pilot plant extraction unit · the temperature rating is ususally set for co2 extraction, but it...

79 rue Marinoni 77013 VAUX LE PENIL CEDEX FRANCE

T : +33 (0) 1 64 10 45 50 F : +33 (0) 1 64 37 62 08

info@top‐industrie.fr www.top‐industrie.com 0917

In view of possible technological advances in our production methods, the products described in this manual are liable to be modified without prior notice.

DESIGN FEATURES :

• Extractor autoclave:

‐ The extraction autoclave is a stainless steel vessel with full opening at the top and a singlescrew type lid. The lid is manufactured in 2 parts and is supplied with special lip seal allowing closingwithout tool. The thread is coated on the surface to prevent damaging the threads and crippling thelid in the vessel allowing intense use.

‐ The autoclave is supplied with a basket used to store the solid material to be extracted. Itconsists in a stainless steel tube closed by 2 filtering disks. As the basket is sealed around vessel wall,the CO2 is forced to percolate through the feed. A safety system prevent pressure accumulation insidethe basket

‐ When processing liquid feed, the basket can be filled with mass transfer packing and the liquidis filled in the basket.

‐ The vessel is heated on the side, with electrical resistance equipped with both temperaturecontrol and safety temperature probe. The temperature rating is usually set for C02 extraction, but itcan also be set so that subcritical water can be used as an option.

The temperature rating is ususally set for CO2 extraction, but it can also be set so thatsubcritical water can be used as a option.

PILOT PLANT EXTRACTION UNIT

Supercritical Pilot plants for semi‐industrial uses and process development.

Extraction Process Principle:Liquid carbon dioxide is pumped by a cooled‐head dosing pump. CO2 is pressurized and sent to a heatexchanger. It is heated, becomes supercritical and is flowing to the main vessel for the extraction orthe process to be realized.

Depending on the process, it will be possible to adapt the flow circulation, use an agitated vessel, fillthe vessel with an adsorbent, or use different instruments for characterization or optimizing thecontact between the product to be treated and the supercritical fluid. It is also possible to add a co‐solvent or other products to change the properties of the fluids.

At the exit of the main vessel, the mixture is depressurized, and products are separated from CO2 inone or more separators working at lower pressure. Depending on separation conditions, productfractionation can be achieved.CO2 leaving the separators can be either vented or recycled through a condenser to be sent again tothe pump.

‐ Complete equipment supply including utilities (warm water at several temperature levels,cooling fluid for solvent condensation...).‐ The supply from the client is limited to electricity, CO2 supply in cylinders, and a ventconnection.‐ Simple and strong equipment with sophisticated automation supplied with spare parts for atleast one year of intense operation (further supply of spare parts is guaranteed).‐ Design and Construction achieved with Quality Assurance and 30 years of High PressureExperience.‐ Start‐up assistance, training on operation, and the experience of process development.

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Main standard sizes are 1L, 2L, 5L and 20L.

‐ For each specific application, TOP INDUSTRIE can advise on the most suitable way to preparethe feed and the best way to contact the feed with the solvent to optimize the extraction.TOPINDUSTRIE can propose different process option around the extraction vessel : reaction/mixingvessel, second vessel.

• Pumps:CO2 pump:‐ Volumetric pumps with jacketed head(s) for efficient cooling. For optimal reliability, and limitmaintenance and operation costs, TOP INDUSTRIE integrates its own HP flow pumps. Similar solutionswill be used for production plants.

‐ CO2 flow rate is regulated by the motor pomp frequency variation. It is controlledautomatically with a frequency variator and a Coriolis mass flow meter that gives an indication of theflow rate of the fluid at the inlet of the extractor.

Option : Co solvent pump. Piston pump with flow rate control, jacketed head, priming valves,pressure safety.

• Cold and heat exchangers:‐ Condenser: The condenser is put on the line before the CO2 pomp. It allows to liquefy thegaseous CO2 coming from CO2 make up or after recycling. It is cooled by a propylene glycol /watermixture.

‐ An air‐cooled chiller is also supplied to provide this propylene glycol /water mixture chilled at0°C and necessary in the condenser and in the pump head. This chiller must be placed outside or in aventilated area.

Pre‐heater: The pre‐heater after the pomp allows to pre‐heat the mix CO2/Solvent before theheater.

‐ Heater: The electrical heater allows to heat the CO2 after the pump in a range of temperaturesfrom 20 to 150° C. It is independently heated from the extractor for an optimum versatility.

• Separators:TOP INDUSTRIE is supplying high pressure / high performance separators allowing an efficient solvent /extract separation with good control of the flow pattern in the separation vessel. The separators canoperate in parallel or in serie at different pressure to make extracts fractionning by the pressure.A special design is proposed to maximize extract recovery in each separator, minimize CO2 losses atthe bottom of separators and minimize plugging issues when viscous extract are collected.With a full and easy opening, it also efficient cleaning to save time and limit cross contaminationbetween batches or between products.Each separation step is pressure controlled and a process temperature probe is supplied for preciseseparation condition knowledge.

OPERATION:Basic configuration is proposed with one step and one separator. Other configurations with two orthree separators can be proposed optionally in our systems.


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The unit is controlled by an operator from a control box where temperature PID controllers, pressureand temperature indicators are displayed. It allows control of alarm parameters choice, detection andrecord.Back pressure regulators control extraction and separator pressures.Flow rates are controlled on the pumps.Process configuration valves are manually operated directly on the equipment. Control from the PC ofall process parameters and data logging is available in option.Optionally, all configuration valves can also be controlled remotely from the PC.

Autoclave sizes and equipments can be taylor‐ made according to your needs and technicalrequirements.

Main standard systems are :

• SFE 1 :‐ Extractor : volume 1 L, service pressure 400 bars, service temperature 150°C‐ One separator : 250 mL, service pressure 200 bars, service temperature 100°C‐ C02 pump : flow rate from 0,5 to 5 L/h

• SFE 2 :‐ Extractor : volume 2 L, service pressure 600 bars, service temperature 150°C‐ 2 separators : 500 mL each, service pressure 200 bars, service temperature 100°C‐ C02 pump : flow rate from 0,5 to 5 L/h

• SFE 5 :‐ Extractor : volume 5 L, service pressure 600 bars, service temperature 150°C‐ 2 separators : 500 mL each, service pressure 200 bars, service temperature 150°C‐ C02 pump : flow rate 0,5 to 5 L/h

• SFE 20 :‐ Extractor : volume 20 L, service pressure 600 bars, service temperature 150°C‐ 2 separators : 1 L each, service pressure 200 bars, service temperature 150°C‐ C02 pump : flow rate 0,5 to 5 L/h

OPTIONS FOR ALL SYSTEMS :‐ Other pressures are possible (400 bar ‐ 1000 bar)‐ Co‐solvent pump‐ CO2 recycling line with CO2 condenser‐ Addition of an visualization cell‐ Second extractor for other processes like extract fractionation‐ Possibility to add an extraction column for liquid fractioning‐ Designed for subcritical water extraction


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Our SFE2 extraction plant

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pilot plant extraction unit · the temperature rating is ususally set for co2 extraction, but it...

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