Pilot Plants

High Pressure Processes Group disposes of some Pilots Plants for the study and analysis of a great variety of processes and technologies. The most representatives are described next.

This pilot plant allows the operation for batch PGSS  and for semibatch PGSS – drying processes. PGSS technology allows the precipitation a micronization of thermal sensitive products minimizing the degradiation risks, as high temperature is not necessary. PGSS – drying technology extends the applicability of the PGSS process to aqueous solutions.

Some of the products obtained by PGSS and PGSS – drying are:

  • Microencapsulation of EGCG with OSA-starch, soybean lecithin and β-glucan
  • Solid lecithin – Pluronic L64® encapsulated quercetin particles
  • Encapsulation of copper nanoparticles in lipid microparticles
  • Resveratrol encapsulation with b – glucans and lecithin

Read more about PGSS and PGSS – drying technology 

PGSS Pilot plant is able to operate with a scCO2 flow rate up to 30 kg/h and an solution or suspension flow rate up to 5 kg/h and a maximun solid concentration up to 40%. Operation conditions, as CO2 and emulsion/suspesion flow rate (20 – 40), pressure and temperature at the stactic mixer (45 – 65 ºC), nozzle dimensions and geometry and conditions at drying chamber, might be carefully selected to ensure the system effiency and to control particle size and distribution.

The multipurpose plant for batch PGSS process and for semicontinuous PGSS-drying is equipped with a syringe pump that enables operation at pseudo-stationary pressure conditions.

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Supercritical Antisolvent tecnology (SAS) uses high solubility of supercritical carbon dioxide into the organic solvents to precipitate microparticles and microencapsulated of temperature sensitive materials minimizing degradation. When a saturated solution of the target product and organic solvent is putted in contact with supercritical carbon dioxide, the scCO2 quickly saturated the organic phase and cause the precipitation of the solvent. The use of supercritical carbon dioxide presents also, some advantage as:

  • Low operational temperature, since critical point of carbon dioxide is reached around 30 ºC and 80 bar.
  • Easily recovering of organic solvent and carbon dioxide, by despressurizing after the recuperation of the solid.
  • Final product is obtained completely free of solvent, so no purification stage is needed.

HPPG has more than 15 years of experience of SAS technology. During these years SAS has been applied to many different materials, including: natural compounds such as carotenoids, quercetin, caffeine or herb extracts, pharmaceuticals such as ibuprofen or mandelic acid, inorganic materials such as hydrides, or polymers such as poly ethylene glycol, poly lactic acid or pluronic copolymers.

Read more about Supercritical Antisolvent technology 

HPP group disposes of a semicontinuous Supercritical Antisolven pilot plant with a precipitator volume up to 1 liter, supercritical carbon dioxide flow rate up to 5 kg/h and capables to treat up to 0.5 kg/h of solution.

Operational pressure and temperature at precipitator must be high enough to ensure that carbon dioxide is supercritical. Typical operation conditions are fixed between 8 – 15 MPa and 35 – 55 ºC, and might be selected carefully since size distribution and shape of the particles depends strongly on pressure and temperature.

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Spray drying is a conventional technique for the drying of microparticles and microencapsulated formulations. Spray drying technique is based in the combine effect of hot air stream and a rotatory nozzle for the traetment of aqueous suspensions (low organic solvent content is mandatory because of safety reasons). Rotary nozzle creates suspension micro drops reducing the time need for drying and minimizing the risk of degradation because the temperature.

High Pressure Processes Group disposes of a pilot plant comercial device for spray drying built and comercialized by Niro Mobile Minor. Spray drying pilot plant is available to test the capacitiy of new development technologies but also for the testing of spray drying technology.

Spray drying pilot plant has been suscesfully used for the obtention of so many products like: vaccines and medicaments encapsulations, encapsulations of lecitin liposomes, lavadin essential oil encapsulated in PEG, suspensions of β-glucans and β-carotene nanoparticles and tebuconazole oil-in-water emulsions. Spray drying can be used in conjunction with other pilot plants to obtain complex formulations.

Read more about Spray Drying technology

Spray drying pilot plant available at High Pressure Processes Group facilities is a GEA Niro Mobile Minor MM-Basic-PSR. The apparatus disposes of a rotatory nozzle able to operate in presence of solid or abrassives and a 800 x 620 mm chamber. The system has a suspension capacity between 180 – 660 mL/h and a hot air flow rate up to 80 kg/h. Maximum operational temperature is limited to 200 ºC.

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Coating of nanoparticles is a common stage during nanoparticles formulation, since this way it is posible to enhance or change particles propiertes and adjust them to the needs of final applications. However nanoparticles coating is not a simple process since strong aglomeration forces are present.

This pilot plant, consists into an experimental device for nanoparticles encapsulation by SAS technology. After heating and pressurizing, supercritical carbon dioxide is feeded into the fluidized bed where the nanoparticles are settled. The scCO2 fluidize the particles to the upper part of the vessel, where an organic solution of the coating agent is introduced through a nozzle into the vessel.  When scCO2 contact the coating agent and the ethanol, the scCO2 is disolved into the ethanol and cause the saturation of the solution, during at the same time coating agent precipitates over the nanoparticles.

The pilot plant is composed by three vessels with 1 litre volume respectively. Vessels acts as intermediate storage stage for scCO2, fluidized bed and CO2 recovery stage. Main variables to be taken into account during the process are: the ratio between the velocity of carbon dioxide through the bed and the minimum fluidization velocity, the density of carbon dioxide (depends on temperature and pressure of operation), the flow rate of solution; the concentration of the solution, and the mass ratio polymer-particle.

Carbon dioxide flow rate is up to 40 kg/h. Maxima pressure and temperature are, respectively, 300 MPa and 40 ºC.

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Supercritical fluid extraction (SFE) uses the special propierties of supercritical fluids, like high difusivity and low viscosity, for the separation of one or more than one compounds (extract) from another (matrix). By using supercritical fluid extraction is posible to reduce the time need for the extraction and to operate with a softer conditions (pressure and temperature) what reduce the degradation risk.

Carbon dioxide is used as solvent for the supercritical fluid extraction process because its relative low critical point, its no-toxicity and no-reactivity.

After the extraction, extracted can be easily separated from the supercritical carbon dioxide, obtaining a solvent free extract and reducing the amount of fresh carbon dioxide need for the extraction.

Supercritical fluid extraction has been used for the obtention of different natural compound including: tobacco wastes extract, orange peel extracts and cereal bran extracts.

Supercritical fluid extraction pilot plant has an extractor capacity of 5L, with operating pressure up to 400 bar and temperature up to 80ºC. The CO2 flow (up to 20 kg/h) can be recycled. The separator is refrigerated (temperature down to -20ºC) so the equipment is especially suited for the extraction of flavour and aromatic compounds.

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Pressurized high temperature water can be used for the extraction of natural compounds from biomass matrix. Pressuried high temperature water (PHW), which refers to liquid water with a temperature comprisses between 100 ºC and 375 ºC and with a pressure higher than the vapour pressure, has been used by several authors as extraction medium because its beneficial propierties.

PHW exhibits lower viscosity but higher diffusivity than water at room temperature, which favors the diffusion into the vegetal matrix and the release of compounds. Also high temperature can help to broke linkages between the matrix and the target compound, enchancing the extraction. Finally, PHW does not presents any disadvantages which are related to the need of performing a purification step as happend when organic solvent are used for extraction, so the extracted products can be used directly without purification.

The pilot plant available at HPPG is a multipurpose multi-bed flexible plant, with no limitations for the study of temperature, flowrate, particle size and different materials. Also, it disposes of on-line and off-line measurements system for the biopolymers and sugar characterization.

Hemicellulose from woody biomass and polyphenols from grape seeds have been extracted with this pilot plant.

The system is able to operated with a quantitie of biomass up to 2 kg per batch and with an extraction operational temperature and pressure up to 180 ºC and 10 bar respectively.

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By Microwave intensification it is possible to reach high levels of extraction efficiency minimizing the degradation of the extracts. HPP Group have worked with MAE technology since 2006 and nowadays the group disposes of a pilot plant for continuous microwave assited extraction. Pilot plant is composed by a continuous microwave oven COMPACT GENERATOR with a microwave generator MUEGUE with a capacity of 3 kW a water refrigeration system.

Until now, continuous microwave for assisted extraction has been used for the extraction of antioxidants and polyphenos from grape marc. However its applications are not limited, and this techology could be easly applied to other  high -value vegetable matrix like medicinal plants, wheat bran or microorganisms (wastewater sludge and microalgae).

This equipment was founded as part of the european project WINESENSE and the regional project VA330U13 founded by Junta de Castilla y León.

Read more about Microwave intensification techniques

Continuous microwave is able to operate with a maximun flow rate up to 20 L/h and a solid concentration up to 0.75 – 1.00 kg/L feed by a perilstaltic pump. Maximum operation temperature is limited to 120 ºC

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This pilot plant uses subcritical water, high pressure and temperature water but below critical point, to hydrolyze biomass for the continuous obtention of hemicellulose and other bioproducts or biopolymers. Subcritical water hydrolisis posseses some advantages respect to the supercritcal water hydrolisis:

  • Lower energetic cost, since lower temperatures and pressures are need
  • Lower product’s degradation ratio, no furfural or HMF produced.
  • No toxic residues are generated, since water is the only reactive used

During the desing and construction of this pilot plant some operational considerations have been take into account:

  • more than 95% of energetic saving is achived thanks to an energetic exchange system at product stream and sample;
  • easily and quick operation with low interaction between the researcher and the aparatus;
  • quick shift of exhausted solid, process stop is not necessary for refilling;
  • no particle size limitations, different biomass could be used.

Until now, continuous multistage pilot plant for biomass hydrolisis whit subcritical water have been used with wood from several trees, wheat bran, coffee by – products and beet pulp.

Multistage pilot plant for subcritical water hydrolysis is constituted by 5 independent reactors that could be used individually or combined as the same system. Each reactor has a volume of 1 l, which it involves a total reactor volumen of 5 l. Maxima operational pressure and temperature are 20 bar and 180 ºC, althought operational conditions has to been selected according to the biomass caractheristics and the final product desired. This pilot plant is capable to operate with a subcritical water flow rate up to 30 l/h.

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Hydrolisis of biomass by supercritical water responds to the the challenge of developing a selective technology to transform biomass into sugars and chemicals in very short reaction times. 

This pilot plant is constructed as a re-scale of the Ultra fast Hydrolysis Pilot Plant (Project FASTSUGARS). By this new design, pilot plant’s capacity have been increseased 3 times.

Also so operational improvements have been desing and development as a filter previous to the expansive stage to recover the non-hydrolized lignin (higher yield) and a multistage heater system more stable than the heater used in previous designs.

This pilot plant for the continuous hydrolisis of biomass with supercritical water is able to operate at conditions up to 400 ºC and 250 bar with a capacity up to 40 kg/h and biomass’ flow rate up to 15 kg/h keeping a reaction time shorter than 1 second.

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The solution/suspension of biomass is continuously pumped to the operation pressure and instantaneously heating by injecting a stream of supercritical water at the inlet of the reactor. The effluent is suddenly depressurized at the outlet of the reactor without previous cooling in order to instantaneously stop the reaction, reducing in this way its temperature down to 150ºC. This system configuration has so main advantages:

  • (a) the reactor can be considered isothermal due to the instantaneous heating and cooling
  • (b) the products are not diluted in the cooling water
  • (c) the residence time can be varied from 0.004 s to 50 s by using different reactors what supposed a great versatility for the process’ analysis

This plant was founded by the national project FASTSUGARS

Read more about Ultra Fast Hydrolysis Technology

Ultra fast Hydrolysis Pilot Plant consists of a continuous sub- and supercritical continuous hydrolysis plant able to work at conditions up to 400ºC and 30 MPa, supercritical water flow of 10 kg/h  and biomass suspension flows of 3 l/h with a solid concentration up to 20%w/w.

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As part of the project AQUA CO2NV,  HPPG has designed and built a new continuous pilot plant for the hydrothermal reduction of carbon dioxide. In presence of a reduction agent and an aqueous medium and high pressure and temperature, carbon dioxide can be transform into chemicals and fuels such as formic acid, methanol or methane. This process presents some advantages in comparisson with other systems form CO2 reduction: can be easily integrated in common industrial processes and no free hydrogen is present in the process (hydrogen is introduced as water).

This pilot plant has been funded by the Spanish Ministry of Economy and Competitiveness through project ENE2014-53459-R, “AQUA-CO2NV”.

The facilities can work with flows between 0.05 and 10 mL/min, which will allow working with residence times from a few seconds to several hours. The working pressure limit is 250 bar. The range of working temperature is between 275ºC and 600ºC.

This new versatile plant will allow to study different technical solutions to develop a continuos process such as working at semi-batch regime, mixing streams with different catalyst or reagents at different steps and residence times or measuring kinetics parameters at different residence times and temperature.

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This plant was designed and built for the study and analisys of the oxidation reaction on conditions above the supercritical point of water. On these conditions supercritical water acts as a solvent for organic substances and is completely miscible with gases including oxygen and carbon dioxide, that minimizes interphase restrictions and mass transfer limitations. This technology has been suscessfully used for the treatment of: ammonia, isopropanol, residues with high concentration of nitrogen compounds and wastewater with high concentration of coolants from mechanical manufacturing. This plant has been development with the founding from several national projects and diferent programms (346/PC/08/3-04.3 and A569/2007/3-04.3 )

Read  more about Supercritical Water Oxidation Technology 

This pilot plant has a maximum treatment capacity of 40 kg/h and uses air as an oxidant. It works with reaction temperatures as high as 600-650 ºC and pressures of 23 MPa (max pressures 30 MPa).

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This demostration plant for Supercritical Water Oxidation was built to complement and validate the experimental results obtained with the SCWO Pilot Plant. It is located in the site of the industrial plant CETRANSA in Santovenia de Pisuerga (Valladolid, Spain), and it has been tested for treatment of aqueous solutions with a high concentration of ammonia and high concentration of isopropanol.

Read  more about Supercritical Water Oxidation Technology 

SCWO Demostration plant has a treatment capacity of 200 kg/h of waste using oxygen as oxidant. It works with reaction temperatures as high as 600-650 ºC and pressures of 23 MPa (max pressures 30 MPa).

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Wet Air Oxidation Pilot Plant uses subcritical water and  air as hydrothermal treatment for high recalcitrant wastewaters that can not be treat by conventional methodos, like regular oxidation or bioprocesses.  Pilot plant disposes also of a heat recovery system that acts as a preheater for inlet stream and reduces energy consumption. This pilot plant was built in collaboration with Repsol as part of common project (WETOXI).

Read more about Wet Air Oxidation tecnology 

WAO pilot plant built and operated by HPP group has a capacity of 10 ml of efluent/min with a volumen reactor of 1 litre and maxima operational pressure and temperature of 100 bar and 300 ºC.

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