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www.buchi.com Information Bulletin Number 52 2008
Introduction drying process. Initially the droplet particle, while being suspended in the
temperature is approaching the drying chamber. If not, the wet or sticky
The two leading suppliers of spray wet-bulb temperature and as the particle hits the wall and either starts
drying systems in their respective particle dries the temperature increases coating the drying chamber or slightly
sectors, Bchi Labortechnik AG in the towards the spray dryer outlet drying air agglomerates with other particles.
laboratory scale and GEA Niro A/S in temperature. The equilibrium of the water in the
the industrial scale have teamed up to Drying takes place within seconds due vapour and the water content in the
offer their combined comprehensive to the very large liquid surface area final product normally depends on
knowledge of spray drying applications of the spray and the high heat transfer temperature and drying air vapour
to their customers. After first trials with coefficients. Hence, it is possible to dry concentration. A drier product is reached
a Bchi Mini Spray Dryer B-290, at moderate temperatures, which with higher outlet temperature and/or
the next task for most users is to go to enables even heat sensitive materials to lower spray dryer outlet drying air
a bigger scale. remain active after spray drying. vapour concentrations.
This leaflet describes a hands-on The rapid drying and consequently Decreasing the liquid feed rate,
approach to perform a scale-up from fast stabilization of solids in the whilst maintaining a constant outlet
initial trials in the research lab with the feed makes spray drying ideal for temperature by reducing the inlet
Mini Spray Dryer B-290 to laboratory particle engineering e.g. encapsulation, temperature, results in a decrease in the
production with the Niro MOBILE production of dry emulsions or drying air vapour concentration.
MINOR TM spray dryer. The MOBILE amorphous material, as well as the The drying time of a particle increases
MINOR TM is itself a natural next step up ability to adjust powder characteristics with spray chamber size setting up the
after the Mini Spray Dryer B-290, as well such as particle size, density, upper limit of the maximum achievable
as being an excellent first trial plant flowability and dispersability. particle size in a given spray dryer. This
when slightly larger feed quantities are The range of product applications limit especially depends on product
available. continuously expands, so that today characteristics and also process
The objectives are to maintain the most spray drying has connections with many parameters. It may be impossible to
important process conditions constant things in daily life: milk powder, baby obtain a usable powder in a small
during scale-up, such as to obtain same food, instant coffee, pharmaceuticals, drying chamber, whereas using a larger
particle sizes and residual humidity in detergents or dyes. chamber a robust process can be
the produced powders. Guidelines designed. When spray drying is
to adjust the droplet size of the spray The key to success is reproducible evaluated as a feasible new technology
and the relationships between water drying conditions when the feed for new product development, one has
evaporation rate, inlet and outlet droplets convert to particles. The to be aware of false negatives if only a
temperature are explained. droplet has to dry to a non-sticking small drying chamber is used. Contact
Bchis and Niros experts at the
Spray drying technology Current market trends in customer test centres for feasibility
spray drying: testing of your product!
Spray drying is a widely applied process
technology in the chemical, food and ! Improved bioavailability of drugs Some materials dried in spray dryers
pharmaceutical industries. It is a single exhibit thermoplastic and/or hygro-
! Drug delivery by inhalable particles
unit operation rapidly transforming scopic behaviour. Such materials
liquids (solutions, emulsions, slurries, ! Biodegradable polymers as matrix require extra attention. Hygroscopic
pastes or even melts) into powders materials for drug encapsulation materials require a higher drying
in one simple and robust continuous temperature and/or a lower drying air
! Biotech products like yeasts and
process. A spray of fine droplets vapour concentration to achieve a
cell cultures
generated by an atomizing device (e.g. desired residual moisture level. Hygro-
nozzles) is mixed with a stream of hot ! Dry powders of agglomerated scopic materials have a strong affinity
air whereby the water evaporates from nanoparticles to the used solvents and need to be
the droplet while suspended in the handled with care because of the easy
! Fuel cell batteries in the
drying air. re-absorption of vapours from the
automotive industry
The evaporation process uses heat from air phase if the temperature drops or
the drying air. Because of the water ! Microencapsulation and masking the vapour concentration rises. Typical
evaporation from the product, the of fragrances and aromas reabsorption places are cold surfaces
droplet and powder temperature remain in the dryer (e.g. non-insulated parts
! Natural products for traditional
at or below the spray dryer outlet of the dryer), final product discharge
Chinese medicine
drying air temperature during the entire containers and, subsequently, during
best@buchi 52 / 2008 en
laboratory analysis of the powder.
For materials exhibiting thermoplastic
2.0
behaviour, e.g. compounds with
1.8 Outlet temperature 40C
low glass transition temperature, the
50C
1.6 temperature range for drying is limited
60C
Evaporation rate [kg/h]
100C
1.0 for the Mini Spray Dryer B-290, the
Drying air flow rate 40 kg/h
30 kg/h water1 evaporation rate and the total air
0.8 flow rate (drying air and atomization air)
20 kg/h
have to be known.
0.6
Firstly, the water evaporation rate is
0.4
1
Although air, water, moisture and humidity
0.2 are used in the text, the descriptions equally
cover processes using nitrogen as drying
0.0
and atomizing gas with solvent vapour and
50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 230
feed liquids based on solvents (e.g. ethanol,
Inlet temperature [C] acetone etc.). Feed is used to describe any
solution or suspension or. The term droplet
Figure 1: Drying air flow rates in the Mini Spray Dryer B-290 as a function of inlet tempera-
is used for atomized feed or solvent before
ture and water evaporation rate at different outlet temperatures.
turning into particles
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calculated from a simple mass balance The drying air flow rate in the Mini Spray Now, the outlet drying air RW vapour
with the following parameters: feed Dryer B-290 is set by the aspirator EVR = FR (1can
concentration TS) FR TS from a
be calculated1 RW
flow rate, total solids content in the feed setting, which is an indicative reading. simple mass balance across the spray
and the residual water content in powder. However, this is not sufficiently accurate dryer. (Formula 1)
The feed flow rate can accurately be for scale-up calculations as the flow rate
found by weighing the feed container changes with the pressure drop across
before and after an experimental run. the plant e.g. due to powder build up in YIN YTFN
GIN + GTFN + EVR
the filter. Instead the accurate inlet and YOUT = 1 + YIN 1 + YTFN
outlet air temperature readings are used. GIN GTFN
RW +
EVR = FR (1 TS) FR TS Applying the heat and mass balance 1 + YIN 1 + YTFN
1 RW
equation across the spray dryer the
(Formula
(Formula 1) 1) evaporation capacity diagrams can be (Formula
(Formula 2)2)
drawn (Figures 1).
EVR = evaporation rate [kg/h] Based on the evaporation rate, the YOUT = outlet drying air vapour
G IN GTFN
FR = feed flow rate [kg/h] inlet and outlet temperatures, the total concentration
YOUT +
TS G
=INtotal Ysolids in the YTFN
feed
1 + Y IN 1 YTFN
+ EVR drying air flow rate (in kg/h) can be [kg vapour/kg dry air]
IN +
+ GTFN
= [kg1 +solids/kg
YIN feed] 1 + YTFN estimated. The error variations due to
EVR =
YIN = inlet dryingYINair vapour YTFN
YOUT GIN GTFN
RW = residualG water
IN
+ in GTFNpowder
the two-fluid nozzle atomization air flow concentration
1 + YIN 1 + YTFN
1 + YIN wet1 +powder]
[kg water/kg YTFN rates are negligible (error < 5%). [kg vapour/kg dry air]
YTFN = two-fluid nozzle atomization
(Formula 3)
40 G IN = FR = EVR
drying air flow rate
1 RW TS
35
GIN GTFN (including water vapour)
YOUT30 + [kg/h] (Formula 4)
1 + Y IN 1 + YTFN
EVR = 25 GTFN = two-fluid nozzle atomization
YIN YTFN air flow rate (including water
G20IN GTFN
15 1 + YIN 1 + YTFN vapour) [kg/h]
10
5 (Formula 3)
If the drying gas is ambient air the
0
water concentration varies significantly
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30
0 ... 60 Atomization air flow rate [kg/h] from day to day; typically this is in the
1 RW range of 2 to 20 g water per kg dry air.
FR = EVR
B-290 atomization
1 RW0.5 TS
air rotameter 1.0 2.0 3.0 4.0 5.0 6.0 Humidity data can be supplied from
reading [mm] MOBILE MINORTM atomization air pressure [bar] local weather stations. To decrease
(Formula 4)
Figure 2: Water droplet size (D50 ) as a function of atomization air flow rate for the
the relative humidity in the inlet air of
MOBILE MINORTM and the Mini Spray Dryer B-290 two-fluid nozzles. the Mini Spray Dryer B-290 the
Dehumidifier B-296 can be used. This
5.0 additional dehumidification step may
80 kg/h drying air flow rate Outlet improve the drying capacity and allows
4.5 temperature 40C
10 kg/h atomization air flow rate
the removal of more water per unit time
Evaporation rate [kg/h]
4.0 50C
60C - especially for hygroscopic materials.
3.5 70C
On the other hand, the compressed air
3.0 80C
90C normally used for the two-fluid nozzle is
2.5
100C very dry and quite consistent - typically
2.0 110C
in the range of 2 to 3 g water per kg dry
1.5 air.
1.0 If the drying gas is fresh nitrogen the
0.5 vapour concentration is zero. In a closed
0.0 loop configuration with a condenser such
50 70 90 110 130 150 170 190 210 230 250 as the Inert Loop B-295, the
Inlet temperature [C]
vapour concentration can be calculated
from the condenser outlet gas tempera-
Figure 3: MOBILE MINORTM inlet drying air temperature as a function of water
ture at 100% saturation using the
evaporation rate and outlet drying air temperature.
Antoine equation for the relevant solvent.
1 RW
(Formula 1)
(Formula 1)
best@buchi 52 / 2008 en
YIN YTFN
GIN + GTFN + EVR
1
YOUT = GIN + YYININ 1 YTFN
YTFN
+
+ GTFN TFN + EVR
YOUT = 1 + YINGIN + G 1 + YTFN
1 +GYININ 1 +GY TFN
TFN
+
1 + YIN 1 + YTFN
(Formula 2)
(Formula 2)
The next part in scaling up is to get provides longer residence times than G IN
GTFN
YOUT GIN + GTFN
the same particle size. In general, the the co-current two-fluid nozzle in the YOUT 1 + YIN + 1 + YTFN
1 + Y IN 1 + YTFN
droplet size distribution emerging from drying chamber and is therefore more EVR =
a two-fluid nozzle depends upon liquid suitable to dry larger droplets of heavy
EVR = GIN YYININ GTFN YYTFN TFN
The droplet size is difficult to estimate MINOR TM required to achieve the same
or measure. A simple approach is to vapour concentration in the outlet air as 11 RW
RW
FR
FR==EVR
EVR
operate the MOBILE MINORTM nozzle at in the Mini Spray Dryer B-290 (Formula 11RW
RW TS
TS
conditions providing similar droplet sizes 3). The feed rate is then determined with
as in the Bchi nozzle for water. This Formula 4. (Formula
(Formula 4)4)
(Formula 4)
MOBILE MINORTM
The MOBILE MINORTM is a flexible, easy-to-handle laboratory spray dryer. Since the introduction in 1948, more than 2100 units
have been sold worldwide. Todays versions meet the increasing demand for safety, sanitary and flexibility. Due to the different
nozzle techniques, the larger chamber diameter and the longer residence time, the MOBILE MINOR TM is a very versatile
instrument to further investigate the spray drying process or to make production batches. Achievable particle size depends
on nozzle selection and the total solids content of the liquid feed. The MOBILE MINORTM may produce particles in the 2 to 80
micron range and the drying air residence time is between 15 and 25 seconds.
The MOBILE MINORTM model with a pneumatically operated chamber roof can be equipped with three alternative atomizing
systems, ensuring an option is available that is best suited to the task. With the two-fluid nozzle in the centre of the chamber
roof, atomization is created by compressed air. The second option is to place a rotary atomizer in the centre of the chamber
roof where an air turbine supplies energy to the atomizer wheel by means of compressed air. Finally, there is the fountain mode
in which the two-fluid nozzle sprays upwards and atomization is created by compressed air. For operation with feeds based
on flammable solvents or powders subject to explosion risk, special designs are available.
best@buchi 52/ 2008 en
Water evaporation capacity 1.0 kg/h, higher for organic solvents 0.5-6.0 kg/h, higher for organic solvents
Weight 48 kg 250 kg
Rotary atomizer, two-fluid nozzle in co-current
Nozzle types Two-fluid nozzle with nozzle cleaning function
or fountain mode
Operating conditions Open, optional closed cycle with Inert-Loop B-295 Open, optional closed cycle Inert Loop
Table 2: Technical features of the Mini Spray Dryer B-290 and the MOBILE MINORTM.
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