FCC catalysts evaluation

The technology developed in CPERI for the evaluation of FCC catalysts is based on a number of laboratory units (bench and pilot scale) by using proprietary evaluation protocols. The most important units used in this field are:

• FCC pilot plant
  The FCC pilot plant is based on our own proprietary design and it uses a continuous circulated fluid bed reactor and consists of a riser, a stripper, a lift line and a fluid bed as the regenerator. The unit simulates a commercial FCCU aiming at catalysts evaluation and to the development of new technologies.
• Laboratory unit for testing FCC catalysts (MAT)
  The Microactivity Test (MAT) unit used in CPERI has been designed according to the ASTM D-3907.
• Cyclic deactivation unit (CDU) for metals tolerance
  The unit simulates the deactivation of FCC catalysts by exposing them in cycles: cracking, stripping and regeneration.

Methodology for FCC catalysts evaluation
The FCC catalysts evaluation is implemented by a combination of the above units. The method is based on a protocol applied to each unit. The type of protocol that will be used depends upon the special requirements of the refinery. For each catalyst, LEFH can give the yields and selectivities of all products as a function of conversion. In addition, the evaluation is completed by the physicochemical characterization of the cracking catalysts.

FCC additives evaluation

Apart from the above described technology, the Laboratory has also developed technology for the evaluation of some FCC additives: DeSOx and BCA (Bottom Cracking additives):

• Evaluation of DeSOx additives
  A laboratory procedure has been developed in LEFH for testing the relative SOx-removal activity of various DeSOx additives. The procedure involves full cycles between SOx adsorption and regeneration of the materials, carried out usually at the conditions of a typical FCC unit.
• Evaluation of BCA additives
  BCA are now very important because of the higher amounts of resid added in the FCC feedstock. The technology developed in CPERI for BCA evaluation is based on the units described above for FCC catalysts. The CDU is the key unit for this evaluation (mettalation procedure) while the final evaluation is carried out in MAT or FCC pilot unit according to a specific protocol.

HDS catalysts evaluation

A special pilot plant unit is used for the evaluation of the various hydrotreating catalysts. The unit can operate in a wide range of operating conditions and for all petroleum fractions.

• Pilot plant unit for hydrotreating petroleum fractions (HDS) (click here for more details on this item)
  The HDS unit consists of two reactors connected in series and contains three independent feed modules (H2, H2/H2S, N2). The unit is fully automated and can operate up to a maximum temperature of 550°C and up to a maximum pressure of 200 bar.
• Methodology for HDS catalysts evaluation
  A standard protocol is applied which depends on the type of catalyst, the type of feedstock and the targets of the hydrotreating process. The catalysts comparison is performed under constant operating conditions according to the degree of hydrogenation achieved by each catalyst.

Fuels quality control

The laboratory team and the equipment are available to industry for standard fuel analysis and fuel quality control. More specifically the following services are offered:

• Quality control of gasoline, naphtha and diesel
• Quality control of other fuels: fuel oil, crude oil, lubricants
• Quality control of gaseous fuels
• Analysis of solids/catalysts
• Analysis of various environmental samples
• Development of new analytical methods

Polymeric Materials – New Technologies

Excellent experimental facilities exist in the Laboratory for the synthesis, analytical characterization and testing of polymers. The laboratory can provide services related to: (a) Polymerization processes, (b) Characterization of polymeric materials, and (c) Chemical modification of polymers under processing conditions. Moreover, the Laboratory can undertake analytical and consultative services concerning the quality control of the polymers and polymeric products.

The services already provided by the LPRE are the following:

1. CAD/CAM OF POLYMERIZATION PROCESSES
   • Investigation of polymerization processes in fully automated high-pressure pilot scale units
   • Development of advanced software for the design, optimization and control of polymerization processes.
2. CHARACTERIZATION OF MOLECULAR PROPERTIES
   • Determination of the viscosity average molecular weight of polymers by Ubbelholde Viscometer.
   • Determination of the molecular weight distribution of polymers by Gel Permeation Chromatography (GPC).
   • Qualitative and quantitative characterization of polymeric and non-polymeric materials (e.g. solutions, membranes, particles and fibers) by Infrared Spectroscopy (FT-IR).
3. CHARACTERIZATION OF THERMOMECHANICAL AND OTHER PHYSICAL PROPERTIES
   • Thermal analysis of polymeric and non-polymeric materials by Differential Calorimetry (DSC).
   • Thermal analysis of polymers and non-polymers by Thermogravimetry (TGA).
   • Measurement of molecular diffusion coefficient of polymers by Dynamic Light Scattering.
4. CHARACTERIZATION OF POLYMERIC PARTICLES AND EMULSIONS
   • Determination of the particle size and drop size distribution by Laser Diffraction Sizer
   • Determination of particle size distribution by Dynamic Light Scattering.
   • Determination of particle and drop size distribution by Optical Microscopy – Image Analysis (400X-5000X).
   • Observation under the optical microscope, sample photographing, digital imaging and advanced image processing.
5. CHEMICAL MODIFICATION OF POLYMERS UNDER PROCESSING CONDITIONS
   • Investigation of the chemical modification of polymeric materials under processing conditions by reactive extrusion using a Mixer-Brabender Plasticorder.

Analysis and Characterization of Solids

The “Laboratory of Analysis and Characterization of Solids” provides analytical -characterization services mainly for solids materials (e.g. catalysts, solid waste, industrial products, ores). The laboratory has been accredited with ISO 9002 for most of the analytical services that it provides.

AVAILABLE SERVICES

1. Surface morphology observation (magnification 10-300.000) with Scanning Electron Microscopy (SEM)
2. Microanalysis (local elemental analysis), element mapping and linescans with X-ray EDS
3. Crystalline phase identification with X-ray Diffraction
4. Unit Cell Size of Zeolites with X-ray Diffraction
5. Thermogravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC) and Differential Thermal Analysis (DTA) of solid materials
6. Material Characterization with Temperature Programmed Methods (TPD-Η2, ΤPD-ΝΗ3, TPO, TPR, pulse chemisorption). Detection with Mass Spectrometer (MS)
7. Elemental analysis of aqueous solutions, inorganic solid materials and organic materials with Inductively Coupled Plasma – Atomic Emission Spectroscopy (ICP-AES)
8. Surface Area (BET) measurement, Area and Volume of micropores (t-plot method) and Pore Size Distribution with nitrogen sorption
9. Pore Volume, Pore Size distribution and Surface Area with Mercury Porosimetry
10. Particle Size Distribution measurement with laser diffraction (wet and dry dispersion methods) and sieving
11. Milling of Solids
12. Supported Catalyst Preparation with the Dry and Wet Impregnation methods