A non-reactive model system comprising a highly concentrated and unstable oil-in-water emulsion was used to investigate the retention of oil by the membrane in producing biodiesel with a membrane reactor. Critical flux was identified using the relationship between the permeate flux and transmembrane pressure along with the separation efficiency of the membrane. It was shown that separation efficiencies above 99.5% could be obtained at all operating conditions up to the critical flux. It was observed that the concentration of oil in all collected permeate samples using the oil-water system was below 0.2 wt% when operating at a flux below the critical flux. Studies to date have been limited to the characterization of low concentrated emulsions below 15 vol.%. The average oil droplet size in highly concentrated emulsions was measured as 3200 nm employing direct light scattering (DLS) measurement methods. It was observed that the estimated cake layer thickness of 20 to 80 mm was larger than external diameter of the membrane tube i.e. 6 mm based on a large particle size. Settling of the concentrated emulsion permitted the detection of a smaller particle size distribution (30-100 nm) within the larger particles averaging 3200 nm. It was identified that DLS methods could not efficiently give the droplet size distribution of the oil in the emulsion since large particles interfered with the detection of smaller particles. The content of the smaller particles represented 1% of the total weight of oil at 30°C and 5% at 70°C. This was too low to be detected using DLS measurements but was sufficient to affect ultrafiltration. In order to study the critical flux in the presence of transesterification reaction and the effect of cross flow velocity on separation, various oils were transesterified in another membrane reactor providing higher cross flow velocity. higher cross flow velocity provides better separation by reducing materials deposition on the surface of the membrane due to higher shearing. The oils tested were canola, corn, sunflower and unrefined soy oils (Free Fatty Acids (FFA< 1%)), and waste cooking oil (FFA= 9%). The quality of all biodiesel samples was studied in terms of glycerine, mono-glyceride, di-glyceride and tri-glyceride concentrations. The composition of all biodiesel samples were in the range required by ASTM D6751 and EN 14214 standards. A critical flux based on operating pressure in the reactor was reached for waste cooking and pre-treated corn oils. It was identified that the reaction residence time in the reactor was an extremely important design parameter affecting the operating pressure in the reactor. / Natural Sciences and Engineering Research Council of Canada (NSERC)

A non-reactive model system comprising a highly concentrated and unstable oil-in-water emulsion was used to investigate the retention of oil by the membrane in producing biodiesel with a membrane reactor. Critical flux was identified using the relationship between the permeate flux and transmembrane pressure along with the separation efficiency of the membrane. It was shown that separation efficiencies above 99.5% could be obtained at all operating conditions up to the critical flux. It was observed that the concentration of oil in all collected permeate samples using the oil-water system was below 0.2 wt% when operating at a flux below the critical flux. Studies to date have been limited to the characterization of low concentrated emulsions below 15 vol.%. The average oil droplet size in highly concentrated emulsions was measured as 3200 nm employing direct light scattering (DLS) measurement methods. It was observed that the estimated cake layer thickness of 20 to 80 mm was larger than external diameter of the membrane tube i.e. 6 mm based on a large particle size. Settling of the concentrated emulsion permitted the detection of a smaller particle size distribution (30-100 nm) within the larger particles averaging 3200 nm. It was identified that DLS methods could not efficiently give the droplet size distribution of the oil in the emulsion since large particles interfered with the detection of smaller particles. The content of the smaller particles represented 1% of the total weight of oil at 30°C and 5% at 70°C. This was too low to be detected using DLS measurements but was sufficient to affect ultrafiltration. In order to study the critical flux in the presence of transesterification reaction and the effect of cross flow velocity on separation, various oils were transesterified in another membrane reactor providing higher cross flow velocity. higher cross flow velocity provides better separation by reducing materials deposition on the surface of the membrane due to higher shearing. The oils tested were canola, corn, sunflower and unrefined soy oils (Free Fatty Acids (FFA< 1%)), and waste cooking oil (FFA= 9%). The quality of all biodiesel samples was studied in terms of glycerine, mono-glyceride, di-glyceride and tri-glyceride concentrations. The composition of all biodiesel samples were in the range required by ASTM D6751 and EN 14214 standards. A critical flux based on operating pressure in the reactor was reached for waste cooking and pre-treated corn oils. It was identified that the reaction residence time in the reactor was an extremely important design parameter affecting the operating pressure in the reactor. / Natural Sciences and Engineering Research Council of Canada (NSERC)

<p>  </p> <p>In the pharmaceutical industry, special care must be taken by companies to guarantee high quality medications that are free from byproducts and impurities. The development process involves various considerations including solvent selection, solubility screening, unit operation selection, environmental, and health impact evaluations. Traditionally, pharmaceutical manufacturing consisted of large, centralized facilities to meet pharmaceutical demands; however, there has been a recent shift toward distributed manufacturing. With distributed manufacturing platforms, rapidly changing supply chain needs can be met regionally in addition to supplying small-volume medications and personalized medicines to hospitals and pharmacies. To produce quality pharmaceuticals, distributed manufacturing platforms should integrate digital design, novel unit operations, and process analytical technology (PAT) tools for quality monitoring and control. In this dissertation, a process design and development framework is proposed and implemented for a small-scale pharmaceutical manufacturing platform: MiniPharm.</p> <p>Various approaches to process design are detailed in this dissertation, which include heuristic-based and digital or simulation-based design. For heuristic-based design, the knowledge of the researchers was utilized to provide unit operation evaluation and screening of process alternatives. In cases when unit operations were highly complex, digital or simulation-based design was utilized to conduct sensitivity analyses and simulation-based design of experiments. With the implementation of simulation-based design, material and time needs were reduced while gaining knowledge about the system. The integration of various unit operations comes with increased understanding of start-up dynamics and operational constraints. What was found to be the most successful approach was the combination of heuristics and digital design to combine researcher knowledge and experience with the information gained from process modeling and simulation to create process alternatives that utilized system dynamics to reach desired process outcomes. </p> <p>Additionally, MiniPharm was used for process model development at the small-scale. Various software packages have been made commercially available that focus on production scale; however, models for small-scale operations are not typically implemented in these packages. Models for unit operations were fit with collected experimental data to estimate model parameters for small-scale synthesis, liquid-liquid extraction, and crystallization unit operations. The models were implemented to better capture the heat and mass transfer of the milli-fluidic scale platform, which consist of unit operations housed within microchannels. MATLAB was utilized for estimation of parameters such as kinetic rate constants and overall mass transfer coefficients. These parameters were used for design space determination and process disturbance simulation. The exploration of the impact of various process parameters on quality attributes helps researchers gain a deeper understanding about the manufacturing process and helps to demonstrate how to control the process. </p> <p>An important aspect of MiniPharm is the process development progress that has been demonstrated. With the construction of a modular and reconfigurable platform, various process alternatives can now be experimentally validated. The integration of unit operations operated at a decreased scale makes MiniPharm an example of process intensification. The implementation of integrated unit operations decreases handling time of intermediates and reduces the overall footprint for manufacturing. Designed to allow for increased flexibility of operation, perfluoroalkoxy alkane (PFA) tubing was used for synthesis and purification. With PFA tubing clean in place procedures can be implemented using continuous solvent flow or the low cost, PFA tubing can be replaced. The modular nature of the platform also allows for the investigation of individual unit operations for performance evaluation. </p> <p>Finally, a novel continuous solvent switch distillation unit operation was designed and constructed along with customized reactor and crystallizers for process alternative screening for the synthesis and purification of two compounds: Diphenhydramine hydrochloride and Lomustine. Diphenhydramine hydrochloride is a low-value, high volume allergy medication commonly found in Benadryl and Lomustine is a high-value, low volume cancer medication used to treat glioblastoma and Hodgkin Lymphoma. The production of the compounds demonstrated the flexibility of the manufacturing platform to produce both a generic and a specialty medication. A versatile platform is needed for distributed manufacturing because of quickly changing supply chain needs. Overall, this dissertation successfully demonstrates the process design, development, and simulation for small-scale manufacturing.</p>

<p>The present work is focused on the synthesis of small-scale (modular processes) to produce olefins from light alkane resources in shale gas.</p> <p>Olefins, which are widely used to produce important chemicals and everyday consumer products, can be produced from light alkanes - ethane, propane, butanes etc. Shale gas is comprised of light alkanes in significant proportion; and is available in abundance. Meanwhile, shale gas wells are small sized in nature and are distributed over many different areas or regions. In this regard, using shale gas as raw material for olefin production would require expensive transportation infrastructure to move the gas from the wells or local gas gathering stations to large central processing facilities. This is because existing technologies for natural gas conversions are particularly suited for large-scale processing. One possible way to take advantage of the abundance of shale resource for olefins production is to place small-sized or modular processing plants at the well sites or local gas gathering stations.</p> <p>In this work, new process concepts are synthesized and studied towards developing simple technologies for on-site and modular processing of light alkane resources in shale gas for olefin production. Replacing steam with methane as diluent in conventional thermal cracking processes is proposed to eliminate front-end separation of methane from the shale gas processing scheme. Results from modeling studies showed that this is a promising approach. To eliminate the huge firebox volume associated with thermal cracking furnaces and allow for a compact cracking reactor system, the use of electricity to supply heat to the cracking reactor is considered. Synthesis efforts led to the development of two electrically powered reactor configurations that have improved energy efficiency and reduced carbon footprints over and compare to conventional thermal cracking furnace configurations.</p> <p>The ideas and results in the present work are radical in nature and could lead to a transformation in the utilization of light alkanes, natural gas and shale resources for the commercial production of fuels and chemicals.</p>

S tím, jak se neustále vyvíjejí nové technologie pro energeticky náročná průmyslová odvětví, stávající zařízení postupně zaostávají v efektivitě a produktivitě. Tvrdá konkurence na trhu a legislativa v oblasti životního prostředí nutí tato tradiční zařízení k ukončení provozu a k odstavení. Zlepšování procesu a projekty modernizace jsou zásadní v udržování provozních výkonů těchto zařízení. Současné přístupy pro zlepšování procesů jsou hlavně: integrace procesů, optimalizace procesů a intenzifikace procesů. Obecně se v těchto oblastech využívá matematické optimalizace, zkušeností řešitele a provozní heuristiky. Tyto přístupy slouží jako základ pro zlepšování procesů. Avšak, jejich výkon lze dále zlepšit pomocí moderní výpočtové inteligence. Účelem této práce je tudíž aplikace pokročilých technik umělé inteligence a strojového učení za účelem zlepšování procesů v energeticky náročných průmyslových procesech. V této práci je využit přístup, který řeší tento problém simulací průmyslových systémů a přispívá následujícím: (i)Aplikace techniky strojového učení, která zahrnuje jednorázové učení a neuro-evoluci pro modelování a optimalizaci jednotlivých jednotek na základě dat. (ii) Aplikace redukce dimenze (např. Analýza hlavních komponent, autoendkodér) pro vícekriteriální optimalizaci procesu s více jednotkami. (iii) Návrh nového nástroje pro analýzu problematických částí systému za účelem jejich odstranění (bottleneck tree analysis – BOTA). Bylo také navrženo rozšíření nástroje, které umožňuje řešit vícerozměrné problémy pomocí přístupu založeného na datech. (iv) Prokázání účinnosti simulací Monte-Carlo, neuronové sítě a rozhodovacích stromů pro rozhodování při integraci nové technologie procesu do stávajících procesů. (v) Porovnání techniky HTM (Hierarchical Temporal Memory) a duální optimalizace s několika prediktivními nástroji pro podporu managementu provozu v reálném čase. (vi) Implementace umělé neuronové sítě v rámci rozhraní pro konvenční procesní graf (P-graf). (vii) Zdůraznění budoucnosti umělé inteligence a procesního inženýrství v biosystémech prostřednictvím komerčně založeného paradigmatu multi-omics.