation of hemicelluloses, lignins and celluloses by different techniques.

ANALYTICAL EQUIPMENT AND METHODS

Accurate and precise analyses provide the cornerstone for successful research studies. LEFH possess a modern fully equipped laboratory (run under a Laboratory Information Management System, LIMS), which employs ASTM methodologies and is capable of performing a total of 55 different analyses.

LEFH’s analytical services have been certified and approved by Lloyd’s Register Quality Assurance to conform to the BC EN ISO 9001 quality management system standard and ISO 17025 quality policy, with respect to the provision of laboratory inspection services related to fuel content and solid characterization. The laboratory is regularly audited as per ISO requirements.

ADVANCED EQUIPMENT

• 2DGC-TOFMS (Pegasus 4D by Leco instruments)
• GC-MS
• GC-FID (for polar compounds)
• FTIR
• Sugar analysis with Ion Chromatography (qualitative and quantitative analysis with ICS-5000 by Dionex)
• HPLC
• XRF

STANDART EQUIPMENT ANALYTICAL METHODS

• N2 physisorption methods (BET, t-plot, PVD)
• XRD
• TPR/TPD/TPO
• ICP
• SEM microanalysis
• TEM
• TGA-MS
• FTIR for catalyst acidities
• Particle size analysis
• ABD
• Grinding/Sieving
• Attrition resistance
• ISO 9002/17025 and LIMS procedures