Chemical engineering range - 11/01 MULTI-FUNCTION DISTILLATION DVI/6000. Version presented DVI/6000 PIGNAT S.A.S. Subject to technical modifications

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1 Chemical engineering range - 11/01 MULTI-FUNCTION DISTILLATION Version presented 1

2 Chemical engineering range- 11/01 Technical description Distillation packing column: 1 20L polyethylene feeding tank. 2 Dosing pump : flow rate 0 to 16 L/h. 3 Electric pre-heater, 1 kw, temperature probe, float switch, safety valve, sampling valve. 4 Feeding manifold. 5 Glass heater, capacity, ND 200, 6L. 2 kw Ex technology electrical heater, low level switch, temperature probe, ND 25 loading hatch, residue overflow tube, draining valve. 6 Packing column made of three ND 50 glass pieces with removable insulation, Multiknit packing, three stainless steel plates equipped for sampling by stainless steel valve and temperature probe. 7 ND 50 glass reflux-divider, with solenoid and equipped with temperature probe. 8 ND 50 Glass condenser, stainless steel coil, thermostat on vent, temperature probe. 9 Differential pressure electronic transmitter. 10 SS coolant, two solenoid valves. 11 ND 50 glass receiver, graduated, 1 L L polyethylene tank. 13 SS coolant. 14 Glass receiver, graduated, 1 L L polyethylene tank. 16 Jacketed azeotropic settler, return column and take-off valves set. Control unit: Electric console containing: General switch. Switch on and emergency switch off. On-off of kettle heater. Failure witness light. Six configurable electronic temperature digital displays. One configurable flow meter digital display. Two PID electronic controllers. Reflux electronic timer. Switch for opening of the solenoid valves. Connection of controllers and digital displays under Modbus protocole to PC. Distillation plate column: 17 Glass heater, ND 200, 6L. 2 kw Ex technology electric heater, low level switch, temperature probe, ND 25 loading hatch, residue overflow tube, three draining valves. 18 Bubble cap trays column made of three ND 50 glass pieces with removable insulation, three SS plates equipped for sampling by SS valve and temperature probe. 19 ND 50 glass reflux-divider, with solenoid and equipped with temperature probe. 20 ND 50 glass condenser, SS coil, thermostat on vent, temperature probe. 21 Differential pressure electronic transmitter. 22 SS coolant, two solenoid valves. 23 ND 50 glass receiver, graduated, 1 L L polyethylene tank. 25 SS coolant. 26 Glass receiver, graduated, 1 L L polyethylene tank. 28 Cold water circuitry: isolating valve, temperature probe, column setting valve, two pressure reducers, con denser, coolant and settler flow rate setting valves, two float flow meters. Control unit: Electric console containing: General switch Switch on and emergency switch off On-off of kettle heater. Failure witness light Five configurable electronic temperature digital displays One PID electronic controller Reflux electronic timer Switch for opening of the solenoid valves (takeoff-man-reflux) Connection of controllers and digital displays under Modbus protocole to PC Frame: Stainless steel tubular framework. Six feet with adjustable plates. Fitting of the frame to the ground or to the wall by spit and screw. 2

3 Chemical engineering range - 11/01 Principle of operation TIC DPIC2 TH EV4 EV3 TI14 EV1 16 EV2 7 8 TH1 DPIC1 10 TIC5 9 TI8 TI12 TI4 TI11 18 TI10 LA3 TI LA2 3 TIC6 4 2 LA1 TI1 TI3 6 TI TI WATER The test rig comprises two distillation columns: - one packed column 6, - one bubble plate column 18. These two columns can be operated independently (in continuous or batch mode) or in series by changing the position of the solenoid valves. The series configuration can be used to distil an azeotropic mixture (water-butanol). Operating principle for heteroazeotropic distillation: The mixture stored in plastic tank 1 is preheated in 3 and continuously fed to column 6. Manifold 4 is used to select one of the three feed plates. The vapours from the mixture boiled in boiler 5 rise up the column and become richer in butanol. The packing enables the descending liquid phase and the rising vapour phase to mix intimately. The vapours are condensed in 8. Part of the condensates (D) are drawn off in 7; the other part (L) returns to the column. The reflux ratio is L/D. The mixture (raffinate or residue) becomes richer in water in the boiler. The residue, cooled in cooler 13, overflows continuously into plastic tank 15. The flow rate is determined by measuring the filling rate in receiver 14. The condensate drawn off from the head is refrigerated 10 then collected in decanter 16. The light phase is reintroduced into column 6; the heavy phase feeds column 18. On the same principle the light phase boils in boiler 17. The raffinate is drawn off at the base by overflow, cooled in cooler 25 then stored in plastic tank 27. The flow rate is determined by measuring the filling rate in receiver 26. The vapours emitted become richer in butanol at each plate and are condensed in 20. Reflux ratio head 19 is used to draw off part of the condensates. This distillate is then cooled in 22 and collected in decanter 16. The composition of the mixture obtained in the decanter becomes closer to that of the azeotropic mixture with each successive rectification. Temperature sensors and sampling tappings on each column are used to: - observe liquid-vapour equilibriums. - determine the materials balance. - determine the thermal balance. The column pressure drop reflects the vapour flow rate. By measuring this pressure (9 and 21), boiling can be controlled and the hydrodynamics of the column characterised. 3

4 Chemical engineering range- 11/01 Educational goals Simultaneous implementation of two distillation units: Discontinuous distillation on the one hand. Continuous distillation on the other hand. Coupling implementation of distillation units: Process of hetero-azeotropic by decantation and regeneration in continuous mode of third casing. Process of ternary distillation. Proposed experiments Each work duration: 4 hours Characterization studies: Dosing pump calibration. Heating power calibration. Calculation of the unit's pressure drops. Calculation of the heat transfer coefficient at condensation. Calculation of exchange surface at condenser. Hydrodynamics of a packed column and of a plate column: evolution of pressure drops. Process control achievement: Determination of operating parameters: feeding flow rate, position of feeding plate, preheating temperature, reflux ratio. Application of the parameters: Continuous or discontinuous distillation of the binary water - Ethanol. Hetero-azeotropic distillation of the binary water - Butanol. Distillation of a ternary mixture. Materials and heat balances, global yield. Determination of columns' efficiency by Mac-Cabe and Thiele construction, determination of theoretical efficiency. Liquid-vapor balance diagram Distillation of a heteroazeotrope y 1 0,9 0,8 0,7 1 column 2 column azeotrope Distillation or Rectification: This is an operation which consists in separating several volatile liquids, complex or simple mixtures, by a series of vaporisations or condensations. It enables to separate several liquids if they have sufficient different volatility or more simply different boiling points. Continuous distillation enables to separate the mixture into two fractions : a volatile fraction, the distillate extracted at the head of the column, and a heavy section, the residue, extracted at the column bottom. 0,6 0,5 0,4 0,3 0,2 0,1 feeding composition 1 column feeding composition 2 column 0 0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9 1 x Discontinuous distillation enables to separate the components according to their boiling points. Certain non-ideal binary mixtures form an azeotrope for a given composition. An azeotrope is a mixture which behaves like a pure substance : it boils at a fixed temperature and gives vapor having a given and constant composition Two types of azeotropes exist: - The homoazeotropes: homogeneous liquid mixtures. - The heterozeotropes : heterogenous liquid mixtures. 4

5 Chemical engineering range - 11/01 Safety and EC certification This distillation unit is safe thanks to: Low level detection system in pre-heater and kettle stopping the heaters if required Explosion proof technology for the Kettle heater Overheating detection device Optional equipment Computer control software: Enables the acquisition of data ( measurement, setting, output) and supervising the unit from a PC (see below) Computer kit: Colour printer, CPU,17"monitor. Ref /O1 Ref /O2 Other available versions Continuous distillation: Ref DVI/3000 Electronic control of parameters Column equipped with Multiknit packings, perforated plates or bubble cap trays. Continuous distillation for hazardous area: Ref DVI/3000/Ex Manual setting of operating parameters. Pneumatic control console. Flame proof technology pump. Steam heating (heat exchanger) Dilatation thermometers Computerized continuous distillation: Ref DVI/3000/I The same unit as the DVI/3000, supplied with control console supervising software and computer kit. Computerized multi-purpose distillation: Ref /I The same unit as the, but supplied with control console supervising software and computer kit. DVI/3000 5

6 Chemical engineering range- 11/01 Recommended complementary equipment Analysis: Portable densimeter. Chromatography. Minimum PC configuration: consult us Utilities and connections Electricity: 240 volts system, single phase, 50 Hz. Power : 5 kw. Connection on 2 phase + G plug, 5 meters of cable. Cold water: Municipal water network. Flow: 1 m 3 /h, pressure 2 bar. Wastewater collection at ground-level towards the gutter. PIGNAT services Unit assembled and tested in the factory : electrical and hydraulic testing carried out before delivery. Unit delivered with technical document (PID scheme, components list, technical data of the components, electrical schemes). Unit delivered with educational textbook presenting different experiments and theoretical reminders, functioning mode and experimental results. Optional services Formation of trainers on site or in our factory by our engineers. Commissioning on site by our technicians. Warranty conditions The units are guaranteed one year according to the terms of the contract. Terms and conditions of sale and guarantee are available upon request. Overall dimensions L x W x H=270 x 60 x 320 cm Empty weight: 150 kg, in use: 250 kg. Unit to fix on the ground or against the wall Pignat S.A.S. 6, rue Calmett, BP Genas CEDEX France Phone Fax Web site pignat@pignat.com 6