Microwave Vacuum Drying for advanced

Process Technology
Rapid and gentle Vacuum Drying for thermo sensitive Products with
low thermal Conductivity
Introduction
Heat-drying has become important in almost all areas of industrial processing. Apart from the
popular conventional procedures based on conduction, convection, or infrared radiation, heat-
drying utilising microwave energy is an attractive solution to many problems in process
technology. In microwave drying, heat is generated by directly transforming the electromagnetic
energy into kinetic molecular energy, thus the heat is generated deep within the material to be
dried. Especially in vacuum drying the fact of volume heating gives an enormous importance in
order to dry bulk and viscous products with low thermal conductivity.

Basics of Microwave Drying

The applied microwave energy will be transformed depending from the depth of vacuum directly
into evaporation heat.

If all the microwave energy is absorbed, the power density can be calculated using the following
formula

P = 2 ⋅ π ⋅ f ⋅ E ² ⋅ εo ⋅ ε ' r ⋅ tan δ in W/m3 (1),

The penetration depth can be calculated with

d = λo ε'r in cm (2).
2⋅π ⋅ε''r
f frequency, measured in Hz
εo absolute dielectric constant (DC) = 8,85x10-12 As/Vm
E electrical field strength, measured in V/m
ε = εo * ( εr’ -j εr’’ ) complex dielectric constant tanδ = εr’’/εr’
δ dielectric loss angle, measured in degrees
λ0 wave length, measured in, λ0 =c / f

[ Reference see company brochure „Dielectrical heating using Microwaves“ (1) or see also the abstract
published under http://www.pueschner.com/de/basics/index.html]
File: pub_mw-vacuum-drying_engl.doc Seite:1

X Produktfeuchte in kg/kg
P am Gerät eingestellte MW-Leistung
3
T Temperatur in °C des Luftstromes in m /h

Figure 1. Comparison between microwave and conventional heating drying Al2O3-Granular, 2mm

PÜSCHNER GMBH + CO KG MikrowellenEnergietechnik Telefon +49 (421) 68853-0

Postfach 1151 D-28784 Schwanewede bei Bremen Fax +49 (421) 68853-10
Steller Heide 14 http://www.pueschner.com [email protected]
 The most important parameter for microwave heating is the dielectric losses of the product to be
dried. For a big range of products the dielectric losses were measured by Hippel [2].
If no dielectric losses are known from literature, we are able to measure these properties in our
laboratory.

Fields of Application for Microwave Vacuum Drying

• Pharmaceutical Industry
• Food Industry
• Chemical Industry of Fine Chemicals
• Semi-Conductor Manufacturing

Advantages
As compared to conventional drying methods, microwaves penetrate into much greater depths.
This so-called volume heating has the following advantages:

1. a temperature gradient directed towards the surface, i.e. temperatures inside are higher than
on the outside giving rise to a higher partial pressure that drives the evaporating liquid to the
surface
2. consequently, the superficial layer does not dry out completely and the surfaces remain
permeable
3. the liquid evaporating inside the product is emitted through the pore structure of the solid
material’s macro-capillary system, resulting in a high drying velocity
4. the heating of water and most organic solvents occurs selectively - due to the greater
dielectric losses of water as compared to the product to be dried
5. swift and thorough drying of moist products with low thermal conductivity
6. stationary drying of thick layers without frictional losses
7. high total efficiency of energy application
8. high-speed control of the energy transport
9. short processing times, i.e. suitable for automated manufacturing

Together with the appropriate vacuum drying technology the following advantages for the product
are available:

1. Low drying temperatures treat the product gentle

2. No oxygen attack for the product
3. Highly nutritious instant properties
4. Better flavour
5. Less hydroscopic final product
6. Minimal product losses
7. Static drying of thick layers without frictional losses, therefore no mechanic stress for the
product

The microwave vacuum technology results in unique process technology giving the following
benefits:
File: pub_mw-vacuum-drying_engl.doc Seite:2

1. Local controlled energy zones with high controller speed

2. Defined and short residence times of the product to be dried
3. Cooling zone at the outlet for viscous products
4. Closed system
5. Simple setting of different plant operation modes for every product
6. Continuous operation mode possible
7. Short process times, high efficiency and full automated guarantees an economic operation
8. Service friendly because of modular system and full-automated cleaning

PÜSCHNER GMBH + CO KG MikrowellenEnergietechnik Telefon +49 (421) 68853-0

Postfach 1151 D-28784 Schwanewede bei Bremen Fax +49 (421) 68853-10
Steller Heide 14 http://www.pueschner.com [email protected]
 Special Conditions for Vacuum Drying
For integration of microwave components into a vacuum system, some important high frequency
specific items have to be taken into consideration. These are in particular:

• Dielectric properties
• Installed transport systems
• Product throughput rate
• Drying parameter
• Used vacuum, in particular the depth of the vacuum

A homogenous microwave energy distribution over the cross section of the product bed is a
significant requirement. Especially in applications of end-drying or in applications using products
with poor dielectric losses, special microwave antenna systems are required in order to achieve
even temperature and drying results.

Also peaks in the electric fields strength have to be avoided using high quality DC microwave
power supplies, because the breakdown field strength is reduced by the vacuum. If the
breakdown field strength is exceeded, the results are sparks and plasma.

The process parameters as well as the microwave applicator or microwave antenna system have
to be evaluated using microwave vacuum trial plants. Figure 2 shows a microwave trial plant,
which can be equipped with different applicators or antenna systems. Using an infrared and
fibre-optical temperature measurement system, core and surface temperatures can be
measured. Additional the weight loss, pressure and the absorbed microwave energy can be
measured also.

Legends:

1) Pyrometer (0..1000°C)
2) Fibre-optical temperature
measurement system
3) Microwave antenna
4) Pressure measurement
5) Circulator (magnetron
protection) incl.
Measurement of the
reflected power
6) 1.2kW/2450MHz
Magnetron incl. DC high-
voltage power supply.
7) Vacuum vessel ca. 200l
8) 10kg load cell, 10.ooo
digits
9) wall heating

Figure 2. Microwave Vacuum Trial Plant µWaveVac0150

File: pub_mw-vacuum-drying_engl.doc Seite:3

In order to perform trials for evaporation of solvents, the vacuum vessel can be inert using
nitrogen. The procedure of applying nitrogen is observed with an oxygen measurement device.

Based on the results of these trials an up-scale plant concept for he final production throughput
rate can be made.

PÜSCHNER GMBH + CO KG MikrowellenEnergietechnik Telefon +49 (421) 68853-0

Postfach 1151 D-28784 Schwanewede bei Bremen Fax +49 (421) 68853-10
Steller Heide 14 http://www.pueschner.com [email protected]
 Combination of an Air/Vacuum/Microwave 2.4qm Disk Dryer
under Explosive Protection and cGMP
For drying of solvents in pharmaceutical products the microwave vacuum dryer µWaveVac0209
was developed. As a 2.4qm disk dryer it can be used with circulating air heating as well as with
vacuum. In order to cover the requirements of explosive protection, the procedure of applying
nitrogen to inert the atmosphere inside the vacuum vessel is controlled with a redundant oxygen
measurement system.

The evaporation of solvent e.g. ethanol is measured with an online infrared measurement system
in order to avoid critical gas concentrations within vacuum vessel. An inbuilt online load cell as
well as an infrared and a fibre-optical enable a controlled drying process using a PLC system.
The microwave vacuum dryer fulfils the requirements of cGMP.

A flexible PLC with a processing control language guarantees the reproducibility of each drying
batch. In end-drying the absolute deviations from all product positions on all disk layers are
smaller than 0.2%. A typical drying curve is shown in Figure 4.

Figure 3. Microwave Disk Dryer for combined Air Circulation and Vacuum Mode µWaveVac0209
File: pub_mw-vacuum-drying_engl.doc Seite:4

Figure 4. Visualized Drying Curve of a thermo sensitive chemical Raw-material

PÜSCHNER GMBH + CO KG MikrowellenEnergietechnik Telefon +49 (421) 68853-0

Postfach 1151 D-28784 Schwanewede bei Bremen Fax +49 (421) 68853-10
Steller Heide 14 http://www.pueschner.com [email protected]
 Continuous Vacuum Drying using the Microwave Belt Dryer
µWaveVac1290
Using conventional vacuum dryer the product is heated using contact heating within several
heating zone. Heated plates are used as heat transfer medium using pressure water, steam,
oil or electrical sources.

Compared to the above mentioned conventional heating systems microwave is the better
alternative. Microwave vacuum belt dryers are used for the continuous and automatic drying
of temperature sensitive products with low thermal conductivity such as herbal extracts, food,
pharmaceutical and chemical products. The drying process is adapted to the desired dry
product quality such as final solids content, solubility, density and others.
The feed of solids is effected by means of a suitably designed feeding device with attached
and product orientated metering and distribution set-up in the dryer. When feeding wet
product a metering pump and an oscillating feeder are allocated. The movement of this feeder
is adjustable during operation. Therefore an easy optimising is possible.
Pump able products pass normally a high viscose and sticky phase during drying. Towards
the end of the drying and influenced by the steam bubbles a dry cake is formed. This cake is
brittle and is broken at the end of the belt and, if required, granulated.
The vacuum belt dryer consists of a casing with built in transporting belt. The belts are made
from selected PTFE coated glass fibres. For the continuous and automatic operation of such a
plant, a belt control device that runs reliably for a long period is imperative.

For the product quality to be achieved, the heating temperature during drying is of essential
influence. In the tradition vacuum belt dryer normally the belts run over 3 or 4 heating zones
and at the end through a cooling zone. These are fed with hot water, steam or thermo oil. With
using microwave heating careful arranged microwave heater with infinitely variable power
making sure an optimum energy transfer into the product. The temperature profile may be
selected to the needs of the product. The product temperature will be controlled with infrared
thermometers installed on top of the dryer. When the product temperature will climb up in a
critical value, the microwave power will be reduced automatically. Microwave heater usage
normally is 1.2/2/3/6kW-2450MHz. The design of the size will be according to the necessary
water evaporation

Legende:

1 Granular product inlet

2 Distribution system
3 Microwave Belt Drying
Zones
4 PTFE coated conveyor
belt
5 Product outlet
6 Hopper with dried
File: pub_mw-vacuum-drying_engl.doc Seite:5

product
7,8 Microwave system (2x)
9 Vacuum control
10 Steam injector
11 Condenser
12 Water ring vacuum pump
13 Gas steam injector
14 Water ring pump in- /
outlet
15, IR-camera (2x)
16

Figure 4. Process Flow Diagram µWaveVac1290

PÜSCHNER GMBH + CO KG MikrowellenEnergietechnik Telefon +49 (421) 68853-0

Postfach 1151 D-28784 Schwanewede bei Bremen Fax +49 (421) 68853-10
Steller Heide 14 http://www.pueschner.com [email protected]
 The normal working vacuum pressure for drying is in the range of 10 to 50mbar abs. The outlet
sluice chamber can also be used as a product buffer hopper. Die material is discharged in a
cyclic way during continuous operation. The vacuum for the inlet and outlet sluice chamber is
provided by a separate vacuum system.

The complete microwave vacuum dryer is controlled by a PLC system. Data recording and
process visualising as well as active process diagrams can be managed with a WINDOWS PC.
Standard protocol interfaces based on RS232 or Ethernet are available. As a http-server the
microwave plant can be set-up in a TCP/IP network and allow web enabled engineering as well
as remote control access via Intra- and Internet.

Figure 5. µWaveVac1290

For cleaning two options are available:

• Integrated cleaning
• External cleaning by removing the complete transport system

The continuous microwave vacuum dryer provides optimal setting in order to achieve best drying
results. The following parameters can be adjusted:

• Flow rate for granular or for viscous products

• Nozzle section, nozzle distance to belt, charge width of viscous products
File: pub_mw-vacuum-drying_engl.doc Seite:6

• Foam of the product while charging the belt

• Closed product foam
• Inlet cycle time and product rate for granular at the inlet sluice chamber
• Belt speed
• Vacuum
• Microwave power
• Outlet cycle time

PÜSCHNER GMBH + CO KG MikrowellenEnergietechnik Telefon +49 (421) 68853-0

Postfach 1151 D-28784 Schwanewede bei Bremen Fax +49 (421) 68853-10
Steller Heide 14 http://www.pueschner.com [email protected]
 Summery
Microwave Drying has a big advantages compared with conventional drying, because in
microwave drying, heat is generated by directly transforming the electromagnetic energy into
kinetic molecular energy, thus the heat is generated deep within the material to be dried.

Especially in microwave vacuum drying this advantages has a big significance for viscous and
bulk products with poor thermal conductivity.

The described microwave vacuum technology is used for high-end drying applications of thermo
sensitive products in order to achieve higher product qualities and shorter drying times.

Using appropriate process control even applications with explosive protection can be managed.

As microwave vacuum technology always has to cover specific application requirements due to
the transport system, microwave applicators, dielectric losses of the product, the effort on
development work is quite high. Therefore this technology is mainly used for high value products.

References
(1) H.A.Püschner
„Dielektrische Erwärmung durch Mikrowellen“
Kongressband Internat. Elektrowärmekongress 1963 Wiesbaden

(2) A.R. von Hippel, Dielectric Materials and Applications, The Technology Press of. M.I.T., 1954
File: pub_mw-vacuum-drying_engl.doc Seite:7

PÜSCHNER GMBH + CO KG MikrowellenEnergietechnik Telefon +49 (421) 68853-0

Postfach 1151 D-28784 Schwanewede bei Bremen Fax +49 (421) 68853-10
Steller Heide 14 http://www.pueschner.com [email protected]