Tailoring the crystal size distribution of an active pharmaceutical ingredient by continuous antisolvent crystallization in a planar oscillatory flow crystallizer

Cruz, Paulo Teixeira da; Álvarez, Carlos Márquez; Rocha, Fernando; Ferreira, António

doi:10.1016/j.cherd.2021.08.030

Cited by 10 publications

(10 citation statements)

References 21 publications

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“…Antisolvent precipitation or organic displacement crystallization is an energysaving alternative that offers interesting possibilities to better control the crystallization process [9]; this technique is based on changing the solubility of the solute and creating a supersaturated solution by adding a water-miscible organic solvent to force the solute to precipitate [10]. This technique is widely used in the pharmaceutical industry [11][12][13][14][15].…”

Section: Introductionmentioning

confidence: 99%

Antisolvent Precipitation for Metal Recovery from Citric Acid Solution in Recycling of NMC Cathode Materials

Xuan

Chagnes

Xiao

et al. 2022

Metals

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Lithium-ion batteries (LIBs) are widely used everywhere today, and their recycling is very important. This paper addresses the recovery of metals from NMC111 (LiNi1/3Mn1/3Co1/3O2) cathodic materials by leaching followed by antisolvent precipitation. Ultrasound-assisted leaching of the cathodic material was performed in 1.5 mol L−1 citric acid at 50 °C and at a solid-to-liquid ratio of 20 g/L. Nickel(II), manganese(II) and cobalt(II) were precipitated from the leach liquor as citrates at 25 °C by adding an antisolvent (acetone or ethanol). No lithium(I) precipitation occurred under the experimental conditions, allowing for lithium separation. The precipitation efficiencies of manganese(II), cobalt(II) and nickel(II) decreased according to the order Mn > Co > Ni. The precipitation efficiency increased when a greater volume of antisolvent to the leachate was used. A smaller volume of acetone than ethanol was needed to reach the same precipitation efficiency in accordance with the difference in the dielectric constants of ethanol and acetone and their associated solubility constants. After adding two volumes of acetone into one volume of the leach liquor, 99.7% manganese, 97.0% cobalt and 86.9% nickel were recovered after 120 h, leaving lithium in the liquid phase. The metal citrates were converted into metal oxides by calcination at 900 °C.

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Section: Introductionmentioning

confidence: 99%

Antisolvent Precipitation for Metal Recovery from Citric Acid Solution in Recycling of NMC Cathode Materials

Xuan

Chagnes

Xiao

et al. 2022

Metals

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“…Control of crystal size and distribution is critical in the pharmaceutical industries to ensure rigorous quality requirements in the manufacturing of APIs . The manufacturing of APIs involves a variety of unit operations including crystallization followed by filtration, drying, and, in many cases, size reduction operations such as milling, which has a direct impact on downstream operations and end-use properties of the product . The control of crystal size most importantly helps in regulating bioavailability and absorption of poorly soluble drugs in the gastrointestinal tract …”

Section: Results and Discussionmentioning

confidence: 99%

Control of Antisolvent Mass Transfer through Porous Membranes for the Crystallization of Organic Compounds

Chergaoui

Debecker

Leyssens

et al. 2023

Crystal Growth & Design

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Crystallization faces great challenges from the point of view of technology readiness, process economics, and energy consumption. Membranes are capable of controlling both energy and mass transfer, and they can lead to major improvements if integrated into antisolvent crystallization processes, for example, limiting unfavorable kinetics and thermodynamics that are responsible for undesired crystal size and shape. In this work, membrane-assisted antisolvent crystallization (MAAC) was used to crystallize the amino acid l-serine. Two commercial membranes made of polyvinylidene fluoride and polypropylene with water contact angles of 130° and 150°, respectively, allowed a controlled antisolvent crystallization. These membranes controlled the transmembrane mass transfer of antisolvent (ethanol) under different feed and antisolvent velocities at ambient conditions. In all cases, a narrow crystal size distribution of l-serine was obtained reflected in a coefficient of variation (CV) of 31–37%, compared with batch antisolvent crystallization or drop-by-drop crystallization where the CV was 63 and 54%, respectively. Thanks to the measurement of l-serine and ethanol concentration along the operating time, the mass transfer coefficient of MAAC was evaluated. Increasing the antisolvent or the crystallizing solution velocity showed that a too high value of one or the other could result in wetting or system blockage (inside the membrane contactor, module, or tubing). This study explains the transmembrane mass transfer in MAAC and the resulting crystal properties.

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“…112 Control over how and where material nucleates will prevent unwanted nucleation on the walls of the reactor, which, if unchecked, will lead to fouling, back-mixing, and eventually blockage. The use of antisolvent addition, 113 rapid cooling, 114 or sonication 115 to force material to nucleate can be highly effective. Flow-focusing geometries can direct the location of nucleation away from the reactor walls, further ameliorating encrustation, particularly in microreactors 116,117 (Figure 3).…”

Section: ■ Solids−the Nemesis Of the Flow Chemist?mentioning

confidence: 99%

Quid Pro Flow

2023

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How do you get into flow? We trained in flow chemistry during postdoctoral research and are now applying it in new areas: materials chemistry, crystallization, and supramolecular synthesis. Typically, when researchers think of "flow", they are considering predominantly liquid-based organic synthesis; application to other disciplines comes with its own challenges. In this Perspective, we highlight why we use and champion flow technologies in our fields, summarize some of the questions we encounter when discussing entry into flow research, and suggest steps to make the transition into the field, emphasizing that communication and collaboration between disciplines is key.

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Tailoring the crystal size distribution of an active pharmaceutical ingredient by continuous antisolvent crystallization in a planar oscillatory flow crystallizer

Cited by 10 publications

References 21 publications

Antisolvent Precipitation for Metal Recovery from Citric Acid Solution in Recycling of NMC Cathode Materials

Antisolvent Precipitation for Metal Recovery from Citric Acid Solution in Recycling of NMC Cathode Materials

Control of Antisolvent Mass Transfer through Porous Membranes for the Crystallization of Organic Compounds

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