Supercritical Fluid Extraction Vessel
- Supercritical fluid extraction systems with pressures upto 700 bar for lab scale units & upto 450 bar for commercial plants
- Semi or fully automated PLC based plants with CO2 recycling
- PED, U stamp, CE, CSA, UL certification optional
- Customizable designs as per client requirements
World-class technology for natural products
- There is a tremendous demand for high purity & residual solvent free extracts of natural products. Also there is increasing requirement of eco-friendly manufacturing processes for the extraction of natural products
- Supercritical fluid extraction technology provides an economical solution toproviding a safe & eco-friendly way for extraction of natural products. Its superiority over the conventional technologies of extraction, especially for natural products in the food and pharmaceutical industry is well recognized
- Supercritical CO2 textile dyeing is an emerging innovative waterless technology for dyeing of textile fabrics that will revive the textile industries
Commercial Applications of SCFE extractor systems
- Extraction of natural products such as spice oil & oleoresins, flavors, fragrances, colors
- Decaffeination of tea & coffee
- Production of uniform &ultra fine particles
- Supercritical CO2 (SCO2) textile dyeing of fabrics
- Supercritical CO2 (SCO2) cleaning of high precision metal components
- Drying of aerogels
Advantages of SCFE system
- Extract with delicacy & freshness close to natural
- High potency of active components
- Longer shelf life extracts
- Eco-friendly & green technology with no residual solvent & effluents
- High flexibility of process conditions
- Simultaneous fractionation of extracts
- High yields compared to solvent extracted products
- Low batch times for extraction
- Recycling of CO2
- Low operating cost
Advantage of CO2 as a solvent
- Carbon dioxide is generally regarded as safe (GRAS) for food products
- Inexpensive & easily available
- Non-toxic, non-flammable and inert to most materials
Process description for lab-scale plants
The Carbon dioxide gas from the cylinder is first liquefied & then pressurized above the critical pressure of CO2 (73.8 bar) to the required pressure necessary for extraction. This high pressure liquid CO2 is then heated above the critical temperature of CO2 (31 °C) to the required temperature. CO2 which is now in supercritical phase (SCCO2) enters the extractor where the raw material is fed in powder form & the extraction is achieved on the basis of solubility. The compounds dissolved in SCCO2 finally come to the separator at atmospheric pressure & get precipitated. CO2 leaving the separator is then measured by passing it through a CO gas flow meter.
Process description for commercial scale plant
The raw material in powder form is fed to the extractor. The liquid carbondioxide from the CO2 tank is precooled by passing it through the precooler. This precooled liquid carbon dioxide is then pressurized by means of a positive displacement plunger pump to a pressure above the critical pressure of CO2 (i.e. 73.8 bar). High pressure liquid CO2 is then heated above the critical temperature of CO2 (i.e 31 °C) by passing it through preheater. CO2 which is now in the supercritical state enters the extractor in which the raw material is loaded. The SCCO2 dissolves substances on the basis of solubility, depending on operating conditions. The SCCO2 with soluble extracts enters the separators where the pressure & temperature are reduced sequentially so that solubility decreases & extract precipitates in the separators. Finally the clean CO2 without any traces is recycled back to the CO2 tank via condenser.
Amar make high pressure reactors are a critical part of supercritical fluid extraction equipment designed and manufactured by us. These units are used for various purposes including Extraction of natural products such as spice oil & oleoresins, flavors, fragrances, colors, Decaffeination of tea & coffee, Production of uniform &ultra fine particles, Supercritical CO (SCO ) textile dyeing of fabrics, Supercritical CO (SCO ) cleaning of high precision metal components, Drying of aerogels, etc. As opposed to the traditional solvent extraction systems, these systems are eco-friendly, more reliable, efficient and safer. End product of very high to ultra high purity can be obtained with the help of accurately designed SCFE systems.
SCFE extractor standard models
|Model No.||Working Volume (ltr)||Feed Capacity* (kg/day)|
Material of Construction: SS316
|Volume (ltr)||Design Pressure (bar)||Design Temperature (°C)|
|0.1 to 2||350||500, 700||100||200|
|5 to 25||500|
|50 to 100||NA||150|
|200 to 1000|
- *The feed capacity is assuming bulk density of 0.4 kg/ltr of feed, 6 batches/day & one extractor. 5 ltr & above can be offered with 2 extractors & the feed capacity shall double the above given capacity.
- 5 ltr & above systems are offered with CO2 recycling & PLC controls.
It consists of SS316 pressure sensor (transmitter) & digital pressure indicator/ controller (mounted on common control panel) with pressure alarm & optionally heater cut off for safety. Digital pressure indicator has pressure reading in bar & psi, where as controller reads any one ofthe units. The controller is normally used with mass flow controllers (MFCs) or solenoid/flow control valves to maintain constant pressure inside the autoclave. With MFC, gas flow indicator & totalizer are also provided on the same panel. The pressure sensor has temperature limitation upto 100°C & hence the same is provided with water cooling jacket. Optional Intrinsically safe pressure sensor. Pressure sensors with Hastelloy C / Inconel wetted parts can be offered on request.
This system is useful to control temperature overshoots for highly exothermic / out of control / runaway reactions as well as for faster cooling upon completion of reaction. The control panel of the autoclave gives 230V, 1Ø output to connect external auto-cooling system. Options available are: Solenoid valve (ACV) for autoclaves upto 25 ltr or Pneumatically actuated ball valves (ACV) for autoclaves above 25 ltr connected at the inlet of the internal cooling coil with external source of water supply. This is standard for 50 ml – 250 ml autoclaves, however for bigger autoclaves if the cold water line pressure is less than 2 bar then it is better to opt for external pump & tank water cooling system. Normal tap water cooling is not effective at higher temperatures due to steam back pressure whereas pump & tank auto cooling system gives positive pressures & faster cooling. Pump & Water Cooling Tank (ACP): It consists of a SS 304 water tank & pump to circulate water in the internal cooling coil of reactors. Cooling starts automatically if the rate of heating rises suddenly. It comes with monoblock pump, tank, pipeline & flexible hose pipes with quick release coupling & is mounted on the autoclave trolley itself. Ice can be put in the water or the hot water can be discharged & fresh water replenished on continuous basis for more effective and faster cooling. Optional: Ex-proof group IIC pump
High pressure autoclaves are provided with built in safety rupture disc, however additionalsafety can be offered by providing pressure safety valve for which release pressure can be setmanually by increasing or decreasing the spring tension or by simply changing the spring. Theset pressure should normally be around the design pressure. Safety relief valves are standardsupply for glass autoclave & shaker hydrogentor where rupture discs are not available for lowpressures. These valves come with PTFE / Kalrez O-rings. Optional: Materials: Hastelloy C, inconel
It is a pressure reactor with magnetic drive stirring, inlet & outlet valves, pressure gauge &nitrogen/vent. Solvent & catalyst are charged in the vessel & the slurry formed by mixing istransferred under nitrogen pressure into the reactor. The pressure rating & volume of thissystem is designed depending on the quantity of catalyst, pressure & temperature rating of theautoclave. Specially designed control system developed by Amar can be offered to charge thecatalyst slurry in continuous mode at a pre-defined flow rate under pressure. This is very usefulfor CSTR, where no suitable pumps are available for slurry. This system is available for anyreactor volume, pressures upto 350 bar & for a wide range materials.
Gas boosters are useful when the cylinder pressures are much lower than the autoclave ratedpressures. In such case the booster takes gas at lower pressure from cylinder & compresses thesame to deliver at higher pressures. They are generally pneumatically operated. Special gasbooster pumps are available for liquid CO used in supercritical fluid extraction system. The 2booster systems are supplied with air filter regulator, pressure relief valves, inlet-outlet pressuregauges, valves & flexible hose pipe. Optional Boosters upto 700 bar pressure
It is used to transfer liquids, slurries or gases in to the autoclave under pressure. It consists of high pressure SS-316 pot designed for working pressure 100 bar or higher with port for nitrogen gas (N ), liquid / slurry inlet with valve & funnel, outlet valve, pressure gauge, pressure safety 2 valve, high pressure hose & NRV. The liquid to be charged is fed into the pot from top funnel & pressurized with N gas until its pressure is higher than the autoclave pressure & then under 2pressure the liquid is charged into the autoclave. The quantity & rate of flow of liquid charged is not known precisely in this system. However a level indicator or sight glass or weighing balance or flow meter can be provided optionally to measure the liquid charged or its flow rate. Pots of different pressure, M.O.C. & sizes can be offered. These pots can also be used for storage of gases when gas cylinders are located at a far away place. With this option approximate quantity or flow of gas consumed can also be determined by measuring the pressure drop. Volume: 250 ml, ½ ltr, 1 ltr, 2 ltr, 5 ltr, 10 ltr Optional: Forward pressure regulators can be provided at the outlet of (FPR) pot if they are used as gas charging. Pots upto 200 bar / 350 bar Pots in MOC Hastelloy C, Inconel, Monel, Titanium
It is a SS-316 shell & tube reverse flow heat exchanger for distillation/condensing vent vapours from the autoclave upto 10 bar pressure. It is offered in different surface areas such as 0.1, 0.2, 0.5, 1 & 2 m². The condensate can be collected separately in a receiver or optionally refluxed back into the reactor. Higher area & pressures upto 350 bar Different materials Corrugated tubes heat exchangers for better efficiency / compact size
These are small 7 microns SS 316 sintered cup filters which are threaded to bottom of thesampling dip tube so that the catalyst does not come out while sampling liquid. It is very usefulwhen the catalyst is expensive or pyrophoric. These filters may reduce the rate/ flow of thesampling liquid due to the resistance offered by the fine mesh, hence they need regularcleaning to prevent choking. Filters are available for 500 ml – 100 ltr autoclaves. Optional: Different micron sizes Materials: Hastelloy C
It is used to collect the vent vapours / gases from the autoclave vent / rupture disc /safety valve port, when the vapour / gas is highly hazardous & cannot be releaseddirectly into the atmosphere. It is a pressure vessel, designed depending on volume ofautoclave & its design pressure. It is provided with inlet, outlet, vent, dip tubes, pressuregauge, safety valve & optionally a flame / flash back arrester. It is normally filled withwater. The gases / vapours collected are safely released through the flame / flash backarrester to avoid any hazard. It is suitable & available for any autoclave volume.
Level transmitter (LT) / switch (LS) with indicator to measure or maintain level inside thereactor under high pressure. Used mainly in CSTR.
MFM can be used to measure accurate mass flow rate of gas (in gm/hr or LPH) & totalized quantity of mass / volume (in gms/ltr) charged in the autoclave at any point. Mass flow controller (MFC) is used to charge the set flow rate of gas into the autoclave at high pressures up to 100 bar or it can be used in pressure control mode to indicate the gas flow & total gas uptake to maintain desired set pressure inside the autoclave (ideal for hydrogenation). The same MFM / MFC can be used for multiple gases by just entering the conversion factor for different gas densities provided the gases are inert to each other. The MFM/MFC comes with high pressure flexible hose, inlet filter with digital gas flow indicator cum totalizer & additional pressure PID controller with pressure sensor if the MFC is used in pressure control mode. User has to specify the maximum flow rate range, pressure, gas & mode (flow control or pressure control) for ordering MFM/MFC. Optional Ex-proof MFM / MFC can be offered on request MFM/MFC upto 300 bar pressure
It consists of SS 316 (EO/PO) horizontal pot with inlet, outlet valves, gas inlet with dip tube, thermowell, pressure gauge & high pressure hose pipe for 10 bar working pressure. It is used for ethoxylation / propoxylation. Volume: 1 ltr, 2 ltr & 5 ltr Optional: Ex-proof weighing balance to measure the quantity of EO/PO charged.
SCADA is a supervisory control & data acquisition software with all controllers / indicatorshaving RS 485 modbus communication port or PLC & HMI / touch panel, for online display, setpoint changes & data logging of various parameters like pressure, temperature, motor RPM,motor current / torque, liquid / gas flow rate with totaliser, heater temperature, level, pH, ORP,turbidity, IR etc. remotely from PC as well as locally from panel. It gives continuous online datalogging at predefined (variable) time interval, online graphical representation as well ashistorical data & graphs on PC for single or multiple autoclaves. RS 485-232 convertor & cableupto 50 m or higher is also supplied. Optional: Wireless data communication from PC to panel or mobile alerts can be supplied onrequest
Suitable rotary vane or diaphragm oil fee vacuum pumps can be supplied for vacuumfrom 100 mbar upto 0.001 mbar in the reactor. It is used either before starting the batchor for high vacuum distillation. Suitable analogue or digital vacuum indicator withcontroller can be offered on request. The reactor fittings would change for very highvacuum & this may limit its pressure rating
Ex-proof certified gas purge panels for electrical accessories / utilities like heating coolingcirculators etc.
These are used for higher & accurate gas or liquid flow rate indication or control in cases where thermal mass flow meters are not suitable. A common meter can be used for different gases & liquids for a particular range of flow. Optional Ex-proof CFM/CFC can be offered on request
This system is used to charge liquid at a desired rate from as low as 1 ml/hr to 100 ltr/hr, when the autoclave is under pressurized condition. The system comes with a metering pump, flow indicator, controller, liquid sump, pressure gauge, strainer & high pressure hose. Pressure safety valve, flow totalizer can be offered on request. Types of pumps offered are: Diaphragm metering pumps for pressures upto 100 bar & minimum flow range of 60-600 ml/hr to maximum 10-100 lit/hr. The flow rates are varied by varying the motor speed with variable frequency drive. Materials: SS316, option: Hastelloy C, Titanium, PTFE High pressure more accurate HPLC type low flow metering pumps for high pressures upto 350 bar & flow range from 0.01 upto 100ml/min. These pumps can be used along with precision weighing scales to measure the total liquid charged at any point of time. Materials: SS316, option: Hastelloy C, Titanium High pressure syringe, PTFE diaphragm, gear, peristaltic pumps can be offered for pumping corrosive chemicals at low / high pressures for specific application & flow rate condition. In line flow meters can be connected to measure & control the flow of the liquids.
It is SS 316 regulator mounted on the vent line of the autoclave & is used for maintainingconstant pressure inside the autoclave upto 350 bar. The pressure is maintained by releasing theexcess pressure into the atmosphere or through a hose to safe area. The pressure can be setinitially on the gauge, by manually varying the knob until the gas comes out. Once the setpressure is exceeded the excess pressure is released until the autoclave pressure becomes equalto or below the set pressure. The pressure release is slow & gradual & the set pressure can bevaried at any point. Optional Electronic actuated digital pneumatic back pressure regulator, where the pressureis set digitally & can be released at preset rate of pressure release (6 bar air supplyis required) Pneumatically actuated pilot operated back pressure regulator (air / N gas supply 2for rated pressure is required to activate the same) Electronic control unit & forward pressure regulator with 4 mtr. hose for activating (b) above Materials: Hastelloy C, PTFE etc.
It consists of vertical SS sintered filter cartridges in a SS housing. After the batch is over thereactor liquid is transferred to the catalyst filter under reactor/nitrogen pressure. After filtrationis over, catalyst is taken back in to the reactor by back washing, thus recycling the same & makingit available for the next batch. Thus catalyst is never exposed to atmosphere & is reused.Generally this system is suitable & available for 2 ltr to 2000 ltr reactor volume. These filters areavailable with zero hold-up volume.
Sampling pot with condenser for cooling / condensing & collecting the sample taken at highpressure & temperature