Equipment

Pope Scientific Inc. Unveils CE-Certified Series of Wiped-Film Still Systems at ACHEMA 2024

Pope Scientific Inc. Unveils CE-Certified Series of Wiped-Film Still Systems at ACHEMA 2024

Pope Scientific Inc., a prominent figure in processing technologies since 1963, proudly announces the launch of its CE-certified series of wiped-film still systems. Renowned for their efficiency and precision, these systems represent a significant advancement in distillation technology, adhering to the highest health, safety, and environmental standards set forth by the European Union.

Pope 2″ WFC-200 Wiped-Film Still

The CE-certified series, comprised of Pope’s 2”, 4”, and 6” still sizes, bears the model designations WFC-200, WFC-400, and WFC-600 respectively. The first unveiling of the WFC-200 model will take place at ACHEMA 2024, showcasing Pope’s commitment to innovation and excellence in the field.

The wiped-film still, pioneered by Pope in 1976, also recognized under alternate names such as molecular stills short-path stills, and wiped-film evaporators, serves a crucial role in separating heat-sensitive materials effectively. Known by whichever moniker depending on application, geography, or industry, the purpose remains consistent: the separation of materials that demand a delicate touch in distillation processes.

Pope’s expertise extends across a wide array of processing industries, with their stills falling into two primary categories: the wiped film molecular (short path) stills designed for high boiling point materials, and the wiped film evaporators with external condensers tailored for lower boiling point distillates.

Constructed within heavy-duty stainless steel portable structures, the WFC series systems incorporate all necessary auxiliary components for seamless operation under diverse conditions. These include condenser types suitable for molecular distillation and/or evaporation/concentration. The turnkey skids also are provided with wiper drive, feed/degasser flask, extra receivers, cold trap, trap chiller, vacuum pump, vacuum gauge, heating/chilling circulators, and a control panel with a single-point power connection.

 

 

 

Pope 6″ WFC-600 Wiped-Film Still

 

Customers can opt for additional features such as feed pumps, discharge pumps, heat tracing, flow meters, vacuum boosters, and more. The systems are offered with a standard glass body, with the option of 316L stainless steel. Moreover, the body heating can be achieved via electric bands or hot oil, with accessibility for cleaning and system reconfiguration.

 

With a wide range of applications spanning pharmaceuticals, biomaterials, edible and essential oils, foods, flavors, vitamins, cosmetics, liquid silicone polymers, and beyond, Pope’s wiped-film still systems offer unparalleled versatility and reliability. Backed by decades of hands-on distillation toll processing, process development, and testing services, Pope ensures exceptional customer service, technical consulting, and client satisfaction.

The WFC series systems are poised to revolutionize experimental R&D, pilot plant studies, and production processing, accommodating a range of capacities from 0.1 to 20 kg/hr depending on model size, body material, and application. The scalability between WFC series models and larger systems in Pope’s portfolio further enhances their appeal to a diverse clientele.

For more information on Pope Scientific Inc. and its CE-certified series of wiped-film still systems, visit www.popeinc.com.

About Pope Scientific Inc.: Pope Scientific Inc. has been globally known for their innovative chemical processing technologies since 1963. With a commitment to excellence and adherence to the highest industry standards, Pope continues to redefine the landscape of distillation technology across various processing industries worldwide.

For media inquiries, please contact: Dean Segal, Pope Scientific, Inc. +1-262-268-9300, sales@popeinc.com

Determining Which Fractional Distillation Process to Use: Batch or Continuous Mode

Determining Which Fractional Distillation Process to Use: Batch or Continuous Mode

Introduction

Distillation is an important method for the separation and purification of liquids in a wide range of industries and laboratories.  For optimal purification in distillation, a vertical column is incorporated into the equipment with either a series of internal stacked plates (trays) or else filled with one of various types of structured or dumped-in packing.  The purpose of the trays or packing is to provide a high degree of vapor-liquid contact which results in multiple equilibrium stages or “theoretical plates”, each one leading to increasing purification all the way up the column, with the purest and lowest boiling point (BP) vaporized component(s) escaping the top of the column to contact a condenser where it leaves the column as a liquid distillate.  The overall result is that specific components of the starting composition have been separated, or fractionated, giving this process the name, fractional distillation.  Fractional stills often operate under pressure or vacuum and have a reflux device section for controlling and optimizing purity vs. throughput rate, however, these and several other topics of distillation equipment are not covered here. In this article, we will take a look at the two different types of fractional distillation; batch mode and continuous mode.

Batch Distillation Mode

Continuous Fractional Distillation Systems

Batch mode is the normal starting point of any distillation process and is the “simpler” of the modes.  Here, a fixed amount of feed material, (a batch) is loaded into a boiling vessel (pot), onto which is mounted a column with a condenser at the top.  The pot is heated and after a certain amount of time, the liquid begins to boil, and portions of it vaporize and travel up the column.  (One well-known example of batch mode is the traditional making of “moonshine” where a fermented mixture is loaded into the pot, heated, and an ethanol-enriched distillate is collected). The first feed components to vaporize are ones with lower boiling points (BP) than the others.  These components move up the column, with the lowest BP component in the feed becoming increasingly purified by means of fractionation finally being condensed and leaving the rest of the mixture as described above, to be collected in a distillate receiver.  This will continue until the first component of lower BP is depleted in the boiling pot.

At this point, if the process is allowed to continue, the next component of BP greater than the first begins to make the travel all the way up to the condenser to be condensed, leaving as another distillate fraction that can be collected in a different receiver than the first.  Some feed materials may contain many components and this means of separating several of them, one after the other, in order of increasing BP, can be continued until the desired product components have been collected at which point, the distillation process is ended by shutting off the heating of the boiling pot.

Examples of batch stills are many and can include anything from isolation of a flavor component in an extracted natural botanical source to recovering certain solvents from a waste mixture for reuse.  A key characteristic of batch mode is that the composition of the feed material in the pot is constantly, incrementally changing throughout the duration of the run.  The composition in the pot at the moment will be different an hour from now or even just a few minutes from now.  The distillate collected will also change in composition over time as each subsequent component is distilled away.  Thus, this is not a steady-state process.

In situations where the quantity of starting feed material becomes quite large, for example well beyond 1000 liters, and feed lots must be processed frequently, for example, at least every day, batch mode will become quite limited in addressing production requirements.  Another method for fractional distillation is then needed and this is when continuous mode must be considered.

Continuous Distillation Mode  

Continuous mode fractional distillation can handle very large quantities of feed without the need for very large boiling vessels.  Instead, feed is pumped at a set flow rate into the distillation system which has a column and condenser which can be similar to a batch-type setup.  However,  in this case, a reboiler replaces the boiling vessel and this is outfitted with apparatus for continuous discharge of residue, often referred to as a “bottoms stream”.  The feed is preheated and enters the column at a height selected to optimize the overall process efficiency.  Distillate leaves the system from the condenser, similar to the case of batch mode.  So, in continuous mode, there is one stream entering the system and two streams exiting the system, the distillate, and the residue.

A key characteristic of continuous mode is that the compositions of these streams and at any point within the distillation equipment do not change over time as in batch mode, instead they remain constant, in a steady state throughout the entire run, the duration of which may go on for a considerable time.  Oil refineries are a well-known example; these typically operate 24/7, being stopped only for maintenance or other technical reasons.  There are exceptions to the 3-stream scheme described above; for example, in addition to the distillate collected at the top of the column, there may be multiple take-off points (side-streams) at various heights of the column.  In the case of oil refinery columns, these will be multiple component cuts including gasoline, diesel, and mixed solvents in the upper column region, and oil cuts of increasing weight and viscosity as the locations get closer to the bottom of the column.  It is important to note that these are never pure single-component cuts, but collections of many components of somewhat similar BP, for example, one stream may become further processed to become 10W-40 motor oil, and another stream may be used to create a variety of lighter lubricants, etc.  The heaviest components of all become the materials used in tars, asphalts, and the like.

Other continuous fractional applications may involve feed streams with several, but far fewer individual components than are found in crude petroleum oil.  Examples include many specialty chemicals such as pharmaceutical intermediates and electronics materials manufactured in reactors.  The target product(s) may be somewhere in the middle of the range of the BP’s of several byproducts that must be removed.  For high-purity products, side draws cannot be utilized, these will not be pure enough.  To isolate pure components, more than a single column is needed, the number being dependent on the number of components in the feed.  For example, the first column may be used to distill away several components which are lower in BP than the desired product.  The residue can then serve as feed to a second column which will distill away the product plus a byproduct of BP near that of the product.  This distillate stream may be fed to a third column which separates the product away from the byproduct that is co-distilled from the second column.  This type of separation of pure components is more easily done with a single batch still if heat sensitivity is not a problem, (waiting for the product to start coming off the column and collecting it separately), however, as mentioned earlier, this is not practical with very large feed quantities; instead, a battery of staged continuous mode columns is called for.

There are many considerations that go into the design of a fractional column distillation system. These factors can vary depending on the scale at which you are manufacturing. When working at a commodity scale it often makes sense to manufacture in a continuous fashion, however, on the pilot and small production scale an important consideration is whether to use a batch approach. In addition to scale, there are a few other factors that play a considerable role such as the quantity of material, purity, energy use, and how many components need to be separated.  These are highlighted in the figure below:

Energy Usage

Energy consumption in continuous distillation is lower than that of batch distillation.  Heat recovery can be utilized, and the process loops optimized for both product quality and energy consumption. Energy usage can also be optimized by both preheating the feed material and selecting the best column entry point for the feed stream, reducing the condenser and reboiler duties.  In batch mode, more energy is required in startup and because much of the heat is applied to evaporating the same material portions multiple times; this effect is reduced in continuous mode operation.

 

Pope Continuous Fractional Distillation System

Pope Batch Fractional Distillation System

Process Development and Scaleup; Lab, Pilot Plant, and Production Scale

As mentioned, in nearly all cases, batch mode is the starting point for fractional distillation.  Even if the long-range goals call for very large production quantities and continuous mode installation will eventually be needed, new product development typically starts with lab scale and this will be batch mode.  Lab scale equipment with boiling vessels of less than 1 liter up to 12 liters is appropriate for process feasibility studies. The lab-scale distillation experimentation may be part of an extensive general product development project.  For example, it may be found that upstream chemistry and reactions need to be changed to allow proper distillation and other downstream operations work well, followed by more experimentation, etc.  If lab studies are successful, it is normally advisable to move on to stainless steel (or other higher alloy if necessary) pilot scale equipment.  This may include batch stills from a few liters in size up to 100 liters or more.  It may also include pilot scale continuous stills with column diameters from 1” to 12” and feed rates from 1 to a few hundred liters/hr. Equipment of the larger end of these ranges can also serve as small or mid-size production systems as needed.  Examples of such equipment are shown.

Pope Scientific offers batch fractional stills in glass from 1 to 22 liters and in stainless steel from 2 to 2000 liters or larger.  Continuous fractional still systems are available in stainless steel with from 1” to 24” column diameters.  All of the above equipment is normally designed and manufactured in skid-mounted modular turnkey form. Instrumentation can range from control elements only to fully integrated PLC control systems.  Semi-turnkey systems and core distillation components alone are also available.  During pilot plant studies, it may be found that the distillation system may need to be reconfigured somewhat in order to optimize the process.  Pope takes this into account in the design of pilot plants, for example, allowing the ability to add or decrease column height or addition of collection receivers, etc.  Control systems for continuous systems are more complex as there are several control loops required to achieve a steady state.  However, the programs required for batch systems can be more extensive than for continuous, depending on what the user wants to accomplish. This is because there are usually several time and event-based changes in operating parameters during the run which may be automated, with routines set up by the operator before the run begins.

Pope maintains a staff highly knowledgeable in applications assistance, chemical engineering, chemistry, and chemical equipment operation, providing the customer with a partner for matching processing needs to equipment optimized for the lab, pilot, or production project. In addition to the provision of equipment, Pope can offer lab and pilot scale studies, depending on the nature of the specific applications.  Experienced personnel in mechanical and electrical engineering, assembly, quality assurance, and documentation assure the equipment will work well from delivery and startup and will last for decades.

The Benefits of Utilizing Data Acquisition Systems in Distillation Processing with Yokogawa

The Benefits of Utilizing Data Acquisition Systems in Distillation Processing with Yokogawa

Data acquisition systems (DAQ) have been around for a long time; however many people aren’t familiar with this technology when inquiring about distillation equipment. Programmable Logic Controllers (PLCs) are used often in chemical processing for controlling key variables such as pressure, flow rates and temperature. While most PLCs will have some sort of data logging capabilities, it is typical that the software associated with the PLC is very cumbersome. Often a programmer will have to spend a good deal of time to incorporate the basic trend information that would come standard on a DAQ system. In addition, data logging on a PLC is often just a CSV file that is dumped to a location after one run. The CSV file must then be further manipulated to show the data on a graph or chart. An actual data recorder can do a much better job with the visualization of data without hours of additional programming. A DAQ system allows the user to look back at any timeframe of data from 60 seconds to possibly several days prior. This data can also be set to be shown as trend information, bar graphs or just plain figures straight out of the recorder. A DAQ system can exist as hardware within a control panel in which it is viewed from a web browser or as external hardware with its own housing touchscreen control. Having such ease of access to these heavily customizable reports can prove to be very useful to an operator, which is why Pope likes to include both in our control systems.

Having hardware and software record data for you, as opposed to someone in the lab handwriting these bits of information, provides many benefits. Ease of access to data can be a strong point for the recorders. If a DAQ system is uploading this information to a hard drive or server, there are many ways this information can be shared and analyzed throughout a group or company from remote locations. This data can be used to ensure reliability or to improve process efficiency. Having access to this data also allows the user to make predictions in maintenance. For example, if a certain heating or cooling element starts to take more time to reach its target temperature, it could imply that that element is starting to fail. Knowing this ahead of time allows a company time to order replacements before a failure actually occurs. This avoids any sort of downtime.

Yokogawa GX20 – image source yokogawa.com

Most DAQ systems will have similar capabilities as those mentioned above – so why do we specifically like Yokogawa’s DAQ? The two main reasons are its easy-to-use interface as well as its ability to comply with GMP environments. Yokogawa has done an excellent job incorporating universal gestures into its touchscreen technology. The same swipe and pinch motions people use every day on their cell phones are incorporated into their recorders. The display is very intuitive in addition to being very bright and colorful. There is no shortage of customization options when it comes to viewing your data. Bar, trend, and digital graphs can be set up to view whatever variables are desired. As noted, the DAQ can be connected via ethernet to view data in real-time from anywhere, or more traditionally exported on a scheduled basis. This data can also be exported in different files types to be observed in other means. In regards to its GMP capabilities, Yokogawa DAQ systems can be compliant with CFR 21 part 11. This specific compliance is the FDA’s regulations for electronic documentation and electronic signatures. Yokogawa’s advanced security add-on allows the users DAQ system to contain an encrypted data file to prevent any manipulation to the data recovered. It’s a one-way road that only allows data to be exported out in an XLS file type. This add-on also contains an onboard audit trail that tracks what changes are made, who made them and when they were made allows for full traceability.

For all of these reasons, Yokogawa DAQ systems are a great asset to distillation equipment. Next time you’re inquiring about a Pope distillation system, be sure to ask how Data Acquisition Systems can be used with your process. Our experts are available to answer any questions and provide recommendations.

Pope Scientific Inc. Upgraded Series 700 Compact Sanitary Mixers

Pope Scientific Inc. Upgraded Series 700 Compact Sanitary Mixers

Pope Scientific Continues to Improve and Upgrade their Line of Stainless Steel Process Mixers

The line consists of Pope’s Series 600, 700, 800, 900 mixers, covering vessels between 0.1 and 1000 liters in size. The focus of the product line is high purity and sanitary use and where pressure and vacuum operation are required. Applications include blending liquids, dissolving or suspending solids, reactions, fermentation, crystallization, high shear mixing with size reduction, or stirring. All are rated for high vacuum and pressure at a wide range of high and low temperatures, with excellent chemical compatibilities as standard. They are designed for critical use in fine high purity chemical, pharmaceutical and food applications, are CIP and SIP capable, and cGMP validatable.

The most recent upgrades have been to the Series 700 Mixer. This is a more compact version of the long-established Pope Series 800 models, sharing all of the high-performance features of the larger sibling, but used for smaller vessels and reactors from 0.1 to 30 liters in volume and where space is limited. It is ideal for laboratory through mid-pilot size operation where compactness, robustness and high performance are key. Experimentation, process scaleup and small-lever production are all possible.

Versatility is built into the design, with options including interchangeability of AC or DC electric motors or air motors of different power, gearing, speed and classification, all quickly removable for mixer autoclaving or storage. Additional choices include impeller types, sizes, quantities and changeable positions. Pope’s default is a 3-lobed marine style impeller; several additional choices include turbine, pitched, radial, anchor, paddle, Rushton, Cowles, and others. Shaft diameter is 0.5”. A “pool cue” type interchangeable shaft option is available to accommodate simple changes in shaft lengths for different vessels, and to allow for impellers to be welded to shafts and polished, without seams, for maximum sanitary requirements. All mixers are equipped with speed controllers. AC motor powered mixers are supplied with VFD speed controllers with calculated RPM indication; optional tachometer sensors also available for exact shaft RPM indication for any AC or DC motors and air motors. Electric motors and/or controllers are available for general, washdown, Div 1, Div 2, ATEX and other classifications.

 

 

316-L stainless steel is standard, Hastelloy or other alloys or coatings optional. Elastomers are Kalrez for greatest possible ranges of chemical solvent compatibility, pH and temperature extremes. Standard wetted metal finish is better than 32 Ra, with optional mechanical and electropolishing to better than 8 Ra. Application-dependent operating ranges are from: 0.01 torr vacuum to 150 psi pressure, -40 to 250° C temperature, maximum speed choices of 1000, 500, 250, 125, 60, 30 RPM.

A Teflon lip seal protects the space between the mechanical seal and the two sets of permanently lubricated and shielded ball bearings. Side ports enable unpressurized cooling or inert blanketing above the mechanical seal. Standard main seal is a single mechanical, dry running, specially pressure balanced type with 316L, Kalrez, carbon, and tungsten carbide materials. Options include double mechanical type for greater speed and pressure use, or internal steam sterilization. The standard mounting is 1-1/2 sanitary clamp type, alternates also available.

Pope’s knowledgeable staff offers application assistance to clients seeking application-specific optimization and/or maximum versatility. In addition to mixers, Pope provides pressure vessels ranging from simple portable containers to blenders, reactors, homogenizers, crystallizers, fermenters, Nutsches, distillation/evaporators, to skid-mounted, fully turnkey PLC operated multistage processing systems.

Pictured: Pope 700 series mixers on a vessel, and the 700 & 800 series mixers.

Updated Pope 3L, 4L, 5L Benchtop Nutsche Filter Dryers Now Available

Updated Pope 3L, 4L, 5L Benchtop Nutsche Filter Dryers Now Available

The latest Pope Benchtop Nutsche Filter Dryers are now available for quick delivery.

Pope nutsche filter dryers are known and used worldwide for critical high purity separations of liquids and solids. The logical leap forward from laboratory Buchner funnels…Solids, crystals, high purity chemicals, pharmaceutical intermediates, etc., are efficiently filtered, washed, reslurried and dried in these portable nutsche filter units, minimizing contamination and exposure.

Design allows withdrawal of filter cake utilizing removable top head, bottom head and filter support assembly. May be pressurized to increase rate of solvent removal; drying is aided by vacuum and heating capability. Useful for experimentation and scale up studies; also for small scale production of high value products.

Updated features in include:

  • New design for support stand
  • Exterior finish now standard with polished welds
  • New CE certification and stamp, (in addition to rated tag on each Benchtop Nutsche)
  • Improved Pressure/temp ratings:
    • Vessel: 100 PSIG/FULL VACUUM @ -76°F/450°F
    • Jacket: 50 PSIG @ -76°F/450°F

Custom design features include manual or motorized raising/lowering cake agitators, conventional mixers, temperature control options, jacketing, valving, special porting, sight glasses, spray nozzle, instrumentation, pumps, etc., plus a wide range of easily replaceable filter media.

Pope also offers Nutsche Filter Dryers in a variety of sizes from lab through pilot plant and production scale, in volumes from 0.2 through 1000 liters. To learn more contact us today! Pope’s team is available to help you select the proper unit and answer any questions you may have.

Benchtop Nutsche Filter-Dryer Systems

Benchtop Nutsche Filter-Dryer Systems

 

Pope 3-liter Benchtop Nutsche Filter with optional motorized raising/lowering filter cake agitator.

Solids, crystals, high purity chemicals, pharmaceutical intermediates, etc., are efficiently filtered, washed, reslurried and dried in these portable nutsche filter-dryer systems, minimizing contamination and exposure. A logical leap forward from laboratory Buchner funnels. Design allows withdrawal of filter cake utilizing removable top head, bottom head and filter support assembly. May be pressurized to increase rate of solvent removal; drying is aided by vacuum and heating capability. Useful for experimentation and scale up studies; also for small scale production of high value products.

Standard models in 3, 4 or 5-liter sizes are stocked for quick delivery. Other lab sizes down to 0.2 liters and pilot/production sizes up to 1000 liters are offered. ASME and optional CE/PED certification for full vacuum to 100 psi, -80 to 250o C. Offered in stainless steel, Hastelloy, or alternate metals; optional food or pharmaceutical grade mechanical and electropolish finishes; Teflon or alternate coatings. Custom design features include manual or motorized raising/lowering cake agitators, mixers, temperature control options, jacketing, valving, special porting, sight glasses, instrumentation, pumps, etc., plus a wide range of easily replaceable filter media.

Custom Vessels & Processing Systems

Custom Vessels & Processing Systems

 

 

Custom Pharmaceutical Processing Skid System with Hastelloy reactor, absorption column, condenser, pumps, transport and feed vessels, control system.

 

Pope Vessels and integrated Processing systems are utilized in production, pilot plants and labs for processing pharmaceuticals, biomaterials, foods, specialty chemicals, etc. High quality materials, welding, and finishing assure integrity and validation in sanitary, ultra-high purity and hazardous applications. ASME stamping is standard; CE/PED, other certifications available. Options may include mixers, pumps, plumbing/valve manifolds, instrumentation, controls, filters, lifts, heating/cooling systems, CIP, SIP and other features. Fabricated with 316L stainless steel; other alloys such as Hastelloy, finishing levels and coatings are also available. Custom designed complete turnkey skid mounted systems, from 1 to 1000 liters, are offered incorporating blenders, reactors, fermenters, nutsche filter/dryers, extractors, distillation columns, feeders, multiple vessels, control systems, etc. Applications assistance and innovative process equipment design is a company specialty.