Batch Evaporation Crystallization

quick overview :

Batch Evaporation Crystallization

Main characteristics of the pilot

• Industrial instrumentation
• Flow switch of the condenser cooling water for operators safety
• Borosilicate glass and stainless steel AISI 316L manufacturing
• Rigid process pipes
• Product vacuum supply system for storing reagents
• Downwards dismantling of reactor vessel without dismantling upper section of reactor
• Temperature control unit with thermal oil medium
• Thermal oil medium or crystallization reactor temperature control
• Interchangeable stirring rotor
• ATEX variable speed stirring motor
• Liquid-ring vacuum pump (Option 1)
• AISI 316L stainless steel bag filter (Option 2)

Principle of Working:

Crystallization allows the separation from a solution of one or more solid compounds dissolved in that solution. On separation, the dissolved compounds change to their solid state when the required operating conditions are met (temperature, concentration). The crystals formed are then separated from the liquid phase by filtration. Crystallization is obtained by the partial evaporation of the solvent, then cooling of the concentrated solution thus obtained. The initial solution is introduced in one part at the start of processing; the evaporation of the solvent is continued until the desired concentration is reached; the crystallization then takes place as the concentrated solution is cooled; the separation of crystals from the mother liquor is carried out using a bag filter under reduced pressure.

Teaching Objectives of Batch Evaporation Crystallization

• Study of the following experimental parameters:
• Batch crystallization of a solution by evaporation then cooling.
• Influence of operating conditions on crystallization of a solution.
• Study of simple reactions under atmospheric or reduced pressure.
• Study of reaction kinetics.
• Study of reversible or irreversible reactions.
• Study of evaporation.
• Total reflux reactions.
• Calculations:
• Heat balance.
• Mass balance.
• Yields.

Technical Specifications of Batch Evaporation Crystallization

• Borosilicate glass feed tank for storing reagents, graduated with product vacuum supply system for filling reagents; 10 litres nominal volume.
• “Grignard” type cylindrical reactor: AISI AISI 316L stainless steel vessel, with insulated double jacket for heating by thermal oil medium and flush mounted drain valve; AISI AISI 316L stainless steel lid.
• Variable speed stirring assembly made of AISI 316L stainless steel with inclined three-bladed rotor.
• Reaction mixture cooling pipe coil made of AISI 316L stainless steel.
• AISI AISI 316L stainless steel one-piece.
• Borosilicate glass column head, with temperature plug.
• Vertical condenser, borosilicate glass body, AISI 316L stainless steel coil heat exchanger.
• AISI 316L stainless steel distillate heat exchanger.
• Graduated borosilicate glass distillate receiver tanks.
• Temperature control unit with thermal oil medium, with circulation pump and temperature control.
• Insulated flexible hoses for heat transfer fluid feed.
• AISI 316L stainless steel connecting tubes for the process and reinforced PVC for cooling fluid tube.
• AISI 316L stainless steel vacuum piping for the various sub-assemblies on the general manifold.
• Borosilicate glass vacuum trap.
• Liquid-ring vacuum pump.
• AISI 316L stainless steel bag filter operating under reduced pressure; capacity 20 litres.
• Support framework with AISI 304L stainless steel tubes, aluminium connecting nuts and adjustable feet.

Instrumentation:

Cooling water feed to condenser fitted with variable area flowmeter with its adjusting valve and water flow switch to turn off heating in case of lack of cooling water. Crystallization reactor cooling water feed chamber fitted with variable area flowmeter and its adjusting valve. Distillate cooler cooling water feed fitted with variable area flowmeter and its adjusting valve. Reflux flow measurement by variable area flowmeter. Reactor and pilot plant pressure measurement by “Bourdon” type pressure gauges. IP55 command and control cabinet fitted with emergency stop, operating buttons and the following interfaces:

• Digital temperature indicator for crystallization reactor with Pt100 Ω type probe.
• Stirrer speed controller.
• Stirrer speed digital indicator.
• Two digital temperature indicators with six Pt100 Ω type probes.

Dimensions and weight

• 1750 mm x 850 mm x 3000 mm ~ 300 kg.

Essential requirements

• 400 V / 50 Hz / 3-phases + N: 10 kW.
• Cold water 10°C / 3 bar: 2 m3/h.