JP2001334101A - Distillation apparatus and distillation method using the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To separate an original liquid into four or more fractions and enrich the purity of each fraction by using only one distillation column. SOLUTION: This distillation apparatus has a distillation column main body 30, the first internal partition wall 31, the second internal partition wall 32, the third internal partition wall 33 which is formed at the prescribed part of the first distillation region 30A partitioned by the partition walls 31 and 32 and formed together with the second distillation region 30B, the first distillation part 25 formed along the third internal partition wall 33, the second distillation part 26 formed adjacently to the column top, the third distillation part 27 formed adjacently to the column bottom and the fourth distillation part 28 formed in the region 30B by making the part communicate with region 30A through an opening. Since the region 30A is divided by the partition wall 33, each fraction can be separated from other fractions without using a plurality of distillation columns.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] The present invention relates to a distillation apparatus and a distillation method using the same.

[0002]

2. Description of the Related Art Conventionally, the following distillation apparatus has been known as a distillation apparatus for distilling a stock solution containing four or more components to separate each component (fraction).

FIG. 2 is a conceptual diagram of a conventional distillation apparatus having three distillation columns.

In the figure, reference numeral 101 denotes a first distillation column, 10
2 is a second distillation column, 103 is a third distillation column, 201, 2
03 and 205 are evaporators, and 202, 204 and 206 are condensers. For example, when distilling a stock solution containing four components A to D having a large relative specific volatility in the order of components A to D,
In the first distillation column 101, the component A and the components BD are separated, and the liquid rich in the component A is separated from the first distillation column 101.
Discharged from the top of the
And the components C and D are separated from each other, and the liquid rich in the component B is discharged from the top of the second distillation column 102, and the third distillation column 1
In step 03, component C and component D are separated, and a liquid rich in component C is discharged from the top of the third distillation column 103, and a liquid rich in component D is discharged from the bottom of the third distillation column 103, respectively. Like that.

[0005] However, in the distillation apparatus, the first
Since it is necessary to repeat heating and cooling in the first to third distillation columns 101 to 103, each of the first to third distillation columns 101 to 103
In addition to the necessity of the evaporators 201, 203, 205 and the condensers 202, 204, 206, pumps and instrumentation (not shown) are required, which increases the cost of the distillation apparatus and increases the utility. The amount of used and the energy consumption increase.

Therefore, there is provided a distillation apparatus which separates the stock solution into components A to D using only one distillation column.

FIG. 3 is a conceptual diagram showing a first example of a conventional distillation apparatus having one distillation column.

In the figure, 111 is a distillation column, 211 is an evaporator, and 212 is a condenser. Inside the column main body 111a of the distillation column 111, one partition 112 is disposed, and each of the enrichment sections AR11, AR13, AR16, and the recovery sections AR12, AR filled with a filling material.
14, AR17 and an intermediate distillation section AR15 are formed;
The first distillation section is formed by the concentrating section AR11 and the collecting section AR12, and the second distillation section is formed by the concentrating section AR13 and the collecting section AR14.
, A third distillation section is formed by the concentration section AR16 and the recovery section AR17. The intermediate distillation section A
R15 is formed to separate component B and component C.

A stock solution containing the four components A to D is supplied via line 311 between the concentrating unit AR11 and the collecting unit AR12. The liquid rich in the component A is supplied to the line 312 via the condenser 212 from the top of the column, and the liquid rich in the component B is supplied to the line 313 from the column side between the recovery part AR14 and the middle distillation part AR15. The liquid rich in C is
The liquid rich in component D is discharged from the side of the column between the middle distillation section AR15 and the concentration section AR16 to the line 314, and the liquid rich in the component D is discharged to the line 315 from the bottom of the column (Kaibel “Chemic”).
al Engineering Technology
y ", Volume 10, p. 92-98, 1987).

FIG. 4 is a conceptual diagram showing a second example of a conventional distillation apparatus having one distillation column.

In the drawing, reference numeral 121 denotes a distillation column, 221 denotes an evaporator, and 222 denotes a condenser. In the column main body 121a of the distillation column 121, three intermediate partitions 122 to 124 are provided. The middle partition 122 is provided on the feed nozzle side, and the middle partitions 123 and 124 are provided on the side cut nozzle side. In the tower main body 121a, the enrichment sections AR21, AR23, AR25, A
R27, AR31, collection units AR22, AR24, AR2
6, AR28, AR32 and middle distillation section AR29, AR
30 is formed, and the first distillation unit is formed by the concentrating unit AR21 and the collecting unit AR22, and the concentrating unit AR23 and the collecting unit AR
24, the third distillation section by the concentration section AR25 and the recovery section AR26, the fourth distillation section by the concentration section AR27 and the recovery section AR28, and the concentration section AR
A fifth distillation section is formed by the 31 and the recovery section AR32. The intermediate distillation units AR29 and AR30 are composed of the component B
And component C are formed.

A stock solution containing four components A to D is supplied between a concentration section AR21 and a recovery section AR22 via a line 321, and a liquid rich in the component A is supplied from the top of the condenser 22 to the condenser 22.
2 through line 322, component B-rich liquid from column side between recovery section AR28 and middle distillation section AR29 to line 323, and component C-rich liquid into middle distillation section AR.
Line 32 from the side of the tower between 30 and the enrichment section AR31
4, the liquid enriched in component D is discharged from the bottom to line 325 (Sargent et al., "Optimum De
sign of Plate Distillatio
n Columns "p. 267-314, published by Academic Press in 1976).

FIG. 5 is a conceptual diagram showing a third example of a conventional distillation apparatus having one distillation column.

In the figure, 131 is a distillation column, 231 is an evaporator, and 232 is a condenser. Inside the column body 131a of the distillation column 131, two intermediate partitions 132, 133 are provided. The middle partition 132 is provided on the feed nozzle side, and the middle partition 133 is provided on the side cut nozzle side. Also,
In the tower main body 131a, the enrichment sections AR41, AR43, AR45, AR47, A
R49 and recovery units AR42, AR44, AR46, AR
48, AR50 are formed, the first distillation section is constituted by the concentration section AR41 and the collection section AR42, the second distillation section is constituted by the concentration section AR43 and the collection section AR44, and the concentration section AR4 is formed.
5 and the recovery unit AR46 to form a third distillation unit, and the enrichment unit AR47 and the recovery unit AR48 to form a fourth distillation unit.
The enrichment section AR49 and the recovery section AR50 form a fifth distillation section.

A stock solution containing four components A to D is supplied via line 331 between the concentration section AR41 and the recovery section AR42, and the liquid rich in component A is supplied from the top of the condenser 23 to the condenser 23.
2 through line 332, the liquid rich in component B from the column side between the concentrating section AR43 and the collecting section AR44 to the line 333, and the liquid rich in component C between the concentrating section AR45 and the collecting section AR46. From the side of the column to the line 334, and the liquid rich in the component D is discharged from the bottom of the column to the line 335 (Agrawal "Industrial &Engi").
nearing Chemistry Research
h ", Vol. 35, No. 4, p. 1059-1071, published in 1996).

[0016]

However, in each of the above distillation apparatuses, liquids rich in components B and C, which are intermediate components, are both discharged from the column side. When a liquid that cannot be sufficiently separated and is rich in components B and C is used as a product, the purity of the product is low.

The present invention solves the above-mentioned problems of the conventional distillation apparatus, and can separate a stock solution into four or more components using only one distillation column, thereby increasing the purity of each product. It is an object of the present invention to provide a distillation apparatus and a distillation method using the same.

[0018]

For this purpose, in the distillation apparatus of the present invention, a column main body and a first partition formed in the column main body so as to extend vertically from the top to the center of the column. And a second space formed by extending vertically from the bottom of the tower to the center of the tower in the tower body, and having a gap between the lower end of the first partition. A partition formed by extending vertically in a predetermined portion of the first distillation region among the first and second distillation regions defined by the first and second intermediate partitions. 3, a first distillation section formed along the third partition, a second distillation section formed at least partly adjacent to the top of the column, and at least partly a column. A third distillation section formed adjacent to the bottom and the second distillation area through the gap to the second distillation section; It is communicated to the distillation zone and communicates with a fourth distillation section formed.

In another distillation apparatus of the present invention, a feed nozzle for supplying a stock solution facing the first distillation section is provided on the side of the tower body.
The first discharge means for distillate is provided at the top of the distillation section in the first distillation area, and the first discharge means for bottoms is provided at the bottom of the first distillation area.
A discharge means for distillate at the top of the second distillation area and a second discharge means for bottoms at the bottom of the second distillation area. You.

In still another distillation apparatus of the present invention, a first supply means for reflux liquid is provided at the top of the first distillation section, and a first supply means for the reflux liquid is provided at a bottom of the first distillation section. A first supply means for the vapor from the evaporator is provided at the top of the second distillation zone,
A second means for supplying steam from the second evaporator is formed at the bottom of the second distillation zone.

In still another distillation apparatus of the present invention, the enrichment section is located above the feed nozzle in the first distillation section, and the recovery section is located below the feed nozzle in the first distillation section. A concentrating section adjacent to the top of the second distillation section,
A collecting unit adjacent to the first distillation unit in the third distillation unit, a concentrating unit adjacent to the first distillation unit in the third distillation unit, and a collecting unit adjacent to the bottom of the third distillation unit in the third distillation unit. A concentration section is formed above the gap in the fourth distillation section, and a recovery section is formed below the gap in the fourth distillation section.

In still another distillation apparatus according to the present invention, each of the cross-sectional areas of the first chamber and the second chamber defined by the third partition in the first distillation area, and the second distillation The positions of the first to third partitions are set such that the sectional area of the region corresponds to the flow rate of steam.

The distillation method using the distillation apparatus according to the present invention comprises the steps of: a column main body; a first partition formed in the column main body so as to extend vertically from the top to the center of the column; Extending vertically from the bottom to the center of the tower, and
A second partition formed with a gap between the first partition and a lower end of the first partition; and a first and a second distillation region defined by the first and second partitions. A third partition formed in a predetermined portion of the first distillation region and extending in the vertical direction, a first distillation section formed along the third partition, and at least a part of the column. A second distillation section formed adjacent to the top, a third distillation section formed at least partially adjacent to the column bottom, and the second distillation section through the gap to the first distillation section; The present invention is applied to a distillation apparatus having a fourth distillation section formed in communication with the distillation region of (1).

Then, a stock solution is supplied to the first distillation section, a first distillate is discharged from the top in the first distillation section, and a first distillate is discharged from the bottom in the first distillation section. The bottoms are discharged, the second distillate is discharged from the top in the second distillation zone, and the second bottoms is discharged from the bottom in the second distillation zone.

In the distillation method using another distillation apparatus according to the present invention, the stock solution may further comprise a mixture of the first to fourth components in descending order of relative specific volatility. The rich liquid is discharged as a first distillate and the second component-rich liquid is discharged as a second distillate;
The liquid rich in the third component is discharged as a second bottoms, and the liquid rich in the fourth component is discharged as a first bottoms.

In the distillation method using still another distillation apparatus according to the present invention, a part of the first distillate is further refluxed to a second distillation section as a reflux liquid, and the second distillate is further refluxed. Part of the liquid is refluxed to the fourth distillation section as a reflux liquid,
A part of the bottoms is vaporized and collected in the third distillation section, and a part of the second bottoms is vaporized and collected in the fourth distillation section.

[0027]

Embodiments of the present invention will be described below in detail with reference to the drawings.

In this case, a distillation apparatus having one distillation column 10 and a distillation method using the same will be described. In the distillation apparatus, the stock solution M supplied to the distillation column 10
Consists of a mixed solution containing components A to D as first to fourth components (fractions), and has a lower boiling point in the order of components A to D,
Large relative volatility. Distillation is performed in the distillation apparatus, and the components A to D are separated.

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

In the drawing, reference numeral 10 denotes a distillation column, and a plate-shaped first partition is provided in a column main body 30 of the distillation column 10 so as to extend vertically from the top to a predetermined position in the center of the column. 31 extends vertically from the bottom of the tower to a predetermined position in the center of the tower to form a second partition 32 in the form of a flat plate. The first and second partitions 31 and 32 form the tower body 30. The inside is partitioned and the first and second extending in the vertical direction
Of the distillation regions 30A and 30B are defined. The first
A predetermined gap is formed between the lower end of the partition 31 and the upper end of the second partition 32, and the gap allows communication between the first and second distillation regions 30A and 30B.

In the first distillation zone 30A, a first section 11 and a second section 1 are sequentially arranged from the top to the bottom.
2, third section 13, fourth section 14, fifth section 15, sixth section 16, seventh section 1
7, the eighth section 18 and the ninth section 19 are formed, and in the second distillation zone 30B, the tenth section 20, the eleventh section 21, the twelfth section 22, the thirteenth section 23 and 14th
Section 24 is formed. The first section 11 and the tenth section 20 are connected to the upper half of the second section 12, the third section 13 and the fourth section 14, and the eleventh section 21 via the first partition 31. However, the lower half of the fourth section 14 and the upper part of the twelfth section 22 are adjacent to each other, and the upper half of the sixth section 16 and the twelfth section 22 are connected via the second partition 32. The lower portion is adjacent to the lower half of the sixth section 16, the seventh section 17, the eighth section 18, and the thirteenth section 23, and the ninth section 19 and the fourteenth section 24 are adjacent to each other. The fifth section 15 and the twelfth section 22
Is communicated with the central portion of the vehicle through the gap.

A predetermined portion in the first distillation region 30A, in the present embodiment, the fourth section 1
A third partition 33 having a flat plate shape is vertically extended over the fourth, fifth and sixth sections 15 and 16, and the fourth partition 14, the fifth section 15, and the third partition 33 are extended by the third partition 33. Sixth Section 16
Are partitioned into first chambers 14A to 16A and second chambers 14B to 16B. The first chambers 14A to 16A and the second chamber 14B
-16B are adjacent to each other.

The cross-sectional area of the first chambers 14A to 16A is S1
And the sectional area of the second chambers 14B to 16B is S2,
When the sectional area of the second distillation region 30B is S3,
Steam flowing through the first chambers 14A to 16A, the second chambers 14B to 1
The positions of the first to third partitions 31 to 33 are set such that the cross-sectional areas S1 to S3 correspond to the respective flow rates of the steam flowing through the 6B and the steam flowing through the second distillation region 30B.

A first distillation section 25 is formed along the third partition 33 by the first chambers 14A to 16A, and the first section 11 and the second section 1 are formed.
2, the second by the third section 13 and the second chamber 14B
Is formed at least partially adjacent to the top of the column, and the second chambers 15B, 16B, the seventh section 1
The seventh, eighth and ninth sections 18 and 19 form a third distillation section 27 at least partially adjacent to the bottom of the column, the tenth section 20, the eleventh section 21, the twelfth section 22, The 13th section 23 and the 14th section 24 make the fourth distillation section 2
8 are formed in communication with the first distillation area 30A via the gap.

The first to third partitions 31 to 3
3 is made to have a heat insulating structure by being formed of a heat insulating material or by evacuating the inside. Therefore,
Since heat transfer via the first to third intermediate partitions 31 to 33 can be reduced, the efficiency of distillation can be increased.

A feed nozzle 41 is formed on the column side of the first distillation area 30A so as to face the first distillation section 25 and communicate with the first chamber 15A. At the top of 30A, a first vapor outlet 42 as a first discharge means for distillate and a first supply means as a first supply means for reflux liquid are communicated with the first section 11. A reflux liquid inlet 43 is formed.
A first bottoms outlet 44 as a first discharge means for bottoms and a first bottoms evaporator (not shown) connected to the ninth section 19 at the bottom of the distillation zone 30A. First steam inlet 4 as first steam supply means
5, the first steam outlet 42 and the first reflux liquid inlet 43 are connected to a first condenser (not shown), and the first bottoms outlet 44 and the first steam inlet 45 are connected to the first condenser. Connected to the evaporator.

Further, a second vapor outlet 46 as a second discharge means for distillate and a second vapor outlet 46 for reflux liquid are connected to the top of the second distillation zone 30B in communication with the tenth section 20. A second reflux liquid inlet 47 is formed as a second supply means, and is connected to the fourteenth section 24 at the bottom of the second distillation zone 30B, and a second discharge means for bottoms is provided. And a second steam inlet 49 as a second supply means of the steam of the second evaporator (not shown), and the second steam outlet 46 and the second steam outlet 49 are formed. The reflux liquid inlet 47 is connected to a second condenser (not shown), and the second bottoms outlet 48 and the second vapor inlet 49 are connected to the second evaporator.

In the first distillation section 25, the enrichment section AR1 is recovered in the first chamber 14A disposed above the feed nozzle 41, and is recovered in the first chamber 16A disposed below the feed nozzle 41. The portions AR2 are respectively formed. In the second distillation section 26, the first
The enrichment section AR3 is adjacent to the second section 12 disposed above the upper end of the distillation section 25 via the top section and the first section 11 below the upper end of the first distillation section 25, The collection unit AR is provided in the second chamber 14B disposed adjacent to the enrichment unit AR1 via the third partition 33.
4 are formed respectively. Further, the third distillation section 2
7, above the lower end of the first distillation section 25, the enrichment section AR5 is placed in the second chamber 16B adjacent to the recovery section AR2 via the third partition 33.
However, recovery sections AR6 are formed adjacent to the eighth section 18 disposed below the lower end of the first distillation section 25 via the ninth section 19 with the column bottom.

Then, in the fourth distillation section 28, above the gap, that is, in the enrichment section AR3,
The enrichment section AR7 is located below the gap in the eleventh section 21, which is disposed adjacent to the upper half of the third section 13 and the recovery section AR4 via the first partition 31, that is, of the enrichment section AR5. The collecting part AR8 is formed in the lower half part, the seventh section 17, and the thirteenth section 23 disposed adjacent to the collecting part AR6 via the second intermediate partition 32. The enrichment sections AR1, AR3, AR5,
AR7 and the recovery units AR2, AR4, AR6, AR8 are filled with a filler composed of one node. In addition, depending on the relative specific volatility between the components to be distilled, in order to secure the number of theoretical plates required for distillation, a filler composed of a plurality of nodes is filled according to the characteristics of the filler used. You can also. In addition, a distributor can be provided between nodes.

The concentration section A in the first section 11
A distributor 61 for distributing the reflux liquid supplied via the first reflux liquid inlet 43 is provided directly above the concentration section AR1 in the third section 13 and a concentration section A directly above the concentration section AR1 in the third section 13.
The distributor 63 that distributes a part of the liquid flowing down from R3, that is, a part of the liquid flowing down, is provided in the third section 13
A distributor 64 that distributes a part of the liquid flowing down from the concentrating unit AR3 directly above the collecting unit AR4 in the fifth section 15 directly above the collecting unit AR2 in the fifth section 15.
Distributor 6 for distributing a mixture of the flowing liquid from 1 and the stock solution M supplied via the feed nozzle 41
7, a distributor 68 for distributing the effluent from the recovery section AR4 immediately above the enrichment section AR5 in the fifth section 15, and a recovery section AR6 in the seventh section 17
The liquid flowing down from the recovery part AR2 and the concentration part AR5 immediately above
7 that distributes the mixture of the flowing liquid from the container
A distributor 72 for distributing the reflux liquid supplied via the second reflux liquid inlet 47 directly above the concentrating section AR7 in the tenth section 20 includes a concentrating section AR7 directly above the collecting section AR8 in the twelfth section 22. A distributor 74 for distributing the liquid flowing down from is provided.

The collector 62 for collecting the liquid flowing down from the enrichment section AR3 is provided immediately below the enrichment section AR3 in the third section 13 and the enrichment section AR in the fifth section 15.
A collector 65 that collects the liquid flowing down from the concentrating unit AR1 directly below the collector 1 and a collector 6 that collects the liquid flowing down from the collecting unit AR4 directly below the collecting unit AR4 in the fifth section 15.
6 is a collector 69 for collecting the liquid flowing down from the collecting section AR2 directly below the collecting section AR2 in the seventh section 17.
However, a collector 70 that collects the flow-down liquid from the enrichment section AR5 immediately below the enrichment section AR5 in the seventh section 17,
Immediately below the concentration section AR7 in the twelfth section 22, a collector 73 for collecting the liquid flowing down from the concentration section AR7 is provided.

The distributors 61, 6
3, 64, 67, 68, 71, 72, 74 and collectors 62, 65, 66, 69, 70, 73 use various types as long as they correspond to the range of the flow rate of each flowing liquid. can do.

It is necessary to appropriately distribute the flowing liquid collected by the collector 62 to the distributors 63 and 64. The distribution ratio depends on the type and composition of the components of the stock solution M, the filling height of each filler, the product Is set in advance on the basis of distillation conditions such as purity required for the reaction. Further, when it is necessary to supply a part of the flowing liquid collected by the collector 66 to the distributor 74 based on the distillation conditions, or to supply a part of the flowing liquid collected by the collector 73 to the distributor 68. If necessary, the collector 66 side and the collector 73 side are connected by a line 75 as shown by a broken line in the figure. In this case, in order to adjust the flow rate of the flowing liquid, the line 75 may be taken out of the tower main body 30, and a flow meter and a control valve may be provided in a portion of the line 75 outside the tower main body 30.

The undiluted solution M supplied to the distillation column 10 having the above configuration
Comprises a mixture containing components A to D, wherein components A to D
And the relative specific volatility is large. Then, when the stock solution M is supplied to the first distillation section 25 via the feed nozzle 41, distillation is performed in the concentration section AR1 and the recovery section AR2, and the components A and B are separated from the components C and D. . That is, in the concentration section AR1, the components A to A are caused by the flowing liquid distributed by the distributor 63.
The components A and B are separated from D, a vapor rich in components A and B is sent above the concentrating unit AR1, and the components A to D are separated from the components A to D by the flowing liquid distributed by the distributor 67 in the collecting unit AR2. C and D are separated,
A liquid rich in components C and D is sent below the recovery section AR2.

When the steam rich in the components A and B is supplied to the second distillation section 26, the enrichment section AR3 and the recovery section A
In R4, distillation is performed, and component A and component B are separated. That is, in the enrichment section AR3, the component A is separated from the components A and B by the reflux liquid distributed by the distributor 61, and the vapor rich in the component A is sent above the enrichment section AR3. The component B is separated from the components A and B by the flowing liquid distributed by the distributor 64, and the liquid rich in the component B is sent below the recovery part AR4.

The vapor enriched in component A is discharged from a first vapor outlet 42 at the top of the tower to a line (not shown), and then sent to the first condenser, where it is condensed by the first condenser. To become the first distillate. Then, a part of the first distillate is sent to a product supply destination (not shown) as a product, and the remainder of the first distillate is passed through a first reflux liquid inlet 43 as a first reflux liquid. To the first section 11.

On the other hand, when the liquid rich in the components C and D is supplied to the third distillation section 27, the enrichment section AR5 and the recovery section AR
At 6 distillation is carried out to separate component C and component D. That is, in the recovery section AR6, the component D is separated from the components C and D by the flowing liquid distributed by the distributor 71 and the steam supplied through the first steam inlet 45 at the bottom of the tower, and the recovery section AR6 , A component-rich liquid is sent to the lower part, and in the concentrating section AR5, the flowing liquid distributed by the distributor 68 separates the component C from the components C and D. Above the concentrating section AR5, the component-rich liquid Steam is sent.

The liquid rich in component D is discharged as a first bottoms from a first bottoms outlet 44 at the bottom of the column to a line not shown. A part of the first bottoms is sent as a product to the product supply destination, and the remainder of the first bottoms is sent to the first evaporator and evaporated by the first evaporator. After being let go, it is returned to the ninth section 19 via the first steam inlet 45.

In the second chamber 15B, the liquid rich in component B flowing down from the recovery section AR4 and the vapor rich in component C sent upward from the enrichment section AR5 are mixed into the components B and C. Rich vapors are formed and the components B, C
Is supplied to the fourth distillation section 28 through the gap. When the vapors rich in the components B and C are supplied to the fourth distillation section 28, distillation is performed in the enrichment section AR7 and the recovery section AR8, and the components B and C are separated. That is, in the concentrating unit AR7, by the reflux liquid distributed by the distributor 72,
The component B is separated from the components B and C, and a vapor rich in the component B is sent above the concentration section AR7. In the recovery section AR8, the falling liquid distributed by the distributor 74 causes the component C to be converted from the components B and C. Is separated, and a liquid rich in the component C is sent below the recovery section AR8.

The vapor rich in the component B is discharged from a second vapor outlet 46 at the top of the column to a line (not shown), and then sent to the second condenser, where it is condensed by the second condenser. Into a second distillate. Then, a part of the second distillate is sent to the product supply destination as a product, and the remainder of the second distillate is passed through the second reflux liquid inlet 47 as a second reflux liquid. It is returned to the tenth section 20.

The liquid rich in the component C is supplied to the second column at the bottom of the column.
Is discharged as a second bottom liquid from a bottom discharge outlet 48 to a line (not shown). A part of the second bottoms is sent as a product to the product destination, and the rest of the second bottoms is
After being sent to the second evaporator and evaporated by the second evaporator, it is returned to the fourteenth section 24 via the second steam inlet 49.

As described above, the column body 3 of one distillation column 10
In the first and second distillation regions 30A, 3A, a first and a second partition 31, 32 extending in the vertical direction within the first and second distillation regions 30A, 3B.
0B, and the first distillation region 30A is divided into first and second chambers 14A to 16A and 14B to 16A adjacent to each other by a third partition 33 extending in the vertical direction.
B, four components A contained in the stock solution M
~ D can be separated without using multiple distillation columns.

Therefore, the number of necessary evaporators and condensers can be reduced, and the number of pumps and instrumentation (not shown) can be reduced, so that the cost of the distillation apparatus can be reduced. In addition, the usage amount and the energy consumption of the utility can be reduced.

It is not necessary to discharge a liquid rich in intermediate components B and C from the column side.
Can be discharged from the top and bottom of the column, so that the four components A to D can be sufficiently separated, and each component A to
When a liquid rich in D is used as a product, the purity of the product can be increased.

Further, in this embodiment, the four components A to D are separated, but the first distillation region 30A and the second distillation region 30B are separated between the first distillation region 30A and the second distillation region 30B. By having the same structure as 30A, five or more components can be separated.

[0056]

Next, the results of distillation calculation by simulation will be described. There are many cases in which the actual plant operation results match the results of distillation calculations by simulation. In this case, for example, a commercially available process simulator “ASPEN PLUS” (made by ASPEN TEC)
It was used. The abbreviations of the chemical components used here are as follows.

Component A MeOH Methanol Component B EtOH Ethanol Component C PrOH 1-Propanol Component D BuOH 1-Butanol [Example] FIG. 6 is a conceptual diagram of a distillation apparatus used in a simulation according to an embodiment of the present invention. In addition,
Parts having the same structure as in FIG. 1 are given the same reference numerals and description thereof is omitted.

In the figure, reference numeral 81 denotes a line for supplying the undiluted solution M to the feed nozzle 41, reference numeral 78 denotes a line for discharging the vapor rich in the component A, and reference numeral 82 denotes a line for discharging the first distillate. , 83 are a line for refluxing the first reflux liquid, 84 is a line for discharging the first bottom liquid, 85 is a line for recovering vapor rich in component D, and 79 is a line for recovering component B. A line for discharging the rich vapor, 86 a line for discharging the second distillate, 87
Is a line for refluxing the second reflux liquid, 88 is a line for discharging the second bottoms, and 89 is a line for recovering the vapor rich in component C.

The line 78 is provided with a first condenser 9 for condensing the vapor rich in the component A into a first distillate.
3, a line 79 is provided with a second condenser 94 for condensing the component B-rich vapor into a second distillate. A first evaporator 91 for heating the first bottom liquid to generate a vapor rich in component D is provided in the line 85, and a second bottom liquid is provided in the line 89 for heating the first bottom liquid. A second evaporator 92 is provided for heating to generate component C rich vapor.

The theoretical number of plates in the distillation column 10 is such that the enrichment section AR1 has 5 stages, the recovery section AR2 has 5 stages, and the enrichment section A
R3 has 10 stages, recovery section AR4 has 5 stages, and enrichment section A
R5 has 5 stages, recovery section AR6 has 10 stages, and enrichment section A
R7 has 10 stages, and the recovery unit AR8 has 10 stages. Further, continuous distillation was performed on a stock solution M containing four components A to D of methanol MeOH, ethanol EtOH, 1-propanol PrOH and 1-butanol BuOH in equal amounts by weight.

First, a stock solution M at 25 ° C. was added to 1000 [k
g / hr (hour)] to the distillation column 10 through the line 81, a part of the first distillate is 250 kg
/ Hr], and the remainder of the first distillate was returned to the line 83 at a flow rate of 4939 [kg / hr] as a first reflux liquid. A part of the second distillate is discharged to the line 86 at a flow rate of 250 [kg / hr], and the remainder of the second distillate is discharged to the line 87 at a flow rate of 1699 [kg / hr]. Was refluxed. Then, the second bottom liquid is discharged to the line 88 at a flow rate of 250 [kg / hr], and the first bottom liquid is discharged at 250 [kg / h].
r] and was discharged to the line 84.

The effluent from the concentrating unit AR3 was distributed to the concentrating unit AR1 and the collecting unit AR4 at a ratio of 1: 1.08. Further, the heat load of the first evaporator 91 is set to 1,400,000 [kcal / hr], and the heat load of the second evaporator 92 is set to 400,000 [kcal / h].
r].

Table 1 shows the results of distillation by the distillation column 10 shown in FIG. In Table 1, the composition is represented by a single unit of [wt%], and the flow rate is represented by a unit of [kg / hr].

[0064]

[Table 1]

Comparative Example 1 In the distillation apparatus shown in FIG. 2, the number of theoretical plates of the first distillation column 101 was 10
The number of theoretical plates in the second distillation column 102 is 10 in the enrichment unit, the number in the recovery unit is 5, and the number of theoretical plates in the second distillation column 102 is 3.
The number of theoretical plates of the distillation column 103 was 10 in the enrichment section and 10 in the recovery section.

As in the case of the distillation column 10, methanol MeOH,
Ethanol EtOH, 1-propanol PrOH and 1
A stock solution M containing the four components A-D of butanol BuOH in equal amounts by weight was distilled continuously.

First, a stock solution M at 25 ° C. was added at 1000 k
g / hr] to the first distillation column 101,
The liquid rich in component A is the distillate of the first distillation column 101, the liquid rich in component B is the distillate of the second distillation column 102, and the liquid rich in component C is the third distillation column. As the distillate of 103, the liquid rich in component D is the third distillation column 103
Was discharged as bottoms. A part of the liquid rich in the component A is the first liquid at a flow rate of 250 [kg / hr].
Is discharged as a distillate of the distillation column 101, and the remainder of the liquid rich in the component A is transferred to the first distillation column 101 by 1882 [kg /
hr] as a reflux liquid. Component B
A part of the liquid enriched in water is discharged as a distillate of the second distillation column 102 at a flow rate of 250 [kg / hr], and the rest of the liquid enriched in the component B is fed into the second distillation column 102 at 2686 kg
/ Hr], a part of the liquid rich in component C is discharged as a distillate of the third distillation column 103 at a flow rate of 250 [kg / hr], and is rich in component C. The remaining liquid is added to the third distillation column 103 at 3350 [kg / h
r], and the liquid rich in component D was discharged from the third distillation column 103 as a bottom liquid at a flow rate of 250 [kg / hr]. The evaporators 201, 2
03 and 205 were both 600,000 [k
cal / hr].

The first to third distillation columns 101 shown in FIG.
Table 2 shows the results of the distillation by using No. to 103. In Table 2, the composition is expressed in units of [wt%] and the flow rate is expressed in [kg / hr].
Expressed in units of

[0069]

[Table 2]

Comparing the distillation result in Table 1 with the distillation result in Table 2, the sum of the heat load of the first and second evaporators 91 and 92 and the sum of the heat load of the evaporators 201, 203 and 205 are found. In order to make them equal, the number of theoretical plates of the distillation portion used for distillation of each of the components A to D in the distillation column 10 and the number of theoretical plates used for distillation of each of the components A to D in the first to third distillation columns 101 to 103 are determined. Despite the fact that the number of theoretical plates in the distillation section was set to be equal, methanol MeO
H, ethanol EtOH and 1-propanol PrOH
In any case, it is understood that the purity is higher when the distillation apparatus including the distillation column 10 is used than when the distillation apparatus including the first to third distillation columns 101 to 103 is used. Then, in order to equalize the purity of methanol MeOH, ethanol EtOH, 1-propanol PrOH and 1-butanol BuOH, when the distillation apparatus including the distillation column 10 is used, the first to third distillation columns 101 to 103 are used. Energy consumption can be reduced as compared with the case where a distillation apparatus is used. Comparative Example 2 In the distillation apparatus shown in FIG. 3, the number of theoretical plates in the distillation column 111 was 10 in the enrichment section AR11, 10 in the recovery section AR12, 5 in the enrichment section AR13, and 5 in the recovery section AR14. And the middle distillation section AR
15 was set to 10 stages, the enrichment unit AR16 was set to 5 stages, and the recovery unit AR17 was set to 5 stages. Further, similarly to the distillation column 10, four components A of methanol MeOH, ethanol EtOH, 1-propanol PrOH and 1-butanol BuOH were used.
Distillation was continuously performed on the stock solution M containing the same amount of ＤD by weight.

First, a stock solution M at 25 ° C. was added at 1000 k
g / hr] via distillation line 111 via line 311.
To the line 312 as a distillate, a liquid rich in the component B as a sidestream liquid in the line 313, and a liquid rich in the component C as a sidestream liquid in the line 312.
In the line 14, the liquid rich in the component D is supplied to the line 31 as a bottom liquid.
5 respectively. Then, a part of the liquid rich in the component A is discharged as a distillate at a flow rate of 250 [kg / hr], and the remainder of the liquid rich in the component A is 6517 [kg / hr] at the top of the distillation column 111. As a reflux liquid. Further, the liquid rich in the component B is 250 [kg /
hr], a liquid rich in component C is discharged as a sidestream liquid at a flow rate of 250 kg / hr, and a part of the liquid rich in component D is 250 kg / h.
r] as a bottom liquid. The enrichment section A
The effluent of R13 was distributed to the concentrating section AR11 and the collecting section AR14 at a ratio of 1: 13.89. Evaporator 21
1, 800,000 [kcal / hr]
And

Table 3 shows the results of distillation by the distillation column 111 shown in FIG. In Table 3, the composition is expressed in units of [wt%], and the flow rate is expressed in units of [kg / hr].

[0073]

[Table 3]

[Comparative Example 3] In the distillation apparatus shown in FIG.
R23, AR25, AR27, AR31, collection unit AR2
2, AR24, AR26, AR28, AR32 and the middle distillation units AR29, AR30 all have 5 stages. Similar to the distillation column 10, methanol MeOH, ethanol EtO
H, 1-propanol PrOH and 1-butanol Bu
Distillation was continuously performed on the stock solution M containing the four components A to D of OH in equal amounts by weight.

First, a stock solution M at 25 ° C. was added at 1000 k
g / hr] through line 321
, A liquid rich in component A as a distillate in line 322, a liquid rich in component B in line 323 as a sidestream liquid, and a liquid rich in component C as a sidestream liquid in line 3
24, a liquid enriched in component D is discharged as a bottom liquid in line 32;
5 respectively. A part of the liquid rich in the component A is discharged as a distillate at a flow rate of 250 kg / hr, and the remainder of the liquid rich in the component A remains at the top of the distillation column 121 at 6458 kg / hr. As a reflux liquid. Further, the liquid rich in the component B is 250 [kg /
hr], a liquid rich in component C is discharged as a sidestream liquid at a flow rate of 250 kg / hr, and a part of the liquid rich in component D is 250 kg / h.
r] as a bottom liquid. The enrichment section A
The effluent of R27 is distributed to the concentrating section AR23 and the collecting section AR28 at a ratio of 7.838: 1.
The effluent of No. 3 was distributed to the concentration part AR21 and the recovery part AR24 at a ratio of 1: 12.54. The calorific load of the evaporator 221 was set to 1,800,000 [kcal / hr].

Table 4 shows the results of distillation by the distillation column 121 shown in FIG. In Table 4, the composition is expressed in units of [wt%], and the flow rate is expressed in units of [kg / hr].

[0077]

[Table 4]

[Comparative Example 4] In the distillation apparatus shown in FIG.
41 has five stages, the recovery part AR42 has five stages, and the enrichment part A
R43 has 10 stages, the recovery unit AR44 has 5 stages, the enrichment unit AR45 has 5 stages, the recovery unit AR46 has 10 stages,
The enrichment section AR47 was made up of 5 stages, the recovery section AR48 was made up of 5 stages, the enrichment section AR49 was made up of 5 stages, and the collection section AR50 was made up of 5 stages. In the same manner as in the distillation column 10, a stock solution M containing four components A to D of methanol MeOH, ethanol EtOH, 1-propanol PrOH and 1-butanol BuOH was equally distilled by weight, and was continuously distilled.

First, a stock solution M at 25 ° C. was added at 1000 k
g / hr] through the line 331
, A liquid rich in component A as a distillate in line 332, a liquid rich in component B in line 333 as a sidestream liquid, and a liquid rich in component C as a sidestream liquid in line 3.
In line 34, a liquid rich in component D is passed as a bottom liquid to line 33.
5 respectively. A part of the liquid rich in the component A is discharged as a distillate at a flow rate of 250 [kg / hr], and the remainder of the liquid rich in the component A remains at the top of the distillation column 131 at 6534 [kg / hr]. As a reflux liquid. Further, the liquid rich in the component B is 250 [kg /
hr], a liquid rich in component C is discharged as a sidestream liquid at a flow rate of 250 kg / hr, and a part of the liquid rich in component D is 250 kg / h.
r] as a bottom liquid. The enrichment section A
The effluent of R47 is distributed at a ratio of 1: 4.87 to the concentration section AR43 and the recovery section AR48, and the recovery section AR48.
The flowing liquid of 7.6 is supplied to the concentration sections AR41 and AR45.
Dispensed in a 9: 1 ratio. The calorific load of the evaporator 231 was 1,800,000 [kcal / hr].

Table 5 shows the results of distillation by the distillation column 131 shown in FIG. In Table 5, the composition is expressed in units of [wt%], and the flow rate is expressed in units of [kg / hr].

[0081]

[Table 5]

A comparison between the distillation results in Table 1 and the distillation results in Tables 3 to 5 shows that the first and second evaporators 91, 9
2 and the respective evaporators 211, 221, 231
So that the total of the theoretical plates of the distillation column 10 and the total of the theoretical plates of each of the distillation columns 111, 121, 131 are set to be equal so that the total of the calorific loads of the methanol MeOH are equal. , Ethanol EtOH, 1
-Both propanol PrOH and 1-butanol BuOH, when using a distillation apparatus comprising a distillation column 10,
It can be seen that the purity is higher than in the case where each distillation apparatus including each of the distillation columns 111, 121 and 131 is used. In particular, in the distillation apparatus including the distillation column 10, the components B and C, which are intermediate components, are discharged as a distillate and a bottom, respectively, so that the purity is extremely high.

The present invention is not limited to the above-described embodiment, but can be variously modified based on the gist of the present invention, and they are not excluded from the scope of the present invention.

[0084]

As described above in detail, according to the present invention, in the distillation apparatus, the column main body and the first column formed in the column main body by extending vertically from the top to the center of the column. A second partition formed vertically in the tower body from the tower bottom to the center of the tower, and with a gap between the lower end of the first partition. A partition formed by extending vertically in a predetermined portion of the first distillation region among the first and second distillation regions defined by the first and second intermediate partitions. 3, a first distillation section formed along the third partition, a second distillation section formed at least partly adjacent to the top of the column, and at least partly a column. A third distillation section formed adjacent to the bottom and the second distillation area through the gap to the second distillation section; It is communicated to the distillation zone and communicates with a fourth distillation section formed.

In this case, in the column body of one distillation column, the first and second partitions which are vertically extended are partitioned and formed in the first and second distillation regions, and the first distillation column is formed. Since the region is divided by the third partition which extends in the up-down direction, each component contained in the undiluted solution can be separated by using only one distillation column without using a plurality of distillation columns. Can be separated.

Accordingly, the number of necessary evaporators and condensers can be reduced, and the number of pumps, instrumentation parts, etc. can be reduced, so that the cost of the distillation apparatus can be reduced. In addition, the usage amount and the energy consumption of the utility can be reduced.

The intermediate components do not need to be discharged from the side of the column, and can be discharged from the top and bottom of the column. Therefore, each component can be sufficiently separated, and the purity of the product can be increased. .

[Brief description of the drawings]

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

FIG. 2 is a conceptual diagram of a conventional distillation apparatus having three distillation columns.

FIG. 3 is a conceptual diagram showing a first example of a conventional distillation apparatus having one distillation column.

FIG. 4 is a conceptual diagram showing a second example of a conventional distillation apparatus having one distillation column.

FIG. 5 is a conceptual diagram showing a third example of a conventional distillation apparatus having one distillation column.

FIG. 6 is a conceptual diagram of a distillation apparatus used for a simulation according to an embodiment of the present invention.

[Explanation of symbols]

 14A-16A 1st chamber 14B-16B 2nd chamber 25-28 1st-4th distillation part 30 Tower main body 30A, 30B 1st, 2nd distillation area 31-33 1st-3rd partition 41 Feed Nozzles 42, 46 First and second steam outlets 43 and 47 First and second reflux liquid inlets 44 and 48 First and second bottoms outlets 45 and 49 First and second steam inlets AR1, AR3, AR5, AR7 Concentration unit AR2, AR4, AR6, AR8 Collection unit

Continued on the front page F term (reference) 4D076 AA12 AA13 AA22 AA23 AA24 BB04 BB27 CA06 CA11 CA13 CC24 DA03 DA25 FA31 FA35 FA37 JA03 JA04

Claims (8)

[Claims] 1. (a) a tower main body; (b) a first partition formed in the tower main body so as to extend vertically from the top to the center of the tower; and (c) inside the tower main body. A second partition formed extending vertically from the bottom of the tower to the center of the tower and having a gap between the lower end of the first partition and (d) the first partition; A third partition formed by extending vertically in a predetermined portion of the first distillation region of the first and second distillation regions partitioned by the second partition; ( e) a first distillation section formed along the third partition; (f) a second distillation section formed at least partly adjacent to the top of the column; and (g) at least a part thereof. A third distillation section formed adjacent to the bottom of the column, and (h) communicating with the first distillation section through the gap to the second distillation section. And a fourth distillation section formed by passing through. 2. A feed nozzle for supplying an undiluted solution facing the first distillation section is provided on the side of the tower main body at the top of the first distillation section.
The first discharge means for bottoms at the bottom of the first distillation area, the second discharge means for distillate at the top of the tower in the second distillation area, The distillation apparatus according to claim 1, wherein a second discharge means for bottoms is formed at the bottom of the second distillation zone. 3. A first supply means for the reflux liquid at the top of the first distillation zone, and a first supply means for vapor from a first evaporator at the bottom of the first distillation area. However, a second supply means for the reflux liquid is formed at the top of the second distillation area, and a second supply means for the vapor from the second evaporator is formed at the bottom of the second distillation area. The distillation apparatus according to claim 2. 4. A concentrating section above the feed nozzle in the first distillation section, and a recovery section below the feed nozzle in the first distillation section, adjacent to the top of the second distillation section. The enrichment section is adjacent to the first distillation section in the second distillation section, the recovery section is adjacent to the first distillation section in the third distillation section, and the enrichment section is adjacent to the third distillation section. The collection unit is formed adjacent to the column bottom in the above, a concentrating unit is formed above the gap in the fourth distillation unit, and a collection unit is formed below the gap in the fourth distillation unit. Distillation equipment. 5. The sectional area of each of the first and second chambers defined by the third partition in the first distillation area and the sectional area of the second distillation area correspond to the flow rate of steam. The distillation apparatus according to claim 1, wherein the positions of the first to third partitions are set as described above. 6. A tower body, a first partition formed in the tower body so as to extend vertically from the tower top to the center of the tower, and extends vertically in the tower body from the bottom of the tower to the center of the tower. And a second partition formed with a gap between the lower end of the first partition and the first and second partitions defined by the first and second partitions. A third partition formed in a predetermined portion of the first distillation region of the first distillation region extending in the vertical direction, and a first distillation unit formed along the third partition. A second distillation section formed at least partially adjacent to the top of the column, a third distillation section formed at least partially adjacent to the bottom of the column, and the second distillation area, Using a distillation apparatus having a fourth distillation section formed in communication with the first distillation area via The method comprising: (a) feeding a stock solution to the first distillation section; (b) discharging a first distillate from the top of the first distillation section; and (c) discharging the first distillation section. Discharging the first bottoms from the bottom of the column,
(D) discharging a second distillate from the top of the second distillation zone, and (e) discharging a second bottoms from the bottom of the second distillation zone. A distillation method using a distillation apparatus. 7. The stock solution comprises a mixture of first to fourth components in descending order of relative specific volatility, and (b) a liquid enriched in the first component in a first distillate. Discharged as a liquid, (c) the liquid rich in the second component is discharged as a second distillate, and (d) the liquid rich in the third component is discharged as a second bottoms. And (e) a distillation method using the distillation apparatus according to claim 6, wherein the liquid rich in the fourth component is discharged as a first bottom liquid. 8. A part of the first distillate is refluxed to the second distillation section as a reflux liquid, and (b) a part of the second distillate is a reflux liquid in the fourth distillation part. Refluxed to the distillation section of
(C) a part of the first bottoms is vaporized and collected in the third distillation unit; and (d) a part of the second bottoms is vaporized and collected in the fourth distillation unit. A distillation method using the distillation apparatus according to claim 7, wherein the distillation apparatus is recovered.