WIPED FILM MOLECULAR DISTILLATION SYSTEM

Wiped-film evaporator for short-path and molecular distillation

The short path distillation system is designed for the distillation of thermally sensitive products under vacuum. The system is used for organic products of high molecular weight and high viscosity at operating temperatures.

The evaporator surface consists of a vertical double mantled glass cylinder, heated by circulating thermal oil. The product is being spread to a thin film on the inner surface of the evaporator by means of rotating PTFE wiper elements. The wipers are being pressed to the inner wall of the surface where they produce a continuously distributed thin liquid film. The condenser is arranged vertically in the center of the glass evaporator to reduce the distance for the vapors and to prevent any pressure drop by large transfer spaces. It is tempered by liquid flow to condensate the evaporated product. This technology enables the operation at high vacuum to reduce the boiling point of thermally sensitive extracts without decomposition.

The rotating wiper basket is made of stainless steel AISI 316 and equipped with PTFE (Teflon) roll wipers.

PILODIST SP1000M is offered as a turn-key system including complete vacuum accessories and three high capacity thermostats to temper feed-vessel, inlet line, evaporator and the condenser including outlet line. The residue outlet is also tempered to prevent solidification of very heavy, waxy residues.

The SP1000M is a system for batch-wise operation and the budget friendly alternative to our fully continuous flagship SP1000CC. Once having installed and operated the system at customers side it can later be upgraded to the continuous more sophisticated version SP 1000 CC.

One of the unique features of the SP1000M is that the vessels of feed and residue are interchangeable: The residue vessel can be used as feed vessel, which allows running a second pass without any refilling. This eliminates refilling losses and saves a lot of handling and cleaning work compared to all other systems available on the market.

It is also possible to collect the sticky residue of the second pass in cheap standard glass bottles with GL45-neck for single use to prevent annoying waste removal.

Due to the smart design and liquid heated lines and vessels no heat gun or other ancillary heating equipment is required.

Technical Data

	Operating temperature:	up to 200°C (250…350°C upon request)
	Vacuum down to:	< 1 x 10-5 Torr abs.
	Feed range:	approx. 1000 – 4000 ml/h, dep. on application (max. 7000 ml/h)
	Evaporator surface:	~1000 cm², short path
	Evaporator MOC:	borosilicate glass/stainless steel 316
	Feed-vessel:	3000 ml, graduated, heated, interchangeable
	Residue receiver:	3000 ml, graduated, heated, interchangeable or GL-45 bottles
	Distillate receiver:	2000 ml, graduated,
	Speed range of stirrer:	30…1000 rpm
	Dimensions (w x h x d):	1750 x 2280 x 820 mm
	Electrical Supply:	6 individual 230V sockets or optional power distribution box for single line supply 230/400V 25A 50/60Hz with CEE 32A plug

Thin film distillation system for laboratory use.

The distillation system has a liquid-tempered evaporator made of borosilicate glass with an integrated condenser and temperature-controlled inlet and outlet.

The system includes all peripheral parts necessary for operation, such as the stirrer drive, vacuum system, control device and an aluminum assembly frame.

The version shown here is optimized for the handling of small sample quantities of aggressive substances in the range of 20-100ml.

To increase the resistance to aggressive products, the O-rings in FEP / PTFE / FFKM design are used and existing metal parts are refined with a hardcoat / ceramic coating.

Technical Data

	Material	borosilicate glass 3.3
	Evaporator area	approx. 100 cm2
	Operating temperature	up to 150°C
	Operating pressure	ATM, 100… 0.1 Torr (other ranges on request)
	Feed template	100ml, tempered
	Residue deposit	100ml, temperature-controlled feed
	Distillate supply	100ml
	Mains Supply	230 / 400V 16A 50Hz
	Dimensions (w x h x d) approx.	1.00 x 2.10 x 0.56 m

PILODIST PD 4929 S

The new PILODIST PD4929S is an automatic distillation apparatus for the sample preparation according to ASTM D4929.

This standard test method for the Determination of Organic Chloride Content in Crude Oil requires a crude oil distillation up to 204°C with a glass apparatus to achieve the naphtha cut for the chloride content analysis. Prior art is the sample preparation done by a complete manual distillation, which is time consuming and requires full attention to achieve a correct and precise cut point.  The new PD4929S performs this distillation in an automatic and precise computer controlled process with an apparatus strictly according to the ASTM standard method. A unique cooling system for the distillate receivers allows and easy, safe and quick receiver interchange and the direct storage of the sample in standardized GL45-bottles.

Beside the standard application for the 204°C naphtha cut, the system contains an additional receiver with free programmable cut point. This allows integrating additional tests in the same procedure, like the common test method at individual temperatures for mercury content to prevent catalyst poisoning in refineries.

The repeatability and reproducibility of this instrument is outstanding, due to the computer controlled process, a calibrated high-precision temperature sensor and an automatic barometric boiling point correction with integrated pressure sensor.

The PD104BD is designed for critical and sensitive products and does not contain any metal parts in direct contact with the sample. The system consists of a double jacketed 10L glass vessel with mechanical stirrer drive, precise oil tempered by a dynamic process thermostat. The silvered Distillation column in DN25 made of borosilicate glass can be equipped with various packing materials, depending on the application. A column heating jacket with automatic temperature sequence control ensures adiabatic operation. The column reflux ratio can individually be adjusted using a time-controlled reflux divider.

The system provides the possibility to discharge via tempered lines a fraction into a single receiver or alternatively into a customized fraction collector providing 6 receivers with the possibility to take out a filled receiver during operation without disturbing the vacuum.

The plant is equipped with a high capacity vacuum system and automatic calculation of the AET (Atmospheric Equivalent Temperature) so that the desired product sections can be entered directly without conversion and the reflux divider automatically switches to total reflux when the preselected cut temperature is reached. This ensures a clean separation even when the system is unattended. Equipped with the processor-based distillation control unit DCD4001, all distillation parameters such as temperature, vacuum, reflux distribution and the fraction collector are controlled via the associated software using an IP65 touchscreen PC. Limit value monitoring and security mechanisms ensures a safe distillation.

Via an integrated WIFI connectivity PILODIST is able to provide remote online service whenever needed. The entire system is integrated into an aluminum frame with an optionally available transparent polycarbonate enclosure with front doors as well as a top nozzle for adaption to an onsite available exhaust system.

Customized distillation system for fractional distillation of samples with high melting point. The system is designed for collection of product in single receivers. The system is supplied with 2 x  interchangeable columns (concentric tube column, DN25 packed column).

Operation range from ATM up to vacuum down to 1 mbar abs. and heated by a high power electrical heating bath this system can be used for versatile fractioning distillations.

The computer controlled distillation control device includes all functions for a smart and easy operation of  heaters, vacuum, reflux divider as well as an sophisticated safety system.

All fractions are discharged out of the vacuum by means of a heated discharge pump and collected in standard Schott receivers with flexible sizes from 500ml to 2000ml. These receivers can be interchanged during operation without any interruption of the vacuum operation.

Botanicals

New high capacity version of our most popular PILODIST 104 HC fractional distillation system series.

The setup includes a 200 L stainless steel flask with a powerful 12kVA electrical flask heater as well as a stirring gear to allow intensive mixing of the flask content for smooth evaporation. A distillation column with 1000 mm separation length and silvered high-vacuum mantle is packed with a DN 100 SULZER EX structured packing to allow a high throughput with an excellent separation efficiency.

The system is equipped with all required accessories for vacuum operation and the complete assembly is mounted in an aluminum rack with front doors in polycarbonate.

All distillation parameters like temperatures, reflux control and fraction-collector can be controlled by the special PILODIST 104 HC software in combination with our sophisticated touch-screen control system including several automation and safety features.

The displayed customized system is used for the distillation of eucalyptus extract to achieve pure fractions of several botanical terpenes, like α-pinene, limonene and cineol.

New combined distillation system PETRODIST 400 CC-A

PILODIST is proud to introduce a new distillation system to combine 2 different distillation procedures according to ASTM D2892 (TBP) and D5236 (POTSTILL) by sharing some essential components. Each of the 2 distillation procedures is designed to work fully-automatically without operator intervention with automatic evaluation including distillation curves. Both distillation set-ups are sharing a central fraction collector, vacuum supply and the thermostats. This new combined system offers full automatization for both distillation procedures, either TBP or POTSTILL. A superordinated software combines both the process results into 1 combined evaluation result with combined TBP-curve.

The system can be customized with several options available to upgrade according to customers needs, taking care of specific endusers safety regulations.

Like all fully-automatic systems, PETRODIST 400 CC-A, consists of a double pressure sensor system for each Procedure to extent the functionally for automatic ambient air pressure correction.

The standard PILODIST IP65 panel PC with glass front can be operated even with lab gloves. It is also equipped with a WIFI connectivity stick for remote online services from our German headquarter.

Wiped-film evaporator for short-path and molecular distillation

This is our new flagship for short path and molecular distillation. The SP 1000 CC is a turnkey ready system for laboratory use and small scale production and is optimized to cover nearly all applications, from high melting to high boiling points and can handle thermal sensitive material, with full flexibility and complete continuous operation.

The molecular distillation also called high vacuum wiped film, thin film or short path distillation, is a well-known process to separate thermal sensitive material in a very thin film at a high vacuum and short distance to the condenser, which allows an unbeatable performance.

The SP 1000 CC is equipped with our unique and patent pending HYBRID-evaporator which combines all positive aspects of glass and stainless steel in one instrument. It is reliable and solid like stainless steel, but with the full visibility of a glass still.

Due to its complete heated inlet and outlet lines in combination with our tempered feed- and discharge pumps, melting points >150°C can be easily handled.

The sophisticated vacuum system is able to handle incondensable volatiles with its dry running chemical resistant scroll pump as well as the air cooled diffusion  pump can reach a system pressure down to 0.00001mbar.

Due to the fully vacuum tight feed and discharge system there is no limitation in the charge or receiver vessel size and the system can run up to 24/7 operation without any interruption in the vacuum process and a throughput up to 7l/h.

Special Advantages of SP 1000 CC:

• Patent Pending Hybrid Evaporator
  • • Combines all the positive characteristics of glass and stainless steel
    • Full visibility of the process
    • Reliable and precise
    • Lowest tolerances in the market (no welding, no forming)
    • Easy cleaning
    • lowest maintenance & repair costs due to changeable glass-cylinders
    • complete heated inlet and outlet lines
    • Lowest hold up due to extreme compact design

• High capacity glass condenser
  • • Reliable and strong design
    • Easy removable for cleaning
    • Full visibility
    • Complete tempered
    • Maximized surface and minimized distance to the evaporator

• Precise Vacuum control system
  • • Digital vacuum controller for high reproducibility
    • Double vacuum sensor system (optional)
    • No problems with incondensable vapors due to high capacity oil free scroll vacuum pump (optional)
    • Vacuum line in huge diameter for maximum performance and easy cleaning
    • Automatic safety circuit for diffusion pump control (optional)
    • Double condensate receiver system to separate light ends
    • High capacity diffusion pump (65l/s → 234m³/h) with oil level indicator (optional)
    • Supersized vacuum cold-trap for outstanding vacuum performance
    • Cold-Trap with drain nozzle for easy maintenance
    • Optional electrical immersion cooler down to -90°C (no dry ice needed)

• Vertical design for optimized product flow without hold-up in useless pumping lines
• Hermetically sealed, high vacuum tight, tempered gear pumps for fully continuous operation
• Complete tempered discharge system without any solidification of heavy residues
• Sophisticated control cabinet for easy handling with CE and UL approval
• All heating/cooling circuits with maximized diameter and minimized length for optimized heat transfer

Technical Data

	Feed range	approx. 1000-7000 ml/h, dep. on application
	Evaporator	borosilicate glass/stainless steel 316
	Feed-vessel	5000 ml, graduated, refillable
	Product receivers	variable (2x 5000ml included)
	Evaporator surface	1000 cm2, short path
	Operating temperature	up to 200°C (250…350°C optional)
	Operating pressure	down to 10-5 mbar (optional)
	Mains Supply	230/400V 25A 3L+N+PE (50Hz or 60Hz available)

Processor controlled crude oil distillation system for flask volumes of 50 L and 100 L for fully automatic operation exactly conforming to ASTM D-2892 (TBP), latest revision.

The system is computer controlled and designed for fully automatic operation throughout the different distillation runs at different pressure levels which includes:

• debutanization
• run at atmospheric pressure
• run at vacuum 100 Torr
• run at vacuum 10 Torr
• run at vacuum 2 Torr

The system design is based on stainless steel flasks with a drain valve at the bottem for easy discharge of residues. Flask and flask heater are mounted on a movable trolley for easy removal oft he flask and possible exchange with other flask volumes.

The flask content is stirred by a powerful mechanical stirrer to ensure an effective mixing to ensure a smooth evaporation. The system can be equipped with interchangeable different flask volumes .

These different distillation runs are performed automatically without any intervention of the operator. The system automatically manages the changes of all involved operation pressure changes from atmospheric to the different vacuum conditions automatically with. The duration of the intermediate cooling procedure in between the different runs is minimized by an intensive cooling of the flask charge as well as introduction of N2 into the system.

The system measures online the volume of each fraction before each cut is being discharged into an automatic fraction collector with 20 receivers. The fraction collector is equipped with an inbuilt electronic balance to measure the weight of each fraction. By replacing filled receivers the system can handle up to 80 cuts for the distillation of one sample. The receiver change is performed according to pre-selected cut temperatures or when a receiver is filled up to continue the cut sampling in the next receiver (to avoid overfilling of the receiver).

After the distillation the operator needs to weigh the gas trap as well as the flask residue by the external balance (part of delivery), the weights are automatically taken by the system and as a result the final data evaluation and TBP-curves in weight-% and volume-% are printed out and can be stored.

The system can optionally be equipped with an online density measurement system.

The system requires for operation water, nitrogen, compressed air and electricity to be supplied by lab infrastructure.

The following video shows the test procedure of the fire alarm system for PETRODIST 100 CC, manually activated.

Mit dem Laden des Videos akzeptieren Sie die Datenschutzerklärung von Vimeo.
Mehr erfahren

Video laden

Vimeo immer entsperren

Fully-automatic high-temperature analysis system

New development from PILODIST for the distillation of high boiling and highly viscous products
with melting points up to 250°C (similar to ASTM D1160)

Fully-automatic distillation system with a process similar to ASTM D1160 with an extended temperature range for the determination of boiling ranges of crude oils and other hydrocarbons under atmospheric or vacuum conditions.

The system is equipped with a completely heated distillation line, to be tempered up to 250°C. It includes also a processor controlled high temperature heating chamber with an automatic optical fiber volume follower system to ensure that products with melting points of up to 250°C can be collected into the final receiver without any cristallization. As a result complete boiling curves from initial boiling point (IBP) up to the end boiling point (EBP) can be produced. The process can be realized in different pressure steps for the analysis of products with a wide boiling range.

The high temperature resistant stainless steel column (AISI 316Ti) enables head temperatures of up to 400°C under atmospheric conditions (depending on product). Temperatures of up to 650°C AET can be achieved under vacuum operation.

The heating is performed by an electrical high-temperature heating bath with quartz-glass isolation and a 500 ml stainless steel flask. By using a highly dynamic tempering system for the condenser circulation very fast cooling or heating rates can be achieved so that distillation and cleaning runs can follow in short sequences.

Advantages of PETRODIST 300 CC-HT

• parameter input, display as well as calculation of distillation & final data and print out of the distillation curve via PILODIST IP65 user interface with 15,6” touch screen and printer
• easy operation due to user-friendly software, operated under WINDOWS
• distillation can be performed under up to 4 pressure steps
• slow evacuation control to avoid foaming
• dynamic vakuum reduction down to 0,1Torr abs. for max. yields
• high performance cold trap with graduated condensate trap
• distillation reports and curves can ever be re-called
• precise vacuum control
• automatic washing run
• Calculation of charge according to receiver temperature and charge density
• Fully-automatic control and supervised distillation processs
• Additional up to 20 flexible selection of analysis yield points in addition to the values for evaluation requested by ASTM (5%, 10%, 20% 30%…)
• In addition to the volume point setting PD300CC offers additionally 5 temperature points to be set for volume determination per each pressure stage
• network connectivity
• distillation results are available in the following formats for LIMS systems:
  • PDF
  • XLS
  • TXT
  • CSV

Customized Computer Controlled Continuous Distillation System

This system, made of high quality borosilicate glassware 3.3, is for universal operation under atmospheric or vacuum conditions.