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REACTION – CRYSTALLIZATION PILOT MP1071

The process of crystallization allows to separate a component from a liquid solution witch is transformed from the liquid phase to the solid phase.

MP1071

The MP1071 bench allows two types of crystallization :
- by cooling of the mixture, while exploiting the reduced solubility of the component to separate, at lower temperature.
In crystallization by cooling, the solution to treat is stocked in a thermostatic vat, and stirred in order to maintain the component to separate in solution. The treatment at high temperature is assured by of hot water circulation (80°C to 90°C) in the jacket of the vat.
When the complete solubility is gotten until the separation of the thermostatic compound, a measuring pump provides on control the transfer of mixture in the crystallizer, this one also include a vat with a double jacket in which circulate the cooling water.
When the crystallization of the product we wants to separate is obtained, the solid part is discharged in a vat, through the bottom vat valve.
- by evaporation of the solvent, while decreasing the solubility of the component to separate in the solution.
In crystallization by evaporation, the solution to treat is immediately loaded in the crystallizer, the thermal fluid is a low-pressure steam (110°C. 1,4 bar). The generated steams are sent then in a condenser, in a cooler, and in a test-tube.
The complete installation can be put under vacuum, in order to decrease the temperature of the heating thermal fluid. In this case, we can use a thermal fluid in liquid state.

 

Teaching objectives

- Study of liquid-liquid and solid-liquid reaction

- Flowing back heating

- Atmospheric pressure and reduced pressure boiling evaporation

- Crystallization by cooling with double jacket and under vacuum

- Study of crystallization : solubility. Over saturation

- Balances mass and energy balance of the process.>

 

Technical specifications

Reactor :
Double jacket reactor in stainless steel
Pressure : 0 (vacuum) to 2 bars (absolute)
Tapping of the products without retention by bottom valve
Heating by refrigerant
Measure of the internal pressure
Cooling by network water circulating in the double jacket or in a coiled device
Variable-speed stirrer 0 to 300 rpm
Loading of solid powders
loading of liquids under vacuum
Sampling tube with tap

Heating unit :
maximum temperature 160°C, minimum temperature 30°C, refrigerant with circulation pump.

Measuring device :
Vacuum loading
Vacuum pump
Variable and controlled flow
Level measurement
Draining valve

Condenser :
Condensation of the water steam
The refrigerant fluid is water from network

Distillate circuit :
An observation device at the outlet of the condenser
A discharge to the recipe
A refrigerant for cooling the distillate : the refrigerant fluid is the network water
A return circuit to the reactor
Distillate flow measuring device

Recipe :
2 recipes,
Level measurement
Breathing
Draining

Breathing circuit :
the breathings are made of stainless steel pipes

OPTION 1 : Vacuum filter
Stainless steel 316 L design
Diameter 400 mm, height 350 mm
Vacuum fitting connexion
Mounted on wheels

OPTION 2 : Vacuum pump, water ring pump

 

Essential requirements

Power supply : 220 V - 50 Hz

Heating unit 140°C, 3 bars, 10 kW