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BIOCON’s membrane systems for ultra- and microfiltrtion.
Application in various branches of industry.
The results of long-term developments in
the field of installation designing for cross flow microfiltration
and ultrafiltration are presented. As filter elements
there are used tubular ceramic membranes from aluminum oxide with silicon
carbide selective layer and roll membranes from polysulphonamide.
There are given many examples of
application of these installations in pharmaceutical, food and dairy, fuel and
energy industries and in water treatment.
There are shown some research results
concerning concentration of cow and soybean milk and microfiltration
of skim milk using new ceramic membranes.
Content:
1. Introduction.
2. Design and operating principles of the BIOCON membrane
systems.
3. Application of the BIOCON membrane systems.
3.1. Pharmaceutical and microbiological industries.
3.1.1. Riboflavin.
3.1.2. Erythromycin .
3.1.3. Vitamin В2.
3.1.4. Lysine.
3.1.5. Enzymes.
3.2. Dairy industry.
3.2.1. Milk concentration.
3.2.2. Whey and lactose concentration.
3.2.3. Milk microfiltration.
3.3. Food industry.
3.3.1. Soybean milk.
3.3.2. Drinks, extracts,
syrups.
3.3.3. Wines.
3.3.4. Water treatment in beer production.
3.4. Fuel and energy industries.
4. Conclusion.
References.
1.
Introduction.
The membrane filtration processes, particularly, ultrafiltration
and microfiltration are separation processes, which
go under pressure on porous polymeric or inorganic materials. For the last 30
years these processes have found application in different industries for
liquids purification or concentration.
Sales of membranes and membrane equipment are increased continuously with
approximately 10-12% annual rate of growth. For example, in 1986 the membrane
market was $ 3,2 billion, in 1990 it was $ 6,1 billion and according to the
experts at the end of 90-s it should be about $10-11 billion [1,2, 3].
Production of membranes
and membrane equipment concentrated mainly in three regions: USA, Western
Europe and Japan, a share of which ones is about 97 % in all production and 75
% in purchase concerning membrane technology. Now in these regions about 100
corporations and plants occupy membrane industry, and only 60 of them produce
membranes and membrane units, others design equipment using membranes as
elements of commercial installations (systems) [4,5].
In 70 -s the ceramic membranes have
appeared in the membrane market of Europe, USA and Japan. The ceramic membranes
made usually on the base of oxides, nitrides and carbides of some metals were
for micro and ultrafiltration of different liquids
that are aggressive or require temperatures more than 100oC for
effective separation, when polymeric (organic) membranes fail or lose their
properties. Beyond their high thermal stability ceramic membranes have a series
of properties, which allow to select them into independent commercial and
technological activity named abroad as "ceramic membrane business".
Among such properties first of all it
should be noted:
- mechanical
stability;
- stability to
chemical and microbiological influence;
- stability of structural
pores and possibility of their control during membrane production;
- possibility of
using backflow through membranes;
- high flow rate
through membranes;
- long service life.
According to the above mentioned
advantages of ceramic membranes, their using as compared to polymeric membranes
allows to reduce maintenance costs (mainly due to their longer service life),
to reduce overall dimensions and weight of filtering installation, that also
lower capital outlays [6, 7].
Despite of dominate position of polymeric
membranes in sectors of West biotechnological industry, ceramic membranes start
gradually expand into this industry due to their lesser effect on protein
curdle on membrane surface, and also because they allow to sterilize them by steam
repeatedly. Ceramic membranes are widely applied in filtration of industrial
sewage, particularly in Germany, where the metalworking industry is highly
developed.
Sales of ceramic membranes in 1988 was $
32 million, in 1993 it was $ 40 million. In 1991 the experts forecasted rough
propagation of inorganic membranes sales in 90s. It was expected, that sales
should be about $ 450 million in 1999 [8, 9]. However, it has not taken place,
that was caused by high ceramic membrane price that was higher than polymeric
membrane price in 3-5 times (ceramic membrane prices were $ 1800 - $ 2500 for 1
sq. meter of membrane surface). The consequent estimations were more
conservative. They predict, that sales of inorganic membranes will be $ 228
million in 2003 at ceramic membranes share of 70 %. [10].
Nowadays in Russia there are small
productions (500 m2 per year) of ceramic membranes, competitive in
quality, for example, RPE"Ceramicfilter"
Co., Ltd. (Moscow, tubular ceramic membranes).
2.
Design and operating principles of the BIOCON membrane systems.
Base BIOCON filtering systems are two kinds of duplicate products:
filtering modules and filtering units, that differ, mainly, by scale parameters
(dimensions and weight).
As filtering material (filter element)
the polymeric membranes in the form of roll membrane elements (ERU-100-1016
type, JSC «Vladipor», Vladimir) or ceramic membranes
in the form of single-channel tubular ceramic elements (CMFE type, RPE"Ceramicfilter" Co., Ltd. Moscow) are
used. Pore size or retain ability of filtering materials is the following:
for ceramic
membranes: 0.05 microns, 0.2 microns,
0.8 microns,
for polymeric membranes: 500, 50000, 10000, 20000,
50000 Dalton.
Ceramic membranes CMFE-150/80 type (see Fig.1) are porous tubes of 800 mm length with inner diameter of 6 mm and
outer dia of 10 mm or multi-canal tubes made from
aluminum dioxide with a selective layer made from silicon carbide on their
inner side.
Polymeric membranes ERU - 100-1016 type (see Fig.2) are
roll membrane elements of 1016 mm length and with outer diameter of 100 mm with
membrane from polysulphonamide.
The filtration module (see Fig. 3)
consists of a cylindrical housing with the face flanges made from stainless
steel. Tubular ceramic or roll membrane filter elements are inserted into the
housing. The hermetic sealing of filtering elements in the module is made in
the face flanges by rubber rings.
There are nipples
and connecting pipes on the housing and face flanges of filtering module for
liquid feeding, for filtrate and concentrate removing.
The
filtration unit (see Fig. 4) consists of one or several filtration modules,
circulating pump (centrifugal type), feeding pump, heat exchanger, inlet and
outlet collectors, platform, valves, pressure gauges, flowmeters,
auxiliary tank (by necessity), connecting quick-detachable fixture, control
desk.
The filtration unit is constructed by
circulating loop principle for creation of cross flow mode of filtration
(tangential filtration).
Liquid for filtration moves in the apparatus
by feeding pump. Inside the apparatus the filtered liquid under circulating pump
is continuously pumped through the flow circuit formed by several filtrating
modules, heat exchanger and circulating pump, that are connected in series (for
ceramic membranes) or connected in parallel (for polymeric membranes).
Part of liquid and particles,
which size is less than pore size are passed through membrane
surface of ceramic elements under pressure of (0,5 - 3,5 bars) and continuously
removed from the apparatus. This part of liquid is named as permeate. Constant
supplying with new liquid for filtration fills up the deficiency of liquid in
the module.
The particles, which size is more than
pore size, are retained by selective layer and collected inside the flow
circuit. This part of flow is named as concentrate. Circulating flow, which rate
is 4-7 m/sec for ceramic membranes and 1-1.5 m/sec for polymeric membranes,
continuously washes off the deposit formed above a membrane.
Fig.4
The
BIOCON industrial systems are designed from several filtration units, control
valves and system of automatic control. The company BIOCON possesses
"know-how" on designing of large industrial systems in the context of
membrane type optimum choice and scales of filtering system for the given
product.
The company BIOCON produces wide spectrum
of filtering systems.
Filtration surface of the base units is:
- for
ceramic membranes: 0,5; 1,1; 4; 8; 10; 20 m2;
- for
roll membranes: 5, 10, 20, 40, 80, 100 m2.
To the present time the multistage installations
with the maximal area of a surface of a filtration 360 m2 - for
polymeric membranes and 320 m2 - for ceramic membranes are issued.
Stored knowledge of ceramic and roll
filter elements using shows that most effective at the following temperatures:
- for
ceramic membranes: 40-90 0 С;
- for
roll elements: 40-55 0 С,
service life for
ceramic membranes makes 3-5 years and for roll elements makes 0,5 - 1 year.
3.
Application of the BIOCON membrane systems.
3.1.
Pharmaceutical
and microbiological industries.
3.1.1. Riboflavin.
The culture broth of vitamin В12 (riboflavin) producer is subjected
to microfiltration on ceramic membranes with pore
size of 0.2 micron at temperatures more than 1100С for biomass
separation from vitamin В12 dissolved at this temperature. The rate
of filtration is 400 l/m2/h. The installation of 20 m2 filtration
surface is used.
3.1.2. Erythromycin. The culture broth of erythromycin producer is diluted twice with water and then subjected
to microfiltration on ceramic membranes with pore
size of 0.2 micron at the temperature of 400С. The rate of filtration is 60-80 l/m2/h. The antibiotic yield at
the stage of microfiltration is 17-21 % higher as
compared to using of filter-presses according to previous plant technique. The
duration of ceramic membranes washing and regeneration makes 30 min. Now the
installation of 112 m2 filtration surface is used (fig.5). Gross
rated capacity of the installation will be 320 m2.
3.1.3. Vitamin В2. The culture broth solution purified of biomass is concentrated in 40 times
by nanofiltration with using of roll elements
ERU-100-1016. The rate of filtration is 8-10 l/m2/h.
3.1.4. Lysine. To make crystalline lysine the culture broth of lysine producer is subjected to the process of preliminary clearing from
biomass by microfiltration on ceramic membranes with
pore size 0.2 micron at the temperature of 500С. The rate of
filtration is 120-160 l/m2/h. According to technology 75 % of
purified solution goes for crystalline lysine production and the biomass
concentrate (25 %) goes for production of feed lysine. Gross rated capacity of
the installation is 160м2.
3.1.5. Enzymes. Alcoholic (70 %) extract of
protein and enzymes is purified in installation with filtration surface of 1.1
м2 using ceramic membranes with pore size of 0.2 microns. The rate
of filtration is 130 l/m2/h (fig.6).
3.2.Diary industry.
Ultrafiltration (UF) is the most popular membrane process
at processing of dairy raw material. Whole milk, skim milk, previously
clabbered milk and also whey are subjected to UF.
Tasks of ultrafiltration are
the following:
а)
Preliminary concentration of milk proteins for production of traditional sorts
of cheese;
b)
Significant change of ratio between proteins and other ingredients for creation
of new cheese sorts;
c)
Normalization of milk on protein for maintenance of homogeneity and
reproducibility of cheese properties beyond any dependence on seasonality;
d) Separation of whey proteins to
receive protein concentrates and lactose solution.
3.2.1. Milk concentration.
Preliminary concentration of milk by UF increases fraction of total mass
of dry substances on average from 12,5 % up to 16 % and allows to double
productivity of subsequent stages. At concentration of whole milk in 2 times
the processing line includes only UF system and the basic operations of cheese
manufacturing are carried out by standard technology.
Further
concentration of milk up to concentration factor of 3-5 (up to 40 % of solids)
for receiving and processing of protein coagulum requires special equipment.
Using of ultrafiltrated milk
increases cheese yield. For example, in Fet cheese production the consumption of milk is reduced
from 8,5 down to 6,5 kg/kg of cheese. Besides, UF concentrating allows to
reduce consumption of milk coagulating enzyme (up to 60 %) and bacterial
ferment, to accelerate cheese ageing and manufacturing process, and also to automize production and control processes.
In
pilot experience the whole cow milk from milk plant was heated up to 600С
then cooled down to 500С. The average composition of milk is the
following:
n
Solids
....... ………… ………… 10,5 %
n
Protein ...............………….. 2,8 %
n
Fat
.......................... …………
3,1 %
n
Ash
........................…………. ..
0,6 %
n
Lactose
………….. ....... ……….… 4,0 %
In the
experiment the BIOCON pilot
membrane installation (Fig.7) was tested. It consists of the following:
n
Filtration module АRS-5 type with ultrafiltration
roll element of ERU-100-1016 type, filtration surface of 5 m2, polysulphonamide membrane, cut off of 50 kD.
n
Centrifugal circulating pump (flow rate 5 m3/h at pressure of 5 kg/сm2);
n
Feed
pump;
n
Circuital
tank (30 l)
n
Heat
exchanger.
In each experiment in the beginning
milk was concentrated up to the concentration factor (CF) of 3 or 5 times in
volume, then permeate was returned in the circuital capacity and the process of
ultrafiltration was carried out at constant CF during
5 hours. Temperature of the ultrafiltration process
was 42-550С. The results of the experiments are given in Table 3.1.
Cleaning and regeneration of membranes
was carried out up to primal water permeability of membrane element (210 - 240 l/m2
h) by standard procedure, routine for cow milk using solution of caustic soda
with sodium hypochlorite adding.
The concentrating milk experiments on
pilot installation were carried out within 3 months on the same roll element
with periodicity of 1 time per week. Thus the results obtained were similar to
the results given above.
For milk concentration in 2-5 times the
filtration installations with roll membrane elements of 50 kD cut off are
used.
Fig.8
The
installations have filtration surface of 240 m2, consist of two
stages (150 m2 and 90 m2), work in automode
and ensures productivity on initial milk 5000 l/h (fig.8).
3.2.2.
Whey and lactose concentration.
The experiments concerning
concentrating of cheesy whey and lactose solutions obtained in the previous
process of ultrafiltration, were carried out on the
pilot installation described above in item 3.2.1. For whey concentration the
roll membrane elements ERU - 100-1016 with cut off of 20 kD
were used, and for lactose concentration the roll membrane elements ERU -
100-1016 with cut off of 400-500 Dalton were used.
The calculation of ultrafiltration process for
production capacity of 100 tons whey per day based on the test data obtained is
given below.
3.2.2.1. Calculation of ultrafiltration
process at whey concentrating.
А) Membrane type: roll polymeric
membrane of ERU - 100-1016 type (cut off of
20 kD)
B) Source data: Whey volume per day -
100000 l;
Process
time: filtration - 20 h;
Regeneration - 4 h;
Operation cyclogram: 10 h + 2 h (washing)
Productivity: -
whey - 5000
l/h;
- permeate ( with allowance for
waters for diafiltration) -
5625 l/h;
- concentrate
- 125 l/h
Concentrate and filtrate yield –
continuous.
Concentration factor: 40 as compared to initial volume.
Temperature
of the process: 50-520С.
During a multistage ultrafiltration at the last 4-th stage is made diafiltration process for decrease of the contents lactose
and salts.
Liquid concentrate of whey proteins is a
result of ultrafiltration at CF=40. After that the
concentrate obtained is dried on a spray drier and the powder with the contents
of whey proteins 80 % is received. This process can be executed using the ultrafiltration installation UFS/5000WPC80 type
Fig.9
Permeate,
obtained after whey ultrafiltration is highly refined
lactose solution, which can be concentrated in 2-2.5 times using of roll
membranes for nanofiltration (retainability
of 400-500Dalton) to lactose content of 9-10 % and solids content of 10.6-11.0
%, the filtration rate at that is 7 -10 l/m2/h. After
that the concentrate obtained is dried on a spray drier and can be used in
food industry at production of drinks, ice cream or in pharmaceutical industry
for nutrient mediums.
3.2.3.
Milk Microfiltration.
Microfiltration of milk is rather new for milk membrane process, that as well as ultrafiltration, separates milk ingredients under pressure in flowing mode at
5 - 7 m/sec rates of liquid above membrane.
Application of ceramic membranes with
pores of 0.2 - 0.8 microns allows to delete bacteria from milk. At whole milk microfiltration most part of fat is deleted simultaneously,
at this membranes with pore size of 0.2 microns delete 99.9 % of fat particles,
and membranes with pore size of 0.8 microns delete 90-98 % of fat. Bacteria
content in milk filtered through membranes with pore size of 0.8 microns is
decreased in 200 times without noticeable retention of proteins.
Microfiltration
of nonfat milk goes at much higher rate as compared to the similar process for
whole milk. For example, at using of ceramic membranes CMFE-150/80 with pore
size of 0.8 microns microfiltration of whole milk (at
550С) goes at the rate of 500 - 700 l/м2/h, and for
nonfat milk it goes at the filtration rate of 2500 - 3500 l/m2/h,
99.6 % of bacteria are deleted from the skim milk.
The Microfiltration
of skim milk can be used for high-yield sterilization of milk, especially in
the cases of strong milk contamination.
The corporation "Alpha-Laval"
(Sweden) has developed the process of milk sterilization named "Bactocatch", at which nonfat milk is subjected to microfiltration using ceramic membranes with pore size of
0.8 – 1.4 microns, and the concentrate obtained in the process, that makes 5-10
% of total milk volume, is mixed with fat concentrate and heat treated at the
temperature of 1300С for 4 sec, then it is mixed with milk microfiltrate in the necessary proportion /11/. The given
technique allows to increase pasteurization
level of milk considerably and
decrease protein denaturizing as compared to standard thermal pasteurization.
The test data obtained by BIOCON at microfiltration of nonfat milk using ceramic membranes CMFE
with different nominal size of pores is given below. The experiments were
carried out on the pilot installation similar in consist to the installation
given in item 3.2.1, instead of modules with roll membranes, there were used
two modules with single tubular ceramic membrane CMFE-150/80 (filtration
surface of 0.015 m2).
The results of the experiments are
given in Table 3.3. The results given in
Table 3.3 show that ceramic membrane with pore size of 0.2 microns
deletes considerable quantity of the solids from nonfat milk, that is connected
with large retention of casein proteins (about 90-95%). The ceramic membrane
with pore size of 1.2 microns shows rather strong drop of filtration rate
during 2 hours of operation and, besides many bacteria can by-pass in the filtrate
at such pore size. With relation to filtration rate and bacteria retention the
optimum pore size of ceramic membrane for milk is 0.8 microns.
Note. There are given mean data of 2-3 repeated
experiments.
For removal of
microorganisms from skim milk the filtration installations with ceramic
membranes CMFE-150/80 (pore size of 0.8 microns) with filtration surface of 8 m2
are used, productivity of installation is 5000 l/h (see Fig.10).
3.3.
Food industry.
3.3.1.
Soybean milk (vegetable extract of soy). Soymilk base
Fig.10
The soybean
milk is produced by high-temperature extraction (900C) of soybeans
in water. The hot extract obtained is centrifuged using screw decanting vessel for
separation of brews (residual soy beans). The soybean milk contains valuable
high molecular substances: vegetative protein (2.2-3.7 %) and fats (1.1-2.5 %), and also undesirable low
molecular substances, the content of which is about 2.4 % (phytic
acid, trypsin inhibitor, lipoxidase).
The low molecular substances can be deleted by ultrafiltration
of soybean milk in combination with diafiltration.
Ultrafiltration
is rather new process for industry of soybean products. In contrast to traditional concentrating methods, for example, vacuum evaporation, the ultrafiltration allows to get various component
combinations in soybean products. During ultrafiltration
the high molecular substances are retained by membrane and concentrated, and
the low molecular substances move with permeate, thus solids content (TS) in
soybean milk rises from 7.5-8 % up to 12 - 22 %. Adding of water during ultrafiltration (so-called diafiltration
process) allows to reduce concentration of low molecular substances to required
level, for example, 1.1-1.2 %. The concentrate of soybean milk with protein
content of 57-60 % and fat of 30 -34 % obtained during ultrafiltration
can be used in production of cottage cheese, mayonnaise, cream, cheeses of
different fat content and other products.
The concentration of soybean milk was carried out using ceramic membranes
with pore size of 0.2 microns and 0.8 microns on a pilot installation described
in item 3.2.1.
Filtration surface
of ceramic membranes was 0.28 m2 in each module. Initial milk volume
was
60 l,
it was concentrated twice in the volume (CF=2) at the temperature of 700С,
then 30 l distilled water was added and then concentrated from 2.5 up to 4
times in different experiments. Soybean concentrates were produced with
concentration of the solids = 12.4 %
(CF=2.5), = 16.4 % (CF=3), = 20.2 %
(CF=4). Solids content in permeate was decreased down to 1.16-1.24 % by diafiltration.
Filtration rate for ceramic membranes with different pore size differed
and made as concentration advanced 69 – 27 l/m2/h (for pore size of
0.2 microns) and 99 – 41 l/m2/h
(for pore size of 0.8 microns) at the temperature of 60-80 0С and transmembrane pressure of 1.1 kgf/m2.
For installations
of 1000 l/h and 2000 l/h productivity the calculations of different technological
schemes for concentration/diafiltration of soybean
milk using ceramic membranes were made.
3.3.2. Drinks, extracts, syrups.
In microfiltration a filter supply stream (raw juice for
instance) is divided into a stream of filtrate (clear juice) and a stream of
concentrate. The concentrate stream contains all turbidity-forming solid
components such as proteins, pectin fragments, macromolecular tanning agents,
cellulose and others in a concentrated form. The clear juice which is available
as the filtrate stream (permeate) contains the typical components of a
clarified juice in their natural percentages.
The fruit
juice industry uses only the so called tubular membranes.
At
clarification of drinks, fruit
and berry extracts and syrups the ceramic tubular membranes with pore size of
0.2 microns are used. The
BIOCON installations have filtration surface of 2 m2, 4 m2,
20 m2 (fig.11).
Microfiltration
of fruit and berry extracts and syrups goes at the temperatures of 70 - 800С.
Depending on product the filtration rate is 60 - 100 l/m2/h. Microfiltration is used in production of viburnum, dogrose, cranberries, sea-buckthorn, haw and etc. syrups.
For purification of vegetative extracts
on maize base in production of red dyes the filtration installation with
filtration surface of 4 m2 and pore size of 0.2 microns is used. The
productivity of the installation on permeate is 700 - 800 l/h.
Fig.11
After microfiltration refined solution is subjected to
concentration in 3-8 times by nanofiltration using roll membranes
ERU-100-1016. The filtration surface of the installation is 80 m2.
Average productivity of nanofiltration installation
is 700 l/h (fig.12).
Fig.11
Clearing of
mineral water obtained from a slit goes using the installation with ceramic
membrane surface of 2 m2 with
productivity on permeate of 1800 l/h.
Research-and-Production Organization of
brewing, nonalcoholic and wine industries has made a conclusion that after microfiltration iron ions are deleted from mineral water
and chemical composition remains constant.
3.3.3. Wines.
There were tested
more than 20 different dry, fortified and table wines, and also
brandy drink (about 360) for microfiltration
of wine materials using ceramic membranes with pore size of 0.2 microns.
According to main laboratory data and estimations of wine-makers (joint-stock
company "Agrofirm"Abrau-Derso", "Crymsovhozvinprom" and other factories) quality of
filtration is very high, the organoleptic indexes
completely meet requirements for the grades. Sugar and alcohol content does not
vary, the removal of 99.99 % micro-organisms is ensured. For wine clearing the
installations with filtration surface of 4 m2, 10 m2 and
20 m2 are used. Mean filtration rate (8 hours of operation) for dry
wines is 150 - 250 l/m2/h, for fortified wine is 60-100 l /m2/h,
for brandy drink is 300 -500 l/m2/h.
3.3.4. Water treatment in beer production.
Purification efficiency of water from admixtures, microorganisms, iron and hardness salts
is of great importance in beer production. In small power production with water use of 5-6 m3 per day at
one shift operation the complex water-purification installation is used (fig. ).
It includes microfiltration block with ceramic
membranes (filtration surface of 5 m2) and blocks for water
softening. Using of microfiltration is necessary in
the cases, when artesian water has heightened content of microorganisms and
iron. Ceramic membrane regeneration goes due to filtrate backflows during
filtration process and periodic (1-2 times per week) washing by alkaline
solution with sodium hypochlorite adding.
The block of softening ensures soft water
volume between regeneration cycles of 5.25 m3 at total hardness of 8
mg-equivalent. The regeneration of the block for water softening is carried out
by 10 % solution of common salt in automode.
3.4.
Fuel and energy industries.
3.4.1. Regeneration of waste transformer oil.
Utilization of waste
transformer oil is a major
problem for energy industry.
Using microfiltration
process on ceramic membranes it is possible to refine waste transformer oil from suspended particles and water and to bring up parameters of transformer
oil purity to the required
norms concerning specific resistance.
The installation for regeneration of transformer oil includes the microfiltration block with
ceramic membranes (filtration surface of 4 m2) and block of
dehydration (fig.13).Water elimination from transformer oil goes under expansion pressure in
permeates outlet zone above developed outer surface of tubular ceramic filters.
The installation allows to increase purity of reclaimed transformer oil from
14 to 7-th class, to reduce humidity
content from 3000 g/t to 20 g/t and
increase essentially electrical resistance of oil from 0 up to 24.5 kW/cm.
Productivity of the installation for purification of transformer oil is 1200
l/h.
4.
Conclusion.
A wide spectrum of domestic filtration
installations using roll organic and tubular ceramic membrane filter elements
was produced as a result of long-term developments of micro- and ultrafiltration equipment in cross flow mode. The
examinations of these installations in new areas of application are carried
out. The membrane systems developed find wide spread application in
pharmaceutical, food and diary, fuel, energy and other industries.
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