JP3329750B2 - Distillation apparatus and distillation method thereof - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] The present invention relates to a distillation apparatus and a distillation method thereof.

[0002]

2. Description of the Related Art Conventionally, when a plurality of distillation columns are combined and a product is obtained by separating each component from a stock solution containing a plurality of components by distillation to obtain a product, if each of the distillation columns is separately constructed, an occupied area increases. I will. Further, in the side column type distillation apparatus, since it is necessary to control the distribution of steam between the respective distillation columns in order to adjust the pressure in each of the distillation columns, the respective distillation columns cannot be operated stably. .

Therefore, there is provided a Petriuk-type distillation apparatus in which an inner cylinder is disposed in an outer cylinder, and a stock solution is supplied into the inner cylinder to perform distillation. However, in this case, it is difficult to support the inner cylinder with respect to the outer cylinder, arrange a line by penetrating the outer cylinder, or attach a feed nozzle to the inner cylinder. Will be expensive. In addition, since it is not possible to sufficiently seal between the line and the outer cylinder and between the feed nozzle and the inner cylinder,
The efficiency of distillation in the distillation column is reduced.

[0004] Since the inner cylinder and the outer cylinder are arranged concentrically and the collecting section and the concentrating section have an annular structure, it is difficult to manufacture trays arranged in the collecting section and the concentrating section. become. Therefore, a distillation apparatus in which the inside is partitioned by a flat partition is provided (US Pat. No. 42305).
No. 33).

[0005] In this case, the distillation apparatus is supplied with a stock solution through an inlet pipe, and has a first concentrating section formed above the inlet pipe and a first collecting section formed below the inlet pipe. And a distillation unit connected to the upper end of the first distillation unit,
A concentration unit formed above the upper end, and a second distillation unit provided below the upper end and provided with a collection unit adjacent to the concentration unit of the first distillation unit via a partition. Connected to the lower end of the first distillation section, formed above the lower end, and formed adjacent to the recovery section of the first distillation section via a partition, and below the lower end. And a third distillation unit provided with a recovered recovery unit.

[0006] Therefore, the cost of the distillation apparatus can be reduced, the efficiency of distillation can be increased, and the packed (balanced) element can be easily manufactured.

[0007]

However, in the conventional distillation apparatus, the liquid that has moved downward from above is appropriately distributed to the concentration section of the first distillation section and the recovery section of the second distillation section. Therefore, not only the flow rate of the liquid supplied from the concentration section of the second distillation section to the concentration section of the first distillation section needs to be adjusted by an analyzer, a flow controller, and a flow control valve, but also the second distillation section. Second from the enrichment section
It is necessary to adjust the flow rate of the liquid supplied to the recovery section of the distillation section by using a level sensor, a flow rate controller, and a flow rate control valve.

Further, in order to properly distribute the liquid which has moved downward from above to the recovery section of the first distillation section and the concentration section of the third distillation section, the stock solution supplied to the first distillation section is Not only the flow rate needs to be adjusted by a flow controller and a flow control valve, but also the amount of product discharged from between the first and second distillation sections needs to be adjusted by a level sensor, a flow controller and a flow control valve. .

[0009] Then, in order to appropriately distribute the vapor that has moved upward from below to the recovery section of the first distillation section and the enrichment section of the third distillation section, the first vapor is recovered from the recovery section of the third distillation section. It is not only necessary to adjust the flow rate of steam supplied to the recovery section of the distillation section by an analyzer and a flow control valve,
It is necessary to adjust the flow rate of steam supplied from the recovery section of the third distillation section to the concentration section of the third distillation section by an analyzer and a flow control valve.

As described above, in order to properly distribute the liquid and the vapor, it is necessary to dispose not only instrumentation equipment such as an analyzer, a flow controller, a flow control valve, and a level sensor, but also to install each instrumentation equipment. Since it is necessary to perform complicated control by operation, the size of the distillation apparatus is increased, and the cost of the distillation apparatus is increased. The present invention can solve the problems of the conventional distillation apparatus, reduce the number of instrumentation, simplify the control, reduce the size, and reduce the cost. An object of the present invention is to provide a distillation apparatus and a distillation method thereof.

[0011]

For this purpose, in the distillation apparatus of the present invention, there is provided a column main body, and a partition which divides the inside of the column main body and forms a first chamber and a second chamber adjacent to each other; A first distilling unit to which an undiluted solution is supplied via a feed nozzle and provided with a concentrating unit formed above the feed nozzle, and a collecting unit formed below the feed nozzle; and a first distilling unit A concentrating unit formed above the upper end, and a collecting unit formed below the upper end and adjacent to the concentrating unit of the first distillation unit via a partition. A second distillation unit, a concentration unit connected to the lower end of the first distillation unit, formed above the lower end, and adjacent to the recovery unit of the first distillation unit via a partition; and A third portion having a collecting portion formed below the lower end; And a distillation unit. Then, the middle partition is eccentric toward the second chamber. In addition, the second
The distribution ratio of the liquid distributed from the concentration unit of the distillation unit to the first chamber and the second chamber is set in accordance with the degree of eccentricity of the partition.

In another distillation apparatus of the present invention, the undiluted solution is passed through a column main body, a partition that divides the inside of the column main body and forms a first chamber and a second chamber adjacent to each other, and a feed nozzle. A first distillation section provided with a concentrating section formed above the feed nozzle, and a recovery section formed below the feed nozzle, and connected to an upper end of the first distillation section; Concentrating part formed above the upper end,
And a second distillation unit formed below the upper end and having a recovery unit adjacent to the enrichment unit of the first distillation unit via a partition, and connected to a lower end of the first distillation unit. And a third distillation section formed above the lower end and provided with a concentrating section adjacent to the collecting section of the first distillation section via a partition, and a collecting section formed below the lower end. And a part. Then, the middle partition is eccentric toward the second chamber. The ratio of the cross-sectional areas of the first chamber and the second chamber to the cross-sectional area of the column body is set by the ratio of the components obtained at the lower end of the second distillation section and the upper end of the third distillation section. Is done. In the distillation method of the distillation apparatus of the present invention, the present invention is applied to a distillation apparatus including a first chamber and a second chamber adjacent to each other via an intermediate partition, and wherein the intermediate partition is eccentric to the second chamber side. . Then, the undiluted solution is supplied through a feed nozzle formed between the concentration section and the recovery section in the first distillation section, connected to the upper end of the first distillation section, and formed above the upper end. The distillate is discharged from the second distillation section provided with a concentrating section, and a collecting section adjacent to the concentrating section of the first distillation section, formed below the upper end, and a partition. A concentrating unit connected to the lower end of the first distillation unit, formed above the lower end, and adjacent to the recovery unit of the first distillation unit via a partition;
And a third portion having a collecting portion formed below the lower end.
The bottom liquid is discharged from the distillation section, and the side cut liquid is discharged from the side cut nozzle formed between the recovery section of the second distillation section and the concentration section of the third distillation section. Further, a distribution ratio of the liquid distributed from the concentration section of the second distillation section to the first chamber and the second chamber is set in accordance with the degree of eccentricity of the partition.

In another distillation method for a distillation apparatus according to the present invention, the distribution ratio is set by adjusting means for adjusting the flow rate.

[0014]

Embodiments of the present invention will be described below in detail with reference to the drawings. FIG. 1 is a conceptual diagram of a combined distillation column according to an embodiment of the present invention, FIG. 2 is a conceptual diagram of a distillation apparatus according to an embodiment of the present invention, and FIG. FIG. 4 is a sectional view of a main part of a combined distillation column according to an embodiment of the present invention.

In the figure, 10 is a combined distillation column,
The combined distillation column 10 includes a first section 11, a second section 12, a third section 13, a fourth section 1
4, a fifth section 15, a sixth section 16, a seventh section 17, an eighth section 18, and a ninth section 19. In the fourth section 14, the fifth section 15 and the sixth section 16, the column main body of the combined distillation column 10 is divided into first chambers 14A to 16A and second chambers by plate-shaped partitions 22 to 24, respectively. 1
4B to 16B, and the first chambers 14A to 16A and the second chambers 14B to 16B are adjacent to each other. Also,
The first distillation section 25 is provided by the first chambers 14A to 16A.
However, the second distillation section 26 is formed by the first section 11, the second section 12, the third section 13, and the second chamber 14B, and the second chamber 15B, 16B, the seventh section 17, the eighth section 18, and Third sections 27 are respectively formed by the nine sections 19.

The partitions 22 to 24 may be formed of a heat insulating material, or the insides of the partitions 22 to 24 may be made to have a heat insulating structure by evacuating the interior of the partitions 22 to 24. In this case, between the first chamber 14A and the second chamber 14B, between the first chamber 15A and the second chamber 15B, and between the first chamber 15A and the second chamber 14B.
Since the heat transfer between 6A and the second chamber 16B can be respectively reduced, the efficiency of distillation can be increased.

The fifth section 15 is disposed substantially at the center of the combined distillation column 10 in the height direction. A feed nozzle 41 is formed in the first chamber 15A, and a side cut nozzle 42 is formed in the second chamber 15B. Is done. The first section 11 is disposed at the top of the combined distillation column 10, and the first section 11 is connected to a condenser 81, and a vapor outlet 43 and a reflux liquid inlet 44 are formed respectively. Further, a ninth section 19 is provided at the bottom of the combined distillation column 10, and the ninth section 19 is provided with an evaporator 82.
To form a bottoms outlet 45 and a steam inlet 46, respectively.

In the combined distillation column 10 having the above-described structure, a mixture containing the components A to C is supplied to the feed nozzle 41 as a stock solution M. In addition, component A is obtained from component B,
Component B has a lower boiling point than component C. The combined distillation column 1
0, the condenser 81, the evaporator 82 and the like constitute a distillation apparatus. In the first distillation section 25,
First chamber 1 disposed above feed nozzle 41
The enrichment section AR1 is formed by 4A, and the collection section AR2 is formed by the first chamber 16A disposed below the feed nozzle 41. The second distillation section 26 is connected to the upper end of the first distillation section 25, and the enrichment section AR is formed by the second section 12 disposed above the upper end.
3, below the upper end of the first distillation section 25,
Second chamber 14B disposed adjacent to the enrichment section AR1
Thereby, the collection portions AR4 are formed. further,
The third distillation section 27 is connected to the lower end of the first distillation section 25, and the recovery section AR2 is located above the lower end.
Enrichment section A by the second chamber 16B disposed adjacent to the
The recovery section AR6 is formed by the eighth section 18 in which R5 is disposed below the lower end of the first distillation section 25.

As described above, the upper end of the first distillation section 25 is located substantially at the center of the second distillation section 26 in the height direction, and the lower end of the first distillation section 25 is located at the height of the third distillation section 27. Each is connected to approximately the center in the direction. Then, in the recovery part AR2, the stock solution M supplied from the feed nozzle 41 moves downward, and the components A and B
From the lower end of the first distillation section 25 to generate a liquid rich in the components B and C in the downward direction.
Is supplied with a liquid rich in components B and C.

Further, the liquids rich in the components B and C are:
The mixture is heated in the third distillation section 27 to become a vapor rich in the components B and C, and the vapor rich in the components B and C is transferred to the undiluted solution M while moving upward in the recovery section AR2.
To generate a vapor rich in components A and B from the stock solution M. Subsequently, the vapors rich in the components A and B move upward in the enrichment section AR1 and are supplied to the second distillation section 26 from the upper end of the first distillation section 25. Further, the vapors rich in the components A and B are cooled and condensed in the second distillation section 26 to become a liquid rich in the components A and B.

Then, a part of the liquid rich in the components A and B is refluxed to the concentrating unit AR1, and is brought into contact with the vapor rich in the components A and B that can be moved upward in the concentrating unit AR1. In this way, vapors 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 the components B and C move downward, and generate vapor rich in the component B at the upper portion and generate liquid rich in the component C at the lower portion. Therefore, the liquid rich in the component C is discharged from the bottom outlet 45 as bottoms. A part of the component-rich liquid discharged from the bottom outlet 45 is sent to the evaporator 82 and heated by the evaporator 82 to be a component-rich vapor. The vapor rich in component C is supplied from the vapor inlet 46 to the ninth section 19, and the liquid enriched in components B and C is moved while moving upward in the ninth section 19 and the recovery part AR6. To generate a component B-rich vapor from the component B and C-rich liquid.

Subsequently, a part of the vapor rich in the component B is
It moves upward in the enrichment section AR5, and comes into contact with the component B-rich liquid from the second distillation section 26 at the upper end of the third distillation section 27 to become a component B-rich liquid. The liquid rich in component B obtained at the upper end of the third distillation section 27 is discharged from the side cut nozzle 42 as a side cut liquid.

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 downward, producing vapors rich in component A above and liquids rich in component B downward. The liquid rich in component B obtained at the lower end of the second distillation section 26 is discharged from the side cut nozzle 42 as a side cut liquid.

Then, the vapor enriched in the component A moves upward in the enrichment section AR3, is discharged from the vapor outlet 43, is sent to the condenser 81, is condensed by the condenser 81, and is condensed by the condenser 81. And is discharged as a distillate. In this way, the vapors rich in components A and B are separated by the second distillation section 26 into a vapor rich in component A and a liquid rich in component B. The liquid discharged from the top is condensed by the condenser 81 to become a liquid rich in the component A, and the liquid rich in the component B is discharged from the side cut nozzle 42 as a side cut liquid. Further, the liquid enriched in components B and C is separated from the liquid enriched in component B and component C by the third distillation section 27.
The liquid rich in component B is discharged from the side cut nozzle 42 as a side cut liquid, and the liquid rich in component C is discharged from the bottom of the column.

In order to increase the efficiency of the distillation of the component A, a part of the liquid rich in the component A is supplied to the reflux liquid inlet 4.
4 and is returned to the enrichment section AR3, where it is brought into contact with vapors rich in components A and B which are moved upward in the enrichment section AR3. Each of the enrichment sections AR1, AR3, AR5
And each recovery section AR2, AR4, AR6 is formed by a packing consisting of one node, but depending on the specific volatility between the components to be distilled, the number of theoretical plates required for distillation is reduced. To ensure, it can also be formed by a multi-node filling, corresponding to the properties of the filling used. In addition, a distributor can be provided between nodes. Further, the feed nozzle 41
It is not always necessary to arrange the side cut nozzles 42 at the same height.

Thus, the stock solution M can be separated into each component without using a plurality of distillation columns.
In addition, since it is not necessary to repeat heating and cooling in a plurality of distillation columns, it is not necessary to provide a large number of instrumentation equipment such as a condenser, an evaporator, and a pump. Therefore, not only the occupied area can 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 about 30 to 100 theoretical plates as a whole, and the fourth section 14 and the sixth section 16 each have about 5 to 30 plates. preferable. Meanwhile, a collector 54 and a channel type distributor 61 are provided in the third section 13, and the liquid collected by the collector 54 is distributed by the distributor 61 at a predetermined distribution ratio to the first chamber 14 </ b> A of the fourth section 14.
And the second chamber 14B.

The first chamber 15A of the fifth section 15
The collector 62 is located immediately above the feed nozzle 41 in FIG.
However, a tubular type distributor 63 is disposed immediately below, and the liquid collected by the collector 62 is:
Along with the stock solution M supplied via the feed nozzle 41, the sixth section 1 is distributed by the distributor 63.
6 is supplied to the first chamber 16A.

On the other hand, the second chamber 15B of the fifth section 15
A chimney hat type collector 65 is disposed directly above the side cut nozzle 42, and a tubular type distributor 66 is disposed directly below the side cut nozzle 42. The liquid collected by the collector 65 is discharged from the side cut nozzle 42 as a side cut liquid. And the second chamber 16 of the sixth section 16 by the distributor 66.
B.

Further, the collector 6 is added to the seventh section 17.
7 and a tubular type distributor 68 are provided, and the liquid that has moved downward from the sixth section 16 is collected by the collector 67 and then supplied to the eighth section 18 by the distributor 68. By the way, in the present embodiment, the liquid that has moved upward, that is, from the second section 12 to the third section 13 is transferred to the first chamber 14 of the fourth section 14.
A and the second chamber 14B are distributed. The distribution ratio depends on the type of the components of the stock solution M, the composition of the stock solution M, the number of theoretical plates in the combined distillation column 10, the purity (quality) required for the product, and the like. Is set in advance based on the distillation conditions.

For this purpose, the distributor 61
Comprises a distributor (not shown) for distributing liquid in a direction perpendicular to the partition 22, and the first
The amount of liquid supplied to the upper part of the chamber 14A (hereinafter, referred to as “upper part of the first chamber”) and the amount of liquid supplied to the upper part of the second chamber 14B (hereinafter, referred to as “upper part of the second chamber”). The amount of liquid is made different.

Since the side cut liquid is discharged from the side cut nozzle 42, the amount of liquid supplied to the upper part of the second chamber is larger than the amount of liquid supplied to the upper part of the first chamber. When it is necessary to change the distillation conditions in order to obtain two or more types of products in the distillation apparatus, it is necessary to change the distribution ratio in accordance with the distillation conditions. Therefore, a plurality of the distribution units are provided, and the distribution ratio is different for each distribution unit. For this purpose, the liquid that has moved downward from the second section 12 is collected by the collector 54 and selectively supplied to the distributor 61 via switching valves 83 and 84 as adjusting means for adjusting the flow rate of the liquid. . For example,
When a product having a purity of 99.98 [% by weight] is obtained, the distribution ratio is adjusted to 4: 6 by adjusting the switching valves 83 and 84. When a product having a purity of 99.999 [% by weight] is obtained, By adjusting the switching valves 83 and 84, the distribution ratio is set to 2: 8. The load factor is 50-100
It is changed to [%].

As described above, since the liquid can be distributed at the optimum distribution ratio only by disposing the distribution section, instrumentation such as an analyzer, a flow controller, a flow control valve, and a level sensor for distributing the liquid can be performed. Not only is there no need to arrange a large number of components, but there is no need to operate each instrumentation and perform complicated control. Therefore, not only the size of the distillation apparatus can be reduced, but also the cost of the distillation apparatus can be reduced. In adjusting the switching valves 83 and 84, a flow meter (not shown) can be provided.

By the way, for example, the amount of the side cut liquid is extremely large with respect to the supply amount of the stock solution M, and the ratio of the amount of the side cut liquid to the supply amount is almost 100 [w%].
If only side cut solution is the product, when the proportion of each component A~C in stock M and F _A to F _C (%), the composition of the stock solution M _{is, F B »F A, F C} (F A ≠ become F _C).

In such a composition of the stock solution M, for example, the partitions 22 to 24 are disposed in the center of the combined distillation column 10 so that the cross-sectional area S1 of the first chambers 14A to 16A and the second chamber 14
Even if the cross-sectional areas S2 of B to 16B are equal, the evaporator 82
There is no increase in the heat load applied to the substrate. On the other hand, the proportion occupied by two components among the components A to C is large, and the proportion occupied by one component is small, and the composition of the stock solution M is F _A , F _B > F _C F _A , F _C> F _B F _B, if either of F _C> F _a, and a large proportion of one component other than the component B, and small ratio of the two components, the composition of the stock solution M, F _{a> F B, F C F} C> F a, F when either of _B, and to equalize the cross-sectional area S1, S2, and the amount of vapor and liquid flows through the first chamber 14A～16A, second Since the amounts of vapor and liquid flowing in the chambers 14B to 16B are different, the first chambers 14A to 16A and the second chamber 1
4B to 16B are unnecessarily wide with respect to the amount of vapor and liquid, and the other is narrow by that amount.
A to 16A and the second chambers 14B to 16B cannot be used effectively. Therefore, the heat load applied to the evaporator 82 increases, and the energy consumed for distillation increases.

Therefore, the above-mentioned partitions 22 to 24 are undiluted M
Corresponding to the composition of the second chambers 14B to 16B, the cross sections S1 and S2 are made different. The ratio γ γ = S1 / S2 of the cross-sectional areas S1 and S2 occupying the cross-sectional area of the column body of the combined distillation column 10 is set to a value closer to 1 as the ratio of the component B increases, and the component B
The smaller the ratio, the larger the value. However, the greater the amount of eccentricity, the lower the degree of freedom in setting the distribution ratio.

As described above, by making the sectional areas S1 and S2 different, the amounts of the steam and the liquid flowing in the first chambers 14A to 16A and the amounts of the steam and the liquid flowing in the second chambers 14B to 16B are reduced. Even if different, the first chambers 14A to 16A and the second chambers 14B to 16B can be used effectively. Therefore, the heat load applied to the evaporator 82 can be reduced, and the energy consumption for distillation can be reduced.

In the distillation method of the distillation apparatus according to the present invention, the first chambers 14A to 14A to 16E are separated from the enrichment section of the second distillation section.
The distribution ratio of the liquid distributed to A and the second chambers 14B to 16B is set in accordance with the degree of eccentricity of the intermediate partitions 22 to 24. Therefore, unnecessary steam does not move upward in the second chambers 14B to 16B.
There is no need to uselessly increase the liquid that is brought into contact with the vapor. As a result, the heat load applied to the evaporator 82 can be reduced, so that the energy consumption for distillation can be reduced.

The supply amount of the stock solution M is determined by the amount of the distillate discharged from the top of the column, the amount of the side cut liquid discharged from the side cut nozzle 42, and the amount of the bottom discharged from the bottom of the column. Since there are more, the partition 22 to 24 is divided into the first chamber 14A.
It is not eccentric to the side of ~ 16A.

[0041]

[Embodiment 1] A combined distillation column 10 of the present invention was used.
Benzene (C₆H₆) With component B
And toluene (C₇H₈) As component C
(C₆H_Four(CH _Three)_Two)) From the stock solution M containing
AC were separated.

The conditions of the stock solution M and the components A to C are as follows. Composition of stock solution _{M: F A, F C>} F B F A 50 [w%] F _B 3 purity [w%] F _C 47 [w%] supply amount 1000 of the stock solution M [kg / h] distillate 99.9 [w%] or more Purity of bottoms 99.9 [w%] or more And the ratio of the cross-sectional areas S1 and S2 is 60 and 40, respectively.
[%], And distillation was performed under the following distillation conditions.

[0043] In this case, the heat load applied to the evaporator 82 is 170,000.
[Kcal / h]. The optimum value of the distribution ratio can be obtained by calculating the differential pressure between the first chambers 14A to 16A and the second chambers 14B to 16B.

The ratio of the cross-sectional areas S1 and S2 was set to 70 and 30%, respectively, and distillation was performed under the following distillation conditions. In this case, the heat load applied to the evaporator 82 is 140,000.
[Kcal / h].

That is, the ratio FB of the component _B is 3 [w%].
And the value is 1 [w%] or more, which is considered to be valid.
The reflux ratio can be made smaller than when the ratios of the cross-sectional areas S1 and S2 are respectively 60 and 40 [%], and the distillate can be increased accordingly. Therefore, since the amount of steam flowing in the tower body can be reduced, the heat load applied to the evaporator 82 is reduced, and the cross-sectional areas S1, S2
Approximately 8 when the ratio of 2 is 60 and 40%, respectively.
0 [%]. [Comparative Example 1] Using a conventional distillation apparatus combining two distillation columns, components A to C were separated from a stock solution M containing benzene as component A, toluene as component B, and xylene as component C. I let it.

The conditions of the stock solution M and each of the components A to C are as follows. Composition of stock solution _{M: F A, F C>} F B F A 50 [w%] F _B 3 purity [w%] F _C 47 [w%] supply amount 1000 of the stock solution M [kg / h] distillate 99.9 [w%] or more Purity of bottoms 99.9 [w%] or more Distillation was performed under the following distillation conditions.

Number of theoretical plates First distillation column 30 stages Second distillation column 30 stages Reflux ratio First distillation column 1.30 Second distillation column 2.23 Temperature (normal pressure) Top of first distillation column 80.2 [° C.] Bottom of first distillation column 135.0 [° C.] Top of second distillation column 110.6 [° C.] Bottom of second distillation column 139.1 [° C.] In this case, the heat load applied to the evaporator 82 is 115000 [kcal / h] in the first distillation column, and the second distillation column is 350 mm [mm].
Was 59000 [kcal / h], and 174,000 [kcal / h] in total. [Comparative Example 2] Using a distilling apparatus in which middle partitions 22 to 24 were arranged at the center of the tower body, each component A was obtained from a stock solution M containing benzene as component A, toluene as component B, and xylene as component C. ~ C were separated.

The conditions of the stock solution M and each of the components A to C are as follows. Composition of stock solution _{M: F A, F C>} F B F A 50 [w%] F _B 3 purity [w%] F _C 47 [w%] supply amount 1000 of the stock solution M [kg / h] distillate 99.9 [w%] or more Purity of bottoms 99.9 [w%] or more Distillation was performed under the following distillation conditions.

[0049] In this case, the heat load applied to the evaporator 82 is 170,000.
[Kcal / h]. [Embodiment 2] FIG. 5 is a first diagram showing distillation conditions in an embodiment of the present invention, FIG. 6 is a second diagram showing distillation conditions in an embodiment of the present invention, and FIG. FIG. 8 is a third diagram showing the distillation conditions, and FIG. 8 is a fourth diagram showing the distillation conditions in the example of the present invention.

Using the combined distillation column 10 of the present invention (FIG. 2)
And methanol (CH _ThreeOH) with component B
As ethanol (C_TwoH_FiveOH), isopropanol
((CH_Three)_TwoCHOH) and isobutanol ((CH
_Three)_TwoCHCH_TwoOH) as component C with water (H_TwoO)
The components A to C were separated from the stock solution M containing Undiluted solution
The conditions of M and each of the components A to C are as follows.

[0051] The live steam is blown into the bottom of the column to lower the concentration of methanol and to assist the heating by the evaporator 82. In this case, methanol is discharged as a product, and water is discharged from the bottom of the tower.

Then, the ratio of the cross-sectional areas S1 and S2 was set to 60 and 40%, respectively, and distillation was performed under the following distillation conditions. In this case, the heat load applied to the evaporator 82 is 547000
[Kcal / h]. In FIG. 5, the temperature, pressure, flow rate, and composition of the stock solution M, live steam, distillate, side cut solution, and bottoms are shown.

Next, the ratio of the cross-sectional areas S1 and S2 was set to 70 and 30%, respectively, and distillation was performed under the following distillation conditions. In this case, the heat load applied to the evaporator 82 is 538000.
[Kcal / h]. In FIG. 6, the temperature, pressure, flow rate, and composition of the stock solution M, live steam, distillate, side cut solution, and bottom solution are shown.

Next, the ratio of the cross-sectional areas S1 and S2 was set to 75 and 25%, respectively, and distillation was performed under the following distillation conditions. In this case, the heat load applied to the evaporator 82 is 532000
[Kcal / h]. In FIG. 7, the temperature, pressure, flow rate, and composition of the stock solution M, live steam, distillate, side cut solution, and bottoms are shown.

Next, the ratio of the cross-sectional areas S1 and S2 was set to 80 and 20%, respectively, and distillation was performed under the following distillation conditions. In this case, the heat load applied to the evaporator 82 is 525,000.
[Kcal / h]. In FIG. 8, the temperature, pressure, flow rate, and composition of the stock solution M, live steam, distillate, side cut solution, and bottoms are shown. In this case,
The heat load applied to the evaporator 82 was changed to 80 in Comparative Example 4 described later.
[%]. Comparative Example 3 Using a conventional distillation apparatus combining two distillation columns, methanol was used as component A, and ethanol, isopropanol and isobutanol were used as component B,
The components A to C were separated from the stock solution M containing water as the component C.

The conditions of the stock solution M and the components A to C are as follows. Then, distillation was performed under the following distillation conditions.

Theoretical plate number First distillation column 30 stages Second distillation column 30 stages Reflux ratio First distillation column 2.1 Second distillation column 3.9 Temperature (normal pressure) First and second distillation columns Distillate 64.6 [° C.] Side cut liquid of the first and second distillation columns 68.4 to 68.9 [° C.] Diameter of the column body First distillation column 500 [mm] Second distillation column 400 [mm] In this case, the heat load applied to the evaporator 82 is 5702 in total.
00 [kcal / h]. Comparative Example 4 FIG. 9 is a diagram showing distillation conditions in a comparative example.

Using a distillation apparatus in which the middle partitions 22 (FIG. 3) to 24 are arranged at the center of the tower body, methanol is used as the component A, ethanol, isopropanol and isobutanol as the component B, and water as the component C. The components A to C were separated from the undiluted solution M. Stock solution M and each component A to C
Are as follows.

[0059] Then, distillation was performed under the following distillation conditions.

[0060] In this case, the heat load applied to the evaporator 82 (FIG. 2) is 554.
000 [kcal / h]. In the figure,
The temperature, pressure, flow rate and composition of the stock solution M, live steam, distillate, side cut solution and bottoms are shown.

The present invention is not limited to the above 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.

[0062]

As described above in detail, according to the present invention, in the distillation apparatus, the column main body and the inside of the column main body are divided, and the first chamber and the second chamber are formed adjacent to each other. An intermediate partition, a first distilling unit provided with an undiluted solution supplied through a feed nozzle, a concentrating unit formed above the feed nozzle, and a collecting unit formed below the feed nozzle; A concentrating section connected to the upper end of the first distillation section and formed above the upper end; and a collecting section formed below the upper end and adjacent to the concentrating section of the first distillation section via a partition. A second distillation section, comprising:
It is connected to the lower end of the first distillation unit, is formed above the lower end, and is formed below the lower end from the enrichment unit, which is adjacent to the recovery unit of the first distillation unit via a partition, and the lower end. And a third distillation section provided with a recovery section. Then, the middle partition is eccentric toward the second chamber. Also,
The distribution ratio of the liquid distributed from the concentration section of the second distillation section to the first chamber and the second chamber is set according to the degree of eccentricity of the partition.

[0063] In this case, the first distillation unit
Since the liquid can be distributed to the chamber and the second chamber, it is not necessary to dispose a large number of instrumentation devices such as an analyzer, a flow controller, a flow control valve, and a level sensor for distributing the liquid. There is no need to operate the instrumentation and perform complicated control. Therefore, not only the size of the distillation apparatus can be reduced, but also the cost of the distillation apparatus can be reduced.

Further, since the cross-sectional area of the first chamber is different from the cross-sectional area of the second chamber, the amounts of the vapor and the liquid flowing in the first chamber are reduced.
Even if the amounts of the vapor and the liquid flowing in the second chamber are different, the first chamber and the second chamber can be effectively used. Therefore, the heat load applied to the evaporator can be reduced, so that the energy consumption for distillation can be reduced.

In the distillation method of the distillation apparatus according to the present invention,
The present invention is applied to a distillation apparatus that includes a first chamber and a second chamber that are adjacent to each other via an intermediate partition, and the intermediate partition is eccentric to the second chamber side. And supplying the undiluted solution via a feed nozzle formed between the concentration section and the recovery section in the first distillation section, connected to the upper end of the first distillation section,
A concentration section formed above the upper end, and a second distillation section formed below the upper end and provided with a recovery section adjacent to the concentration section of the first distillation section via a partition. Discharging the distillate, connected to the lower end of the first distillation unit, formed above the lower end, and adjacent to the collection unit of the first distillation unit via a partition, and a concentrating unit; The bottom liquid is discharged from a third distillation section having a recovery section formed below the lower end, and is formed between the recovery section of the second distillation section and the concentration section of the third distillation section. The side cut liquid is discharged from the side cut nozzle. Further, a distribution ratio of the liquid distributed from the concentration section of the second distillation section to the first chamber and the second chamber is set in accordance with the degree of eccentricity of the partition.

[0066] In this case, the first distilling section starts with the first distilling section.
Since the distribution ratio of the liquid distributed to the chamber and the second chamber is set according to the degree of eccentricity of the partition, the first
Unnecessary vapor does not move upward in the chamber and the second chamber. Therefore, there is no need to uselessly increase the liquid that is brought into contact with the vapor, so that the heat load applied to the evaporator can be reduced. As a result, energy consumption for distillation can be reduced.

[Brief description of the drawings]

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

FIG. 2 is a conceptual diagram of a distillation apparatus according to an embodiment of the present invention.

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

FIG. 4 is a sectional view of a main part of the combined distillation column in the embodiment of the present invention.

FIG. 5 is a first diagram showing distillation conditions in an example of the present invention.

FIG. 6 is a second diagram showing distillation conditions in an example of the present invention.

FIG. 7 is a third diagram showing distillation conditions in the example of the present invention.

FIG. 8 is a fourth diagram illustrating distillation conditions in the example of the present invention.

FIG. 9 is a diagram showing distillation conditions in a comparative example.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 10 Combined distillation tower 14A-16A 1st chamber 14B-16B 2nd chamber 22-24 Partition 25-27 1st-3rd distillation part 41 Feed nozzle 42 Side cut nozzle 81 Condenser 82 Evaporator 83 Switching valve 84 Switching valve AR1, AR3, AR5 Concentration unit AR2, AR4, AR6 Recovery unit

──────────────────────────────────────────────────続 き Continued on front page (51) Int.Cl. ⁷ Identification code FI C07C 15/06 C07C 15/06 15/08 15/08 29/80 29/80 31/04 31/04 31/08 31/08 31/10 31/10 31/12 31/12 Examiner Keiko Ogawa (56) References JP-A-11-314003 (JP, A) JP-A-11-314002 (JP, A) (58) Fields investigated ( Int.Cl. ⁷ , DB name) B01D 3/00-3/42

Claims (4)

(57) [Claims] 1. (a) a tower main body; (b) a partition dividing the inside of the tower main body and forming a first chamber and a second chamber adjacent to each other; and (c) a stock solution via a feed nozzle. Is provided, and a first unit including a concentrating unit formed above the feed nozzle and a collecting unit formed below the feed nozzle
(D) connected to the upper end of the first distillation section, formed as an enrichment section above the upper end, and formed below the upper end, and the first evaporator section through a partition. (E) connected to the lower end of the first distillation section, formed above the lower end, and via a partition. And a concentrating section adjacent to the collecting section of the first distillation section, and a third distillation section having a collecting section formed below the lower end, and (f) the intermediate partition is a second chamber. (G) first and second chambers from the enrichment section of the second distillation section
Distribution ratio of the liquid distributed to the eccentricity of the partition
The degree to be set corresponding is distillation apparatus according to claim Rukoto. 2. A (a) tower main body, and (b) a first chamber and a first chamber which are separated from each other and are adjacent to each other.
And (c) an undiluted solution is supplied via a feed nozzle,
A concentrating section formed above the feed nozzle;
A first portion provided with a collecting portion formed below the feed nozzle;
And (d) connected to the upper end of the first distillation section and above the upper end.
The concentrating part formed on the side, and formed below the upper end
And a concentrating unit of the first distillation unit via a partition
And (e) connected to the lower end of the first distillation section, and
The first steam is formed above and through a partition.
The enrichment section adjacent to the recovery section of the retaining section, and below the lower end
And a third distillation unit having a recovery unit formed in
Both, (f) said in partition is caused to eccentrically to the second chamber side, (g) wherein the first chamber occupies the cross-sectional area of the tower body and a second
The ratio of each cross-sectional area of the chamber is determined by the lower end of the second distillation section and the third section.
At the top of the distillation section
Distillation apparatus characterized in that it is specified. 3. A distillation method for a distillation apparatus, comprising: a first chamber and a second chamber adjacent to each other via an intermediate partition, wherein the intermediate partition is eccentric to the second chamber side. Supplying the undiluted solution via a feed nozzle formed between the concentration section and the recovery section in the distillation section, and (b) connected to the upper end of the first distillation section and formed above the upper end. And discharging a distillate from a second distillation section formed below the upper end and provided with a recovery section adjacent to the enrichment section of the first distillation section through a middle partition; (c) A) a concentrating 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 formed below the lower end; Discharging the bottoms from the third distillation section provided with the recovered section; (d) the second distillation section; Discharging a side cut liquid from a side cut nozzle formed between the recovery section of the distillation section and the concentration section of the third distillation section, and (e) a first chamber and a first chamber from the concentration section of the second distillation section. A distillation method for a distillation apparatus, wherein a distribution ratio of a liquid distributed to a second chamber is set in accordance with a degree of eccentricity of the partition. 4. The distillation method according to claim 3 , wherein the distribution ratio is set by adjusting means for adjusting a flow rate.