Distillation Unit

Distillation units are often used for small scale production of fine chemicals and pharmaceuticals (API’s) & Pilot Plants.

The standard configuration of Distillation Unit allows performing a variety of processes like:

Distillation, Reflux, Rectification

Azeotropic distillation (phase separation)

• Evaporation to desired consistency
• Multi component reactions
• Gas dispersion into liquid phase
• Extraction/phase separation in reactor
• Crystallization
• Cryogenic / low temperature reaction

Since used for multiple processes and different products, fast and efficient cleaning of such reactors systems is very important. This issue must be respected already in the planning stage by the choice of used materials in such units, as well as in the design of the complete unit to shorten the down time during product changes.

Additional accessories to our Distillation Units are scrubber, glass reactors or mixing vessel.

A TYPICAL UNIT BASICALLY CONSISTS OF;

·        Reactor with Multiple Necks on TOP, with a bottom Flush Valve for Outlet for flushing OFF the remains.

·        Fractional Column of usually 1Mtr of height with or without Packings required as per theoretical stages.

·        Shell & tube Heat Exchanger (Condenser) with Top Vent

·        SS316 Pipes, Fittings & Valves as a connecting medium (Flanged / TC Clamp Joint End connections)

·        SS316 Valves for Vacuum Release.

·        Flush Bottom Valve for minimum Hold up in the main flask.

·        SS316 Surge Tanks (Receivers) for Phase Separations, Reflux & Collection.

·        Glass / SS316 Addition Vessels

·        Dip pipes for feed and as a insert for temperature reading sensors, etc

·        SS316 Stirrer Shaft with detachable & height adjustable Blades with Maintenance free & Zero Leak Magnetic Drive for High Vacuum & Pressure Reactions.

·        Flame Proof Motor (of 0.5HP; 3Phase Electric) with Lov Jov Coupling

These all are mounted on Box Pipe frame Structure (Either SS304 or Powder Coated, as per Client’s requirement) which is suitably designed for the calculated weight.

Quick Installation Steps:

“It is always a good practice to start the assembling of the unit for Bottom to Top”

1.   Assemble the Pipe Structured Frame as per the drawings provided. (Please maintain the dimensions given in the drawings, as these are based on calculation of the load on per stage of glass assembly accordingly)

2.   Check twice for assuring the bolts of fittings are tightened, as one loose bolt can call havoc.

3.   First Place the complete SS Reactor as per Site Location.

4.   Then Place the Shell & tube on the Pipe Structure with proper Nut & Bolt Support provided.

5.   Then Place the Column on the Vapor Nozzle (either by Flange / TC clamp Joint) as per Design Data.

6.   Then Adjust the height of Shell & tube Heat exchanger along with the entire frame section on which it has been mounted, to match the end joint of Column Pipe.

7.   Then start Fitting the surge Tank / s as per GA drawing provided.

8.   Fill the HFCU (Hot Fluid Circulation Unit) with the Oil Provided (Or with Therminol Oil, if Oil is in Client’s Scope; or equivalent Oil as per Process Requirement.)

9.   Connect the HFCU to the Main Reactor with Insulated Hose provided along with the Unit.

10. Fill The Reactor with the material and Start the Distillation to fix any leaks in the system.

DETAILS FOR ASSEMBLING THE UNIT:

Water For The Condenser

The easiest thing you can do is to use tap water to circulate water through the condenser. Water goes “IN FROM THE BOTTOM and OUT FROM THE TOP” of the condenser. Tap water will work just fine, and you can drain the exiting water to your sink drain. Experts say chilled water is better, and recirculating it with a pump (optional but not provided with the kit) conserves this precious resource. If you use the pump, use a bucket of ice water to circulate chilled water through the condenser and back to the bucket. In any case, the water only needs to be a trickle, but IT MUST ALWAYS BE MOVING. Once the distillation gets underway, you will be able to tell if your flow is enough by feeling the temperature of the water coming out...if it is cold to Luke warm, your flow is enough. If it's warm or hot, increase the flow. If you use the pump instead of tap water, plan on using a good amount of ice in the bucket per distillation.

Be sure to plug the hoses on to the condensers' glass hose-bibs snugly... a hose popping off in the middle of a distillation is a good way to make a real mess! The hose may seem difficult to get on to the condenser fittings- if so, simply warm the end of the hose with hot water or over a lighter or candle flame (don't burn it!) and it will then stretch easily and slip on. (you may have to cut it off with a razor blade later)

BASICALLY THAT'S IT

Turn on the condenser water; Make sure the stopcock on the receiver is CLOSED.

The Distillation Process

As the water heats up and starts to boil, you'll see steam starting to finally come out the top as the biomass flask heats up. This takes about half an hour or so depending on the volume. Eventually you'll finally see that first drip make it's way down the condenser and into the receiver.

Cleaning

Usually just swirl a lot of soapy water around in the parts, and use a bristle brush to clean everything. It's a good idea to first wipe as much of the joint grease out as you can with a paper towel or so.

BE CAREFUL to not clunk the glass of The Window provided against any hard surfaces as most glass wares are broken during cleaning!!

If the toughened Glass bump into a hard object like a tile counter or porcelain sink, they may develop little tiny "star" cracks. These are dangerous, they can be repaired, but if left un-noticed, they can easily cause a flask to crack or break apart at the most inconvenient time, like when it's full of boiling water

Using a 1/2" diameter dowel or plastic rod is helpful for quickly poking plant matter and stems out of the biomass flask. Don't be tempted to use metal

Gunk in the boiling flask that builds up from the mineral deposits of your tap water can quickly be removed with an overnight soak in vinegar, Methanol or a good soak with soap solution with Lime in it will probably work just as well.

BE CAREFUL while using chemicals, as a cleaning agent.

Usually do not remove the water hoses from the condenser- simply circulating a little soapy water inside the tube, plugging the ends with the fingers, and giving it a good shake is usually all that's necessary to clean the condenser

It's a lot easier to just leave the hoses on for storage than risk breaking things trying to get them off each time you use the system.

If you do have to remove them and they are stubborn, just use a sharp knife and slit the hose at it's base, and it will come off easily.

Hot fluid Circulators and Electricals:

Test the HFCU for any leaks from the joints and rectify it before charging the Oil.

Ensure the Drain Valve is closed before charging the oil.

Ensure that the Electrical terminals are well placed as per the electrical drawing provided with proper insulation and precautions.

On the heater and set the heating temperature as per the given instructions.

Check and assure that the heater switches to OFF at the “Set OFF” temperature before starting the distillation process.

Do’s

Don’t s

·        Apply & Release the Vacuum gradually.

·        Always provide a Pressure Release Valve to the water supply Main lines

·        Start Circulation of cooling water 15mins prior to switching ON the Oil Bath Heater.

·        Stop Circulation of Cooling water only after the contents of the Main flask have reached to room temperature.

·        Always Drain the water from condenser and keep it dry when the unit is not in use.

·        Always assure the Flow of Cooling water to Optimum.

·        Never Heat the Unit when the Main Flask is Empty.

·        Cooling water pressure should not exceed 1.5Kg/Sq.cm.

·        Never “DRY” heat the HFCU

·        Never fill the Main Flask more than 2/3rd of its total volume.

·        Never Light a lighter when the distillation process is ON

·        Avoid any dripping of cold water on the Main Flask when the process is ON (It can create sudden temperature stress on the Glass Body which the rupture the whole Flask)

HAVE A EFFECTIVE DISTILLATION PROCESS……..