Poster Reception
Session Chair:
- Anne Mohan, Merck
Session Description:
The poster reception will feature a mix of poster presentations from both industry and academia. As attendees mingle between posters, hors d'oeuvres and drinks will also be served.
As process development scientists, we face wide variety of issues from sensitive reactions to complex separations as we move from lab scale research to pilot scale demonstrations. It is essential to create a smooth transition to commercialization to bring a new product to market successfully. This poster session will cover diverse topics from experimental to modeling studies in process optimization to process scale-up issues across industries from pharmaceuticals to specialty chemicals. The purpose of this session is to allow presenters and symposium participants to have lively discussions on specific topics as well as give them immense opportunity to learn from each other’s experiences.
*All session and speaker information is subject to change pending finalization
Schedule:
The Poster Session will formally take place from 5:00pm - 6:00pm, followed by open networking. Posters will be available for viewing throughout the full reception.
Abstracts:
Process Development of Opteon® yf – Innovating to Meet Market Challenges
Karl Krause, The Chemours Company
Regulatory response to climate change, first enacted in Europe, required development of a low global warming potential (GWP) refrigerant for vehicles on an accelerated timetable. Innovative approaches to identify a drop-in replacement for the legacy refrigerant, achieve market acceptance, develop a process for first-to-market commercial production, and develop an improved process for larger scale production will be described in this poster. Key aspects include parallel process development programs, partnerships for process development and commercialization, strong intellectual property protection, leveraging of existing processes coupled with development of new technology, and process simplification.
Enabling Rapid Process Development for a Challenging Salt Crystallization
Anne Mohan, Merck
The final chemical transformation and isolation in the synthesis of an Active Pharmaceutical Ingredient (API), referred to as the Pure Step, is often chemically simple but scientifically, operationally and strategically the most challenging. Pure step development is critical because it is used to determine and support the critical quality attributes (CQAs) for the API, which will have lasting impacts on the process. This poster will detail specific challenges for an API that is isolated as a citrate salt, crystallized out of methanol and isopropanol. This citrate salt is then formulated via direct compression to make the deliverable for the patient. The salt crystallization is particularly challenging due to: (1) the propensity of the citrate salt crystal to form solvates, (2) the particle size control requirements, and (3) the variability in starting material purity. The team has had to execute targeted, rapid process development in order to support pilot plant API batches which will supply clinical trials. This work has required not just the technical capabilities of the team, but has also required streamlined collaboration and flawless communication across both drug substance and drug product space. This poster will detail the comprehensive and hefty process development work which was executed to support the Pure Step, focusing on the drug substance crystallization, and the impacts on the drug product space.
Scale Up of Fluidized Bed Reactors: What Can Be Calculated and What Needs to Be Measured
Ben Freireich, PSRI
Fluidized beds are commonly used for the manufacturing of a wide range of products including syngas, fuels including gasoline, acrylonitrile, polyolefins, and ultra-high purity silicon. These units provide unsurpassed heat transfer along with the ability to flow solids during operation. However, scale-up of these units can be challenging with respect to productivity and reliability. For fast reactions, the fluidized bed is usually mass-transfer limited and mass-transfer is strongly dependent on bed hydrodynamics. Thus, scale-up parameters need to include gas compression, bubble growth, solids mixing, and particle cohesive forces all of which need to be obtained on a large-scale. Many of the available correlations were either obtained on too small of a test unit to be relevant with commercial application, or simply don’t consider parameters that affect to mass transfer.
Thus, understanding key hydrodynamic parameters such as bed density profiles, bubble hydrodynamics, entrainment, pressure loop profiles and jet-penetration lengths, all of which are depend on particle properties, can yield a commercial-scale design that mimics pilot-plant performances with reliability goals similar to other unit operations. While modeling efforts can provide good approximations of what is and is not important with scale up. Yet, most models are based on “ideal” or “standard” conditions and properties and rarely consider micro-scale effects such as interparticle forces (coulombic, capillary, van der Waals) or other surface interactions (collisional stresses). Thus, experiments from cold flow to pilot studies are needed to understand controlling hydrodynamic parameters as relevant to the operation conditions of the process and the physical properties of the powder or catalyst.
Selection of Isolation Methods for Micron Sized Particles
Mrunmayi Kumbhalkar, The Dow Chemical Company
Solid-liquid separations are commonly used in industrial processes and are approached in a distinctive way based on the desired component- solid or liquid. The separation technique is dependent on a combination of factors- how the feed suspension was prepared, total volume, solid concentration, and particle shape and size distribution of the solids. Investigating the performance of various separation equipment is time consuming and this search can be narrowed down by utilizing specific laboratory scale tests to predict the behavior of a separation technique before scale-up. Herein, the processes of technology selection for situations where solids are the desired fraction with particle size < 10 μm are discussed. The choice of cake filtration methods such as vacuum and pressure filtration is often based on the average flux, which indicates the time required for filtration. Filter media with small channel sizes are required to isolate the micron sized particles. The cake deposited always exhibits high resistance and the small particles may block the channels leading to unacceptably long filtering time. Sedimenting centrifuges such as tubular, or stacked disc can be used for isolating sub-micron particles since they do not use a filter medium for separation and avoid the challenges of media fouling. The selection of sedimenting centrifuge can be based on laboratory scale feasibility tests performed with a benchtop centrifuge by varying the centrifugal force and residence time and observing the sediment compactness and supernatant clarity. Other filtration methods including thin cake filtration and cross-flow filtration can also be considered for systems with small particles.
Design and Characterization of a Lab Scale Pump Loop System
Jennifer Larimer, The Dow Chemical Company
Turbulent immiscible liquid-liquid systems produce functionalized highly branched polymers via hydrolysis and condensation reactions. Due to simultaneous and interdependent physics, including coalescence, dispersion, heat and mass transfer, and competitive consecutive chemical reaction, time dependent mixing characteristics impact the resulting material produced.
Well characterized mixing equipment such as stirred tank reactors have well established rules for designing and scaling mixing dependent processes. Specific guidelines exist for both geometric and operational parameters such as load volumes, tank and impeller diameters, impeller types, number and location, and reactant addition strategies. Pump loop systems, however, have not been explicitly studied in the literature; therefore, scaling guidance for these systems is limited. Parallels can be drawn between well characterized stirred tank systems and pump loop operation, however, there are more independent design and operational variables in pump loop systems that increase the level of difficulty in process scaling over that of the stirred tank design.
Additionally, highly branched polymers can grow in three dimensional space as a function of time. Reaction conditions as a function of time influence how the structure of these species build[1]. Different mixing conditions throughout different zones of a pump loop system can shift the instantaneous growth of a molecule between different reaction mechanisms. Therefore understanding what aspects of pump loop system design have the largest influence in how molecules build is essential to successfully scaling a process. This poster highlights the challenges associated with designing and tuning a pump loop process asset.
REFERENCES
1. Brinker, C.J., “Hydrolysis and Condensation of Silicates: Effects on Structure”, Journal of Non-Crystalline Solids, V100, 1988, Pg 31-50, North Holland, Amsterdam. Elsevier Science Publishers B.V.
Modular Chemical Process Intensification (MCPI): A Perspective from the RAPID Manufacturing Institute
Ignasi Palou-Rivera, RAPID Manfacturing Institute
In December 2016, the Department of Energy announced the establishment of the 10th Manufacturing USA Institute, representing a critical step in the federal government’s effort to double U.S. energy productivity by 2030. The Rapid Advancement in Process Intensification Deployment (RAPID) Institute (https://www.aiche.org/rapid) is focused on addressing barriers to enable the development of breakthrough technologies to boost energy productivity and energy efficiency through manufacturing processes in industries such oil and gas, pulp and paper and various domestic chemical manufacturers. RAPID will leverage approaches to modular chemical process intensification (MCPI) — such as combining multiple process steps as mixing, reaction, and separation into single more complex and intensified processes — with the goal of improving productivity and efficiency, cutting operating costs, and reducing waste.
This poster will present the approach used by the RAPID Manufacturing Institute to advance MCPI in the selected Focus Areas of Chemical and Commodity Processing, Renewable Bio Products, Natural Gas Upgrading, Modeling and Simulation, Intensified Process Fundamentals, and Module Manufacturing. Achievements to date such as the compile roadmap and plans for 2018 and beyond will be the cornerstones of the presented material.
Polysaccharide and Fructose Syrup Production using Glucosyltransferase Enzymes
Kevin D. Nagy, DuPont Industrial Biosciences
Commercialization of chemicals and materials derived from bio-based sources requires finding opportunities that have the right balance between performance, cost, and sustainability. A significant challenge using fermentation technology is the loss of carbon to CO2; carbon yields significantly lower than 50% are the norm, and these low yields have substantial implications on both the process economics and environmental footprint. One approach to improve these metrics is to use enzymatic processes instead of microbial fermentations.
The production of engineered polysaccharides using glucosyltransferase enzymes is an example of a technology that allows for 100% of the carbon to be recovered as valuable products. These enzymes convert sucrose into a polysaccharide comprising glucose while simultaneously generating an enriched fructose stream. This method of producing fructose is also advantaged compared to the typical starch process.
Commercial fructose syrup products contain 42-55 wt% dry weight basis (DWB) fructose. The 55 wt% DWB fructose stream cannot be produced directly and requires several chromatographic steps to achieve an intermediate stream containing 90+ wt% DWB fructose. This high purity fructose stream is then back blended to achieve the right composition. Overall, this incumbent process is extremely energy intensive due to the large amount of water evaporated in the chromatography process. Comparatively, the glucosyltransferase approach outlined above directly generates a high purity fructose syrup containing 75+ wt% DWB fructose suitable for blending while completely avoiding chromatography and the associated evaporation requirements. These glucosyltransferase based processes thus enable the production of new polysaccharide materials while simultaneously streamlining the production of fructose syrup.
Simulated Moving Bed Reactor for Enhancing the Productivities of Equilibrium Limited Reactions
Balamurali Sreedhar, The Dow Chemical Company
Equilibrium-limited reactions are ubiquitous in the chemical industry. Those with highly unfavorable equilibrium constants face very energy intensive operations for conversion and recovery of the product, often needing extensive recycle. Chances are also that such severely equilibrium-limited reactions using conventional reactors are written off at an early stage and are never scaled up to production.
In this work, we demonstrate the potential of simulated moving bed reactor (SMBR) in increasing the productivity of strongly equilibrium-limited reactions and possibly rendering them economically feasible. In an SMBR, in-situ chromatographic separation of the products aids in shifting the equilibrium, thereby improving the conversion.
Liquid phase transesterification of propylene glycol methyl ether (DOWANOL™ PM) to propylene glycol methyl ether acetate (DOWANOL™ PMA) using a homogeneous catalyst is considered as a case study to compare the performance of SMBR with that of a conventional batch reactor. Here, DOWANOL™ PM is used both as a reactant and desorbent for the chromatographic separation inside the SMBR. In the SMBR process, an anion exchange resin, AMBERLITE™ IRA904 in chloride form is used as a non-catalytic adsorbent, while sodium alkoxide of PM is supplied as a homogeneous catalyst in the desorbent. Using model based optimization, we demonstrate the advantage of employing a non-catalytic adsorbent in the SMBR for the homogeneously catalyzed reaction. With the ability to independently tune the separation of the product in the SMBR, it is demonstrated that the productivity of the process increases with increasing separation factor. Presence of an optimal product separation factor is observed with respect to the amount of DOWANOL™ PM used for reaction and separation. At a fixed conversion of 95%, SMBR outperforms a batch reactor by increasing the productivity by 85% and reducing DOWANOL™ PM usage to 50% of what is required by the batch reactor.
Chemicals from Biomass: The Design of a Succinic Acid Production Facility
Serdar Ozturk, Milwaukee School of Engineering
Using SuperPro Designer, a process simulation software, our team explored a biochemical route to producing succinic acid that uses the rumen bacteria Actinobacillus succinogenes to ferment corn stover. Key steps of the facility include feedstock pretreatment, bacterial fermentation, recovery of the final product by crystallization, and power generation.
The model was used to assess the quality of the theoretical product and the economic and environmental impact of the facility to ultimately determine if the design could compete with both the petrochemical process and existing bio-based solutions. The team’s design is on par with the current market by producing 11.55 kilotons of 99.7% pure succinic acid annually, and offering a payback time under 5 years. Our team created a biorefinery design that maximizes profitability for a feasible and sustainable solution.