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Temperature Control




                                     high precision thermoregulation




                                           Whitepaper


                    Temperature Control
            for Chemical Research and Production




Peter Huber Kältemaschinenbau GmbH                       Contents:
Werner-von-Siemens-Strasse 1                             Introduction to Temperature Control	                 2
77656 Offenburg / Germany                                Unistat Principal - Control and Heat Transfer	     3-5
Phone: +49 781 9603-0                                    Unistat Technology	                                6-7
Fax: +49 781 57211                                       Unistat Hybrid for High Volume Reactors	           8-9
info@huber-online.com                                    Practical Advantages	                               10
www.huber-online.com                                     Case Studies	                                    11-14




                                                   -1-
Temperature Control




Temperature Control
for Chemical Research and Production
Precise temperature control has a significant influence on performance and quality in chemical
process engineering. The Unistat range of temperature control systems ensure accurate temperatures
and stable process conditions in research laboratories, pilot plants and kilolabs worldwide. The new
Unistat Hybrid technology, offers solutions for temperature control of large scale production reactors,
enabling an affordable partial modernisation of existing central plant cooling/heating systems.


When it comes to chemical reactions in production processes the          Fig 1: Unistat temperature systems
                                                                         allow scale-up in small reactors
right temperature is critical and so accordingly, is the need for an     used in process development,
appropriate heating/cooling solution. For process engineers it is        to production volume
essential to find a compromise between yield quality and produc-
tivity. Over the years, and with the support of process engineers
from the chemical and pharmaceutical industry, the Unistat range
has been developed and refined. This collaboration has ensured
that Unistats remain at the forefront of technology, making them
suitable for controlling the temperature of chemical and bioreac-
tors, autoclaves, reaction blocks & calorimeters in mini, pilot and
distillation plants. As a result of their thermodynamic characteris-
tics, Unistats offer cutting edge performance regardless of the ap-
plication, excelling even under heavily changing system conditions.

To demonstrate the performance of the Unistat range over 200 case
studies have been created to show the Unistats unique ability to ad-
apt to process requirements, offering precise stability and control.



                                                                   -2-
Temperature Control


The Unistat Principal                                     Key to good heat transfer is pump per-                  Low Operating Costs
Reliable temperature control of a chemical                formance. In order to achieve optimal cir-              Compared to conventional heating and
process, is critical to success and, is depen-            culation, high flow rates, with low pump                cooling circulators, Unistats achieve gre-
dent on effective thermal transfer. With                  pressure are required. This allows heating              ater efficiency and reduce resource con-
traditional “Open bath” thermostats, limi-                and cooling energy to be transported very               sumption. Operating costs (electricity,
tations occur with; the flash points of ther-             effectively by the temperature control sys-             cooling water, thermal fluids, etc.) are less
mal fluids at high temperatures, causing a                tem so fast ramps are possible (Fig. 4).                than other systems.
narrow safe operating temperature range.
Degridation of thermal fluid due to eva-                  For a comparison of thermal dynamics it is
poration, water absorption and oxidation                  essential to take into account cooling po-
which dramatically reduces the thermal                    wer density [W / l]. Cooling power density
conductivity of the fluid. The large volume               is particularly important for applications
of fluid required for the bath puts a con-                with a continuously changing reaction
straint on performance and severely limit                 mass. Precise temperature control and
the dynamics of heating and cooling.                      process stability are crucial factors in ob-
                                                          taining the desired temperature result and
Unistat principle, (Fig. 2) unlike conventional           the better the heat transfer the quicker the
technology uses no internal bath. Instead a               temperature change. When endothermic
low internal volume in conjunction with an                or exothermic reactions occur, the Unistats
expansion vessel is used to compensate for                impressive ability to react to the process,
volume change induced by heating and coo-                 quick temperature changes and intergra-
ling. This principle reduces the mass of fluid            ted process safety feature allows the reac-
and as a result dramatically increases the rate           tion to be kept under tight control without Figure 2: The Unistat principle com-
of temperature change, achieving cooling ra-              over or undershoot, resulting in higher pu- bines powerful thermodynamics and
                                                                                                       modern microelectronics
tes of several hundred degrees per hour.                  rity levels, and better efficiency (Fig. 3).


                                                                                            Temperature °C
Selectivity
                                                                Reaction Speed

                              Optimum Temperature



                                                 Temperature

                                                    Interval




                                                                                                                                                Setpoint temperature
                                                                                                                                                Jacket temperature
                                                                                                                                                Process Temperature




                                Temperature                                                                                                                   Time (min)

Figure 3: Temperature control of a chemical reaction has a                                Figure 4: Regulation of an exothermic reaction in a reactor
significant influence on selectivity and reaction rate. The op-                           is fast and reliable and destruction of the reactor contents is
timum is often in a narrow temperature interval.                                          avoided.



 Thermal reactions are compensated quickly and reliably (Figure 4):
  Exothermic reaction starts 		                   The Unistat compensates by rapid cooling		             Process temperature rise is brought under control 	
  The reaction is cooled to setpoint temperature	 As the process temperature drops the Unistat heats	    The process is brought back to the desired temperature



                                                                                    -3-
Temperature Control



Power according to DIN 12876
DIN – Deutsches Institut für Normung, is                                                   Typical Unistat Applications:
the national standards body for Germany.                                                   »» Reaction Systems, Autoclaves
                                                                                           »» Pilot Plant
DIN 12876, demands that the quoted                                                         »» Mini Plant
cooling capacity is to be measured at                                                      »» Process Development
full pump power using water as a HTF.                                                      »» Double jacketed vessels
Reducing pump power reduces the heat
                                                                                           »» Reaction Calorimetry
entering the system leading to more net
                                                                                           »» Distillation
cooling capacity and makes lower tem-
                                                                                           »» Plant testing
peratures possible. Reducing the pump
                                                                                           »» Material Testing
speed increases cooling power and in
                                                                                           »» Combinatorial Chemistry
some cases 30 to 50 Watts and up to 5 °C
                                                                                           »» Semiconductor Industry
lower end temperatures can be achieved.
Huber always quote cooling power at full                                                   »» Kilolab
pump power.                                                                                »» Vacuum Chambers


Unistats have a very low filling volume     Figure 5: Unistats are in use in many industries - particularly in reactor
and therefore a very high cooling power     temperature control.
density [W / l]. This shows how quickly a
system changes temperature. A crucial pa-
rameter in terms of safety.




                                                               -4-
Temperature Control



True Adaptive Control                            a multi-dimensional model of the process,                         User defined ramp rates allow for faster
Varying research criteria and process de-        TAC is able to automatically adjust PID pa-                       or slower response (Fig. 6). If TAC is not
mands change the thermal load on the             rameters to cope with and respond rapidly                         required, the user can manually adjust the
temperature control system; what does            to sudden changes in the process.                                 PID parameters.
not change is the requirement for good
control.                                         Operating in both „Jacket” and „Process”,
                                                 TAC provides responsive and close control
The solution is True Adaptive Control (TAC)      with rapid changes with no overshoot to
which has the capability to automatically        the process - automatically and under all
change with those demands. By building           conditions.


    Rapid Ramping (no overshoot)                    Faster Ramping (minimal overshoot)




                                   Setpoint                                                Setpoint
                                   With TAC                                                With TAC
                                   Without TAC                                             Without TAC




Figure 6: TAC generates a multidimensional model of the process to achieve the                                     Figure 7: Large cross-sections and pump
desired temperature in the shortest times without overshoot                                                        connections minimise pressure losses
                                                                                                                   and provide optimum heat transfer




Optimised heat transfer                                                                                  Pump Curves
The Unistat range has improved pump
connections, with wide internal diameters
to minimise flow losses and internal pres-
sure. Wider bores, low pressure and low
flow resistance allow higher flow rates.
This has a significant influence on heat
transfer and results in improved cooling
                                                                      Pressure/bar




and heating capacity, improved process
control and faster response times. Large
Unistats are equipped with M24 x 1.5
pump connections (Fig. 7). Bench top mo-
dels are supplied with M16 x 1 adaptors
as standard; allowing existing connections
and hoses be used without modification.


                                                                                                                   Flow Rate l/min

                                                                                                    Measured according to DIN 12876 with water at 20 °C


                                                               Figure 8: Pump curves show reduced flow as pressure increases




                                                                                     -5-
Temperature Control



Practical features
In temperature control importance is
placed on the primary function of a system
such as heating and cooling power, but
often secondary attributes play a decisi-
ve role in performance. High heating and
cooling capacities are worthless if pres-
sure from the pump is too high. Pressure
reduces flow which causes heat transfer
to be restricted and this has a dramatic
effect on performance. With low pressure
and high flow smaller, less expensive units
are required.
                                              Figure 9: The Unistat range offers over 50 standard models for temperature con-
                                              trol applications in research, pilot plant and production from -120 to +425 ° C
Huber systems offer users numerous func-
tions and settings which make control
                                              ware against breakage and compensating        can be written and stored and a range of
simpler. These settings allow very fine
                                              for pressure changes in the thermal fluid.    safety features allow Unistats to run unat-
tuning of the application; for example,
                                              Intelligent temperature control techniques    tended. The Unistat-Pilot can be removed
True Adaptive Control (TAC) intelligent
                                              ensure minimum pressure with maximum          from the Unistat and mounted remotely
temperature control system, continuously
                                              flow for optimum heat transfer.               to allow flexible control. Further features
analyzes the system, learning with the ap-
                                                                                            such as: the programmer, adaptive casca-
plication so the more you use it the better
                                              Water Separation System                       de control, ramp functions, calendar start,
control. VPC – Variable Pressure Control,
                                              Occasionally water from previous applica- individual user menus, sensor calibration
with soft start, protecting delicate glass-
                                              tions, cleaning or moisture absorbed from and analogue and digital interfaces for in-
                                              the atmosphere during storage can build tegration in process control systems round
                                              up within the heat transfer fluid circuit. off the Unistats functionality.
                                              Unistats offer the unique water separati-
                                              on system, which allows residual water to Analogue and Digital Interfaces
                                              be removed. If water is not removed, ice Numerous data interfaces allow Huber
                                              builds up during low temperature work, systems to integrate into equipment or
                                              preventing heat transfer and in some ca- process control systems. Standard fea-
                                              ses resulting in costly repairs.              tures include an RS232/RS485 interface
                                                                                            and various analogue interfaces comply-
                                              Unistat-Pilot                                 ing to NAMUR standards are available.
                                              Unistats offer full functionality in the Uni- The optional Web.G@te module (Fig. 11)
                                              stat-Pilot controller. This 5.7 inch colour
                                              touch screen controller can be customised
                                              to display all the important parameters for
                                              the applications such as setpoints, actual
                                              values and limits clearly. Temperature gra-
                                              dients can be displayed in a real time gra-
                                              phic format and the unit can be switched
Figure 10: Unistat were developed with        from Celsius to Fahrenheit. In addition the
process engineers in chemical and phar-
maceutical companies
                                              Unistat-Pilot offers interfaces in 6 langua- Figure 11: WebG.@te enables instru-
                                                                                            ment control and data transfer via
                                              ge options, temperature control programs network or Internet

                                                                 -6-
Temperature Control


provides additional ports for Ethernet and      Performance in the smallest space The Petite Fleur comes with the Com.G@
USB, enabling the exchange of data over         High heating and cooling capacities, so-        te interface which offers RS232/RS485, a
corporate networks, the Internet or the         phisticated safety features and an extensi-     potential free contact, analogue interface
storage of data and profiles on USB sticks.     ve list of features - all in compact housing,   (0/4-20mA or 0-10V) and connection for
                                                with small footprints.                          external control signals (ECS). The Petite
Unistats stand out in safety and economy!                                                       Fleur is available in two versions for either
The efficient energy management system          According to DIN12876 cooling power is          temperature control of externally closed or
keeps electrical power consumption to a         divided by the size of the housing to give      externally open applications.
minimum. Reduced operating costs and            power density in watts/dm3 = kW/ms.
minimal use of water further saves on utility   Truly compact units occupy the smallest         Models for process technology
consumption. The hydraulically sealed con-      space whilst at the same time ensuring          The Unistat product range offers many
struction of the Unistat range prevents the     a high cooling power density (watts/litre)      models with the power to control a range
formation of oil vapours and oxidation, ex-     for temperature rates of several hundred        of reactors from small scale to 1,000 lit-
tending the lifetime of costly thermal fluids   degrees per hour.                               res or more depending on the application.
by years. The Unistat Pilot offers Compre-                                                      The product range has recently expanded
hensive safety features and continuously        Even the Petite Fleur, the smallest Unistat     with the addition of the new Unistats 905,
monitors the process allowing Unistats to       in the range, (Fig. 12) offers the best ther-   905w, 912w and 915w (Fig. 13). These
run remotely. In the event of an emergen-       modynamic properties and full functionali-      new models are suitable for many typical
cy, alarms are activated and, depending on      ty despite being incredibly compact with a      applications in process and process engi-
the user defined settings, the system will      small footprint. The working temperature
then either, turn off or, the emergency over-   range of the Petite Fleur is from -40°C
temperature protection function will be         to +200°C with cooling powers of 480
activated; switching the machine to 100%        watts, when measured at full pump speed
cooling in the event of a thermal runaway.      in accordance to DIN 12876. Decreasing
                                                the pump speed allows additional cooling
                                                power to become available – in some ca-
                                                ses an extra 50 watts can be achieved!

                                                The powerful variable speed pump gu-
                                                arantees optimum circulation with flow
                                                and pressure rates of 33l / min and 0.9
                                                bar. Unistats, including the Petite Fleur of-
                                                fer many safety options, such as TAC, VPC
                                                and Process Safety feature.




                                                        Figure 13: The new Unistats 905,
                                                      905w 912w and 915w are suitable
                                                          for applications in process and
                                                      process technologies, such as reac-
Figure 12: As the smallest of the Uni-                 tors, autoclaves, mini plant, pilot
stats, the Petite Fleur is suitable for               plants, reaction blocks, distillation
the research laboratories.                                                  columns, etc.


                                                                    -7-
Temperature Control


                                              and digital interfaces for connection to
                                              process control systems. The Unistat series
                                              offers cooling capacities up to 150 kW
                                              and operating temperatures from -120 °C
                                              to +425 °C.

                                              In addition options for weather protection
                                              and/or winter operation are available, al-
                                              lowing units to be located outdoors and
                                              controlled remotely with the detachable
                                              controller (Fig. 14). For Unistats sited in
                                              ATEX zones 1 & 2, Huber offers two so-
                                              lutions. The Unistat can either be placed
                                                                                               Figure 15: Ex-p Pressurised cabinet for
                                              in an Ex-p pressure chamber (Fig. 15). or
                                                                                               use within hazardous areas in ATEX
                                              an ATEX certified controller can be moun-        zones 1 & 2.
                                              ted in the ATEX area whilst the Unistat
Figure 14: The removable Unistat Pilot
can be used as a remote controller            remains in the safe zone.

                                              Production reactors
                                                                                               interaction of the individual energy sour-
                                              of 10 m³ or more
neering, e.g. temperature control of biore-                                                    ces and control temperature accordingly.
                                              The introduction of the new Unistat Hyb-
actors, autoclaves and reaction blocks in                                                      This results in faster heating times for lar-
                                              rid technology extends the range of Huber
Mini and Pilot Plants. All models cover a                                                      ge volume reactors heated by steam or re-
                                              systems allowing temperature control of
temperature range of -90 to +250 °C and                                                        spectively faster cooling times with liquid
                                              large volume reactors of 10,000 litres or
offer a heating capacity of 6 kW. Cooling                                                      nitrogen or cooling water. The advanta-
                                              more. The Unistat Hybrid combines the
capacities range from 4.5 to 11 kW de-                                                         ges of this technique are precise control,
                                              precise control of the Unistat range, with
pending on the model. The variable speed                                                       an extended temperature range, more
                                              the power of existing energy resources in
circulation pump achieves flow rates up to                                                     heating and cooling power and reliable
                                              a production facility such as steam, coo-
110 l/min.                                                                                     control of thermal reactions. Linking the
                                              ling water or liquid nitrogen (fig. 16), offe-
                                                                                               Unistat Hybrid into an existing centralised
                                              ring powerful process control and a parti-
The Unistat-Pilot enables further auto-                                                        cooling/heating system results in better
                                              al cost effective modernisation of existing
mation of work processes with features                                                         process conditions and improved produc-
                                              resources.
which include a programmer, ramp func-                                                         tion output.
                                              Using a Unistat Hybrid system (Fig. 17) in
tion, calendar, start, customisable user
                                              this way, allows the Unistat to manage the
menus, sensor calibration and analogue




Figure 16: Complete solution: The Unistat hybrid temperature control system used in conjunction with external heat ex-
changers and various energy sources (steam, cooling water, nitrogen) and controls the interaction.


                                                                   -8-
Temperature Control


Professional Scale-up                         Roche requires that chillers are HCFC, HFC                        Dynamics of the Unistat


Over 50 models are available in the Unis-     & PFC free. Now the entire Huber range
tat product group, offering precise tempe-    is offered with natural refrigerants as an
rature control from -120 to +425 °C. They     option or as standard.
range from very compact units to powerful
models for controlling temperature of pro-    The energy management system keeps
duction reactors, to the Unistat Hybrid for   energy consumption to a minimum. The
production scale. A range of accessories      Unistats highly efficient energy conversion
including: Heat transfer fluid, hose con-     from electrical power to temperature control
                                                                                                          Dynamics of conventional technology
nections, booster pumps, explosion proof      and the speed and accuracy of Huber saves
equipment, maintenance contracts are          resources, time and money. With a Huber
available.                                    chiller consumption of water can be reduced
                                              to zero and in addition to this, the materials
Environmental Commitment                      used in manufacturing are recyclable stain-
1995 signalled the end of the use of CFC‘s    less steel, copper and high grade polymers.
as refrigerants. In 1991, four years ahead
of the ban all Huber systems were built       For Huber, the eradication of CFC‘s is good
without CFC‘s and R22, which was later        but not sufficient, the current target is to     Figure 18: A comparison of the thermo-
banned in 2000. As a result Huber custo-      phaze out all FC‘s, well before the dead-        dynamics of Unistats and conventional
                                                                                               technology illustrates the practical
mers were the first to buy machines that      line in 2015. Reducing energy consumpti-         benefits. Time savings in research tasks
reached -120°C, fully Chlorine free and       on in the build and operation of systems         and an improved production through-
                                                                                               put are the main arguments.
environmentally friendly. Bespoke tempe-      remains a priority but the current units are
rature control systems developed in ac-       a great start, leading the way in reduced
cordance with the global K6 directive from    energy consumption.
                                                                                                 Modernisation of Che-
                                                                                                 mical Plants with the
                                                                                                 Unistat Hybrid
                                                                                                 Chemical and pharmaceutical production
                                                                                                 plants, often use central Cooling and Heating
                                                                                                 systems in production processes for tempera-
                                                                                                 ture control. The Unistat Hybrid system opti-
                                                                                                 mises existing systems by connecting a hyd-
                                                                                                 raulically sealed temperature control unit. The
                                                                                                 available cooling and heating capacity is incre-
                                                                                                 ased and the range of temperatures expanded.

                                                                                                 Benefits
                                                                                                 •	 Higher heating and cooling capacities
                                                                                                 •	 Use of existing energy resources such as
                                                                                                    steam, cooling water, LN2 liquid nitrogen, etc.
                                                                                                 •	 Temperature range extension in existing
                                                                                                    facilities
                                                                                                 •	 Precise control of the process temperature
                                                                                                 •	 Reliable compensation of thermal reactions
                                                                                                 •	 Low cost modernisation of existing
                                                                                                    facilities
                                                                                                 •	 Avoids costly and time consuming system
                                                                                                    renovations


Figure 17: With a Unistat Hybrid system production reactors of 10,000 liters and
more can be controlled. Advantages are a high precision control and reliable com-
pensation of thermal reactions.


                                                                  -9-
Temperature Control




                                                                              Process Safety
     Practical Advantages:                                               1
                                                                              Unistats provide an option to allow the circulation
                                                                              pump and compressor to continue to work despite
                                                                              an over temperature trip. This allows controlled
                                                                              heat removal and protects your thermally controlled
                                                                              products from being destroyed.
          Heat Transfer
          Powerful circulation pumps and a large
          hose cross section ensure maximum
                                                     10
          flow rates and optimum heat transfer.
                                                                                                              De-Gassing

                                                                                                      2
                                                                                                              Unistats only require de-gassing
                                                                                                              after each application set up. As
                                                                                                              a result uncontrolled conditions
                                                                                                              during normal operation will be
     Space saving design                                                                                      minimised.
     Unistats have a compact design requi-
     ring little space. The power to volume
     ratio (Watts/cm3) according to DIN
     12876 documents the extremely small
                                                  9
     space requirement of the Unistats.
                                                                                                                   Hydraulically sealed
                                                                                                                   Volume changes due to fluid temperature

                                                                                                           3       fluctuations are equalised by the expansi-
                                                                                                                   on vessel. The fluid in the expansion vessel
    Power / Volume                                                                                                 hydraulically seals the fluid circuit and
    Unistats have a high power to vo-                                                                              prevents early Oxidation.
    lume ratio (Watts/Litre). In practice,
    Unistats offer a very high speed of
    temperature change in the region of
                                              8
    several hundreds of Kelvin per hour.


                                                                                                                Touchscreen Colour
                                                                                                                Display

                                                                                                       4
                                                                                                                The large, graphic touchscreen aids
     Pressure Control
                                                  7
                                                                                                                operation and shows convenient display
     The pressure control VPC continuously
                                                                                                                of temperature runs directly on the
     monitors the pressure in the connected
                                                                                                                machine. Therefore essential application
     application and therefore protects the
                                                                                                                parameters are always in view.
     sensitive glass reactor from breakage.



                     Temperature Control                                                    Data Communication
                     The intelligent temperature control TAC
                     analyses the controlled fluid circuit conti-
                     nuously, and adjusts the control parameters     6              5       Unistats offer numerous possibilites for data
                                                                                            communication. RS232/RS485 interfaces are
                                                                                            fitted as standard, as well as various analogue
                     automatically. The result is the best control
                                                                                            interfaces. The optional Web.G@te offers additi-
                     results even with difficult applications.
                                                                                            onal interfaces for Ethernet, Internet and USB.




Peter Huber Kältemaschinenbau GmbH
Werner-von-Siemens-Strasse 1
77656 Offenburg / Germany
Phone: +49 781 9603-0
Fax: +49 781 57211
info@huber-online.com
www.huber-online.com
                                                                                  high precision thermoregulation


                                                                         - 10 -
Temperature Control




Case Study:
Unistat® 615w
Heating & cooling a Buchi 250 litre glass lined
stainless steel reactor through 60 K

Requirement
This case study shows the remarkable power trans-
fer capabilities of the Unistat range in using a Unistat
615w to heat and cool a 250-litre Buchi Glas Uster
GLSS reactor.

Method
The Unistat was connected to the reactor using two
2 metre insulated metal hoses. The reactor was filled
with 200 litre of Ethanol.

Results
The Unistat cools the process from 20 °C to -40 °C
(60 K) in approximately 150 minutes. It can be seen
from the jacket temperature that the system is “com-
fortable” with this load. The heat up time back to
20 °C takes approximately 60 minutes.




                                                                    Setup details
                                                                    Temperature range:	       –60...200 °C
                                                                    Cooling power: 	          9.5 kW @ 200…0 °C
                                                                    		                        8.0 kW @ -20 °C
                                                                    		                        4.8 kW @ -40 °C
                                                                    		                        1.2 kW @ -60 °C
                 Jacket temperature
                                                                    Heating power: 	          12 kW
                 Process temperature                                Hoses: 		                 M38x1,5; 2x2 m
                 Setpoint                                           HTF: 		                   DW-Therm (#6479)
                                                                    Reactor: 		               Buchi Glas Uster CR252
                                                                    		                        250 litre glass lined
                                                                    		                        (enameled) steel reactor
                                                                    Reactor content: 	        200 litre Ethanol
                                                                    Reactor stirrer speed:	   90 rpm
                                                                    Control: 		               process




                                                           - 11 -
Temperature Control




                                                    Case Study:
                                                    Unistat® 1005w
                                                    Cooling an Asahi 10 litre triple wall reactor to
                                                    -110 °C

                                                    Requirement
                                                    Temperatures required to carry out chemistry in spe-
                                                    cialised cryogenic research have become lower and
                                                    lower. This case study demonstrates that the process
                                                    temperature inside an Asahi vacuum insulated glass
                                                    reactor can be comfortably cooled and controlled at
                                                    -110 °C by using a Unistat 1005w.

                                                    Method
                                                    The Asahi reactor was connected to the Unistat
                                                    1005w using two 1.5 metre insulated metal hoses.
                                                    Under process control, a process set-point of -110 °C
                                                    was entered and the results recorded using the Huber
                                                    “SpyControl”.

                                                    Results
                                                    The jacket temperature cools quickly in a linear
                                                    fashion to -100 °C in approximately 55 minutes ramp
                                                    rate of 2 K/min) before slow.




Setup details
Temperature range:-120...100 °C
Cooling power:	 1.5 kW @ 100…-40 °C
	                 1.4 kW @ -60… -80 °C                                                  Jacket temperature
	                 1.0 kW @ -100°C                                                       Process temperature
Heating power:	 2.0 kW                                                                  Setpoint
Hoses:	 x1.5 m; M30x1.5
                  2
                  (#6386)
HTF:	             Kryothermal S
Reactor:	 litre insulated
                  10
                  jacketed glass reactor
Reactor content:	 10 litre M90.055.03
Stirrer speed:	   ~ 200 rpm
Control:	process


                                                                  Tmin Jacket -120 °C


                                                                                         On the point control




                                           - 12 -
Temperature Control




                                                                                           Case Study:
                                                                                           Unistat® 510w
                                                                                           Controlling a simulated 300  W (258  kcal  /  hr)
                                                                                           exothermic reaction in a 15 litre Buchi Glas Uster
                                                                                           reactor

                                                                                           Requirement
                                                                                           This case study shows the temperature profile of a
                                                                                           specific test while undergoing a simulated exother-
                                                                                           mic reaction.

                                                                                           Method
                                                                                           A Unistat 510w has been selected to control the pro-
                                                                                           cess temperature inside a 5 litre glass lined (ename-
                                                                                           led) steel reactor which is 2/3 filled with M20.235.20.

                                                                                           Results
                                                                                           The 300 W exothermic reaction increases the process
                                                                                           temperature by approx. 1.7 K and the Unistat com-
                                                                                           pensates the temperature difference in 9 minutes.
                                                                                           After a while the heater is removed out of the reactor
                                                                                           and the process temperature goes down to approx.
                                                                                           18.3 °C. The Unistat takes 12 minutes to bring back
                                                                                           the process temperature to its set-point.




                                                                                              Setup details
                                                                                              Unistat® 510w  Buchi Glas Uster reactor

                                                                                              Temperature range:	-50...250 °C
Heater „On“ at a value of                                                                     Cooling power:	 5.3 kW @ 0…250 °C
300 W (258 Kcal/hr)
                                                                                              	                  2.8 kW @ -20 °C
                                      Process temperature                                     	                  0.9 kW @ -40 °C
                                      back at set-point and                                   Heating power:	 6.0 kW
                                      controlled during
                                      simulated reaction                                      Hoses:	            2x1.5 m; M30x1.5
                                                                                              	(#6386)
                                                                                              HTF:	              DW-Therm (#6479)
                                                                                              Reactor:	 litre glass lined (enameled)
                                                                                                                 15
                               Heater „Off“                                                                      steel reactor
                                                                                              Reactor content:	 litre M20.235.20 (#6162)
                                                                                                                 10
                                                                                              Stirrer speed:	    80 rpm
                                                              Jacket ramps  8 K/min. to      Control:	process
                                                              recover the process to its
                                                              set-point




                     Jacket ramps  5.6 K/min. to create a           Jacket temperature
                     wide DT to make the extra entergy flow          Process temperature
                     out into the jacket
                                                                     Setpoint




                                                                          - 13 -
Temperature Control



                                                  Case Study:
                                                  Unistat® 705w
                                                  Unistat® 705w cooling a 2 litre reactor to Tmin

                                                  Requirement
                                                  This case study demonstrates the minimum achiev-
                                                  able process temperature when a Unistat 705 is con-
                                                  nected to a Radleys “Reactor Ready” system config-
                                                  ured with 2 litre vacuum insulated reactor.

                                                  Method
                                                  The reactor was filled with 1,5 litres of “P20.275.50”
                                                  as a thermal load, the stirrer set to 250 rpm and the
                                                  control to “Process”. The results were recorded on
                                                  the Huber “SpyControl” software.

                                                  Results
                                                  As can be seen from the graphic, the jacket rapidly
                                                  cools to -61 °C with a corresponding minimum pro-
                                                  cess temperature of -59 °C.

                                                  The ramp time back to 20 °C sees the jacket tempera-
                                                  ture increase to 47 °C before ramping back to bring
                                                  the process temperature exactly to its 20 °C set point.




Jacket temperature                                   Setup Details:
Process temperature
Setpoint
                                                     Temperature range:	 - 70...250 °C
                                                     Cooling power:	         0,6 kW @ -20 °C
                                                     	                       0,6 kW @ -40 °C
                                                     	                       0,3 kW @ -60 °C
                                                     Heating power:	         1,5 / 3,0 kW
                                                     Pump speed:	            3500 rpm
                                                     Hoses:	                2x1 m; M24x1,5
                                                                             (#9325)
                                                     HTF:	SilOil P20.275.50
                                                                             (#6157)
                                                     Reactor:	 litre vacuum 2
                                                                             jacketed glass reactor
                                                     Reactor content:	 litre P20.275.50
                                                                             1.5
                                                                             (#6259)
                                                     Reactor stirrer speed:	 250 rpm
                                                     Control:	Process




                      Over 200 Case Studies available to download at:
                          www.huber-online.com

                                        - 14 -

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Temperature Control for Reactors - a Huber Whitepaper

  • 1. Temperature Control high precision thermoregulation Whitepaper Temperature Control for Chemical Research and Production Peter Huber Kältemaschinenbau GmbH Contents: Werner-von-Siemens-Strasse 1 Introduction to Temperature Control 2 77656 Offenburg / Germany Unistat Principal - Control and Heat Transfer 3-5 Phone: +49 781 9603-0 Unistat Technology 6-7 Fax: +49 781 57211 Unistat Hybrid for High Volume Reactors 8-9 info@huber-online.com Practical Advantages 10 www.huber-online.com Case Studies 11-14 -1-
  • 2. Temperature Control Temperature Control for Chemical Research and Production Precise temperature control has a significant influence on performance and quality in chemical process engineering. The Unistat range of temperature control systems ensure accurate temperatures and stable process conditions in research laboratories, pilot plants and kilolabs worldwide. The new Unistat Hybrid technology, offers solutions for temperature control of large scale production reactors, enabling an affordable partial modernisation of existing central plant cooling/heating systems. When it comes to chemical reactions in production processes the Fig 1: Unistat temperature systems allow scale-up in small reactors right temperature is critical and so accordingly, is the need for an used in process development, appropriate heating/cooling solution. For process engineers it is to production volume essential to find a compromise between yield quality and produc- tivity. Over the years, and with the support of process engineers from the chemical and pharmaceutical industry, the Unistat range has been developed and refined. This collaboration has ensured that Unistats remain at the forefront of technology, making them suitable for controlling the temperature of chemical and bioreac- tors, autoclaves, reaction blocks & calorimeters in mini, pilot and distillation plants. As a result of their thermodynamic characteris- tics, Unistats offer cutting edge performance regardless of the ap- plication, excelling even under heavily changing system conditions. To demonstrate the performance of the Unistat range over 200 case studies have been created to show the Unistats unique ability to ad- apt to process requirements, offering precise stability and control. -2-
  • 3. Temperature Control The Unistat Principal Key to good heat transfer is pump per- Low Operating Costs Reliable temperature control of a chemical formance. In order to achieve optimal cir- Compared to conventional heating and process, is critical to success and, is depen- culation, high flow rates, with low pump cooling circulators, Unistats achieve gre- dent on effective thermal transfer. With pressure are required. This allows heating ater efficiency and reduce resource con- traditional “Open bath” thermostats, limi- and cooling energy to be transported very sumption. Operating costs (electricity, tations occur with; the flash points of ther- effectively by the temperature control sys- cooling water, thermal fluids, etc.) are less mal fluids at high temperatures, causing a tem so fast ramps are possible (Fig. 4). than other systems. narrow safe operating temperature range. Degridation of thermal fluid due to eva- For a comparison of thermal dynamics it is poration, water absorption and oxidation essential to take into account cooling po- which dramatically reduces the thermal wer density [W / l]. Cooling power density conductivity of the fluid. The large volume is particularly important for applications of fluid required for the bath puts a con- with a continuously changing reaction straint on performance and severely limit mass. Precise temperature control and the dynamics of heating and cooling. process stability are crucial factors in ob- taining the desired temperature result and Unistat principle, (Fig. 2) unlike conventional the better the heat transfer the quicker the technology uses no internal bath. Instead a temperature change. When endothermic low internal volume in conjunction with an or exothermic reactions occur, the Unistats expansion vessel is used to compensate for impressive ability to react to the process, volume change induced by heating and coo- quick temperature changes and intergra- ling. This principle reduces the mass of fluid ted process safety feature allows the reac- and as a result dramatically increases the rate tion to be kept under tight control without Figure 2: The Unistat principle com- of temperature change, achieving cooling ra- over or undershoot, resulting in higher pu- bines powerful thermodynamics and modern microelectronics tes of several hundred degrees per hour. rity levels, and better efficiency (Fig. 3). Temperature °C Selectivity Reaction Speed Optimum Temperature Temperature Interval Setpoint temperature Jacket temperature Process Temperature Temperature Time (min) Figure 3: Temperature control of a chemical reaction has a Figure 4: Regulation of an exothermic reaction in a reactor significant influence on selectivity and reaction rate. The op- is fast and reliable and destruction of the reactor contents is timum is often in a narrow temperature interval. avoided. Thermal reactions are compensated quickly and reliably (Figure 4):  Exothermic reaction starts  The Unistat compensates by rapid cooling  Process temperature rise is brought under control  The reaction is cooled to setpoint temperature  As the process temperature drops the Unistat heats  The process is brought back to the desired temperature -3-
  • 4. Temperature Control Power according to DIN 12876 DIN – Deutsches Institut für Normung, is Typical Unistat Applications: the national standards body for Germany. »» Reaction Systems, Autoclaves »» Pilot Plant DIN 12876, demands that the quoted »» Mini Plant cooling capacity is to be measured at »» Process Development full pump power using water as a HTF. »» Double jacketed vessels Reducing pump power reduces the heat »» Reaction Calorimetry entering the system leading to more net »» Distillation cooling capacity and makes lower tem- »» Plant testing peratures possible. Reducing the pump »» Material Testing speed increases cooling power and in »» Combinatorial Chemistry some cases 30 to 50 Watts and up to 5 °C »» Semiconductor Industry lower end temperatures can be achieved. Huber always quote cooling power at full »» Kilolab pump power. »» Vacuum Chambers Unistats have a very low filling volume Figure 5: Unistats are in use in many industries - particularly in reactor and therefore a very high cooling power temperature control. density [W / l]. This shows how quickly a system changes temperature. A crucial pa- rameter in terms of safety. -4-
  • 5. Temperature Control True Adaptive Control a multi-dimensional model of the process, User defined ramp rates allow for faster Varying research criteria and process de- TAC is able to automatically adjust PID pa- or slower response (Fig. 6). If TAC is not mands change the thermal load on the rameters to cope with and respond rapidly required, the user can manually adjust the temperature control system; what does to sudden changes in the process. PID parameters. not change is the requirement for good control. Operating in both „Jacket” and „Process”, TAC provides responsive and close control The solution is True Adaptive Control (TAC) with rapid changes with no overshoot to which has the capability to automatically the process - automatically and under all change with those demands. By building conditions. Rapid Ramping (no overshoot) Faster Ramping (minimal overshoot) Setpoint Setpoint With TAC With TAC Without TAC Without TAC Figure 6: TAC generates a multidimensional model of the process to achieve the Figure 7: Large cross-sections and pump desired temperature in the shortest times without overshoot connections minimise pressure losses and provide optimum heat transfer Optimised heat transfer Pump Curves The Unistat range has improved pump connections, with wide internal diameters to minimise flow losses and internal pres- sure. Wider bores, low pressure and low flow resistance allow higher flow rates. This has a significant influence on heat transfer and results in improved cooling Pressure/bar and heating capacity, improved process control and faster response times. Large Unistats are equipped with M24 x 1.5 pump connections (Fig. 7). Bench top mo- dels are supplied with M16 x 1 adaptors as standard; allowing existing connections and hoses be used without modification. Flow Rate l/min Measured according to DIN 12876 with water at 20 °C Figure 8: Pump curves show reduced flow as pressure increases -5-
  • 6. Temperature Control Practical features In temperature control importance is placed on the primary function of a system such as heating and cooling power, but often secondary attributes play a decisi- ve role in performance. High heating and cooling capacities are worthless if pres- sure from the pump is too high. Pressure reduces flow which causes heat transfer to be restricted and this has a dramatic effect on performance. With low pressure and high flow smaller, less expensive units are required. Figure 9: The Unistat range offers over 50 standard models for temperature con- trol applications in research, pilot plant and production from -120 to +425 ° C Huber systems offer users numerous func- tions and settings which make control ware against breakage and compensating can be written and stored and a range of simpler. These settings allow very fine for pressure changes in the thermal fluid. safety features allow Unistats to run unat- tuning of the application; for example, Intelligent temperature control techniques tended. The Unistat-Pilot can be removed True Adaptive Control (TAC) intelligent ensure minimum pressure with maximum from the Unistat and mounted remotely temperature control system, continuously flow for optimum heat transfer. to allow flexible control. Further features analyzes the system, learning with the ap- such as: the programmer, adaptive casca- plication so the more you use it the better Water Separation System de control, ramp functions, calendar start, control. VPC – Variable Pressure Control, Occasionally water from previous applica- individual user menus, sensor calibration with soft start, protecting delicate glass- tions, cleaning or moisture absorbed from and analogue and digital interfaces for in- the atmosphere during storage can build tegration in process control systems round up within the heat transfer fluid circuit. off the Unistats functionality. Unistats offer the unique water separati- on system, which allows residual water to Analogue and Digital Interfaces be removed. If water is not removed, ice Numerous data interfaces allow Huber builds up during low temperature work, systems to integrate into equipment or preventing heat transfer and in some ca- process control systems. Standard fea- ses resulting in costly repairs. tures include an RS232/RS485 interface and various analogue interfaces comply- Unistat-Pilot ing to NAMUR standards are available. Unistats offer full functionality in the Uni- The optional Web.G@te module (Fig. 11) stat-Pilot controller. This 5.7 inch colour touch screen controller can be customised to display all the important parameters for the applications such as setpoints, actual values and limits clearly. Temperature gra- dients can be displayed in a real time gra- phic format and the unit can be switched Figure 10: Unistat were developed with from Celsius to Fahrenheit. In addition the process engineers in chemical and phar- maceutical companies Unistat-Pilot offers interfaces in 6 langua- Figure 11: WebG.@te enables instru- ment control and data transfer via ge options, temperature control programs network or Internet -6-
  • 7. Temperature Control provides additional ports for Ethernet and Performance in the smallest space The Petite Fleur comes with the Com.G@ USB, enabling the exchange of data over High heating and cooling capacities, so- te interface which offers RS232/RS485, a corporate networks, the Internet or the phisticated safety features and an extensi- potential free contact, analogue interface storage of data and profiles on USB sticks. ve list of features - all in compact housing, (0/4-20mA or 0-10V) and connection for with small footprints. external control signals (ECS). The Petite Unistats stand out in safety and economy! Fleur is available in two versions for either The efficient energy management system According to DIN12876 cooling power is temperature control of externally closed or keeps electrical power consumption to a divided by the size of the housing to give externally open applications. minimum. Reduced operating costs and power density in watts/dm3 = kW/ms. minimal use of water further saves on utility Truly compact units occupy the smallest Models for process technology consumption. The hydraulically sealed con- space whilst at the same time ensuring The Unistat product range offers many struction of the Unistat range prevents the a high cooling power density (watts/litre) models with the power to control a range formation of oil vapours and oxidation, ex- for temperature rates of several hundred of reactors from small scale to 1,000 lit- tending the lifetime of costly thermal fluids degrees per hour. res or more depending on the application. by years. The Unistat Pilot offers Compre- The product range has recently expanded hensive safety features and continuously Even the Petite Fleur, the smallest Unistat with the addition of the new Unistats 905, monitors the process allowing Unistats to in the range, (Fig. 12) offers the best ther- 905w, 912w and 915w (Fig. 13). These run remotely. In the event of an emergen- modynamic properties and full functionali- new models are suitable for many typical cy, alarms are activated and, depending on ty despite being incredibly compact with a applications in process and process engi- the user defined settings, the system will small footprint. The working temperature then either, turn off or, the emergency over- range of the Petite Fleur is from -40°C temperature protection function will be to +200°C with cooling powers of 480 activated; switching the machine to 100% watts, when measured at full pump speed cooling in the event of a thermal runaway. in accordance to DIN 12876. Decreasing the pump speed allows additional cooling power to become available – in some ca- ses an extra 50 watts can be achieved! The powerful variable speed pump gu- arantees optimum circulation with flow and pressure rates of 33l / min and 0.9 bar. Unistats, including the Petite Fleur of- fer many safety options, such as TAC, VPC and Process Safety feature. Figure 13: The new Unistats 905, 905w 912w and 915w are suitable for applications in process and process technologies, such as reac- Figure 12: As the smallest of the Uni- tors, autoclaves, mini plant, pilot stats, the Petite Fleur is suitable for plants, reaction blocks, distillation the research laboratories. columns, etc. -7-
  • 8. Temperature Control and digital interfaces for connection to process control systems. The Unistat series offers cooling capacities up to 150 kW and operating temperatures from -120 °C to +425 °C. In addition options for weather protection and/or winter operation are available, al- lowing units to be located outdoors and controlled remotely with the detachable controller (Fig. 14). For Unistats sited in ATEX zones 1 & 2, Huber offers two so- lutions. The Unistat can either be placed Figure 15: Ex-p Pressurised cabinet for in an Ex-p pressure chamber (Fig. 15). or use within hazardous areas in ATEX an ATEX certified controller can be moun- zones 1 & 2. ted in the ATEX area whilst the Unistat Figure 14: The removable Unistat Pilot can be used as a remote controller remains in the safe zone. Production reactors interaction of the individual energy sour- of 10 m³ or more neering, e.g. temperature control of biore- ces and control temperature accordingly. The introduction of the new Unistat Hyb- actors, autoclaves and reaction blocks in This results in faster heating times for lar- rid technology extends the range of Huber Mini and Pilot Plants. All models cover a ge volume reactors heated by steam or re- systems allowing temperature control of temperature range of -90 to +250 °C and spectively faster cooling times with liquid large volume reactors of 10,000 litres or offer a heating capacity of 6 kW. Cooling nitrogen or cooling water. The advanta- more. The Unistat Hybrid combines the capacities range from 4.5 to 11 kW de- ges of this technique are precise control, precise control of the Unistat range, with pending on the model. The variable speed an extended temperature range, more the power of existing energy resources in circulation pump achieves flow rates up to heating and cooling power and reliable a production facility such as steam, coo- 110 l/min. control of thermal reactions. Linking the ling water or liquid nitrogen (fig. 16), offe- Unistat Hybrid into an existing centralised ring powerful process control and a parti- The Unistat-Pilot enables further auto- cooling/heating system results in better al cost effective modernisation of existing mation of work processes with features process conditions and improved produc- resources. which include a programmer, ramp func- tion output. Using a Unistat Hybrid system (Fig. 17) in tion, calendar, start, customisable user this way, allows the Unistat to manage the menus, sensor calibration and analogue Figure 16: Complete solution: The Unistat hybrid temperature control system used in conjunction with external heat ex- changers and various energy sources (steam, cooling water, nitrogen) and controls the interaction. -8-
  • 9. Temperature Control Professional Scale-up Roche requires that chillers are HCFC, HFC Dynamics of the Unistat Over 50 models are available in the Unis- & PFC free. Now the entire Huber range tat product group, offering precise tempe- is offered with natural refrigerants as an rature control from -120 to +425 °C. They option or as standard. range from very compact units to powerful models for controlling temperature of pro- The energy management system keeps duction reactors, to the Unistat Hybrid for energy consumption to a minimum. The production scale. A range of accessories Unistats highly efficient energy conversion including: Heat transfer fluid, hose con- from electrical power to temperature control Dynamics of conventional technology nections, booster pumps, explosion proof and the speed and accuracy of Huber saves equipment, maintenance contracts are resources, time and money. With a Huber available. chiller consumption of water can be reduced to zero and in addition to this, the materials Environmental Commitment used in manufacturing are recyclable stain- 1995 signalled the end of the use of CFC‘s less steel, copper and high grade polymers. as refrigerants. In 1991, four years ahead of the ban all Huber systems were built For Huber, the eradication of CFC‘s is good without CFC‘s and R22, which was later but not sufficient, the current target is to Figure 18: A comparison of the thermo- banned in 2000. As a result Huber custo- phaze out all FC‘s, well before the dead- dynamics of Unistats and conventional technology illustrates the practical mers were the first to buy machines that line in 2015. Reducing energy consumpti- benefits. Time savings in research tasks reached -120°C, fully Chlorine free and on in the build and operation of systems and an improved production through- put are the main arguments. environmentally friendly. Bespoke tempe- remains a priority but the current units are rature control systems developed in ac- a great start, leading the way in reduced cordance with the global K6 directive from energy consumption. Modernisation of Che- mical Plants with the Unistat Hybrid Chemical and pharmaceutical production plants, often use central Cooling and Heating systems in production processes for tempera- ture control. The Unistat Hybrid system opti- mises existing systems by connecting a hyd- raulically sealed temperature control unit. The available cooling and heating capacity is incre- ased and the range of temperatures expanded. Benefits • Higher heating and cooling capacities • Use of existing energy resources such as steam, cooling water, LN2 liquid nitrogen, etc. • Temperature range extension in existing facilities • Precise control of the process temperature • Reliable compensation of thermal reactions • Low cost modernisation of existing facilities • Avoids costly and time consuming system renovations Figure 17: With a Unistat Hybrid system production reactors of 10,000 liters and more can be controlled. Advantages are a high precision control and reliable com- pensation of thermal reactions. -9-
  • 10. Temperature Control Process Safety Practical Advantages: 1 Unistats provide an option to allow the circulation pump and compressor to continue to work despite an over temperature trip. This allows controlled heat removal and protects your thermally controlled products from being destroyed. Heat Transfer Powerful circulation pumps and a large hose cross section ensure maximum 10 flow rates and optimum heat transfer. De-Gassing 2 Unistats only require de-gassing after each application set up. As a result uncontrolled conditions during normal operation will be Space saving design minimised. Unistats have a compact design requi- ring little space. The power to volume ratio (Watts/cm3) according to DIN 12876 documents the extremely small 9 space requirement of the Unistats. Hydraulically sealed Volume changes due to fluid temperature 3 fluctuations are equalised by the expansi- on vessel. The fluid in the expansion vessel Power / Volume hydraulically seals the fluid circuit and Unistats have a high power to vo- prevents early Oxidation. lume ratio (Watts/Litre). In practice, Unistats offer a very high speed of temperature change in the region of 8 several hundreds of Kelvin per hour. Touchscreen Colour Display 4 The large, graphic touchscreen aids Pressure Control 7 operation and shows convenient display The pressure control VPC continuously of temperature runs directly on the monitors the pressure in the connected machine. Therefore essential application application and therefore protects the parameters are always in view. sensitive glass reactor from breakage. Temperature Control Data Communication The intelligent temperature control TAC analyses the controlled fluid circuit conti- nuously, and adjusts the control parameters 6 5 Unistats offer numerous possibilites for data communication. RS232/RS485 interfaces are fitted as standard, as well as various analogue automatically. The result is the best control interfaces. The optional Web.G@te offers additi- results even with difficult applications. onal interfaces for Ethernet, Internet and USB. Peter Huber Kältemaschinenbau GmbH Werner-von-Siemens-Strasse 1 77656 Offenburg / Germany Phone: +49 781 9603-0 Fax: +49 781 57211 info@huber-online.com www.huber-online.com high precision thermoregulation - 10 -
  • 11. Temperature Control Case Study: Unistat® 615w Heating & cooling a Buchi 250 litre glass lined stainless steel reactor through 60 K Requirement This case study shows the remarkable power trans- fer capabilities of the Unistat range in using a Unistat 615w to heat and cool a 250-litre Buchi Glas Uster GLSS reactor. Method The Unistat was connected to the reactor using two 2 metre insulated metal hoses. The reactor was filled with 200 litre of Ethanol. Results The Unistat cools the process from 20 °C to -40 °C (60 K) in approximately 150 minutes. It can be seen from the jacket temperature that the system is “com- fortable” with this load. The heat up time back to 20 °C takes approximately 60 minutes. Setup details Temperature range: –60...200 °C Cooling power: 9.5 kW @ 200…0 °C 8.0 kW @ -20 °C 4.8 kW @ -40 °C 1.2 kW @ -60 °C Jacket temperature Heating power: 12 kW Process temperature Hoses: M38x1,5; 2x2 m Setpoint HTF: DW-Therm (#6479) Reactor: Buchi Glas Uster CR252 250 litre glass lined (enameled) steel reactor Reactor content: 200 litre Ethanol Reactor stirrer speed: 90 rpm Control: process - 11 -
  • 12. Temperature Control Case Study: Unistat® 1005w Cooling an Asahi 10 litre triple wall reactor to -110 °C Requirement Temperatures required to carry out chemistry in spe- cialised cryogenic research have become lower and lower. This case study demonstrates that the process temperature inside an Asahi vacuum insulated glass reactor can be comfortably cooled and controlled at -110 °C by using a Unistat 1005w. Method The Asahi reactor was connected to the Unistat 1005w using two 1.5 metre insulated metal hoses. Under process control, a process set-point of -110 °C was entered and the results recorded using the Huber “SpyControl”. Results The jacket temperature cools quickly in a linear fashion to -100 °C in approximately 55 minutes ramp rate of 2 K/min) before slow. Setup details Temperature range:-120...100 °C Cooling power: 1.5 kW @ 100…-40 °C 1.4 kW @ -60… -80 °C Jacket temperature 1.0 kW @ -100°C Process temperature Heating power: 2.0 kW Setpoint Hoses: x1.5 m; M30x1.5 2 (#6386) HTF: Kryothermal S Reactor: litre insulated 10 jacketed glass reactor Reactor content: 10 litre M90.055.03 Stirrer speed: ~ 200 rpm Control: process Tmin Jacket -120 °C On the point control - 12 -
  • 13. Temperature Control Case Study: Unistat® 510w Controlling a simulated 300  W (258  kcal  /  hr) exothermic reaction in a 15 litre Buchi Glas Uster reactor Requirement This case study shows the temperature profile of a specific test while undergoing a simulated exother- mic reaction. Method A Unistat 510w has been selected to control the pro- cess temperature inside a 5 litre glass lined (ename- led) steel reactor which is 2/3 filled with M20.235.20. Results The 300 W exothermic reaction increases the process temperature by approx. 1.7 K and the Unistat com- pensates the temperature difference in 9 minutes. After a while the heater is removed out of the reactor and the process temperature goes down to approx. 18.3 °C. The Unistat takes 12 minutes to bring back the process temperature to its set-point. Setup details Unistat® 510w Buchi Glas Uster reactor Temperature range: -50...250 °C Heater „On“ at a value of Cooling power: 5.3 kW @ 0…250 °C 300 W (258 Kcal/hr) 2.8 kW @ -20 °C Process temperature 0.9 kW @ -40 °C back at set-point and Heating power: 6.0 kW controlled during simulated reaction Hoses: 2x1.5 m; M30x1.5 (#6386) HTF: DW-Therm (#6479) Reactor: litre glass lined (enameled) 15 Heater „Off“ steel reactor Reactor content: litre M20.235.20 (#6162) 10 Stirrer speed: 80 rpm Jacket ramps 8 K/min. to Control: process recover the process to its set-point Jacket ramps 5.6 K/min. to create a Jacket temperature wide DT to make the extra entergy flow Process temperature out into the jacket Setpoint - 13 -
  • 14. Temperature Control Case Study: Unistat® 705w Unistat® 705w cooling a 2 litre reactor to Tmin Requirement This case study demonstrates the minimum achiev- able process temperature when a Unistat 705 is con- nected to a Radleys “Reactor Ready” system config- ured with 2 litre vacuum insulated reactor. Method The reactor was filled with 1,5 litres of “P20.275.50” as a thermal load, the stirrer set to 250 rpm and the control to “Process”. The results were recorded on the Huber “SpyControl” software. Results As can be seen from the graphic, the jacket rapidly cools to -61 °C with a corresponding minimum pro- cess temperature of -59 °C. The ramp time back to 20 °C sees the jacket tempera- ture increase to 47 °C before ramping back to bring the process temperature exactly to its 20 °C set point. Jacket temperature Setup Details: Process temperature Setpoint Temperature range: - 70...250 °C Cooling power: 0,6 kW @ -20 °C 0,6 kW @ -40 °C 0,3 kW @ -60 °C Heating power: 1,5 / 3,0 kW Pump speed: 3500 rpm Hoses: 2x1 m; M24x1,5 (#9325) HTF: SilOil P20.275.50 (#6157) Reactor: litre vacuum 2 jacketed glass reactor Reactor content: litre P20.275.50 1.5 (#6259) Reactor stirrer speed: 250 rpm Control: Process Over 200 Case Studies available to download at: www.huber-online.com - 14 -