NZ622298B2 - Process and apparatus for the separation of the components of a liquid mixture - Google Patents
Process and apparatus for the separation of the components of a liquid mixture Download PDFInfo
- Publication number
- NZ622298B2 NZ622298B2 NZ622298A NZ62229812A NZ622298B2 NZ 622298 B2 NZ622298 B2 NZ 622298B2 NZ 622298 A NZ622298 A NZ 622298A NZ 62229812 A NZ62229812 A NZ 62229812A NZ 622298 B2 NZ622298 B2 NZ 622298B2
- Authority
- NZ
- New Zealand
- Prior art keywords
- liquid
- ofthe
- bubbles
- tank
- water
- Prior art date
Links
- 239000007788 liquid Substances 0.000 title claims abstract description 126
- 238000000926 separation method Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000000203 mixture Substances 0.000 title claims description 10
- 238000009835 boiling Methods 0.000 claims abstract description 31
- 239000007791 liquid phase Substances 0.000 claims abstract description 13
- 239000012159 carrier gas Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 52
- 238000004821 distillation Methods 0.000 abstract description 7
- 238000005194 fractionation Methods 0.000 description 10
- 239000007789 gas Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 9
- 239000012467 final product Substances 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- 238000012856 packing Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- XLYOFNOQVPJJNP-ZSJDYOACSA-N Heavy water Chemical compound [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 230000000630 rising effect Effects 0.000 description 4
- 238000004508 fractional distillation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 238000003892 spreading Methods 0.000 description 3
- 239000012808 vapor phase Substances 0.000 description 3
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 229910052805 deuterium Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011067 equilibration Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000005501 phase interface Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229910000906 Bronze Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical class CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000010974 bronze Substances 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000003921 oil Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/0064—Feeding of liquid into an evaporator
- B01D1/007—Feeding of liquid into an evaporator the liquid feed being split up in at least two streams before entering the evaporator
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/14—Evaporating with heated gases or vapours or liquids in contact with the liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/0005—Degasification of liquids with one or more auxiliary substances
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/008—Liquid distribution
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
- B01D5/006—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with evaporation or distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D59/00—Separation of different isotopes of the same chemical element
- B01D59/02—Separation by phase transition
- B01D59/04—Separation by phase transition by distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D59/00—Separation of different isotopes of the same chemical element
- B01D59/22—Separation by extracting
Abstract
Disclosed is a process and an apparatus for the separation of liquid components having different boiling points (distillation). From a liquid outlet tap (3), liquid is taken from the liquid tank (1) to a liquid pump (12) which feeds the water to a bubble generator (13) that is feed with a carrier gas (15). The liquid taken from the out let (3) is reintroduced into the liquid tank (1) via a liquid inlet (2) with bubbles that have a diameter of 5-200 µm to increase the liquid-vapour interface area and allow rapid concentration of the more volatile component in the air space of the bubble thereby separating the components within the liquid phase itself. After said bubbles leave the liquid phase (7), the released vapour content of the bubbles are condensed (9) and collected (11) and the obtained liquid enriched in the more volatile component(s) is separated from the carrier gas (29). s (15). The liquid taken from the out let (3) is reintroduced into the liquid tank (1) via a liquid inlet (2) with bubbles that have a diameter of 5-200 µm to increase the liquid-vapour interface area and allow rapid concentration of the more volatile component in the air space of the bubble thereby separating the components within the liquid phase itself. After said bubbles leave the liquid phase (7), the released vapour content of the bubbles are condensed (9) and collected (11) and the obtained liquid enriched in the more volatile component(s) is separated from the carrier gas (29).
Description
Process and Apparatus for the Separation of the Components ofa Liquid Mixture
The invention relates to an apparatus and process for separation and concentration ofliquids with
different boiling point.
Prior art
Fractional distillation has been used in the industry for decades to separate substances ofdifferent
boiling point. Separation ofalcohol from water, or obtaining mineral oil products of boiling points are well-
known examples. In both‘ the difference in the boiling points ofthe components to be separated is large, up to
several tens rces centigrade (°C), so separation by fractional lation is vely easy and economical
— what shows that alcohol, and oil derivatives, produced this way are ctured and used in the order of
million tons per year. Major challenge is separation of substances with slightly different [0.5 — 2°C difference)
boiling point and have, hence, low fractionation constant. Such materials can be separated only in s of
very high (theoretical or physical) plate number at considerable energy expenditure. Separation of compound
containing stable isotopes is such a difficult task. The present invention is primarily an apparatus for separation
and concentration of water molecules containing the stable es ofhydrogen (H20, H00, D30) and a
s to operate the said apparatus.
The technology of manufacturing deuterium-depleted water (DDW) exists, and is based on classical
onal distillation, making use ofthe boiling point ence of H20 and HDO (05°C) and H20 and 020
(15°C). Separation essentially means that, in equilibrium state. the product of lower boiling point (here: HZO)
will be minimally (at 100°C. to [2%) concentrated in the vapor phase. The fractional distillation columns used
today are built to e for stable water-vapor equilibrium on physical or theoretical “plates” where vapor,
rising from plate to plate, gradually loses the components with higher boiling point (in this case: HDO, D20),
and DDW can be obtained at the top ofthe column by condensing the vapor, The higher is the plate number for
separating normal and heavy water, the lower will be the ium level in the product.
The cliicicncy ofseparation is determined by several parameters. Decisive factors are the amount of
vapor flowing in the column, the area providing for water-vapor equilibrium. and the fractionation
(concentration) nt (the lower separation temperature s in, higher onal constant). Fractionation
constant defines to what percent the more volatile component is more concentrated in the vapor than in the liquid
phase at a given temperature For H20 and H00. the fractionation constants are given in the table below from 0
to 100 °C, in 5°C steps.
Temperature (”C) Fractionation Change (ppm)
constant (%)
0 10.2 | 5.6
H‘ "i
9.5 14.25
8.9 13.35
RT '— 8.3 12.45
7.8 I 1.7
7.3 10.95
6.8 Tfi
Generation of DDW is, ofcourse, tional to the amount of vapor flowing h the column
(while D concentration rises in the water at the ). it is a case ofpoint, that although the fractionation
constant is higher at lower temperatures, the corresponding partial vapor pressures are much lower, so at low
temperatures the amount of water carried in the vapor is low which will limit productivity. Furthermore, it
should be noted that the minimal difference in boiling points requires that only [/1 5 to l/l 8 part ofthe product is
led offto upkeep the equilibrium in the column. So, practically. by using one ton of vapor per hour only 5565
liters of DDW can be manufactured.
The efficiency ration highly depends on the size ofthe water-vapor contact area, to obtain the
water—vapor brium at the given temperature as fast as possible. Several methods have been developed in the
past decades to increase the contact area. A known classical solution uses bubble caps. In this case, every plate in
the column is covered by a water layer ofa few centimeters, where the steam rising from the lower plate is
forced to bubble through by the use of bubble cup. In this process, vapor is present in the water phase only for
l time, and the contact area is determined largely by the column diameter and the area of the water layer
on the plates. in a l m diameter column. this area is 0.785 ml. Another way to increase the contact area is to fill
the column with a porous material which gives large area in small volume. lfthe area is sufficiently wettable by
water, there will be increased equilibration n the rising vapor and the water layer on the solid surface over
a unity oflength and the efficiency ofseparation will approximate the theoretical maximum. A generally used
form ofcolumn packing is Raschig rings, the porous ceramic surface of which provides the area for separation of
substances with different boiling points. Better separation per volume unit can be achieved using a so-called
ordered packing. in which maximum surface per volume unit is given by a precisely bent meshwork made of fine
metal wires. In case of manufacturing DDW or heavy water. an extra cost is ed because ess steel is
not well wetted by water so the packing must have a phosphorous bronze finish.
In all these procedures. separation happens essentially at the contact surface ofthe liquid and vapor, and
some solid “scaffold“ is used to create the liquid surface. in case of bubble caps, the trays themselves give the
solid part, in packed columns, it is the c filling, ordered g or some other solid substance. The
ng methods of manufacturing DDW haVe the following disadvantages: l. One distillation column has low
capacity, even at high energy input; 2. ing the column at l00 °C, fractionation constant is low,
necessitating high plate number for attaining the theoretical maximum D level decrease. ing in elevated
investment costs; 3. Higher fractionation constant can be ed by distilling in vacuum at a lower
temperature, but the control system is then more complicated, and ty is decreased because less water
investment costs,
present in the vapor phase at lower temperature; 4. Distillation columns ent high
increased further by the auxiliary equipment (high-throughput boilers, tall building for the columns, large
cooling capacity).
Summary of the Invention
The primary object ofthe invention is an apparatus, able to separate components of different boiling
points more efficiently than the methods available at present.
This ion is based on the recognition that by generating bubbles in the liquid to be separated to
components, the liquid-vapor phase interface area can be largely increased. This area will be sufficient to allow
rapid concentration of the more volatile component in the air space ofthe bubbles, and the liquid-vapor
equilibrium at the given temperature will be reached relatively y. in contrast to the ng procedures
(using trays. Raschig rings or an ordered packing) the invention s to create the surface. where the
ents ofdifferent boiling points separate according to their Fractionation constant, within the liquid phase
itself. When the bubbles burst on reaching the surface ofthe liquid, their gas content, together with the vapor
enriched in the more volatile component, goes to the space above the liquid.
Further, as smaller (micro) bubbles stay longer in the liquid phase, sufficient time is given for the
liquid~vapor equilibrium to settle.
So the invention relates primarily to such a process for separation of components ofa liquid with
different boiling points, in which bubbles are generated in the liquid phase by a carrier gas, where the more
le component(s) of the liquid is/are trated; and as the bubbles enriched in the more le
component(s) leave the liquid phase, the vapor released is collected and condensed, and the resulting liquid —
being rich in the volatile component(s) — is separated form the r gas.
Further, of advantage is a s according to the above, where the diameter ofthe bubbles is 5-5000
tun.
Further, of advantage is a process according to the above, where at least 70% ofthe bubbles has 5-200
um diameter.
Further, ofadvantage is a s according to the above, where 70% ofthe bubbles is till in the liquid
phase after 5 minutes.
Further, ntage is a process according to the above, wltere at least 70% ofthe bubbles has 500-
5000 um diameter, or even more advantageously 750-3000 pm diameter.
Further, of age is a process according to the above, where the carrier gas used to generate bubbles
is a mixture ofone or more gases of low boiling point: practically air.
Further, ofadvantage is a process according to the above, where the liquids ofdifferent boiling points to
be separated are H30, H00 and D20 (a blend ofthese, as it is found in natural waters) and the concentration step
ofthe process is performed at 5—100 C’C, preferably at 40—70 E’C.
Further, ofadvantage is a process according to the above, where the release of gas mixture from the
bubbles is promoted by spreading the liquid on a solid surface.
r object ofthe invention is an apparatus set up for implementation ofthe process. So the
inventiOn also relates to an apparatus for separation of components ofa liquid with different boiling points, said
apparatus comprising:
at least one liquid tank (1) with at least one liquid inlet (2), at last one liquid outlet (3), and at least one
gaseous medium outlet (4);
at least one feed line (6) connecting the liquid tank (1) via the liquid inlet (2) with a liquid source (5);
a condenser unit (9) in hrough contact with the inner space (7) ofthe liquid tank (1) via the
gaseous medium outlet (4) and a ting pipe (8);
a collector tank (1 ected to the outlet (10) ofthe condenser unit (9) via pipe (30);
characterized in that:
in the feed line (6) between liquid source (5) and liquid inlet (2), a liquid pump (l2) and a bubble
generator (13) connected to the outlet ofthe former are included;
the gaseous medium inlet (l4) ofthe bubble generator (13) is connected to the outlet (16) ofthe gaseous
medium compressor (15);
the liquid outlet (3) ofthe liquid tank (1) is connected to the inlet ofthe liquid pump (12) via the return
line (i7) and a unifier-distributor unit (18) which is connected also to the liquid source (5);
the outlet (31) ofthe collector tank (I 1) connected to the outlet (l0) ofthe condenser unit (9) is
connected, via another distributor unit (32) to the inlet ofthe final product collector tank (29) but also to
an additional liquid inlet (i9) ofliquid tank (1); and
the air space (33) ofthe collector (l l) is connected to the vacuum pump (27).
Ofadvantage is an apparatus according to the above, where the bubble generator (13) works with
ceramic tubcs penctrable for gaseous medium;
Further, of advantage is an apparatus according to the above, where (Figure 2 and 3) the outlet (20) of
the bubble tor (13) is connected to one liquid inlet (2) in the lower part (expediently in the lower third) of
the liquid tank (1) and to another liquid inlet (22) in the upper part (expediently in the upper third) ofthe liquid
tank (l). via the distributor unit (2|). Element (21) can be a directional control valve.
Further, ofadvantage is an apparatus according to the above, where the bubble generator (I 3) is one
generating bubbles of 5-5000 um. it is expedient lithe bubble generator (13) is generating a total bubble volume
ofa few cm‘i/min to a few mJ/min.
it is of advantage ifthe condenser (9) ses a tubular heat exchanger (23).
It is of advantage if unifier-distributor unit (18) is a directional l valve or a manifold valve, and
can be remote controlled.
it is if advantage ofthe liquid tank (1) is standing, cylindrical and closed.
er, ofaclvantage is an apparatus according to the above, where the inner space (7) of the liquid
tank (I ) contains a e-enlarging element (24). It is expedient ifthis element has a grid structure.
Further, of advantage is an apparatus according to the above, where a heat-transfer unit (25) is attached
to the tank(|). [t is ent ifunit (25) is placed inside (7) ofthe liquid tank, near to its bottom, or, more
practically, in contact with that. Heat transfer unit (25) can be a'tubular heat exchanger or an electric heater.
Further‘ of advantage is an apparatus aceording to the above, where the liquid tank (I) has an overflow
outlet.(26). It is expedient if at least one ofthe upper or lower sections ofthe tank (1) is jacket-walled in which a
fluid ofdifferent temperatures can circulate.
Further, ofadvantage is an apparatus according to the above (Figure 3) which contains l liquid
tanks (l)connected in series in such a way that the gaseous medium outlet (4) ofa previous tank (1) ed in
the upper part ofit is connected to the inlet (28) ofthe compressor ( l 5) beionging to the subsequent tank (I), and
the gaseous medium outlet (4) ofthe last liquid tank (I) in the series is connected to the inlet (34) ofthe
condenser unit (9), and the overflow outlet (26) ofa liquid tank (I) being forward to another one in the series is
connected to the additional liquid inlet (19) ofthe previous tank via the connecting line (35).
The apparatus containing several liquid tanks (I) can be constructed so that the liquid outlet (3) ofa
given liquid tank (I) is connected to the inlet ofthe liquid pump (l2) ofone ofthe previous tanks (1).
Carrier gas is fed in the system at the inlet (36) ofthe compressor.
As described above. the apparatuses can be connected in series to se separation. in such a ,
it is ent to connect in series one after r, and the vapor from one tank air space (7), enriched in the
component oflower boiling point, is used to generate bubbles in the next tank. By increasing the number of
bubble generators in the system the separation ofcomponents with ent volatility can be increased to any
level.
ed ption of the ion
The liquid mixture can be any kind containing ents ofdifferent boiling point, Obviously, the
process is most advantageous in case ofmixtures where there is little difference (eg. 0.5-3°C) between the
boiling points ofthe ents; but it can be also applied, of , when the boiling point difference is
higher (eg. 3-30°C). The invented process is highly suitable for manufacturing deuterium~dcpleted water, DDW
(that is for separation of H20, HBO and 020 which have nearly the same boiling point). in the examples and the
advantageous implementation forms. DDW production is described. but the basic idea ofthe invention —
sing the liquid-vapor interfacial area by generating bubbles ~ can clearly be adapted by a skilled person for
other mixes (eg. water-alcohol mixtures, mixed organic solvents).
According to the invented technical solution, the diameter ofthe bubbles can vary widely (is practically
between 5 and 5000 pm). Decreasing the size ofthe bubbles will increase the the time to stay in the liquid.
Microbubbles (of 5-200 um diameter) can be also used. Ofthese, 70% remains in the liquid even afier 5 minutes.
Although with ubbles the equilibrium to be reached is more close to the theoreticai liquid-vapor
equilibrium at the given temperature, an additional task is to make microbubbles leave the liquid phase and
rge their contents in the space above the liquid. This can be promoted by spreading the liquid partially or
fully saturated with microbubbles, that is, by letting it flow over a large surface to promote make the bubbles
merge and/or burst.
Microbubbles are produced in a so-called microbubble generator. Several companies manufacture and
sell such devices, so the most appropriate device can be picked from a broad choice. Depending on type‘ bubbles
ot'ca. 5-200 um diameter can be produced by microbubble generators.
in r advantageous embodiment, bigger bubbles are generated. In this case the content ofthe
bubbles are transferred easier in the air space. e.g. by letting the liquid flow along a surface. in case of such
bigger bubbles (ca. 500—5000 pm. or even more preferably 750—3000 um diameter) it is advantageous to
ulate the bubble-containing liquid into the tank several times, to ensure sufficiently long contact time of
liquid and vapour (preferably 7O % ofthe bubbles falls into this range). The advantageous constructions shown
in the figures are ofthis kind.
Hereafter, “bubbles” mean both ubbles and bigger bubbles, and any mixture e (unless the
sizes are specified).
To generate bubbles, a led carrier gas is required. The boiling point ofthe carrier gas should be
much lower than that ofthe components to be separated, it is advantageous ifthe gas at the temperature of use is
above its critical temperature. This way the gas will not liquefy in the condenser which can be advantageously a
heat exchange or it can work on the basis ensation achieved by pressure increase.
At separating substances of different boiling point, one ofthe ve factors is the sufficiently large
area where the components can separate according to their boiling point. The invention also relates to an
apparatus which provides the sufficient separation area by means of bubbles.
In an advantageous embodiment, temperature gradient is created in the liquid tank (practically a
cylindric tank) so that the top ofthe water column is warmer than the bottom. This way. the rising bubbles will
expand ng layers ofever higher temperatures, increasing the lilting force acting on the bubble and driving
these to the water surface where their contents are discharged in the space being over the water.
In actual implementation ofthe invention, it has to be determined experimentally for a given material to
be separated bubbles of what size will ~ depending on the y, viscosity. boiling point etc. ofthe liquid and
other physicochemical parameters (such as external pressure) — remain stably in the liquid, and at which size and
temperature will change the floating behaviour ofthe bubbles and they rise to the surface on the effect oflifting
force. In operating the apparatus, the size of bubbles and the temperature gradient ofthe column have to be set
ingly.
An another advantageous implementation, surfacing ofthe bubbles can be promoted also by creating
ions, at a given distance from the top in the water column, which accelerate the coalescence of bubbles and
ubbles, and the size increase will force the resulted big bubbles to the surface.
Further, the annihilation ofthe bubbles at the surface and the transfer oftheir content to the air space
being over the water can be ed ifa porous material or some other material, the collision with which
induces bubble annihilation, touches the water surface.
Further, ing the bubbles can also be promoted by leading the liquid leaving the bubble generator,
or a fraction of it, to the top ofthe tank and letting it flow down the tank wall or an extra large-surface element,
e.g. a sieve-like matter, Flowing down, the s reach the surface with high probability. burst, and the
ents carried in them are emptied in the air space. Surface-enlarging ts other than sieves (porous
ceramics, wire mesh packing, etc.) can be also applied; and these elements can be used in several layers or
se. with the liquid flowing from one to r.
To increase enrichment ofthe more volatile component, implementation is possible also in such a way
in which the gaseous medium above the liquid (practically steam-containing air, hereafter: steam) and within it
the components in the gas phase (present in steam form at the applied temperature and pressure) is pumped in the
bubble generator ofa subsequent tank unit (cg. is led through the bubble‘generating ceramic or other elements).
This will achieve further concentration ofthe component with lower boiling point. it is expedient to connect so
many apparatuses according to the invention in series with which the required enrichment can be reached.
In a further advantageous implementation ofthe invention, the continuous separation and the
continuous operation ofthe plant are d by moving the liquid and the steam used in the bubble generators in
rcurrent. Steam taken from one unit is led to the next unit via the bubble generator, and the liquid
condensed at the end ofthe system is returned to the last unit. This will raise the liquid level there and will flow
back to the previous unit. practically in a gravitational overflow. Final product is taken away from the
condensate at the end ofthe system, where the proportion oftakeoffis d to the extent of separation and
productivity. In case of water, l/12to 1/15 ofthe condensate can be taken offas final product.
By the forward flow of steam and backward flow ofliquid, the ratio ofcomponents with different
g points slowly changes in the whole system. the mount ofthe more volatile component increases from
unit to unit. So that the less le component is not ed, fresh liquid has to be fed into the first column.
As described here above. the large water-steam interface area (or any liquid-steam interface area) for
separation ofthe components having different boiling points is achieved not by means ofa solid structure (as in
the decades-old process used by now) but by bubbles t within the liquid. This idea may enable the
production of any amount of DDW required by the pharmaceutical industry (possibly several n liters a
day) by relatively cheap equipment and without high energy consumption. Separation ofany other liquid
material my also be done more economically. Another major advantage ofthe apparatus and process is that it can
be deployed anywhere with little preparatory work and additional investment.
The surface-related parameters ofthe apparatus according to the invention are exemplified with the
calculations below:
A bubble~cap column for fractional distillation, as used today, provides the following area per plate for
equilibration of water and steam, ing on column diameter:
Column diameter0.6 m l.0 m 1.5 m
Plate area 0.27 m2 0.78 m2 1.76 m2
In contrast, by introducing merely 10 cmJ of air per minute in the system, e.g. through the -
generating ceramic elements. the water-steam phase interface area is, depending on bubble size:
Bubble diameter 5 pm 10 um 50 pm 100 um
steam contact area [.17 m2 0.58 m2 0.1] m2 0.04 m2
During operation, the amount ofair introduced in the liquid phase and that ofthe bubbles leaving the
water should be in equilibrium. lfthe flow of lo cm3 per minute can be maintained, the bubble area generated in
the water per hour is, ing on bubble diameter, as follows:
Bubble diameter 5 um 10 um 50 pm 100 um
Area generated per work hour 70.2 m2 34.8 m2 6.6 m2 2.4 m2
The ageous properties ofthe apparatus created according to the invention. and the process, are as
follows:
- Separation is done at a ion/er temperature. saving considerable energy;
- At lower temperature, fractionation constant is higher than with boiling at l00°C, so the required
ment is reached in fewer steps;
- The apparatus can built more simply and cheaply than the traditional distillation towers of l0-3O m
height;
— The supplementary equipment (gas~fired boiler, cooling capacity, structural elements ofa distillation
tower, etc.) are not needed, or their size and costs are much smaIIer than for the distillation equipment known
today;
- N0 Several s high structure is needed, the units ofthe apparatus can be placed next to each other
in one hall;
- The number ofunit5, and so the grade chment, can be varied any time as required by the
production process.
Explanation of the figures
Figure I shows a stand-alone (one unit) apparatus.
In Figure 2, the system already includes an area-enlarging element, to which a fraction ofwater leaving
the bubble generator is directly led. In the variation shown, a part ofthe bubble-enriched liquid flows to the top
of the tank, and there, to the area-enlarging element.
Figure 3 shows a system formed by connecting two ofthe units shown in Figure 2. It should be noted
also here that, in theory, any number ofthe base units (one liquid tank 1 with its fixtures) can be connected in the
above way.
Legend to the Figures:
l liquid tank
2 liquid inlet
3 liquid outlet
4 gaseous medium outlet
liquid source
6 feed line
7 inner space of the liquid tank
8 connecting pipe
9 condenser unit
l0 outlet of condenser unit
I l collector tank
12 liquid pump
13 bubble generator
14 s medium inlet
l5 compressor
l6 compressor outlet
l7 return line
l8 unifier—distributor unit
l9 additional liquid inlet
bubble generator outlet
2] distributor unit
22 liquid inlet ed in the upper part ofthe tank
23 r heat exchanger
24 surface-enlarging unit
heat er unit
26 overflow outlet
27 vacuum pump
28 compressor inlet
29 final product collector tank
pipe
31 collector tank outlet
32 unifier-distributor unit
33 tor tank air space
34 condenser inlet
connecting line
36 ssor inlet
The invention is interpreted, without limiting the scope of patent protection, by the following examples:
Example I
A tank of 15 L volume and 25 cm diameter is filled with 10 L water. The liquid tank (I) can be heated
from below by the heat transfer unit (25) so water temperature can be set to any value. At the top ofthe tank (I)
are connected the thermometer (but is not shown on the Figure because it is obvious) and the condenser unit (9)
(a r heat exchanger). Liquid inlet (2) and outlet (3) are built in the side ofthe tank (l).
The liquid inlet (2) connects the liquid tank (I) to the liquid pump (12) which delivers water, drawn
from the liquid tank (1) via the liquid outlet (3), through the bubble generator (13) and the liquid inlet (2) back to
the liquid tank. A compressor (15) is connected to the bubble generator (13) and feeds it continuously with air.
The required water amount is fed into the system from the liquid source (5) by the unifier-distributor unit (18).
The liquid condensing at the bottom ofthe water-cooled ser unit (9) goes to the tor tank (1 l) which
is connected to a vacuum pump (27) providing for under pressure in the system and so for sufficient steam flow.
A fraction ofthe water from the collector tank (1 l) is divided by the unifier-distributor unit (32), one line
delivering the final product to the final product collector tank (29), and the other leading the remaining liquid
back to the system via the additional liquid inlet (19).
This setup is shown in Figure 1.
1n the first production test, water temperature was kept at 60°C and the microbubble generator was fed
with 20 ch/min air. The generator produced bubbles oi‘SO-lOO pm diameter and the pump moved 5-8L/min
water through the generator. The D content ofthe condensate was 6.7 ppm lower than that ofthe feed water, in
good agreement with the calculated theoretical value.
Example 2
Using the above prototype but running it at 80°C, the decrease ofD content in the produced water was
only 4.6 ppm. This showed that tion s with increasing temperature, proving the correctness ofthe
theoretical background ofthe invention.
Example 3
An apparatus set up from the elements in example 1. but ed as follows:
The liquid tank is l m high, 25 cm in diameter and contains 15 L water. The pipe leaving the bubble
generator (13) is bifurcated in the distributor unit (2|). One line delivers (as in e (1) bubble-saturated
water to the bottom ofthe liquid tank (l) through liquid pump (12) and liquid inlet (2). The other line goes to the
liquid inlet (22) arranged in the upper part ofthe liquid tank ( l ), and the -saturated water flows down
spreading on the wall ofthe tank, or down an extra surface-enlarging unit (24), expediently a sieve~like surface,
to the bottom ofthe tank. The distributor unit (21) before the bifurcation regulates in what proportion the bubble-
ted water delivered by the liquid pump (12) goes to the two branches. This construction ensures that the
bubbles leave the water flowing on the wall ofthe liquid tank (1) and so the amount of evaporated water is
greatly increased.
Example 4
The same setup as in example 3 but with 0 um diameter bubbles.
Example 5
The same apparatus as in example 3, but the bubble size varies between 500 and 5000 pm (mean: 500~
800 um). During operation. the distributor unit (21) after the bubble generator (13) directs 20% ofthe liquid flow
in the bottom ofthe tank and 80% to its top. At larger bubble size (750-3000 pm) more water (40-75%) is led to
the tank bottom; while at 5000 um bubble diameter 80% goes to the bottom and 20% to the top of the tank.
Example 6
Five liquid tanks (l) onO cm diameter and 50 cm , containing water 40 cm high. A ceramic
bubble generator ( l3) connects to the bottom ofthe first cylinder through the liquid inlet (2) and brings 10
ch/min air in the water fed in by the liquid pump (12) in form of to pm bubbles. The cylindric liquid tank (1)
has a IO cm widejacket between 30 and 40 cm height in which water of60 °C temperature is flowing. The
lowest 10 cm section ofthe tank has an identicaljacket with 20°C water. Air and evaporated water from the
inner space (7) of the first liquid tank is fed via a second ceramic bubble generator (13) in the next liquid tank (1)
which is identical to the first one; and this ce is repeated for three more times. Steam from the r inner
space (7) ofthe last liquid tank (I) is condensed in a condenser unit (9) and led to the collector tank (1 1). A part
of the water taken from the collector tank is bifurcated [by the unifier-distributor unit (32)]. The final product
going to the final product collector tank (29). and the remaining water being returned to the system via the
additional liquid inlet (19).
[n the bed process, the al moves from the first liquid tank (I) to the last one through the
bubble tor (13). Constant water level in the liquid tanks (1) is secured by placing every tank 0.5-! cm
higher than the previous one, and connecting it via the w outlet (26), placed at 40 cm height, and a pipe to
the bottom of the previous liquid tank (l). This way, the liquid returning to the last liquid tank (I) after
condensation flows via the overflow outlet (26) to the previous tank (I) where the liquid will also surpass 40 cm
height level and will flow on to the preceding tank.
Five units described in example 3 are connected so that the air is taken from the inner space (7) of one
tank (l) and is fed to the microbubble generator (l3) ofthe next tank.
An apparatus with identical structure to that in example 1, but with a cylindrical liquid tank (1) is of l m
height and 50 cm diameter. Air input is 100 cm3 per minute.
The above examples demonstrate that ation of bubbles in separation technology —— more exactly
the idea that separation ofcomponents with different boiling points is possible in the bubbles, without the need
of any solid surface — opens up unlimited possibilities in the area. The size ofthe apparatus and the bubbles, the
amount ofair or other gas fed in, the number ofcylinders in series, the temperature distribution. etc. can be
varied at will or be optimized to the actual separation task.
Comprises/comprising and grammatical variations f when used in this specification are to
be taken to specify the presence of stated features, integers, steps or components or groups
thereof, but do not preclude the presence or addition of one or more other features, integers,
steps, components or groups thereof.
Claims (1)
1. Process for separation of components of a liquid mixture with different boiling , wherein bubbles are generated in the liquid mixture by a carrier gas, the bubbles become ed in one or more volatile components, and when the s leave the liquid phase the vapor released from them is ted and sed to separate the volatile component(s) obtained from the applied carrier gas, wherein at least 70% of the bubbles have a diameter of 5-
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| HU1100435A HUP1100435A2 (en) | 2011-08-12 | 2011-08-12 | Apparatus and method for distillation of liquids with different boiling point |
| HUP1100435 | 2011-08-12 | ||
| PCT/HU2012/000069 WO2013024310A1 (en) | 2011-08-12 | 2012-08-13 | Process and apparatus for the separation of the components of a liquid mixture |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| NZ622298A NZ622298A (en) | 2015-04-24 |
| NZ622298B2 true NZ622298B2 (en) | 2015-07-28 |
Family
ID=
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US9675903B2 (en) | Process and apparatus for the separation of the components of a liquid mixture | |
| US6254734B1 (en) | Barometric evaporation process and evaporator | |
| CN104338417B (en) | Carbon dioxide separating and capturing system and method of operating same | |
| CA2716624C (en) | Method and apparatus for dewatering a mixture of ethanol and water | |
| JP5923367B2 (en) | Heat exchange type distillation equipment | |
| CN103237580B (en) | Low energy Distallation systm and method | |
| JP2012518667A (en) | Post-treatment by distillation of methanol / water-mixture and production of alkali metal methylate | |
| WO2014009762A1 (en) | Rectification tower with internal heat and mass exchange and method for separation of multi-component mixtures into fractions using a rectification tower with an internal heat and mass exchange | |
| US20140007576A1 (en) | Method and device for energy conversion | |
| CN103432761A (en) | Distillation equipment and method for separating dichlorobenzene isomers | |
| US10350510B2 (en) | Mass transfer column of cross flow of liquid and gas (vapour) phases | |
| CN106730968A (en) | A kind of integrated air rectification and purification device | |
| NZ622298B2 (en) | Process and apparatus for the separation of the components of a liquid mixture | |
| CN205833144U (en) | A kind of pilot scale rectifier unit | |
| RU2393904C1 (en) | Rectification plant | |
| WO2013089584A2 (en) | Method and device for producing a krypton/xenon mixture | |
| HUP2400258A1 (en) | Apparatus without packing and process for separating and enriching liquids with different boiling points | |
| JP6312614B2 (en) | Hydrous ethanol distillation apparatus and method for producing absolute ethanol | |
| CN208287528U (en) | A kind of rectifying tower of double ports and built-in demister, many places redistributor | |
| CN202460158U (en) | Distillation cooling device | |
| JP2903096B2 (en) | Method and apparatus for separating azeotropic mixed solution | |
| CN206549204U (en) | A kind of integrated air rectification and purification device | |
| JP2000140501A (en) | Distillation apparatus and distillation method thereof | |
| CN108355367A (en) | Naphthalene vaporising device in phthalic anhydride preparation process | |
| CN103611327B (en) | Controlling temp type knockout tower and separation method |