MIXCEL : Une cellule calorimétrique haute pression agitée

MIXCEL : Une cellule calorimétrique haute pression agitée (2014). Magazine Emergence(s) : les faits marquants de la recherche à l’UPP

Cellule de mesure calorimétrique haute pression agitée mécaniquement avec système de contrôle dynamique de pression, et dispositif de support pour cette cellule (High-pressure calorimetric measurement cell)

La présente invention concerne un ensemble d’une cellule de mesure calorimétrique et d’un dispositif de support de cette cellule de mesure, ainsi qu’un calorimètre comportant un tel ensembl

Development of a new type of high pressure calorimetric cell, mechanically agitated and equipped with a dynamic pressure control system: Application to the characterization of gas hydrates

A novel prototype of calorimetric cell has been developed allowing experiments under pressure with an in situ agitation system and a dynamic control of the pressure inside the cell. The use of such a system opens a wide range of potential practical applications for determining properties of complex fluids in both pressurized and agitated conditions. The technical details of this prototype and its calibration procedure are described, and an application devoted to the determination of phase equilibrium and phase change enthalpy of gas hydrates is presented. Our results, obtained with a good precision and reproducibility, were found in fairly good agreement with those found in literature, illustrate the various interests to use this novel apparatu

Experimental and modeling investigations of adsorption-induced swelling and damage in microporous materials

International audienceThe purpose of this work is to achieve a better understanding of the coupling between adsorption and swelling in microporous materials. This is typically of utmost importance in the enhancement of non-conventional reservoirs or in the valorization of CO 2 geological storage. We consider here the case of fully saturated porous solids with pores down to the nanometer size (≤ 2nm). Hardened cement paste, tight rocks, activated carbon or coal are among those materials. Experimentally, different authors tried to combine gas adsorption results and volumetric swelling data, especially for bituminous coal. However, most results in the literature are not complete in a sense that the adsorption experiments and the swelling experiments were not performed on the exact same coal sample. Other authors present simultaneous in-situ adsorption and swelling results but the volumetric strain is extrapolated from a local measurement on the surface sample or by monitoring the two-dimensional silhouette expansion. Only elastic and reversible swellings are reported in the literature. Theoretically, most continuum approaches to swelling upon adsorption of gas rely on a coupling between the adsorption isotherms and the mechanical deformation. A new poromechanical framework has been recently proposed to express the swelling increment as a function of the increment of bulk pressure with constant porosity. However, this framework has to be extended to take into account the porosity evolution upon swelling. This paper aims at presenting a new experimental setup where both adsorption and strain are measured in-situ and simultaneously and where the full-field swelling is monitored by digital image correlation. Permanent strain and damage are observed. On the other hand, we present an extended poromechanical framework where the porosity is variable upon swelling. A new incremental nonlinear scheme is proposed where the poromechanical properties are updated at each incremental pressure step, depending on the porosity changes. Interactions between swelling and the adsorption isotherms are examined and a correction to the classical Gibbs formalism is proposed. Predicted swellings are compared with results from the literature

Kinetics of CO2 Capture by Hydroquinone Clathrates

Organic clathrates formed by combining hydroquinone (HQ) and CO2 could offer very interesting prospects in the near future, particularly in the field of CO2 capture and storage. However, one of the main limitations hindering the large-scale deployment of this type of clathrate-based technology is the slow enclathration kinetics. Our experiments, performed at different pressures (1.5, 3.0, and 4.5 MPa) and temperatures (298, 323, and 348 K), with HQ in different forms (HQ powder, HQ pellets, and HQ–silica composites, each different in nature and in terms of pore size and HQ content) demonstrated that (i) an increase in both pressure and temperature enhances the enclathration rate, (ii) the textural properties of HQ significantly impact kinetics, and composite materials remain the most efficient for improving HQ clathrate formation kinetics

An Innovative High Pressure Mixing Cell for Microcalorimetry: Application to Gas Hydrates.

High pressure differential scanning calorimetry (HP-DSC) is of importance in several fields involving “gas hydrates”, such as oil and gas production, flow assurance, carbon dioxide capture and storage, and refrigeration. Gas hydrates are icelike crystals that contain gas molecules in molecular cavities. To improve classical calorimetric cells used for gas hydrates characterization, we present here our last prototype: a calorimetric cell equipped with an in-situ mechanical agitation system, which allow performing experiments both under pressure and agitated conditions. The m-cell, called MICROMIXCELL®, was developed for micro-calorimetry analysis (experiments carried out using a mDSC7 evo from SETARAM Instrumentation). In this work, thermophysical properties of the cyclopentane hydrate − a “model” clathrate hydrate which forms at atmospheric pressure − were measured. Technical details of the system and results are given and commented. The use of such novel calorimetric mixing cells opens a wide range of possibilities for the analysis of complex fluids, which must be analyzed in both pressurized and agitated conditions

A novel stirred microcalorimetric cell for DSC measurements applied to the study of ice slurries and clathrate hydrates

A novel prototype of a microcalorimetric cell with in-situ stirring has been developed to per-form DSC measurements under atmospheric or pressure conditions. After a brief technical description of the apparatus, preliminary tests are presented which analyzed the influ-ence of the stirrer rotation on the heat-flow signal. Experiments were then performed with complex fluids such as ice slurries and clathrate hydrates formed with cyclopentane and with carbon dioxide. They took place in stirred and non-stirred conditions and the results obtained were then compared. It was proven that the rotation of the microstirrer in the measuring cell does not disrupt the heat-flow signal during the analysis. As regards the prac-tical applications tested, the in-situ stirrer efficiently reduces crystallization metastability, increases the water-to-hydrate conversion, and reduces the amount of time needed for anal-ysis. The dissociation enthalpy of cyclopentane (CP) hydrates was measured at atmospheric pressure; it is effectively very difficult to analyze this system with non-stirred calorimetry techniques because the two liquid phases are immiscible. The experimental results, in good agreement with other data found in the literature, showed complete water-to-CP hydrate conversion within a short period of time using a simple protocol. Experiments were also performed under pressure to demonstrate that CO2 hydrate phase equilibrium data could be obtained rapidly and easily. It is therefore our opinion that the potential of this novel technology has been thoroughly demonstrated

Recent improvements in the differential scanning calorimetry methods applied to the study of gas hydrates.

Recent improvements in the differential scanning calorimetry methods applied to the study of gas hydrates

Recent improvements in the high pressure differential scanning calorimetry method applied to the study of gas hydrates.

A novel prototype of calorimetric cell has been developed and the technical details of the system and typical results are presented. It was demonstrated that this invention allows performing experiments under pressure, potentially up to 200bar with an in situ stirring system. The demonstration focuses particularly on the determination of the enthalpy variation and temperature of dissociation of CO2 hydrate and a positive comparison with published data. The use of such a system thus opens a wide range of potential practical applications for determining properties of complex fluids in both pressurized and agitated conditions

Media réactif comprenant un support poreux imprégné d’un composé organique capable de former des clathrates de gaz, et son utilisation pour la séparation et le stockage de CO2

L'invention concerne un média réactif comprenant un support poreux sur lequel est déposé, sous forme solide, un composé organique capable de former des clathrates de gaz. L'invention concerne également un procédé de séparation du CO2, présent dans un mélange de gaz, dans lequel une capture du CO2 est réalisée par enclathration au moyen dudit média réactif. L'invention porte aussi sur des réacteurs permettant la mise en oeuvre dudit procédé