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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. PILOT PLANT MIXED UNIT This system is design to be very modular and to be adapted to all current supercritical fluid processes like extraction, liquid fractionation, reaction, impregnation. Our "mixed units" are gathering the best features of our batch extraction units for solid feedstocks and of our liquid fractioning columns for liquid feedstocks. Extraction : The extraction equipment is composed of CO2 and co solvent pumps, CO2 heater, extraction vessel with different extraction cells, and 2 to 3 separators in series. A sampling loop system also allows to collect extract under pressure and in parallel to the separators for real time on‐line analysis on analytical equipment. For more information about the extraction process, please refer to the datasheet "Pilot plant ‐ extraction unit". Liquid fractionation column: In the standard extraction system, a liquid feed is injected in batch mode in the extractor. In this system we propose a complementary counter‐current column filled with mass transfer packing for a continuous and more selective treatment of a liquid feed to be fractionated by CO2. CO2 is injected in an injector close to the bottom of the column, as the feed is injected close to the top or between the jacket sections. Light extract is recovered at the top of the column and non‐ extracted part of the liquid (called raffinate) is recovered at the bottom. For more information about the fractionning process, please refer to the datasheet "Pilot plant ‐ Fractionning unit". Reaction : The vessel can be equipped with a magnetic mixer with a propeller to provide an efficient mixing of the mixture. The reaction can then be carried out either in batch or in continuous mode as the 2 pumps allows to inject. A second smaller vessel is supplied equipped with sapphire windows. The operation can observe phase behaviour when filled with a mixture of components. Particle formation : The system will be designed to be configured with the 2 main particle formation process described in literature call RESS and SAS. Impregnation : As this system enclosed 2 high pressure vessels, we can configure impregnation processes. This can be implemented by extracting a component in the first vessel and operating the second vessel in different conditions. We can this way imagine processes like deposition or impregnation of a naturel extract on an excipient. DESIGN FEATURES For extractor autoclave, pomps, fractionning columns, separators, cold and heat exchangers, pumps, please refer to "Fractionning unit" and "Extraction unit" datasheets. Pressure collection Pressure is controlled very precisely with back‐pressure regulator. The mixture is heated in the case of CO2 extraction, cooled in the case of subcritical water extraction. T2cA

PILOT PLANT MIXED UNIT - top-supercritical.com...The extraction equipment is composed of CO2 and co solvent pumps, CO2 heater, extraction vessel with different extraction cells, and

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Page 1: PILOT PLANT MIXED UNIT - top-supercritical.com...The extraction equipment is composed of CO2 and co solvent pumps, CO2 heater, extraction vessel with different extraction cells, and

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.

PILOT PLANT ­ MIXED UNIT

This system is design to be very modular and to be adapted to all current supercritical fluid processeslike extraction, liquid fractionation, reaction, impregnation.Our "mixed units" are gathering the best features of our batch extraction units for solid feedstocks andof our liquid fractioning columns for liquid feedstocks.

Extraction :The extraction equipment is composed of CO2 and co solvent pumps, CO2 heater, extraction vesselwith different extraction cells, and 2 to 3 separators in series. A sampling loop system also allows tocollect extract under pressure and in parallel to the separators for real time on‐line analysis onanalytical equipment.For more information about the extraction process, please refer to the datasheet "Pilot plant ‐extraction unit".

Liquid fractionation column:In the standard extraction system, a liquid feed is injected in batch mode in the extractor.In this system we propose a complementary counter‐current column filled with mass transfer packingfor a continuous and more selective treatment of a liquid feed to be fractionated by CO2.

CO2 is injected in an injector close to the bottom of the column, as the feed is injected close to thetop or between the jacket sections. Light extract is recovered at the top of the column and non‐extracted part of the liquid (called raffinate) is recovered at the bottom. For more information aboutthe fractionning process, please refer to the datasheet "Pilot plant ‐ Fractionning unit".

Reaction :The vessel can be equipped with a magnetic mixer with a propeller to provide an efficient mixing ofthe mixture. The reaction can then be carried out either in batch or in continuous mode as the 2 pumpsallows to inject.A second smaller vessel is supplied equipped with sapphire windows.The operation can observe phase behaviour when filled with a mixture of components.

Particle formation :The system will be designed to be configured with the 2 main particle formation process described inliterature call RESS and SAS.

Impregnation :As this system enclosed 2 high pressure vessels, we can configure impregnation processes.This can be implemented by extracting a component in the first vessel and operating the second vesselin different conditions. We can this way imagine processes like deposition or impregnation of a naturelextract on an excipient.

DESIGN FEATURESFor extractor autoclave, pomps, fractionning columns, separators, cold and heat exchangers, pumps,please refer to "Fractionning unit" and "Extraction unit" datasheets.

Pressure collectionPressure is controlled very precisely with back‐pressure regulator.The mixture is heated in the case of CO2 extraction, cooled in the case of subcritical water extraction.

T2cA

Page 2: PILOT PLANT MIXED UNIT - top-supercritical.com...The extraction equipment is composed of CO2 and co solvent pumps, CO2 heater, extraction vessel with different extraction cells, and

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

Extract is collected at atmospheric pressure into vials, filled or not with solvent.Three separators are supplied to have versatile extract fractionation possibilities.These stainless steel separators are working under pressure up to 200 bar, and allow CO2 recycling (inthe CO2 configuration). Working with HP separator allows to minimize solvent consumption, ease theseparation, raise collection efficiency and limits plugging problems.They also permit extract fractionation operating them at different pressure.

The 3rd separator is designed to be used either like the first two to fractionate the extract accordingto pressure, or as an adsorption bed that would be more efficient for volatile fraction collection.

Extract is collected at atmospheric pressure in vials.

Continuous liquid feed treatment moduleThis module is placed on a separate skid. It is a turn‐key solution for liquid fractionation and iscomposed of a liquid pump to feed the fractionation column with all valves and instrumentationmounted on a skid. Column is heated with a jacket and a view port allows to control liquid level at thebottom of the column. A programmable automated valve controls the raffinate recovery.

OPERATIONThe unit is controlled from a PC ensuring the following functionalities:• Display of all parameters in a synoptic view of the process• Process parameter choice and record• Alarm parameters choice, detection and record• Curve display of all parameters• Storage of all process parameters on data files

Configuration valves remains manually operated by the operator directly on the equipment.

Autoclave size and equipments are taylor‐ made according to your needs and technical requirements.

PILOT PLANT ­ MIXED UNIT

OUR MAIN STANDARD SYSTEMS ARE :

• SCF 1 :‐ Extractor : 1 L, C02 extraction service pressure up to 1000 bar and temperature up to 150°C,subcritical water (and other organic solvents) extraction service pressure up to 300 bar andtemperature to 250°CSecond 100 mL vessel equipped with 2 Sapphire windows‐ 2 to 3 separators : service pressure 200 bar‐ CO2 pump : service flow rate from 0 to 60 L/h of C02 at 1000 bar, from 0 to 100 mL/h of water orliquid solvent at 300 bar‐ Co‐solvent pump : 0 to 5 L/h up to 400 bar‐ Fractionation column : column height 2 m with 2 levels, diameter 17 mm, design pressure 350 bar,design temperature 150°C‐ Full automation for remote control

T2cA

Page 3: PILOT PLANT MIXED UNIT - top-supercritical.com...The extraction equipment is composed of CO2 and co solvent pumps, CO2 heater, extraction vessel with different extraction cells, and

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

PILOT PLANT ­ MIXED UNIT

Our fractionning and extraction plantin Perou

OUR MAIN STANDARD SYSTEMS ARE :

• SCF 2 :‐ Extractor : 2 L, C02 extraction service pressure up to 1000 bar and temperature up to 250°C‐ 2 to 3 separators : service pressure 700 bar, service temperature from 20 to 100°C‐ CO2 pump : service flow rate from 4 to 25 L/h of liquid C02 at 350 bar‐ Co‐solvent pump : 0 to 5 L/h‐ Fractionation column : column height 3 m with 3 levels, diameter 30 mm‐ Full automation for remote control‐ Options available : second 30 L extractor with service pressure 350 bar, service temperature 100°Cfor other processes like adsorption/chromatography or extraction PGSS, C02 pump service pressure at700 bar and flow at 30 L/h

• SCF 5 :‐ 2 extractors : 5 and 20 L, C02 extraction service pressure up to 600 bar and temperature from 20 to100°C‐ 2 to 3 separators : 1 L, service pressure 350 bar, service temperature from 20 to 100°C‐ CO2 pump : service flow rate from 20 to 100 L/h at 600 bar‐ Co‐solvent pump : from 4 to 15 L/h, load pump from 1 to 5L/h‐ Fractionation column : column height 4 m with 4 levels, diameter 60 mm, design pressure 350 bar,design temperature from 20 to 140°C‐ Full automation for remote control

OPTIONS FOR ALL SYSTEMS :­ Other pressures are possible‐ Longer column‐ Addition of an extraction cell‐ CO2 recycling line with CO2 condenser

T2cA