JP2003088703A - Distillatory apparatus and distillation method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To enhance rectifying effect. SOLUTION: The distillatory apparatus has a first distillation part 25 equipped with a column main body Tw, an intermediate partition 22, a concentration part AR1 and a recovery part AR2, a second distillation part 26 connected to the upper end of the first distillation part 25 and equipped with a concentration part AR3 and a recovery part AR4, a third distillation part 27 connected to the lower end of the first distillation part 25 and equipped with a concentration part AR5 and a recovery part AR6 and a cooling device for taking out the liquid condensed in the second distillation part 26 through a liquid take-out port to cool the same and returning the cooled liquid into the column main body Tw to reflux the same to the concentration part AR3. Since it is unnecessary to arrange the condenser to the column top, the column main body Tw and a filler can be made light.

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to a distillation apparatus and a distillation method.

[0002]

2. Description of the Related Art Conventionally, in order to separate each component by distilling a stock solution containing a mixture containing a plurality of components and recovering a predetermined component as a product, for example, a single partition whose interior is partitioned by a partition is used. There is provided a distillation apparatus having a type distillation column.

FIG. 2 is a conceptual diagram of a conventional distillation apparatus.

In the figure, 10 is a combined distillation column,
In the combined distillation column 10, a predetermined inner portion is divided by a flat plate-shaped partition 22, and a first chamber and a second chamber are formed adjacent to each other. Then, a feed nozzle 41 is formed on the first chamber side of the combined distillation column 10 on the column side, and the feed nozzle 41 is provided with components A to C.
A line L51 for supplying a stock solution M consisting of a mixture containing is connected. The component A has a lower boiling point than the component B, and the component B has a lower boiling point than the component C. The component A constitutes a low boiling point component, the component B constitutes an intermediate component, and the component C constitutes a high boiling point component.

In the main body of the combined distillation column 10, a concentrating part AR1 formed above the feed nozzle 41 in the first chamber and a recovery part formed below the feed nozzle 41 in the first chamber. A first distillation section having a section AR2, a concentration section AR3 connected to the upper end of the first distillation section and formed above the upper end of the first distillation section, and the first distillation in the second chamber A second distillation section that is formed below the upper end of the section and that has a recovery section AR4 that is adjacent to the concentrating section AR1 via a partition 22; and is connected to the lower end of the first distillation section, A concentrating section AR formed above the lower end of the first distillation section in the second chamber and adjacent to the recovery section AR2 via the partition 22.
5 and a third distillation section having a recovery section AR6 formed below the lower end of the first distillation section.

A vapor outlet 43 is formed at the top of the combined distillation column 10, and a line L57 for discharging the vapor rich in the component A is connected to the vapor outlet 43. Further, the line L is provided at the top of the combined distillation column 10.
A condenser 81 is connected via 57, and the vapor rich in component A discharged from the top of the column is cooled and condensed by a cooling liquid such as cooling water supplied from a cooling liquid supply source (not shown) and condensed. Generated as effluent, lines L58, L60
Is discharged through. A vacuum generator (not shown) is connected to the condenser 81 via a line L61,
Due to the negative pressure generated by the vacuum generator, the vent gas generated in the column body of the combined distillation column 10 is sucked and discharged into the atmosphere. Further, a reflux liquid inlet 44 is formed at the top of the combined distillation column 10, and a part of the distillate discharged to the line L58 is returned to the inside of the column body via the line L59 and refluxed to the concentrating section AR3. It is refluxed as a liquid.

In this case, the condenser 81 is connected to the line L6.
A vacuum generator is connected via 1, but in the case of a combined distillation column in which the inside of the column body is placed under normal pressure or under pressure, a condenser is used. 81
It is not necessary to connect a vacuum generator to.

A side cut nozzle 42 is formed on the second chamber side of the combined distillation column 10 on the side of the column, and a liquid rich in component B is discharged to the side cut nozzle 42 as a side cut liquid. The line L56 is connected.

A bottoms outlet 45 is formed at the bottom of the combined distillation column 10, and a line L5 for discharging a liquid rich in component C as bottoms to the bottoms outlet 45.
2, L55 are connected. Further, the combined distillation column 1
An evaporator 82 is connected to the bottom of column 0 through the lines L52 and L53, and a part of the bottom liquid is sent to the evaporator 82 for heating supplied from a heating vapor supply source (not shown). It is heated by the vapor and evaporates to become vapor rich in component C. Then, the vapor inlet 46 is formed at the bottom of the combined distillation column 10, and the vapor rich in the component C generated in the evaporator 82 is supplied into the column main body through the line L54. A distillation apparatus is constituted by the combined distillation column 10, the condenser 81, the evaporator 82 and the like.

[0010]

However, in the conventional distillation apparatus, the distillate produced by condensing the vapor by the condenser 81 is used as the reflux liquid. Since it is difficult to adjust the temperature of, the rectification effect cannot be improved by the reflux liquid.

It is an object of the present invention to provide a distillation apparatus which can solve the problems of the conventional distillation apparatus and improve the rectification effect.

[0012]

To this end, in the distillation apparatus of the present invention, a column main body and a partition which divides the inside of the column main body and adjoins each other to form a first chamber and a second chamber, A first distilling section having a concentrating section formed above the feed nozzle and supplied with a stock solution through a feed nozzle, and a collecting section formed below the feed nozzle; and the first distilling section. A concentrating part formed above the upper end and a collecting part formed below the upper end and adjacent to the concentrating part of the first distillation part through a partition. A second distillation section, a concentration section connected to the lower end of the first distillation section, formed above the lower end, and adjacent to the recovery section of the first distillation section via a partition; and Third with a recovery part formed below the lower end Cooling device for distilling the liquid condensed in the second distilling unit through the liquid outlet, cooling the liquid, returning the liquid inside the tower main body through the liquid returning port, and returning the liquid to the concentrating unit. Have and.

In another distillation apparatus of the present invention, further, the liquid in the second distillation section is taken out from the inside of the tower body through the liquid take-out port, cooled, and then inside the tower body through the liquid return port. It has a heat exchange device for returning to.

In still another distillation apparatus of the present invention, a heat exchange section is further formed in the tower body between the liquid return port and the liquid takeout port.

In still another distillation apparatus of the present invention, the concentration section, the recovery section and the heat exchange section are further filled.
The thing is filled.

In still another distillation apparatus of the present invention, the concentration section, the recovery section and the heat exchange section have a tray structure.

In still another distillation apparatus of the present invention, further, in the cooling apparatus, the liquid is subcooled to a temperature lower than the boiling point.

In the distillation method of the present invention, the column solution is supplied through a tower body, a partition which divides the inside of the tower body and adjoins each other to form a first chamber and a second chamber, and a feed nozzle. A first distillation section having a concentrating section formed above the feed nozzle and a collecting section formed below the feed nozzle, connected to the upper end of the first distillation section, and formed above the upper end Concentrated distillation section, and a second distillation section including a recovery section formed below the upper end and adjacent to the concentration section of the first distillation section via a partition, and the first distillation A collecting section connected to the lower end of the section, formed above the lower end, and adjacent to the collecting section of the first distillation section via a partition, and a collecting section formed below the lower end. Applicable to a distillation apparatus equipped with a third distillation section It is.

Then, the liquid condensed in the second distillation section is taken out through the liquid take-out port, cooled, and then returned into the column main body through the liquid return port and refluxed to the concentrating section.

[0020]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.

FIG. 1 is a conceptual diagram of a distillation apparatus according to the first embodiment of the present invention, and FIG. 3 is a conceptual diagram of a combined distillation column according to the first embodiment of the present invention.

In the figure, 10 is a combined distillation column,
In the column body Tw of the combined distillation column 10, the first section SC1, the second section SC2, the third section SC
3, 4th section SC4, 5th section SC5, 6th section SC6, 7th section SC7, 8th section SC8, 9th section SC9, 10th section SC10, 11th section SC11, 12th section SC12 and 13th section SC13 is formed.

Inside the tower body Tw, in the eighth section SC8, the ninth section SC9, and the tenth section SC10, the flat chamber-shaped partition 22 is used to form the first chambers 14A to 16A and the second chambers 14B to 16B. The first chamber 14A-16A and the second chamber 14B-16B
And are adjacent to each other. In addition, the first chamber 14A ~
16A causes the first distillation section 25 to change the first section SC1, the second section SC2, and the third section SC.
3, 4th section SC4, 5th section SC5, 6th section SC6, 7th section SC7, 2nd chamber 1
4B and the upper half of the second chamber 15B allow the second distillation section 2
6 is the lower half of the second chamber 15B, the second chamber 16B, the first
The third distillation section 27 is formed by the 1st section SC11, the 12th section SC12 and the 13th section SC13, and the second distillation section 26 is provided at the upper end of the first distillation section 25 and the third distillation section 27. Is connected to the lower end of the first distillation section 25.

The partition 22 is formed of a heat insulating material, or the interior of the partition 22 is evacuated,
The partition 22 may have a heat insulating structure. In this case, between the first chamber 14A and the second chamber 14B, the first chamber 15A
And the second chamber 15B, and the first chamber 16A and the second chamber 16
Since the heat transfer with B can be reduced respectively, the efficiency of distillation can be improved.

On the tower side of the combined distillation column 10, the feed nozzle 41 is exposed to the first chamber 15A.
However, a side cut nozzle 42 is formed facing the second chamber 15B, and a line L for supplying a stock solution M composed of a mixture containing components A to C to the feed nozzle 41.
51 is a line L for discharging the liquid rich in component B to the side cut nozzle 42 as a side cut liquid.
56 is connected. The boiling point of component A is lower than that of component B, and that of component B is lower than that of component C. Then, the side cut liquid is discharged as a product.

A vent gas outlet 49 is formed at the top of the combined distillation column 10 so as to face the first section SC1, and a line L101 for discharging the vent gas is connected to the vent gas outlet 49. A vacuum generator (not shown) is connected to the combined distillation column 10 via a line L101, and in the distillation process of a reduced pressure system,
The inside of the combined distillation column 10 is decompressed by the negative pressure generated by the vacuum generator, the vent gas generated inside the combined distillation column 10 is sucked, and the line L1
It is discharged into the atmosphere via 01.

In the present embodiment, the vent gas outlet 49 and the line L10 are provided at the top of the combined distillation column 10.
A vacuum generator is connected via 1, but a vacuum is generated in the case of a combined distillation column in which the inside of the tower body Tw is placed under normal pressure or under pressure. No need to connect equipment.

At the top of the combined distillation column 10, a distillate outlet 71 as a liquid outlet for facing the third section SC3 is provided as a liquid return outlet for facing the first section SC1. A reflux liquid inlet 72 is formed, and a line L102 is provided at the distillate outlet 71 and the reflux liquid inlet 72 is provided.
The line L103 is connected to. And the line L
A pump p11 is connected to 102, and a first heat exchanger 85 is connected to the pump p11 via a line L104,
The reflux liquid inlet 72 is connected to the first heat exchanger 85 via a line L105 and the line L103. The pump p11 uses the liquid rich in the component A in the tower main body Tw as a distillate through the distillate take-out port 71 to form a line L1.
02, and supply to the first heat exchanger 85 via line L104. The first heat exchanger 85 functions as an overhead cooler, and the distillate supplied through the line L104 is combined with a cooling liquid such as cooling water supplied from a first cooling liquid supply source (not shown). Part of the distillate is returned to the inside of the tower body Tw through the lines L105, L103 and the reflux liquid inlet 72 and is refluxed as the first reflux liquid to the concentrating part AR3 to distill The rest of the liquid is line L
It is discharged to 106. The lines L102 to L105,
The pump p11 and the first heat exchanger 85 constitute a cooling device.

On the side of the combined distillation column 10 facing the seventh section SC7, the liquid outlet 4 is provided.
7, the liquid return port 48 facing the fifth section SC5
The line L73 is connected to the liquid return port 48, and the line L71 is connected to the liquid outlet 47. A pump p1, a line L72 and a second heat exchanger 83 are connected between the lines L71 and L73, and the liquid inside the tower body Tw is taken out to the line L71 via the liquid take-out port 47 by the pump p1. And is supplied to the second heat exchanger 83 via the line L72. The second heat exchanger 83 functions as a side cooler, and the liquid rich in component A supplied through the line L72 is cooled by cooling water or the like supplied from a second cooling liquid supply source (not shown). It is cooled by heat exchange with the liquid, returned to the inside of the tower main body Tw via the line L73 and the liquid return port 48, and is refluxed to the concentrating sections AR1 and AR5 as the second reflux liquid. The line L
71-L73, the pump p1, and the 2nd heat exchanger 83 comprise a heat exchange device.

Further, a bottom liquid outlet 45 is formed at the bottom of the combined distillation column 10 so as to face the 13th section SC13, and a liquid rich in component C is discharged into the bottom liquid outlet 45. Lines L52 and L55 for discharging as liquid are connected. Then, an evaporator (reboiler) 8 is provided at the bottom of the combined distillation column 10 via the lines L52 and L53.
2 is connected, a part of the bottom liquid is sent to the evaporator 82, and is heated and evaporated by the heating steam supplied from the heating steam supply source (not shown) to become a steam rich in the component C. Further, at the bottom of the combined distillation column 10, the first
The vapor inlet 46 is formed so as to face the one section SC11, and the vapor rich in the component C generated in the evaporator 82 is supplied into the column body Tw via the line L54. The combined distillation column 10, the evaporator 82, the first,
A distillation apparatus is constituted by the second heat exchangers 85, 84 and the like.

In the first distillation section 25, the concentration section AR1 is collected by the first chamber 14A arranged above the feed nozzle 41, and the concentration section AR1 is collected by the first chamber 16A arranged below the feed nozzle 41. The parts AR2 are respectively formed. Then, in the second distillation section 26, the concentration section AR3 is arranged below the upper end of the first distillation section 25 by the fourth section SC4 arranged above the upper end of the first distillation section 25. , The concentration section A
The second chamber 14B disposed adjacent to R1 allows the recovery part AR4 to be disposed between the reflux liquid inlet 72 and the distillate outlet 71, that is, above the concentrating part AR3. 2 section SC2 with first heat exchange section ZN11
Between the liquid return port 48 and the liquid outlet 47, that is, the concentration part AR3, the concentration part AR1 and the recovery part A.
A second heat exchange section ZN1 is formed in the sixth section SC6 arranged between the second section and R4.

Further, in the third distillation section 27, above the lower end of the first distillation section 25, the concentration section AR5 is provided by the second chamber 16B arranged adjacent to the recovery section AR2. The recovery section AR6 is formed by the twelfth section SC12 arranged below the lower end of the first distillation section 25.

A tubular type distributor 28, which is a cylindrical body having holes for distribution (not shown) formed in the bottom, is disposed in the first section SC1, and is returned through the reflux liquid inlet 72. A part of the effluent is distributed to the second section SC2. And the third section S
A collector 29 and a tubular distributor 31 are arranged in C3, and the liquid collected by the collector 29 is taken out to a line L102 through a distillate outlet 71 and is distributed to the fourth section SC4 by the distributor 31. To be done. Further, the collector 32 and the tubular type distributor 33 are arranged in the fifth section SC5, and the liquid returned through the liquid return port 48 and the liquid collected by the collector 32 are collected by the distributor 33 in the sixth section SC5. It is distributed to SC6.

A chimney hat collector 34 (having the same shape as the collector 32 may have a cover formed by forming a gap at the upper end of a vertical cylindrical body in the seventh section SC7. .), And a channel-type (trough-type) distributor 35, which is composed of a grooved body having an opening at the top and a hole (not shown) for distribution formed at the bottom, and the liquid collected by the collector 34 is The eighth section SC is taken out to the line L71 through the liquid take-out port 47 and at a predetermined distribution ratio preset by the distributor 35.
8 first chamber 14A and second chamber 14B.

Also, the first chamber 15 of the ninth section SC9
A collector 36 and a tubular-type distributor 38 are disposed in A, and the stock solution M supplied through the feed nozzle 41 and the liquid collected by the collector 36 are supplied to a tenth position by the distributor 38.
It is distributed to the first chamber 16A of the section SC10.

On the other hand, the second chamber 15 of the ninth section SC9
A collector 37 and a tubular-type distributor 39 are disposed in B, and the liquid collected by the collector 37 is discharged to the line L56 via the side cut nozzle 42 and the distributor 3
9 is distributed to the second chamber 16B of the tenth section SC10.

Further, a collector 51 and a channel type distributor 52 are arranged in the eleventh section SC11, and the liquid collected by the collector 51 is distributed by the distributor 52 to the twelfth section SC12.

In the present embodiment, the tubular type distributors 28, 31, 33, 38, 39,
And the channel type distributors 35 and 52 are used. Instead of the tubular type distributors 28, 31, 33, 38 and 39, the channel type distributors are replaced with the channel type distributors 35 and 52. A tubular type distributor can also be used.

Next, the operation of the combined distillation column 10 will be described.

When the undiluted solution M is supplied through the feed nozzle 41, the undiluted solution M moves downward in the recovery section AR2, and vapors rich in the components A and B in the upper part become the component B in the lower part. And a liquid rich in C are generated, and from the lower end of the first distillation section 25 to the third distillation section 27.
Is supplied with a liquid rich in components B and C.

Further, the liquid rich in the components B and C is
The vapor is heated in the third distillation section 27 to become vapor rich in components B and C, and the vapor rich in components B and C is moved upward in the recovery portion AR2, while being concentrated into the stock solution M.
To produce a vapor rich in components A and B from the stock solution M.

Subsequently, the vapor rich in the components A and B is
The first distilling unit 25 is moved upward in the concentrating unit AR1.
Is supplied to the second distillation section 26 from the upper end. Further, the vapor rich in components A and B is cooled and condensed in the second distillation section 26 to become a liquid rich in components A and B.

Then, a part of the liquid rich in the components A and B is refluxed to the concentrating part AR1 and brought into contact with the vapor rich in the components A and B which is moved upward in the concentrating part AR1.

In this way, the vapor rich in components A and B can be supplied from the upper end of the first distillation section 25 to the second distillation section 26.

In the recovery section AR6, the liquids rich in components B and C move downward, and vapors rich in component B are generated in the upper part and liquids rich in component C are generated in the lower part. Therefore, the liquid rich in the component C is discharged as the bottom liquid through the bottom liquid outlet 45.

Further, a part of the liquid rich in component C discharged through the bottom liquid outlet 45 is sent to the evaporator 82 and heated by the evaporator 82 to become vapor rich in component C. . The vapor rich in the components C is supplied to the thirteenth section SC13 through the vapor inlet 46 and is rich in the components B and C while being moved upward in the thirteenth section SC13 and the recovery unit AR6. The liquid rich in components B and C is contacted with the liquid to generate a vapor rich in component B.

Subsequently, a part of the vapor rich in the component B is
The liquid moves up in the concentrating unit AR5 and comes into contact with the liquid enriched with the component B that is refluxed from the second distillation unit 26 at the upper end of the third distillation unit 27 to become a liquid enriched with the component B. In this way, the liquid rich in component B obtained at the upper end of the third distillation section 27 is discharged as the side cut liquid through the side cut nozzle 42.

On the other hand, the recovery section AR of the second distillation section 26
In 4, the liquids rich in components A and B move downwards, producing vapors rich in component A in the upper part and liquids rich in component B in the lower part. In this way, the liquid rich in component B obtained at the lower end of the second distillation section 26 is discharged as the side cut liquid through the side cut nozzle 42.

Then, the vapor rich in the component A moves upward in the concentrating section AR3 to reach the first heat exchanging section ZN11.
And is condensed in the first heat exchange section ZN11 to become a liquid rich in component A and collected by the collector 29, and a part of the liquid rich in component A is passed through the distillate outlet 71. And is taken out as a distillate in the line L102.

In this way, the vapor rich in components A and B is separated into the vapor rich in component A and the liquid rich in component B by the second distillation section 26, and rich in component A. The vapor is condensed in the first heat exchange section ZN11 to become a liquid rich in component A (overhead fraction), taken out as a distillate via a line L102, and a liquid rich in component B (intermediate). The distillate) is discharged as a side cut liquid through the side cut nozzle 42. Further, the liquid rich in components B and C is separated into the liquid rich in component B and the liquid rich in component C by the third distillation section 27, and the liquid rich in component B serves as a side cut liquid. The liquid (column bottom fraction) rich in component C discharged through the side cut nozzle 42 is discharged from the column bottom.

Then, in order to increase the efficiency of distillation of the component A, a part of the distillate is returned through the reflux liquid inlet 74 and is refluxed to the concentrating section AR3 as the first reflux liquid,
Components A and B that can be moved upward in the concentration unit AR3
Contacted with rich steam.

Incidentally, each of the concentrating sections AR1, AR3, AR
5, each of the recovery parts AR2, AR4, AR6 and the first and second heat exchange parts ZN11, ZN1 are filled with packing such as ordered packing and irregular packing composed of one node. However, depending on the relative volatility of each component to be distilled, in order to secure the theoretical plate number required for distillation, it is formed by a packing composed of multiple nodes corresponding to the characteristics of the packing used. You can also

Further, a distributor may be arranged between the nodes. Further, the feed nozzle 41 and the side cut nozzle 42 do not necessarily have to be arranged at the same height.

In this way, the stock solution M can be separated into the components A to C without using a plurality of distillation columns. Further, since it is not necessary to repeat heating and cooling in each of a plurality of distillation columns, it is not necessary to provide a large number of instrument parts such as a condenser, an evaporator and a pump. Therefore, not only can the area occupied by the distillation apparatus be reduced, but also the usage amount and energy consumption of the utility can be reduced, and the cost of the distillation apparatus can be reduced.

The combined distillation column 10 has a theoretical plate number of about 30 to 100 plates as a whole, and the sixth section SC6 and the eighth section SC8 are each provided with about 5 to 30 plates. preferable.

By the way, in the present embodiment, the first,
Since the liquid taken out from the tower body Tw is supplied to the second heat exchangers 85 and 83, it can be placed separately from the combined distillation tower 10. Moreover, it is not necessary to dispose a condenser in the combined distillation column 10.

Therefore, since the tower top of the tower body Tw can be lightened, the support of the combined distillation column 10 can be stabilized, and the reinforcing member for preventing the combined distillation column 10 from tipping over. The plate thickness can be reduced. Further, since the moment applied to the foundation of the combined distillation column 10 can be reduced, the foundation work can be simplified.

Further, no condenser is arranged at the top of the column, the vapor is condensed in the first heat exchange section ZN11 formed in the second section SC2, and the liquid collected in the collector 29 is distilled as distillate. Line L1 from the outlet 71
02, and is cooled to a predetermined temperature in the first heat exchanger 85. Therefore, the temperature of the distillate returned to the first section SC1 via the reflux liquid inlet 72 and the reflux to the concentrating section AR3. The temperature of the first reflux liquid can be freely set.

Therefore, through line L104, the first
Of the liquid supplied to the heat exchanger 85 of the first heat exchanger 8
In 5, supercooling to a temperature below the boiling point and returning liquid below the boiling point to the first section SC1 enables reflux by the supercooled first reflux liquid, that is, cold reflow. , Concentration part AR3
In, the amount of liquid moving downward is increased, and the rectification effect is improved. In order to cool the liquid in the first heat exchanger 85 to a temperature lower than the boiling point, the amount of cooling water supplied to the first heat exchanger 85 is increased or the temperature of the cooling water is lowered.

By the way, in the depressurizing distillation process, the negative pressure generated by the vacuum generator sucks the vent gas generated in the combined distillation column 10 and discharges it into the atmosphere through the line L101. However, if a process fluid such as a vapor rich in component A is mixed in the vent gas, it disturbs the performance of the vacuum generator. In particular, when the process fluid is composed of a high melting point component, a corrosive component, a malodorous component, a component having a bad influence on the human body, etc., it becomes impossible to stably operate the vacuum generator.

However, in the present embodiment, the temperature of the reflux liquid can be set freely, so that the line L
The temperature of the gas exhausted via 101, ie the exhaust gas, can be adjusted and the composition of the exhaust gas can be adjusted. Therefore, the vacuum generator can be operated under stable and operating conditions adapted to the process. Note that, also in the case of the normal pressure system, the conditions of the exhaust gas discharged through the line L can be selected.

A second heat exchanging portion ZN1 is formed in the sixth section SC6, and a part of the liquid collected by the collector 34 is removed by the seventh section SC7.
From the liquid through the liquid outlet 47, is cooled in the second heat exchanger 83, and is discharged through the liquid return port 48 into the fifth region.
It is returned to the section SC5 and, together with the liquid collected by the collector 32, is distributed by the distributor 33 to the fourth section SC4. And the second
The vapor moving upward in the heat exchanging section ZN1 and the liquid moving downward in the second heat exchanging section ZN1 come into direct contact on the surface of the packing, and the vapor is cooled and condensed by the liquid.

Therefore, the fifth liquid is returned through the liquid return port 48.
Since the liquid returned to the section SC5 is refluxed to the concentration units AR1 and AR5 as the second reflux liquid, the distillate returned to the column main body Tw at the top of the column is the first distillate required in the concentration unit AR3. Since only the amount of the reflux liquid is required and the amount of the second reflux liquid can be reduced, the concentration part AR3
In, it is possible to reduce the amount of liquid moving downward in the tower body Tw. In addition, the second heat exchange section ZN1
The amount of vapor moving upward in the tower body Tw in the concentrating portion AR3 can be reduced by the amount of vapor condensed in. As a result, not only can the column diameter of the combined distillation column 10 be reduced while maintaining the rectification effect in the column body Tw, but also the first heat exchange section ZN1.
Since the size of 1 can be reduced, the distillation apparatus can be downsized. Further, since the load on the top of the combined distillation column 10 can be reduced, the combined distillation column 10 can be stably supported.

Since the filling capacity of the packing in the concentrating section AR3 can be reduced, the amount of liquid droplets floating in the tower body Tw (dynamic liquid holdup amount) can be reduced, Extra process system hold-up in the collector 32, the distributor 33, etc. can be reduced. Therefore, the total filling capacity of the combined distillation column 10 can be reduced, and the distillation apparatus can be further downsized.

Further, usually, when the composition of the stock solution M changes, the reflux ratio (reflux amount) of the distillate returned at the top of the tower through the reflux liquid inlet 72 is increased or decreased, or the heating in the evaporator 82 is performed. Although the composition of the distillate is adjusted by increasing or decreasing the amount, by adjusting the temperature of the distillate returned through the reflux liquid inlet 72, the composition of the stock solution M can be changed. Then, the composition of the distillate can be easily adjusted. Therefore, the rectification effect can be improved and the purity of the distillate can be increased.

Further, in general, when the composition of the stock solution M changes, the reflux ratio of the distillate returned through the reflux liquid inlet 72 at the top of the tower is increased or decreased, or the heating amount in the evaporator 82 is increased or decreased. The composition of the side-cut liquid is adjusted by adjusting the temperature of the liquid returned via the liquid return port 48, so that the composition of the side-cut liquid can be adjusted in accordance with the fluctuation of the composition of the stock solution M. Can be easily adjusted. Therefore, the rectification effect can be improved, and the purity of the side cut liquid can be increased.

Since the condenser is designed mainly for the purpose of condensing the vapor, it is difficult to further subcool the distillate as the condensate in the condenser. Since the first and second heat exchangers 85 and 83 are designed mainly for cooling the distillate and the liquid, the cooling temperature of the distillate and the liquid can be freely adjusted.

In the present embodiment, the filler is arranged in the first and second heat exchange parts ZN11 and ZN1, and the liquid is
The steam is moved downward along the surface of the packing so that the steam moves upward through the clearance of the packing, and the steam is filled in the first and second heat exchange parts ZN11, ZN1. Without arranging objects, disposing an injection device such as a sprue nozzle,
The liquid is jetted toward the space inside the first and second heat exchange units ZN11 and ZN1, and the first and second heat exchange units ZN11 and ZN are injected.
It is also possible to bring 1 into direct contact with the steam moving upwards.

Further, in the present embodiment, the concentration section A
The second heat exchange section ZN1 is arranged below R3, but the second heat exchange section is formed integrally with the concentrating section AR3, and the liquid is taken out from immediately below the concentrating section AR3. After cooling, it can also be returned directly above the concentration part AR3.

Furthermore, in the present embodiment, the first,
Although the second heat exchange units ZN11 and ZN1 are arranged, only the first heat exchanger ZN11 can be arranged.

Next, a second embodiment of the present invention will be described. In addition, about the thing which has the same structure as 1st Embodiment, the description is abbreviate | omitted by giving the same code | symbol.

FIG. 4 is a conceptual diagram of a distillation apparatus according to the second embodiment of the present invention.

In the figure, 73 is the seventh section SC7.
Is a liquid return port formed immediately below the liquid outlet 47, and the line L73 and the liquid return port 73 are lines L
Connected by 108. And the second heat exchanger 8
Part of the liquid cooled by 3 is returned to the fifth section SC5 via the line L73 and the liquid return port 48, and is returned to the concentrating units AR1 and AR5 as the second reflux liquid, and the rest of the liquid is returned to the line L108. And liquid return port 7
It is returned to the seventh section SC7 via 3 and is directly refluxed to the concentrating units AR1 and AR5 as the third reflux liquid.

The lines L71 to L73, L108,
The heat exchange device is configured by the pump p1 and the second heat exchanger 83.

Next, a third embodiment of the present invention will be described. In addition, about the thing which has the same structure as 1st Embodiment, the description is abbreviate | omitted by giving the same code | symbol.

FIG. 5 is a conceptual diagram of a distillation apparatus according to the third embodiment of the present invention.

In this case, L109 is a line formed by branching the line L73. 7th section SC7
In, a liquid rich in component A ′ close to component A can be obtained, so a liquid rich in component A ′ (intermediate fraction)
Can be discharged to the line L109 as a side cut liquid.

Next, a fourth embodiment of the present invention will be described. In addition, about the thing which has the same structure as 1st Embodiment, the description is abbreviate | omitted by giving the same code | symbol.

FIG. 6 is a conceptual diagram showing a main part of a distillation apparatus according to the fourth embodiment of the present invention.

As shown in the figure, a collecting part AR4 is formed adjacent to the concentrating part AR1, and a concentrating part AR5 is formed adjacent to the collecting part AR2. Between the collecting part AR4 and the concentrating part AR5, and A collecting part AR4 'is formed so as to be slightly adjacent to the concentrating part AR1 and the collecting part AR2.
Between the collecting part AR4 'and the collecting part AR4'
However, a side cut liquid nozzle 102 is formed between the recovery unit AR4 'and the concentration unit AR5. From the side cut liquid nozzle 101, a component B'containing mainly component B and containing component A in a predetermined amount is formed. The rich liquid (intermediate fraction) is discharged to the line L111 as a side-cut liquid, and the liquid rich in component B (intermediate fraction) is discharged to the line L112 from the side-cut liquid nozzle 102 as a side-cut liquid.

Next explained is the fifth embodiment of the invention. In addition, about the thing which has the same structure as 1st Embodiment, the description is abbreviate | omitted by giving the same code | symbol.

FIG. 7 is a conceptual diagram showing a main part of a distillation apparatus according to the fifth embodiment of the present invention.

As shown in the figure, the collecting section AR4 is adjacent to the concentrating section AR1, the concentrating section AR5 is adjacent to the upper end of the collecting section AR2, and the lower end of the collecting section AR2 is below the concentrating section AR5. And a side cut liquid nozzle 103 is formed between the collection unit AR4 and the concentration unit AR5, and a side cut liquid nozzle 104 is formed between the concentration unit AR5 and the concentration unit AR5 '. A liquid (middle distillate) rich in component B is discharged from the side cut liquid nozzle 103 to the line L113 as a side cut liquid, and the side cut liquid nozzle 104 mainly contains the component B and a predetermined amount of the component C. The liquid rich in component B'containing only (the middle distillate) is used as the side cut liquid in line L.
It is discharged to 114.

Next explained is the sixth embodiment of the invention. In addition, about the thing which has the same structure as 1st Embodiment, the description is abbreviate | omitted by giving the same code | symbol.

FIG. 8 is a conceptual diagram of a distillation apparatus according to the sixth embodiment of the present invention.

As shown in the figure, the concentration section in the second distillation section 26 is divided into a concentration section AR3 and a concentration section AR3 ', and the concentration section AR3 is provided between the first and second heat exchange sections ZN11, ZN1. However, a concentration section AR3 'is formed between the second heat exchange section ZN1 and the concentration sections AR1 and AR4.

In this case, in the seventh section SC7, the liquid return port 73 is formed immediately below the liquid outlet 47, and the line L73 and the liquid return port 73 are connected to the line L11.
6, L117 are connected. Also, the line L11
6 is branched to form a line L118. The lines L71 to L73, L116, L117, and the pump p1
The second heat exchanger 83 constitutes a heat exchange device.

Then, a part of the liquid cooled by the second heat exchanger 83 is returned to the fifth section SC5 through the line L73 and the liquid return port 48, and is concentrated as a second reflux liquid AR3 ', Refluxed to AR1 and AR5, the rest of the liquid flows through the line L116, and a part of the liquid flows through the line L117 and the liquid return port 73 to the tower main body Tw.
It is returned to the inside and is directly concentrated as the third reflux liquid
It is refluxed to 3 ', AR1, AR5.

In this case, the concentration section in the second distillation section 26 is divided into the concentration section AR3 and the concentration section AR3 ', and the second heat exchange section ZN is provided between the concentration section AR3 and the concentration section AR3'.
Since 1 is formed, it is possible to freely set the amounts of the first to third reflux liquids that are refluxed to the concentrating portions AR3 and AR3 '. Therefore, the product recovery rate can be made higher than the product recovery rate in the first embodiment, and if the supply amount of the undiluted solution M is the same, the recovered product amount can be increased. If the same amount of products are
The supply amount of the stock solution M can be reduced. Further, the distillation apparatus can be downsized.

Next explained is the seventh embodiment of the invention. In addition, about the thing which has the same structure as 1st Embodiment, the description is abbreviate | omitted by giving the same code | symbol.

FIG. 9 is a conceptual diagram of a distillation apparatus according to the seventh embodiment of the present invention.

By the way, in the middle part of the combined distillation column 10, for example, below the seventh section SC7, the temperature in the column is usually higher than the temperature of the stock solution M, so that heat is recovered from the liquid taken out from the column. can do.
Therefore, in the present embodiment, the pump p1 and the second heat exchanger 83 are the line L121 and the third heat exchanger as a preheater.
Connected via a heat exchanger 86 and a line L123 of
In the third heat exchanger 86, the liquid supplied via the line L121 and the stock solution M supplied via the line L51 are heat-exchanged, and the stock solution M supplied into the tower body Tw is the liquid. Preheated by.

Therefore, the amount of heat in the evaporator 82 can be reduced and the energy consumption can be reduced.

The lines L71, L73, L121,
L123, the pump p1 and the second and third heat exchangers 83,
A heat exchange device is constituted by 86.

Next, an eighth embodiment of the present invention will be described. In addition, about the thing which has the same structure as 1st Embodiment, the description is abbreviate | omitted by giving the same code | symbol.

FIG. 10 is a conceptual diagram of a distillation apparatus according to the eighth embodiment of the present invention.

By the way, when the temperature of the column top is high and the temperature of the liquid taken out from the column top is higher than the temperature of the stock solution M,
Heat can be recovered from the liquid removed from the top of the column.

Therefore, in the present embodiment, the pump p11 and the first heat exchanger 85 are connected via the line L122, the fourth heat exchanger 87 as a preheater and the line L124, and the fourth In the heat exchanger 87, the distillate supplied through the line L122 and the line L51
Heat exchange with the undiluted solution M supplied through the tower main body Tw
The undiluted solution M supplied inside is preheated by the distillate.

Therefore, the amount of heat in the evaporator 82 can be reduced and the energy consumption can be reduced.

Lines L102, L105, L12
2, 2, L124, the pump p11, and the first and fourth heat exchangers 85 and 87 constitute a cooling device.

Next explained is the ninth embodiment of the invention. In addition, about the thing which has the same structure as 1st Embodiment, the description is abbreviate | omitted by giving the same code | symbol.

FIG. 11 is a conceptual diagram of a distillation apparatus according to the ninth embodiment of the present invention.

In the middle part of the combined distillation column 10, for example, below the seventh section SC7, usually,
Since the temperature in the tower is higher than the temperature of the stock solution M, heat can be recovered from the liquid taken out from the tower. Further, the temperature at the top of the tower is high, and the temperature of the liquid taken out from the top of the tower is
If the temperature is higher than the above temperature, heat can be recovered from the liquid taken out from the top of the column.

Therefore, in the present embodiment, the pump p11 and the first heat exchanger 85 are connected via the line L122, the fourth heat exchanger 87 as a preheater and the line L124, and In the heat exchanger 87, the distillate supplied through the line L122 and the line L51
Heat exchange with the undiluted solution M supplied through the tower main body Tw
The undiluted solution M supplied inside is preheated by the distillate.

Further, the pump p1 and the second heat exchanger 83 are in the line L121, and the third heat exchanger 86 as a preheater.
, And the liquid M supplied via the line L121 and the stock solution M supplied via the line L51 are heat-exchanged in the third main heat exchanger 86, and inside the tower body Tw. The undiluted solution M supplied to is further preheated by said liquid.

Lines L102, L105, L12
2, L124, the pump p11 and the first and fourth heat exchangers 85 and 87 constitute a cooling device, and a line L7
The 1, L73, L121, L123, the pump p1, and the second and third heat exchangers 83, 86 constitute a heat exchange device.

Therefore, the heating amount in the evaporator 82 can be further reduced, and the energy consumption can be further reduced.

Next explained is the tenth embodiment of the invention. In addition, about the thing which has the same structure as 1st Embodiment, the description is abbreviate | omitted by giving the same code | symbol.

FIG. 12 is a conceptual diagram of a distillation apparatus according to the tenth embodiment of the present invention.

In this case, the concentration sections AR1, AR3, AR
5, each of the recovery parts AR2, AR4, AR6 and the first and second heat exchange parts ZN11, ZN1 have a tray structure formed by stacking a plurality of trays.

Then, the concentrating section AR1 and the collecting section AR
The partition 22 is arranged from the tray at the upper end of 4 to the tray at the lower end of the collection unit AR2 and the concentration unit AR5, and the first partition and the second chamber are formed adjacent to each other.

[0112]

EXAMPLE Next, for the hydrocarbon type C12 to C20, the gas-liquid amount balance in the column of the conventional distillation apparatus and the gas-liquid amount balance in the column of the distillation apparatus of the present invention are compared.

FIG. 13 is a diagram showing the gas-liquid amount balance in the column of the conventional distillation apparatus, and FIG. 14 is a diagram showing the gas-liquid amount balance in the column of the distillation apparatus according to the first embodiment of the present invention.

In this case, in the conventional distillation apparatus, the reflux ratio RR is set to 5.56, and the amount of the reflux liquid refluxed not only to the concentrating section AR3 but also to the concentrating sections AR1 and AR5 is adjusted by the reflux rate according to the reflux ratio RR. Secure. At this time, since the flow rate of the component A discharged to the line L60 is 5,000 [kg / h], assuming that the latent heat of vaporization of the component A is 67 [kcal / kg], the vapor moving upward in the enrichment section AR3. Heat quantity Q1
Is about 2,200,000 [kcal / h].

On the other hand, in the distillation apparatus according to the first embodiment, the reflux ratio RR is set to 1.1, and the amount of the first reflux liquid refluxed to the concentrating portion AR3 is secured by the reflux amount according to the reflux ratio RR. . At this time, since the flow rate of the component A discharged to the line L106 is 5,000 [kg / h], when the latent heat of vaporization of the component A is 67 [kcal / kg], the vapor moving upward in the enrichment section AR3. Q2 is about 703
It becomes 500 [kcal / h]. The heat quantity Q3, which is the difference between the heat quantity Q1 and Q2, is 1,496,500 [kcal / h], and the steam corresponding to the heat quantity Q3 is cooled in the second heat exchange section ZN1 and secondly supplied to the enrichment sections AR1 and AR5. Is refluxed as a reflux liquid of.

Common equipment specifications of the conventional distillation apparatus and the distillation apparatus in the first embodiment are as follows.

Theoretical plate number NTS: Concentrating part AR1, AR3, AR5: 15 plate, 20 plate, 15 plate Collecting part AR2, AR4, AR6: 15 plate, 15 plate, 10 plate Raw material supply amount: 14,000 [kg / h] Emission of component A: 5,000 [kg / h] Emission of component B: 7,000 [kg / h] Emission of component C: 2,000 [kg / h] First chamber 14A to 16A To the second chambers 14B to 16B LB: 18,900 [kg / h] Column top, first heat exchange section ZN11 and enrichment section AR3 Pressure: 6.67 [kPa] (50 [Torr]) Process temperature of column top, first heat exchange section ZN11 and enrichment section AR3 T1: 75 [° C] between enrichment section AR3 and enrichment section AR1 and recovery section AR4 Process temperature T2: 180 [° C] Process temperature T3 between the part AR1 and the recovery part AR2: 200 [° C] Process temperature T4: 220 [° C] at the bottom of the column and the recovery part AR6 Heating amount Q: 1,880,000 [kcal / h] of the evaporator 82 ] Also, a combined distillation column 10 at the top of a conventional distillation apparatus
The device specifications are as follows.

Column top diameter ID: 2200 [mm] Packing material for the enrichment section AR3: 250Y (manufactured by Sumitomo Heavy Industries, Ltd.) Packing height: 9000 [mm] Packing capacity: 34.2 [m ³ ] where: The process temperature in the tower top and the enrichment section AR3 is T1, and the inlet temperature of the vapor in the condenser 81 is tvi.
And the outlet temperature of the distillate is tvo, the inlet temperature of the cooling water is twi, and the outlet temperature of the cooling water is two, the inlet temperatures tvi, twi and the outlet temperatures tvo, tw
Let o be tvi = T1 = tvo = 75 [° C.] twi = 32 [° C.] two = 37 [° C.] At this time, if the outlet side temperature difference in the condenser 81 is Δto, the inlet side temperature difference is Δti, and the logarithmic average temperature difference is Δtav [° C.], the outlet side temperature difference Δto, the inlet side temperature difference Δti, and the logarithmic average temperature. Difference Δtav [° C]
Is Δto = 75−37 = 38 [° C.] Δti = 75−32 = 43 [° C.] Δtav = (Δto−Δti) / k1 · log (Δto / Δti) = 40.5 [° C.] However, k1 is a coefficient, which is 2.3 in the present embodiment.

When the overall heat transfer coefficient in the condenser 81 is U [kcal / hr · m ² · ° C], U = 200 [kcal / hr · m ² · ° C] The thermal area A1 [m ² ] is A1 = Q1 / (Δtav · U) = 2,200,000 / (40.5 × 200) ≈272 [m ² ].

On the other hand, the equipment specifications of the combined distillation column 10 at the top of the distillation apparatus of the first embodiment are as follows.

Tower top diameter ID: 1300 [mm] Packing of the first heat exchanger ZN11 and the enrichment section AR3: 2
50Y (Sumitomo Heavy Industries, Ltd.) Filling height: 9000 [mm] Filling capacity: 12 [m³] Flow rate of the cooling liquid supplied to the second heat exchanger 83: 4,0
00 [kg / h] In this case, in the conventional distillation apparatus,
The top diameter ID was 2200 [mm],
Column top diameter ID of the distillation apparatus of the embodiment is 1300 [mm]
Therefore, in the distillation apparatus of the first embodiment,
The cross-sectional area ratio of the tower top can be set to 35%. That
In the conventional distillation apparatus, the packing capacity at the top of the column is 34.2.
[M³] Was that of the distillation apparatus of the first embodiment.
The filling capacity at the top of the tower is 12 [m ³], So the first implementation
In the distillation apparatus in the form of
It can be [%].

Here, the inlet temperature of the distillate in the first heat exchanger 85 is tui, and the outlet temperature of the distillate is tuo.
When the inlet temperature of the cooling water is twi and the outlet temperature of the cooling water is two, the inlet temperatures tui, twi and the outlet temperatures tuo, two are: tui = T1 = tuo = 75 [° C.] twi = 32 [° C. ] When two = 37 [° C.], the logarithmic average temperature difference Δtav [° C.] becomes Δtav = 40.5 [° C.], and the overall heat transfer coefficient is U [kcal / hr · m ² ·.
[° C] is U = 200 [kcal / hr · m ² · ° C], so the heat transfer area A2 of the first heat exchanger 85 is
[M ² ] is A2 = Q2 / (Δtav · U) = 703, 000 / (40.5 × 200) ≈87 [m ² ]. The first heat exchanger 85 is operated in an optimum state by performing a cascade control of the process temperature T1 and the outlet temperature tuo by a controller (not shown).

Further, since the process temperature T2 between the concentrating section AR3 and the concentrating section AR1 and the recovering section AR4 is equal to the process temperature T2 in the second heat exchanging section ZN1, the second heat exchanger 83 has the same temperature. Liquid inlet temperature is tq
i, the outlet temperature of the liquid is tqo, the inlet temperature of the cooling water is tri, and the outlet temperature of the cooling water is tro, the inlet temperatures tqi, tri and the outlet temperatures tqo, tr
Let o be tqi = T2 = 180 [° C.] tqo = 117 [° C.] tri = 32 [° C.] tro = 37 [° C.]. Then, assuming that the outlet side temperature difference in the second heat exchanger 83 is δto, the inlet side temperature difference is δti, and the logarithmic average temperature difference is δtav [° C], the outlet side temperature difference δt.
o, inlet side temperature difference δti and logarithmic average temperature difference δtav
[° C.] is δto = 117-37 = 80 [° C.] δti = 180-32 = 148 [° C.] δtav = (δto−δti) / k1 · log (δto / δti) = 111 [° C.] Heat transfer area A3 [m ² ] of the heat exchanger 83 of No. ²
A3 = Q3 / (Δtav · U) = 1,496,500 / (111 × 200) ≈67 [m ² ]. The second heat exchanger 83 controls the process temperature T2 and the outlet temperature to tqo by the control device.
By performing cascade control of and, they can be operated in an optimum state.

Also, the heat transfer area is from the heat transfer area A1 of 272 [m ² ] of the condenser 81 to the heat transfer area A2 of 87 [m ² ] of the first heat exchanger 85 and the second heat exchange area. The heat transfer area A3 of the vessel 83 is reduced to 154 [m ² ] which is the total of 67 [m ² ] (heat transfer area ratio 57 [%]), and the equipment can be made compact.

The heat transfer area A3 of the second heat exchanger 83 is smaller than the difference between the heat transfer area A1 and the heat transfer area A2 of the condenser 81 because the process temperature T1 in the enrichment section AR3 is small. While the temperature is 75 [° C.], the liquid inlet temperature tqi of the second heat exchanger 83 is 180 [° C.], which is 105 between the liquid inlet temperature tqi and the process temperature T2.
This is because there is a temperature difference of [° C]. Due to this temperature difference, the logarithmic average temperature difference Δtav in the condenser 81 is 4
While 0.5 [° C.], the logarithmic average temperature difference δtav in the second heat exchanger 83 becomes 111 [° C.],
70.5 [° C] between the logarithmic average temperature difference Δtav and δtav
A difference in temperature is formed, and the amount of heat exchanged can be increased by the difference in temperature. Therefore, the second heat exchanger 83 can be downsized, and the distillation apparatus can be downsized.

In the conventional distillation apparatus, if a condenser having a heat transfer area A1 of 272 [m ² ] is integrally formed at the top of the combined distillation column 10, the operating load W is 10,000 [k].
g], on the other hand, as shown in the first embodiment of the present invention, the heat transfer area A2 is provided at the top of the combined distillation column 10.
When the first heat exchanger 85 of 87 [m ² ] is disposed, the operating load W becomes 3,500 [kg] and the second heat exchanger 83 having the heat transfer area A3 of 67 [m ² ] , The operating load W becomes 3,300 [kg], and the total operating load W
Becomes 6,800 [kg]. The first and second heat exchangers 85 and 83 are placed separately from the combined distillation column 10.

Therefore, since the column main body Tw and the packing can be lightened, the support of the combined distillation column 10 can be stabilized, and a reinforcing member for preventing the combined distillation column 10 from tipping over. The plate thickness can be reduced.
Further, since the moment applied to the foundation of the combined distillation column 10 can be reduced, the foundation work can be simplified.

Incidentally, in the first embodiment, the first and second heat exchangers 85 and 83 are arranged, but only the first heat exchanger 85 is arranged. In such a distillation apparatus, the heat transfer area A of the first heat exchanger 85 is
2 [m ² ] is A2 = Q1 / (Δtav · U) = 2,200,000 / (40.5 × 200) ≈272 [m ² ].

However, since the first heat exchanger 85 can be placed separately from the combined distillation column 10, the column body Tw and the packing can be lightened.

Next, the gas-liquid balance in the column of the distillation apparatus according to the seventh embodiment of the present invention will be described. In addition, about the same content as the column gas-liquid balance of the distillation apparatus in the first embodiment, the description thereof will be omitted by describing each variable in the figure.

FIG. 15 is a diagram showing the gas-liquid amount balance in the column of the distillation apparatus according to the seventh embodiment of the present invention.

As described above, while the process temperature T1 in the enrichment section AR3 is 75 [° C.],
Process temperature T2 in the heat exchange section ZN1 of the
[° C.] and 105 between the process temperatures T1 and T2.
There is a temperature difference of [° C]. Therefore, the energy of the liquid of 180 [° C.] taken out through the liquid outlet 47 is used to preheat the stock solution M of 60 [° C.] to 150 [° C.] by the third heat exchanger 86. ing. Along with this, the liquid of 180 [° C] becomes 148.5 [° C].

In this case, when the quantity of heat that the stock solution M acquires from the liquid in the third heat exchanger 86 is Q4 and the liquid specific heat cp of the stock solution M is 0.6 [kcal / kg.degree. C.], the supply rate of the stock solution is Is 14,000 [kg / h], the heat quantity Q4 is Q4 = 14,000 × (150-60) × 0.6 = 756,000 [kcal / h]. When the amount of heat that the liquid gives to the stock solution M is Q4 ', the amount of heat Q4' is: Q4 '= 40,000 x (180-148.5) x 0.6 = 756,000 [kcal / h] Has an inlet temperature of 180 ° C, an outlet temperature of 148.5 ° C, and an inlet temperature of the stock solution M of 60 ° C.
[° C.] and the outlet temperature is 150 [° C.], so the logarithmic average temperature difference δtam δtam = 54.1 [° C.] based on the inlet side temperature difference and the outlet side temperature difference in the third heat exchanger 86. Can be calculated. Therefore, the heat transfer area A4 of the third heat exchanger 86 is: A4 = Q4 / δtam · U = 756,000 / 54.1 · 200 ≈70 [m ² ] And in the third heat exchanger 86, Since the temperature of the liquid cannot be lowered sufficiently, the second heat exchanger 8
It is necessary to lower it further in 3. That is, the second,
In the third heat exchangers 83 and 86, the heat quantity Q3 of the difference between the heat quantities Q1 and Q2, that is, 1,496,500 [kca
1 / h], the second heat exchanger 8
When the amount of heat released in 3 is Q5, the amount of heat Q5
Becomes Q5 = 1,496,500−756,000 = 740,500 [kcal / h].

In this case, the heat transfer area A5 required in the second heat exchanger 83 is A5 = Q5 / (δtav · U) = 740,500 / 97.7 · 200≅38 [m ² ]. .

In this way, when the third heat exchanger 86 is not provided, the heat transfer area A3 of the second heat exchanger 83 is 67.
On the other hand, when the third heat exchanger 86 is provided, the heat transfer area A5 of the second heat exchanger 83 is 38 [m ² ].
[M ^2] a is, the heat transfer area A4 of the third heat exchanger 86 is a 70 [m ^2], a second, a third heat exchanger 83,8
The total heat transfer area ΣA of 6 becomes 108 [m ² ] and the heat transfer area increases by 41 [m ² ].

However, by preheating the stock solution M, the heat quantity Q4, that is, 756,000 [kcal / h]
The energy consumption can be reduced by 34% in terms of the energy ratio. For example, about 1 year of heating steam is required to heat the steam in the evaporator 82.
It can be reduced by 1,000 [ton].

Also, the amount of cooling water required in the distillation apparatus can be reduced. That is, in the case of the conventional distillation apparatus, if the cooling water amount required in the condenser 81 is CW1, the cooling water amount CW1 is the liquid specific heat c of the cooling water.
When the p 1.0 [kcal / kg · ° C.], the CW1 = 2,200,000 / (37-32) · 1.0 = 440 [m ³ / h].

On the other hand, in the case of the distillation apparatus of the seventh embodiment, the amount of cooling water required in the first heat exchanger 85 is CW2, and the amount of cooling water required in the second heat exchanger 83 is Let CW5 be the cooling water amount CW2, CW
CW2 = 703,500 / (37−32) · 1.0 ≈141 [m ³ / h] CW5 = 740,500 / (37−32) · 1.0 ≈148 [m ³ / h] Become. Therefore, the first and second heat exchangers 83, 83
The total cooling water amount ΣCW is ΣCW = CW2 + CW5 = 289 [m ³ / h], and the difference between the cooling water amounts CW1 and ΣCW, that is, the cooling water amount difference ΔCW ΔCW = 440-289 = 151 [m ³ / h] Cooling water can be reduced.

In the distillation apparatus of each of the above embodiments, hydrocarbons, halogenated hydrocarbons, alcohols, ketones, ethers, acetals, esters, fatty acids, phenols, nitrogen compounds are used. , Organic compounds such as heterocyclic compounds and fragrances can be separated by distillation. Then, as the hydrocarbons, benzene, toluene, xylene, biphenyl, naphthalene, etc. are separated, as the halogenated hydrocarbons, methyl chloride, methylene chloride, carbon tetrachloride, etc. are separated, and as the alcohols, methanol is used. , Ethanol, propanol, butanol, heptanol, octanol, etc. are separated, as ketones, acetone, methyl ethyl ketone, methyl isobutyl ketone, etc. are separated, and as ethers, isopropyl ether, butyl ether, benzyl ether, etc. are separated, and acetal As a kind,
Dioxane, furfural, hydrofuran, etc. are separated, as esters, ethyl acetate, butyl acetate, methyl acetate, butyl acrylate, etc. are separated, and as fatty acids, acetic acid, butyric acid, fatty acids, higher alcohols, etc. are separated. As phenols, phenol, cresol, xylenol, etc. are separated, as nitrogen compounds, dimethylamine, triethylamine, aniline, pyridine, picoline, quinoline, etc. are separated, and as heterocyclic compounds, sulfolane, etc. are separated. As the fragrance, it is possible to separate methyl anthranilate, methyl benzoate, isoeugenol, ethyl caproate, eugenol, graniol and the like.

In addition to acidic solutions containing precious metals, non-precious metals, etc., solutions containing inorganic compounds, etc., nuclear technology,
It is also possible to separate organic compounds such as gas and solution used in petroleum refining technology. Then, as the acidic solution containing noble metals, gold, silver, etc. are separated, as the acidic solution containing non-noble metals, nickel, copper, etc. are separated, and as the solution containing an inorganic compound, water, sodium hydroxide, etc. , Salt, etc. can be separated.

The present invention is not limited to the above-mentioned embodiments, but can be variously modified within the scope of the present invention, and they are not excluded from the scope of the present invention.

[0142]

As described in detail above, according to the present invention, in the distillation apparatus, the tower main body and the inside of the tower main body are divided, and the first chamber and the second chamber are formed adjacent to each other. A first distilling section having a middle partition, a concentrating section formed above the feed nozzle and supplied with a stock solution through the feed nozzle, and a collecting section formed below the feed nozzle; A concentration part formed above the upper end of the first distillation part and a recovery part formed below the upper end and adjacent to the concentration part of the first distillation part via a partition. A second distillation section having a section,
A concentrating unit that is connected to the lower end of the first distillation unit, is formed above the lower end, and is adjacent to the recovery unit of the first distillation unit via a partition, and is formed below the lower end. The third distillation section having a recovery section and the liquid condensed in the second distillation section are taken out through the liquid take-out port, cooled, and then returned into the column main body through the liquid return port. And a cooling device for refluxing to the concentrating section.

In this case, not only can the heat exchanger of the cooling device and the combined distiller be placed separately, but it is not necessary to dispose a condenser at the top of the column.

Therefore, since the column main body and the packing can be lightened, the support of the combined distillation column can be stabilized, and the plate thickness of the reinforcing body for preventing the combined distillation column from tipping over can be increased. Can be made smaller. Further, since the moment applied to the foundation of the combined distillation column can be reduced, the foundation work can be simplified.

Further, since the condenser is not provided at the top of the tower and the liquid is cooled to a predetermined temperature in the cooling device, the temperature of the liquid returned to the inside of the tower body and the reflux of the liquid refluxed inside the tower body. The temperature of the liquid can be set freely.

Further, since the reflux by the supercooled reflux liquid becomes possible, the rectification effect can be improved.

In addition, usually, when the composition of the stock solution changes,
The composition of the distillate is adjusted by increasing or decreasing the reflux ratio of the distillate at the top of the column or by increasing or decreasing the heating amount in the evaporator. By adjusting the temperature, the composition of the distillate can be easily adjusted according to the change in the composition of the stock solution M. Therefore, the rectification effect can be improved and the purity of the distillate can be increased.

In another distillation apparatus of the present invention, further, the liquid in the second distillation section is taken out from the inside of the tower body through the liquid take-out port, cooled, and then inside the tower body through the liquid return port. It has a heat exchange device for returning to.

In this case, the liquid in the second distillation section was taken out from the inside of the tower main body through the liquid take-out port, cooled, and then returned to the inside of the tower main body through the liquid return port and returned. Since the liquid is refluxed as the reflux liquid to the concentration parts of the first and third distillation parts, the reflux liquid refluxed in the combined distillation column at the top of the column is refluxed to the concentration part of the second distillation part. It only needs to be enough. That is, the amount of the reflux liquid refluxed to the concentrating section of the second distillation section at the top of the column can be reduced by the amount of the returned liquid, so that the inside of the column main body in the concentrating section of the second distillation section can be reduced. The amount of liquid moving downward can be reduced.

Further, the amount of vapor moving upward in the column main body in the concentrating section of the second distillation section can be reduced by the amount that the vapor is condensed below the concentrating section of the second distillation section. it can. As a result, it is possible not only to reduce the column diameter of the combined distillation column while also maintaining the rectification effect in the column main body, but also to reduce the size of the cooling device. You can Further, since the load on the top of the combined distillation column can be reduced, it is possible to stabilize the support of the combined distillation column.

Further, it is possible to reduce the amount of liquid droplets floating in the tower body, and to reduce extra process system hold-up in the collector, the distributor and the like. Therefore, the total filling capacity of the combined distillation column can be reduced, and the distillation apparatus can be further downsized.

Usually, if the composition of the stock solution changes,
The composition of the side cut liquid is adjusted by increasing or decreasing the reflux ratio of the reflux liquid at the top of the tower, or by increasing or decreasing the heating amount in the evaporator, but the temperature of the liquid returned to the inside of the tower is adjusted. By doing so, it is possible to easily adjust the composition of the side cut solution in response to the fluctuation of the composition of the stock solution. Therefore, the rectification effect can be improved, and the purity of the side cut liquid can be increased.

In still another distillation apparatus of the present invention, further, in the cooling apparatus, the liquid is supercooled to a temperature lower than the boiling point.

In this case, since the liquid is supercooled to a temperature lower than the boiling point in the cooling device, the amount of the liquid moving downward in the concentration section of the second distillation section increases,
The rectification effect is improved.

In the vacuum distillation process,
By the negative pressure generated by the vacuum generator,
The vent gas generated in the combined distillation column is sucked and discharged into the atmosphere. However, if the process fluid is mixed in the vent gas, the performance of the vacuum generator is disturbed.

However, since the temperature of the reflux liquid can be freely set by the cooling device, the temperature of the exhaust gas can be adjusted and the composition of the exhaust gas can be adjusted. Therefore, the vacuum generator can be operated under stable and operating conditions adapted to the process.

[Brief description of drawings]

FIG. 1 is a conceptual diagram of a distillation apparatus according to a first embodiment of the present invention.

FIG. 2 is a conceptual diagram of a conventional distillation apparatus.

FIG. 3 is a conceptual diagram of a combined distillation column according to the first embodiment of the present invention.

FIG. 4 is a conceptual diagram of a distillation apparatus according to a second embodiment of the present invention.

FIG. 5 is a conceptual diagram of a distillation apparatus according to a third embodiment of the present invention.

FIG. 6 is a conceptual diagram showing a main part of a distillation apparatus according to a fourth embodiment of the present invention.

FIG. 7 is a conceptual diagram showing a main part of a distillation apparatus according to a fifth embodiment of the present invention.

FIG. 8 is a conceptual diagram of a distillation apparatus according to a sixth embodiment of the present invention.

FIG. 9 is a conceptual diagram of a distillation apparatus according to a seventh embodiment of the present invention.

FIG. 10 is a conceptual diagram of a distillation apparatus according to an eighth embodiment of the present invention.

FIG. 11 is a conceptual diagram of a distillation apparatus according to a ninth embodiment of the present invention.

FIG. 12 is a conceptual diagram of a distillation apparatus according to a tenth embodiment of the present invention.

FIG. 13 is a view showing a gas-liquid amount balance in a column of a conventional distillation apparatus.

FIG. 14 is a diagram showing a gas-liquid amount balance in a column of the distillation apparatus according to the first embodiment of the present invention.

FIG. 15 is a diagram showing a gas-liquid amount balance in a column of a distillation apparatus according to a seventh embodiment of the present invention.

[Explanation of symbols]

10 Combined-type distillation towers 14A-16A 1st chamber 14B-16B 2nd chamber 22 Partition 25-27 1st-3rd distillation part 41 Feed nozzle 47 Liquid extraction port 48 Liquid return port 71 Distilled liquid extraction port 72 Reflux Liquid inlet 73 Liquid return port 82 Evaporators 85, 83, 86, 87 First to fourth heat exchangers AR1, AR3, AR5 Concentrating sections AR2, AR4, AR6 Recovery sections L71 to L73, L102 to L105, L117, L1
21-L124 Line M Undiluted solution p1, p11 Pump Tw Tower body ZN11, ZN1 First and second heat exchange parts

   ─────────────────────────────────────────────────── ─── Continued front page    (72) Inventor Toru Fukumasa             2-1-1 Yatocho, Nishi-Tokyo, Tokyo             Inside the Tanashi Works of Tomo Heavy Industries F term (reference) 4D076 AA23 AA24 BB04 BB05 BB23                       BB30 DA35 DA37 JA04

Claims (7)

[Claims] 1. A (a) tower main body, (b) a partition that divides the inside of the tower main body and adjoins each other to form a first chamber and a second chamber, and (c) a stock solution via a feed nozzle. Is supplied, the concentrating portion formed above the feed nozzle,
And a first distillation section having a recovery section formed below the feed nozzle, (d) a concentration section connected to the upper end of the first distillation section and formed above the upper end, and A second part having a collecting part formed below the upper end and adjacent to the concentrating part of the first distilling part through a partition.
And (e) a concentrating unit that is connected to the lower end of the first distillation unit, is formed above the lower end, and is adjacent to the recovery unit of the first distillation unit via a partition, And a third distillation section having a recovery section formed below the lower end, and (f) the liquid condensed in the second distillation section is taken out through a liquid take-out port and cooled, A distillation device comprising: a cooling device that returns the liquid to the inside of the tower body through a liquid return port and recirculates it to the concentration part. 2. The heat exchanging device for removing the liquid in the second distillation section from the inside of the tower body through the liquid outlet, cooling it, and returning it to the inside of the tower body through the liquid return port. The distillation apparatus according to 1. 3. The distillation apparatus according to claim 1, wherein a heat exchange section is formed between the liquid return port and the liquid extraction port in the tower body. 4. The distillation apparatus according to claim 1, wherein a packing material is filled in the concentrating section, the collecting section and the heat exchanging section. 5. The distillation apparatus according to claim 1, wherein the concentration section, the recovery section and the heat exchange section have a tray structure. 6. The distillation apparatus according to claim 1, wherein in the cooling device, the liquid is subcooled to a temperature lower than the boiling point. 7. A tower main body, a partition that divides the inside of the tower main body and adjoins each other to form a first chamber and a second chamber, and a stock solution is supplied through a feed nozzle and is formed above the feed nozzle. A first distillation section having a concentrated concentration section and a recovery section formed below the feed nozzle, a concentration section connected to the upper end of the first distillation section and formed above the upper end, and A second distillation section formed below the upper end and having a recovery section adjacent to the concentration section of the first distillation section via a partition, and connected to the lower end of the first distillation section A third distillation section including a concentration section formed above the lower end and adjacent to the recovery section of the first distillation section via a partition, and a recovery section formed below the lower end In the distillation method of a distillation apparatus comprising: The liquid that is condensed in part, taken out through the liquid outlet, after cooling, distillation method is returned to the tower body through the liquid return port, characterized by refluxing in concentrated portion.