JP2014168740A - Solution treatment device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a solution treatment device capable of sufficiently reducing the content of a high boiling point organic solvent in a distillate, while sufficiently increasing the content of the high boiling point organic solvent in a concentrated liquid, by separating a processed liquid into the concentrated liquid and the distillate.SOLUTION: A solution treatment device 1a comprises: a treatment tower 2 for taking out the concentrated liquid L2 from a tower bottom part, by distilling distillate steam L3 from a tower top part, by separating the processed liquid L1 into the concentrated liquid L2 and distillate steam L3 of becoming the distillate L3; first heating means 6a for heating the processed liquid L1 supplied to the tower bottom part of the treatment tower 2; first gas-liquid contact means 3a installed inside the treatment tower 2 and contacting the processed liquid L1 and processed steam L1 of becoming a gas shape by being heated by the first heating means 6a; and supply means 4 for supplying the processed liquid L1 to the inside of the treatment tower 2 from above the first gas-liquid contact means 3a.

Description

  The present invention relates to a solution treatment apparatus for treating water (liquid to be treated) containing a high-boiling organic solvent used in a cleaning process, a manufacturing process, or the like in various industrial fields, and in particular, contains a high-boiling organic solvent. The present invention relates to a solution processing apparatus for separating a liquid to be treated into a concentrated liquid having a high content of a high-boiling organic solvent and a distillate having a low content of a high-boiling organic solvent.

In the manufacturing process of various products in the electrical and electronic fields and the chemical field, high-boiling organic solvents are used when cleaning parts and manufacturing equipment, etc., and water cleaning is performed for the purpose of rinsing after the cleaning. A large amount of water containing a boiling organic solvent is discharged. In the resin film production process, a large amount of water is used to extract the high-boiling organic solvent in the process of extracting the high-boiling organic solvent in the resin and forming the film. A large amount of contained water is discharged.
In recent years, with the growth of these industrial fields, the amount of high-boiling organic solvent used has increased, and at the same time, the amount of water (liquid to be treated) containing the high-boiling organic solvent has increased.

Here, since many high-boiling organic solvents have a high value to be reused, the high-boiling organic solvent in the liquid to be recycled (processed liquid) is selected based on the viewpoint of effective use of resources. There is a desire to concentrate, purify and reuse.
In addition, since high-boiling organic solvents may contribute to environmental pollution, the content of high-boiling organic solvents in liquids (liquids to be treated) to be discarded based on the viewpoint of reducing environmental impact There is also a desire to reduce as much as possible.

  In order to satisfy the above-mentioned demand, a liquid to be treated containing a target solvent such as a high boiling point organic solvent is separated into a concentrated liquid having a high content of the target solvent and a distillate having a low content of the target solvent. Technology to do is being researched.

  For example, Patent Document 1 includes a first evaporator, a second evaporator, and a vapor transfer pipe that transfers the vapor of the processing liquid generated in the second evaporator to the first evaporator, and the vapor transfer pipe Is connected to the first evaporator so that the vapor generated in the second evaporator is returned to the processing liquid stored in the first evaporator, and the first evaporator discharges the vapor of the processing liquid to the outside. A concentrating device is disclosed which includes a discharge pipe for the purpose.

JP 2009-82883 A

However, in the evaporator disclosed in Patent Document 1, the relationship between the concentration (content) of the high-boiling organic solvent in the distillate vapor and the concentration of the high-boiling organic solvent in the concentrate is a gas-liquid equilibrium relationship. Will be decided automatically.
Therefore, according to the evaporator disclosed in Patent Document 1, for example, when the content of the high-boiling organic solvent in the concentrated liquid is increased, the content of the high-boiling organic solvent in the distillate is also vapor-liquid equilibrium. Therefore, it is difficult to sufficiently reduce the content of the high boiling point organic solvent in the distillate vapor. On the other hand, when the content of the high-boiling organic solvent in the distillate is to be reduced, the content of the high-boiling organic solvent in the concentrate also decreases according to the vapor-liquid equilibrium relationship. It is difficult to sufficiently increase the content of the high-boiling organic solvent.
As a result, the technique disclosed in Patent Document 1 attempts to solve the above problem by providing two evaporators, a first evaporator and a second evaporator. However, since the individual evaporators have the above-mentioned limitations, the fundamental problem has not been solved.
That is, in the technique disclosed in Patent Document 1, the content of the high-boiling organic solvent in the concentrate is sufficiently increased and the high-boiling point in the distillate vapor at the same time, despite the increase in size and complexity of the equipment. There was room for improvement in terms of sufficiently reducing the content of the organic solvent.

  Therefore, the present invention separates the liquid to be treated into a concentrated liquid and a distillate, sufficiently increases the content of the high-boiling organic solvent in the concentrated liquid, and contains the high-boiling organic solvent in the distillate. It is an object to provide a solution processing apparatus capable of sufficiently reducing the amount.

  As means for solving the above problems, the present invention provides a liquid containing a high-boiling organic solvent, a concentrated liquid containing a high content of high-boiling organic solvent, and a distillate containing a low content of high-boiling organic solvent. A liquid treatment apparatus that separates the liquid to be treated into a concentrate and a distillate vapor to be a distillate, distills the distillate from the top of the tower, and removes the concentrate from the bottom of the tower. And a first heating means for heating the liquid to be processed (concentrated liquid to be processed) supplied to the bottom of the processing tower, and the liquid to be processed is installed inside the processing tower. A first gas-liquid contact means for contacting the vapor to be treated which has become gaseous by being heated; and a supply means for supplying the liquid to be treated to the inside of the treatment tower from above the first gas-liquid contact means; A solution processing apparatus comprising:

According to such a configuration, the liquid to be processed supplied from above the first gas-liquid contact means to the inside of the processing tower is first supplied to the first gas-liquid contact means. The liquid is in a state immediately after being supplied, that is, a state in which the high-boiling organic solvent is not concentrated (a state in which the content of the high-boiling organic solvent is low). Therefore, in the first gas-liquid contact means, the liquid to be processed in this state is brought into contact with the vapor to be processed that has been heated to be in a gas state, as compared with the case where the liquid to be processed in a state of advanced concentration is brought into contact. As a result, distillate with a very low content of high-boiling organic solvent can be distilled from the top of the treatment tower. Can be obtained.
When the distillate obtained from the solution treatment apparatus is treated as waste water, the content of the high-boiling organic solvent in the distillate is sufficiently reduced, so that the load on the subsequent treatment apparatus is reduced. Can be reduced.

On the other hand, in the first gas-liquid contact means, the liquid to be treated in a state where the high boiling point organic solvent is not concentrated is brought into contact with the vapor to be treated which is heated by the heating means to become a gaseous state. Can be supplied to the bottom of the processing tower. Therefore, it is possible to obtain a concentrate having a sufficiently high content of the high-boiling organic solvent.
In addition, when recycling the concentrate obtained from the solution processing apparatus, since the content of the high-boiling organic solvent in the concentrate is sufficiently high, the load on the purification apparatus used thereafter is reduced. be able to.

  Further, the solution processing apparatus preferably does not have a reflux means for condensing the distillate vapor distilled from the top of the treatment tower to form a distillate and returning the distillate to the inside of the treatment tower.

  According to such a configuration, by not having the reflux means, it is possible to reliably avoid the enormous energy consumption required in the reflux operation. As a result, it is possible to obtain a distillate in which the content of the high-boiling organic solvent is sufficiently suppressed and a concentrated liquid in which the content of the high-boiling organic solvent is sufficiently increased, and at the same time energy saving (running The effect of suppressing an increase in cost) can be obtained.

  In the solution processing apparatus, the liquid to be processed supplied from the supply unit preferably has a high-boiling organic solvent content of 10.0 wt% or less.

  According to such a configuration, the liquid to be processed supplied into the processing tower is first supplied to the first gas-liquid contact means. At this time, the content of the high-boiling organic solvent in the liquid to be processed Is a sufficiently small state of 10.0 wt% or less. As a result, in the first gas-liquid contact means, it is possible to reliably distill distillate having a very low content of high-boiling organic solvent from the top of the treatment tower. The effect of lowering the solvent content can be made more reliable.

  Moreover, the solution processing apparatus preferably includes a gas-liquid separation unit that separates droplets accompanying distillate vapor distilled from the top of the processing tower and returns the liquid droplets to the inside of the processing tower.

  According to such a configuration, the droplets accompanying the distillate distilled from the top of the processing tower, that is, a high boiling point content equal to or higher than the liquid to be processed at the time of being supplied to the processing tower. Since the liquid containing the organic solvent can be returned to the treatment tower, the effect of reducing the content of the high-boiling organic solvent in the distillate can be further ensured.

  The solution processing apparatus further includes a compression unit that compresses and raises the temperature of the distillate distilled from the top of the treatment tower, and the distillate vapor that has been compressed by the compression unit and heated is It is preferably used as a heating source for the heating means.

  According to such a structure, since the distillate vapor | steam which was compressed and heated up by the compression means is used as a heating source of a heating means, the energy required for a heating source can be reduced.

  Further, in the solution processing apparatus, the compression means is configured so that the temperature of the distilled steam distilled from the top of the processing tower is 2 ° C. or higher than the liquid to be processed at the bottom of the processing tower. It is preferable to compress and raise the temperature.

  According to such a configuration, the distillate vapor heated by the compression means is suitable as a heating source, and the effect of reducing the energy required for the heating source can be further ensured.

  Further, in the solution processing apparatus, the liquid processing apparatus is disposed inside the processing tower and below the first gas-liquid contact means, and contacts the liquid to be processed and the vapor to be processed which has become gaseous by being heated. A second gas-liquid contact means to be installed, and is installed inside the processing tower and between the first gas-liquid contact means and the second gas-liquid contact means, and is supplied from the first gas-liquid contact means Holding a predetermined amount of the liquid to be processed, holding means for supplying the liquid to be processed exceeding the predetermined amount to the second gas-liquid contact means, and compressing the distillate vapor distilled from the top of the processing tower And a second heating unit that heats the liquid to be treated held in the holding unit, and the first heating unit converts distillate vapor that has been compressed by the compression unit and raised in temperature. And as a heating source of at least one of the second heating means It is preferable to have.

According to such a configuration, in the second gas-liquid contact means, the liquid to be treated which is concentrated by the high boiling point organic solvent supplied from the first gas-liquid contact means (holding means) is heated and turned into a gaseous form. By bringing it into contact with the processing steam, the liquid to be processed in a further concentrated state can be supplied to the bottom of the processing tower. As a result, a concentrated liquid having a very high content of high boiling point organic solvent can be obtained.
And since the distillate vapor | steam compressed and heated by the compression means is used as a heating source of at least one among a 1st heating means and a 2nd heating means, the energy required for a heating source can be reduced.

  Further, in the solution processing apparatus, the high-boiling organic solvent of the liquid to be treated supplied from the supply means is a solvent having a boiling point higher than water, completely dissolved in water, and not azeotropic with water, N-methylpyrrolidone, N-ethyl-2-pyrrolidone, N, N-dimethylformamide, N, N-dimethylacetamide, dimethyl sulfoxide, ethylene glycol, diethylene glycol, triethylene glycol, propylene glycol, butyl diglycol, 1,4-butanediol, monoethanol One or more solvents selected from the group consisting of amine, diethylene glycol monomethyl ether and 1,3-dimethyl-2-imidazolidinone are preferred.

  In the solution processing apparatus, the high-boiling organic solvent of the liquid to be processed supplied from the supply means is N-methylpyrrolidone (1-methyl-2-pyrrolidone), and is a distillation distilled from the top of the processing tower. The output steam has a high-boiling organic solvent content of 0.5 wt% or less, and the concentrated liquid taken out from the bottom of the treatment tower has a high-boiling organic solvent content of 60.0 wt% or more. Is preferred.

  According to the present invention, the liquid to be treated is separated into a concentrate and a distillate, the content of the high-boiling organic solvent in the concentrate is sufficiently increased, and the content of the high-boiling organic solvent in the distillate is included. The amount can be reduced sufficiently.

It is a schematic diagram of the solution processing apparatus which concerns on 1st Embodiment of this invention. It is a schematic diagram of the solution processing apparatus which concerns on 2nd Embodiment of this invention.

Hereinafter, an embodiment (embodiment) for carrying out a solution processing apparatus according to the present invention will be described with reference to the drawings as appropriate.
In addition, about the solution which is a process target of the solution processing apparatus which concerns on this invention, the thing before being supplied to a processing tower and the thing in a processing tower are to-be-processed liquid L1 (gaseous thing is to-be-processed vapor | steam L1). The liquid after being removed from the bottom of the processing tower is indicated as concentrated liquid L2 (the gaseous one is the concentrated vapor L2), and after being distilled from the top of the processing tower, the liquid L3 ( A gaseous thing is shown as distillate vapor | steam L3).

First, the outline of the solution processing apparatus 1a according to the first embodiment will be described with reference to FIG.
<< Outline of Solution Processing Apparatus According to First Embodiment >>
The solution processing apparatus 1a according to the first embodiment uses a liquid L1 containing a high-boiling organic solvent, a concentrated liquid L2 containing a high content of high-boiling organic solvent, and a distillate containing a low content of high-boiling organic solvent. This is a device that separates into L3.
As shown in FIG. 1, the solution processing apparatus 1 a includes a processing tower 2, a first gas-liquid contact means 3 a that is installed inside the processing tower 2 and that contacts the liquid L1 to be processed and the vapor L1 to be processed, The supply means 4 for supplying the liquid to be processed L1 from above the first gas-liquid contact means 3a to the inside of the processing tower 2 and the liquid to be processed L1 at the bottom of the processing tower 2 are heated (in detail, the concentrated liquid L2 is The first heating means 6a for heating and returning to the tower bottom of the processing tower 2 raises the temperature of the liquid to be treated L1 and indirectly heats the liquid to be treated L1 and distills from the tower top of the processing tower 2 Gas-liquid separation means 7 that separates droplets accompanying the distillate vapor L3 and returns them to the inside of the processing tower 2, and compression means 8 that compresses and raises the temperature of the distillate vapor L3 distilled from the top of the treatment tower 2. And comprising.

And the solution processing apparatus 1a is equipped with the gas-liquid separator 5 which prevents entrainment in the inside of the processing tower 2. FIG. Further, the solution processing apparatus 1a includes a concentrated liquid heat exchanger 10 and a distillate liquid heat exchanger 11 in order to preliminarily heat the liquid to be processed L1 supplied from the supply means 4 to the inside of the processing tower 2. . Furthermore, the solution processing apparatus 1a includes first heating auxiliary means 9 that assists heating of the first heating means 6a. In addition, the solution processing apparatus 1a includes a cooler 13 that cools the distillate vapor L3 distilled from the processing tower 2 so as not to leak out of the system (a vacuum pump (not shown)) to form a distillate L3, A holding can 12 that is provided upstream of the cooler and stores condensed condensed distillate L3.
The solution processing apparatus 1a includes pipes t1 to t20 for flowing liquid or gas between the devices, and includes pumps P1, P2, and P3 for flowing liquid or gas in a predetermined direction.

Next, each device of the solution processing apparatus 1a according to the first embodiment will be described with reference to FIG.
<Processing tower>
The treatment tower 2 separates the liquid to be treated L1 into a concentrated liquid L2 and a distillate vapor L3.
The processing tower 2 has a cylindrical shape as a whole, and includes a first gas-liquid contact means 3a described later, and a gas-liquid separator 5 above the first gas-liquid contact means 3a. Further, the processing tower 2 includes a supply unit 4 described later between the first gas-liquid contact unit 3 a and the gas-liquid separator 5.

  The treatment tower 2 is provided with an outlet (distillation outlet) for the distilled steam L3 at the top of the tower, and the outlet is connected to the inlet of the gas-liquid separation means 7 via a pipe t4. The processing tower 2 is provided with two outlets of the concentrate L2 at the bottom of the tower, and one outlet (can outlet) is connected to the inlet of the first heating means 6a via the pipe t14, the pump P2, and the pipe t15. The other outlet is connected to the pipe t20 that goes to the outside of the system via the branched pipe t16, and the other outlet is connected to the inlet of the first heating auxiliary means 9 via the pipe t17.

<First gas-liquid contact means>
The first gas-liquid contact means 3a is means for bringing the vapor separated from the liquid L1 to be processed into liquid-liquid contact.

  The 1st gas-liquid contact means 3a is provided in the inside of the processing tower 2, and can use a shelf. This shelf may be a single tray or two or more trays stacked at a predetermined interval in the vertical direction, such as perforated plate trays, valve trays, bubble bell trays, lift trays, etc. Any of the contact trays may be used.

The first gas-liquid contact means 3a is not particularly limited as long as it can appropriately contact the liquid L1 to be processed and the vapor L1 to be processed. Known gas-liquid contact means such as regular packing can be used.
The number of trays (the number of trays) and the bed height of the packing may be determined based on the desired high boiling point organic solvent content of the concentrated liquid L2, physical properties, and the like.

<Supply means>
The supply means 4 is a means for supplying the liquid L1 to be processed into the processing tower 2.
The supply means 4 is provided above the first gas-liquid contact means 3a and has a tubular shape so that the liquid L1 to be treated flows.
In FIG. 1, the supply means 4 is provided so as to protrude inward from the inner wall of the processing tower 2, but is a means capable of supplying the liquid L1 to be processed above the first gas-liquid contact means 3a. If there is, it will not specifically limit, For example, a spray nozzle may be sufficient so that the to-be-processed liquid L1 can be supplied to the upper whole surface of the 1st gas-liquid contact means 3a.
<First heating means>
The 1st heating means 6a is a means to heat the to-be-processed liquid L1 supplied to the tower bottom part of the processing tower 2. As shown in FIG.
The first heating means 6a heats the concentrate L2 supplied from the outlet at the bottom of the processing tower 2 via the pipe t14, the pump P2, and the pipe t15 by exchanging heat with a heating source (heat medium). The concentrated liquid L2 that is a heater and is heated by the heater is supplied into the processing tower 2 in a liquid or gas state via the pipe t18. As a heating source of the heater, distillate vapor L3 compressed by the compression means 8 and heated is used.

  The inlet of the distillate vapor L3 (heating source) of the first heating means 6a is connected to the outlet of the compression means 8 via the pipe t7, and the outlet of the distillate L3 (heating source) of the first heating means 6a is The holding can 12 is connected to the inlet via the pipe t8.

When using the heater which heats the concentrated liquid L2 as described above and returns it to the processing tower 2 as the first heating means 6a, a multi-tube heat exchanger, a plate heat exchanger, a shell plate heat exchanger, a spiral A known heat exchanger such as a heat exchanger can be used.
And as a heating source (heat medium) of a heater, well-known heating sources, such as the steam heated up by means other than the compression means 8, and an electric heater other than the distillate vapor | steam L3 heated up by the compression means 8, are used. Can do.

  The first heating means 6a is not particularly limited as long as it can appropriately heat the liquid L1 to be treated. In addition to the heater for heating the concentrated liquid L2 and returning it to the processing tower 2, Known heating means such as a heater for heating the liquid L1 to be processed in the processing tower 2 using a heat medium such as steam can be used.

<Gas-liquid separation means>
The gas-liquid separation means 7 is means for separating the droplets accompanying the distillate vapor L3 distilled from the top of the processing tower 2 and returning it to the inside of the processing tower 2.
The gas-liquid separation means 7 can use a cyclone type gas-liquid separation device. This cyclone type gas-liquid separation device is provided with piping and a plurality of blades that are inclined around an axis along the flow direction (horizontal direction) of the distillate vapor L3 inside the piping. In the cyclone type gas-liquid separator, the inclined blades give a swirling flow to the distillate vapor L3, the gaseous distillate vapor L3 moves straight while swirling, and the accompanying droplet is pressed against the inner wall surface. It becomes. As a result, the cyclone type gas-liquid separator can separate the accompanying droplets from the distillate vapor L3.

The inlet of the distilling vapor L3 of the gas-liquid separating means 7 is connected to the outlet of the top of the processing tower 2 via a pipe t4, and the outlet of the distilling vapor L3 of the gas-liquid separating means 7 is connected via a pipe t6. It is connected to the inlet of the compression means 8.
And the discharge port which discharges | emits the droplet isolate | separated by the gas-liquid separation means 7 was provided in the tower side vicinity (above 1st gas-liquid contact means 3a) vicinity of the tower | column top of the processing tower 2 via piping t5. Connected to the supply port.

The gas-liquid separation means 7 is not particularly limited as long as it is a means capable of appropriately separating the entrained droplets and returning them to the processing tower 2. In addition to the cyclone-type gas-liquid separation device, a baffle plate Known gas-liquid separation means such as a type gas-liquid separator and a wire mesh type gas-liquid separator can be used.
However, among these gas-liquid separation means 7, it is preferable to use a cyclone-type gas-liquid separation device that can suppress pressure loss.

<Compression means>
The compression means 8 is a means for compressing and raising the temperature of the distillate vapor L3 distilled from the top of the processing tower 2.
And the compression means 8 compresses the distillate vapor | steam L3 distilled from the tower top part of the processing tower 2 so that temperature may become 2 degreeC or more higher than the to-be-processed liquid L1 of the tower bottom part of the processing tower 2. Raise the temperature. Thereby, the distillate vapor | steam L3 used as a heating source of the 1st heating means 6a becomes 2 degreeC or more higher than the to-be-processed liquid L1 of the tower bottom part of the processing tower 2 which is heating object, Distilled vapor | steam L3 becomes It is suitable as a heating source.

  The inlet of the distillate vapor L3 of the compression means 8 is connected to the outlet of the gas-liquid separation means 7 via the pipe t6, and the outlet of the distillate vapor L3 of the compression means 8 is connected to the first heating means 6a via the pipe t7. Connected to the entrance.

  The compression means 8 is not particularly limited as long as it is a means capable of compressing and raising the temperature of the distillate vapor L3. If it is a mechanical compression device, it can be a multi-stage turbo blower, screw type compression, in addition to a roots blower. Known compression means such as a machine, a vane compressor, a diaphragm compressor, and other ejectors can be used. The compression means 8 may be selected from known compression means according to the degree of pressure increase required, the amount of distillate vapor generated, economy, and the like.

<Other configuration of the solution processing apparatus according to the first embodiment>
(Gas-liquid separator)
The gas-liquid separator 5 is a mesh-like structure that is provided at the top of the processing tower 2 and prevents entrainment of the distillate vapor L3, and is, for example, a mist eliminator.
As shown in FIG. 1, the solution processing apparatus 1a may be configured to include both the gas-liquid separator 5 and the gas-liquid separating means 7 in order to reliably prevent entrainment of droplets, but only one of them may be used. May be provided.

(First heating auxiliary means, concentrate heat exchanger, distillate heat exchanger)
The first heating auxiliary means 9, the concentrate heat exchanger 10, and the distillate heat exchanger 11 use known heat exchangers, and steam S, concentrate L2, and distillate L3 are used as heat media, respectively. Use.
Note that the heat medium of the first heating auxiliary means 9 may be an electric heater.

  The inlet of the concentrated liquid L2 of the first heating auxiliary means 9 is connected to the outlet of the bottom of the processing tower 2 via the pipe t17, and the outlet of the concentrated liquid L2 (liquid and gaseous) of the first heating auxiliary means 9 Is connected to a supply port provided on the side of the tower near the bottom of the processing tower 2 via a pipe t19.

  The inlet of the liquid to be processed L1 of the concentrate heat exchanger 10 is connected to the outside via the pipe t1 and the pump P1, and the outlet of the liquid to be processed L1 of the concentrate heat exchanger 10 is distilled through the pipe t2. It is connected to the inlet of the liquid heat exchanger 11. The inlet of the concentrate L2 of the concentrate heat exchanger 10 is connected to the outlet of the bottom of the processing tower 2 via the pipe t16, the pump P2, and the pipe t14, and the concentrate L2 of the concentrate heat exchanger 10 is connected. The outlet is connected outside the system via a pipe t20.

  The outlet of the liquid L1 to be treated of the distillate heat exchanger 11 is connected to the supply means 4 via a pipe t3. The inlet of the distillate L3 of the distillate heat exchanger 11 is connected to the outlet of the holding can 12 via the pipe t12, the pump P3, and the pipe t11, and the distillate L3 of the distillate heat exchanger 11 is connected. Is connected to the outside via a pipe t13.

(Cooler, holding can)
The cooler 13 is a device that cools the distillate vapor L3 to a distillate L3 so that the distillate vapor L3 does not leak out of the system (a vacuum pump (not shown)).
The holding can 12 holds the distillate L3 made liquid by the first heating means 6a and the distillate L3 made liquid by the cooler 13 on the bottom side.

The inlet of the distilling steam L3 of the cooler 13 is connected to the outlet of the holding can 12 via a pipe t9, and the outlet of the steam of the cooler 13 is connected to the outside of the system (a vacuum pump not shown) via the pipe t10. To do.
The inlet of the distillate L3 of the holding can 12 is connected to the outlet of the first heating means 6a via the pipe t8, and the outlet of the distillate L3 of the holding can 12 is connected via the pipe 11, the pump P3, and the pipe t12. And connected to the inlet of the distillate heat exchanger 11.

≪About reflux means≫
The solution processing apparatus 1a does not have a reflux means. In other words, the solution processing apparatus 1a is an apparatus related to evaporation (simple distillation) not using the refluxing means, not the rectification using the refluxing means.
Here, the reflux means is a means for condensing the distillate vapor L3 distilled from the top of the treatment tower 2 into a distillate L3 and returning the distillate L3 to the inside of the treatment tower 2.

  According to the solution processing apparatus 1a, the distillate L3 having a sufficiently low content of the high-boiling organic solvent and the concentrate L2 having a sufficiently high content of the high-boiling organic solvent can be obtained. There is no need to have.

In addition, since the solution processing apparatus 1a does not have the reflux means, it is possible to reliably avoid the enormous energy consumption required in the reflux operation.
However, the energy consumption is not limited, and when the content of the high-boiling organic solvent in the distillate L3 must be further reduced, a reflux means may be provided in the solution processing apparatus 1a.

  The solution processing apparatus 1a may be provided with an internal reflux means. Here, the internal reflux means is means for condensing the vapor L1 to be processed inside the processing tower 2 and supplying the condensed liquid L1 to be processed to a gas-liquid contact means or the like inside the processing tower 2. When applied to the solution processing apparatus 1a, for example, a known cooler may be provided as an internal reflux means inside the processing tower 2 and above the gas-liquid separator 5.

Next, the liquid L1 to be processed in the solution processing apparatus according to the present invention will be described, and the concentrated liquid L2 and the distillate L3 obtained by processing the liquid L1 will be described.
≪Processed liquid≫
The liquid L1 to be treated is a solution containing a high-boiling organic solvent and water, and more specifically, water (solution) containing a high-boiling organic solvent used in washing processes and manufacturing processes in various industrial fields. ).

The high boiling point organic solvent of the liquid L1 to be treated is a solvent having a boiling point higher than that of water, completely dissolved in water, and does not azeotrope with water.
High boiling point organic solvents include N-methylpyrrolidone (NMP), N-ethyl-2-pyrrolidone (NEP), N, N-dimethylformamide (DMF), N, N-dimethylacetamide (DMAc), dimethyl sulfoxide ( DMSO), ethylene glycol (EG), diethylene glycol (DEG), triethylene glycol (TEG), propylene glycol (PG), butyl diglycol (BDG), 1,4-butanediol (1,4-BD), monoethanol The solvent is preferably one or more solvents selected from the group consisting of amine (MEA), diethylene glycol monomethyl ether (DGME), and 1,3-dimethyl-2-imidazolidinone (DMI).
Since these high-boiling organic solvents are highly reusable solvents, the solution processing apparatus according to the present invention contributes to recycling by sufficiently concentrating the high-boiling organic solvents in the concentrate L2. The effect can be made more certain.

  The content of the high-boiling organic solvent in the liquid to be treated L1 is preferably 10.0 wt% or less, and more preferably 5.0 wt% or less. If the content of the high-boiling organic solvent in the liquid to be treated L1 is not more than a predetermined value, the effect of lowering the content of the high-boiling organic solvent in the distillate L3 can be made more reliable. is there.

  When the high boiling point organic solvent is NMP, the content of NMP in the liquid to be treated L1 is preferably 10.0 wt% or less. This is because when the NMP content of the liquid to be treated L1 is 10.0 wt% or less, the effect of reducing the NMP content in the distillate L3 can be made more reliable.

≪Concentrate≫
The concentrated liquid L2 is a solution having a high content of high-boiling organic solvent compared to the content of the high-boiling organic solvent in the liquid L1 to be processed, and the liquid L1 is processed by the solution processing apparatus according to the present invention. It is a solution obtained by doing.

  When the high boiling point organic solvent is NMP, the content of NMP in the concentrate L2 is preferably 60.0 wt% or more, and more preferably 80.0 wt% or more. When the NMP content of the concentrate L2 is 60.0 wt% or more, it becomes advantageous in terms of cost when recycling the NMP of the concentrate L2, and the concentrate L2 can be handled as a valuable resource. Moreover, it is because the load concerning the refiner | purifier used after processing with the solution processing apparatus of this invention can be reduced that it is 80.0 wt% or more.

  However, when the high boiling point organic solvent is NMP, if the NMP content of the concentrate L2 is 85.0 wt% or more, it is regarded as a dangerous substance by the Fire Service Act. In this case, the NMP content of the concentrate L2 The amount is preferably less than 85.0 wt%.

Table 1 shows an example of the NMP vapor-liquid equilibrium relationship at 53.3 kPa.
From Table 1 below, regarding the content of NMP in the solution (NMP liquid composition), the temperature difference between 0.0 and 60.0 wt% is only 4.5 ° C, but 0.0 to 80.0 wt% It can be seen that the temperature difference between% is 11.7 ° C. Here, if the temperature difference of the distillate vapor | steam 3 in the inlet side (pipe t6 side) and the exit side (pipe t7 side) of the compression means 8 becomes large, the motive power (energy) required for the compression means 8 will also become large.
That is, in order to obtain the concentrated liquid L2 when the NMP content is about 80.0 wt%, compared to the case where the NMP content is about 60.0 wt%, the concentrated liquid L2 is heated. Since the temperature difference of the distilled steam L3 needs to be 2.5 times or more by the compression means 8, the energy required for the compression means 8 is significantly increased.
Therefore, according to the solution processing apparatus of the present invention, it is necessary to consider the performance of the compression means 8 to be used, the energy required for the compression means 8, and the like, but the content of the high-boiling organic solvent in the concentrate L2 is set to 60. It can be seen that it can be 0.0 wt% or more and 80.0 wt% or more.

≪Distillate≫
The distillate L3 is a solution having a low content of the high-boiling organic solvent compared to the content of the high-boiling organic solvent in the liquid L1 to be treated. The liquid L1 is treated by the solution treatment apparatus according to the present invention. It is a solution obtained by processing. The distillate L3 is obtained by condensing and condensing the distillate vapor L3 distilled from the processing tower 2 by increasing the pressure and raising the temperature by the compression means 8 and passing through the first heating means 6a.

  When the high boiling point organic solvent is NMP, the content of NMP in the distillate L3 is preferably 0.5 wt% or less. This is because, when the content of NMP in the distillate L3 is 0.5 wt% or less, it is possible to reduce the load on the processing apparatus after processing by the solution processing apparatus according to the present invention.

Table 2 shows an example of the NMP vapor-liquid equilibrium relationship at 53.3 kPa.
From Table 2 below, when the NMP content in the solution (NMP liquid composition) is 5.0 wt%, the NMP content in the vapor (NMP vapor composition) becomes 0.2 wt%, and the NMP content in the solution It can be seen that when the amount (NMP liquid composition) is 10.0 wt%, the NMP content (NMP vapor composition) in the steam is 0.5 wt%.
That is, when the NMP content of 10.0 wt% is used as the liquid L1 to be processed, according to the solution processing apparatus according to the present invention, in the first gas-liquid contact means 3a based on the gas-liquid equilibrium relationship, Distilled vapor L3 having an NMP content of 0.5 wt% can be distilled from the treatment tower 2.
Therefore, according to the solution processing apparatus which concerns on this invention, it turns out that content of the high boiling point organic solvent of the distillate L3 can be 0.5 wt% or less.

Next, the processing method of the to-be-processed liquid L1 by the solution processing apparatus 1a which concerns on 1st Embodiment is demonstrated using FIG.
<< Processing Method for Liquid to be Processed by Solution Processing Apparatus According to First Embodiment >>
First, when the pump P1 is operated, the liquid L1 to be treated is supplied to the concentrate heat exchanger 10 through the pipe t1. In the concentrated liquid heat exchanger 10, heat exchange is performed between the supplied liquid L1 and the concentrated liquid L2, and the liquid L1 is heated and the concentrated liquid L2 is cooled.

Next, the to-be-processed liquid L1 heated up in the concentrate heat exchanger 10 is supplied to the distillate liquid heat exchanger 11 through the piping t2. In the distillate liquid heat exchanger 11, heat exchange is performed between the supplied liquid L1 and the distillate L3, the liquid L1 is heated, and the distillate L3 is cooled.
And the to-be-processed liquid L1 heated up in the distillate liquid heat exchanger 11 is supplied in the process tower 2 through the piping t3 and the supply means 4. FIG.

  The liquid L1 to be processed supplied into the processing tower 2 is first supplied to the first gas-liquid contact means 3a. Here, the liquid L1 to be processed is in a state immediately after being supplied into the processing tower 2, that is, in a state in which the high-boiling organic solvent is not concentrated. Therefore, the to-be-processed liquid L1 in this state comes into contact with the to-be-processed vapor L1 rising from the bottom side of the processing tower 2. As a result, the vaporization phenomenon of the liquid to be treated L1 occurs on the basis of the vapor-liquid equilibrium relationship of the solution having a small content of the high boiling organic solvent, so that the vapor to be treated L1 having a very low content of the high boiling organic solvent is treated. Ascend to the tower top side of tower 2.

<Distillate side>
The to-be-processed vapor | steam L1 which rose to the tower | column top side of the processing tower 2 passes the gas-liquid separator 5, passes through piping t4 from the exit (distillation port) of a tower | column top part, and is vapor-liquid separation means 7 as the distillate vapor | steam L3. To be supplied. Note that the liquid to be processed L1 is trapped by the gas-liquid separator 5 so that the liquid to be processed L1 supplied from the supply unit 4 remains in a liquid state and does not distill as the distillate L3 (that is, does not entrain with droplets). , Supplied to the first gas-liquid contact means 3a.
Further, the droplets accompanying the distillate vapor L3 supplied to the gas-liquid separation means 7 are separated from the distillate vapor L3 by the gas-liquid separation means 7, and the separated droplets pass through the pipe t5 and pass through the processing tower. Returned to 2.

Next, the distillate vapor L3 from which droplets have been removed in the gas-liquid separation means 7 is supplied to the compression means 8 through the pipe t6. In this compression means 8, the supplied distillate vapor | steam L3 is compressed and it heats up.
And the distillate vapor | steam L3 heated up in the compression means 8 is supplied to the 1st heating means 6a through the piping t7. In the first heating means 6a, heat exchange is performed between the supplied distillate vapor L3 and the concentrate L2, the distillate vapor L3 is condensed, and the concentrate L2 recovers the latent heat of vaporization of the distillate vapor L3. As a result, the temperature rises and a part of the gas is vaporized.

Next, the distillate L3 condensed in the first heating unit 6a is supplied to the holding can 12 through the pipe t8.
Cooling provided between the pipe t9 and the pipe t10 so that the distillate vapor L3 does not leak out of the system (vacuum pump not shown) through the pipe t8, the holding can 12, the pipe t9, and the pipe t10. Cooled by the cooling water W in the vessel 13. Then, the distillate L3, which has been cooled and condensed, flows down in the cooler 13, passes through the pipe t9, and is stored on the bottom side of the holding can 12.
In addition, the pressure of the solution processing apparatus 1a is brought into a desired reduced pressure state by suctioning the solution processing apparatus 1a through the pipe t10, the cooler 13, the holding can 12 and the like by a vacuum pump (not shown).

The distillate L3 stored on the bottom side of the holding can 12 is supplied to the distillate heat exchanger 11 through the pipe t11 and the pipe t12 by the pump P3 that operates. In the distillate heat exchanger 11, as described above, heat exchange is performed between the supplied distillate L3 and the liquid to be treated L1, the temperature of the distillate L3 is lowered, and the liquid to be treated L1 is raised. Warm up.
Finally, the distillate L3 cooled in the distillate heat exchanger 11 flows out of the system of the solution processing apparatus 1a through the pipe t13.

<Concentrate side>
On the other hand, in the first gas-liquid contact means 3a, the liquid L1 having a high content of high-boiling organic solvent flows down in the first gas-liquid contact means 3a and is supplied to the bottom of the processing tower 2. And the to-be-processed liquid L1 supplied to the tower bottom part of the processing tower 2 is supplied to the 1st heating means 6a by the pump P2 which act | operates as a concentrate L2 through the piping t14 and the piping t15. The part passes through the pipe t14 and the pipe t16 and is supplied to the concentrate heat exchanger 10. Further, a part of the liquid L1 to be processed supplied to the bottom of the processing tower 2 is supplied as the concentrated liquid L2 to the first heating auxiliary means 9 through the pipe t17.

  In the 1st heating means 6a, as above-mentioned, heat exchange is performed between the supplied concentrate L2 and the distillate vapor | steam L3, the concentrate L2 evaporates partially, and the distillate vapor | steam L3 condenses. Moreover, in the 1st heating assistance means 9, heat exchange is performed between the supplied concentrate L2 and the steam S, and the concentrate L2 will partially evaporate. Then, the concentrated liquid L2 heated by the first heating means 6a and the first heating auxiliary means 9 passes through the pipe t18 and the pipe t19 and returns to the inside of the processing tower 2 to be evaporated by being heated. The treated vapor L1 rises to the tower top side (the first gas-liquid contact means 3a side) of the treatment tower 2 and the liquid L1 to be treated which remains in the liquid state is supplied to the tower bottom of the treatment tower 2.

In the concentrate heat exchanger 10, as described above, heat exchange is performed between the supplied concentrate L2 and the liquid L1 to be processed, the temperature of the concentrate L2 is decreased, and the temperature of the liquid L1 to be processed is increased. .
Finally, the concentrated liquid L2 cooled in the concentrated liquid heat exchanger 10 flows out of the solution processing apparatus 1a through the pipe t20.

Next, an outline of the solution processing apparatus 1b according to the second embodiment will be described with reference to FIG.
In the description of the second embodiment, the description of the configuration common to the first embodiment will be omitted, and the description will focus on the configuration that is different.

<< Outline of Solution Processing Apparatus According to Second Embodiment >>
Similarly to the solution processing apparatus 1a according to the first embodiment, the solution processing apparatus 1b according to the second embodiment converts the liquid L1 containing the high-boiling organic solvent into the concentrated liquid L2 containing a high content of the high-boiling organic solvent. And a distillate L3 having a low content of high-boiling organic solvent.

As shown in FIG. 2, in addition to the configuration of the solution processing apparatus 1a shown in FIG. 1, the solution processing apparatus 1b is a second installed inside the processing tower 2 and below the first gas-liquid contact means 3a. A gas-liquid contact means 3b; a holding means 14 installed in the processing tower 2 between the first gas-liquid contact means 3a and the second gas-liquid contact means 3b; Second heating means 6b for heating the treatment liquid L1.
And the solution processing apparatus 1b is provided with the control valve 15 and the condenser 16 in addition to the structure of the solution processing apparatus 1a shown in FIG.
The solution processing apparatus 1b includes pipes t1 to t30 for flowing liquid or gas between the devices, and includes pumps P1 to P4 for flowing liquid or gas in a predetermined direction.

Next, each device of the solution processing apparatus 1b according to the second embodiment will be described with reference to FIG.
<Second gas-liquid contact means>
The second gas-liquid contact means 3b is means for bringing the vapor separated from the liquid L1 to be processed into liquid-liquid contact.
The second gas-liquid contact means 3b is provided inside the processing tower 2 and below the first gas-liquid contact means 3a. As the second gas-liquid contact means 3b, known gas-liquid contact means such as a shelf, regular packing, and irregular packing can be used as in the case of the first gas-liquid contacting means 3a.
The first gas-liquid contact means 3a and the second gas-liquid contact means 3b may be the same type of combination (for example, a shelf and a shelf) or different types of combinations (for example, a shelf and a regular packing). May be.

<Holding means>
The holding unit 14 is a unit that holds a predetermined amount of the liquid L1 supplied from the first gas-liquid contact unit 3a and supplies the liquid L2 that exceeds the predetermined amount to the second gas-liquid contact unit 3b. .
The holding means 14 is installed inside the processing tower 2 and between the first gas-liquid contact means 3a and the second gas-liquid contact means 3b. And the holding means 14 can use the chimney tray 14a and the pipe t26 for supplying the liquid L1 to be processed held in the chimney tray 14a to the second gas-liquid contact means 3b.

The chimney tray 14a includes a tray having a through hole, and a stand pipe that protrudes upward from the through hole of the tray and allows the steam L1 to flow from the lower side to the upper side of the tray. The pipe t26 supplies the liquid L1 to be processed held on the tray portion of the chimney tray 14a to the second gas-liquid contact means 3b at a predetermined flow rate.
The holding means 14 is not particularly limited as long as it can hold a liquid, and a liquid collector other than a chimney tray may be used.

<Second heating means>
The 2nd heating means 6b is a means to heat the to-be-processed liquid L1 hold | maintained at the holding means 14. FIG.
As the second heating means 6b, a heater similar to the first heating means 6a can be used. This heater heats the liquid L1 supplied from the holding means 14 of the processing tower 2 via the pipe t21, the pump P2, and the pipe t22 by exchanging heat with a heating source (heat medium). The liquid L1 heated by the heater is supplied in a liquid or gas state to the inside of the processing tower 2 (above the holding means 14) via the pipe t23. As a heating source of the heater, distillate vapor L3 compressed by the compression means 8 and heated is used.

  The inlet of the liquid to be processed L1 (heating target) of the second heating means 6b is connected to an outlet provided on the side of the tower near the installation of the holding means 14 of the processing tower 2 via the pipe t22, the pump P2, and the pipe t21. The outlet of the liquid L1 to be processed (heating target) of the second heating means 6b is connected to a supply port provided on the side of the tower near the installation of the holding means 14 of the processing tower 2 via a pipe t23.

And the 1st heating means 6a and the 2nd heating means 6b may be the same kind combination (for example, the heater of the composition which returns the heated liquid to processing tower 2, and the heater of the same composition as the heater), Different combinations (for example, a heater configured to return the heated liquid to the processing tower 2 and a heater that directly heats the liquid L1 to be processed in the processing tower 2) may be used.
In FIG. 2, the solution processing apparatus 1 b includes a compression unit 8 corresponding to the second heating unit 6 b, but a compression unit corresponding to the first heating unit 6 a (compression ratio than the compression unit 8). (High compression means) may be further provided.

<Other configuration of the solution processing apparatus according to the second embodiment>
(Control valve, condenser)
The control valve 15 is provided between the pipe t6 and the pipe t24, and adjusts the flow rate of the distillate vapor L3 flowing to the pipe t24 side by opening and closing.
And the condenser 16 is a well-known heat exchanger which condenses the distillate vapor | steam L3 by cooling with the cooling water W, and makes it the distillate L3.

Next, the processing method of the to-be-processed liquid L1 by the solution processing apparatus 1b which concerns on 2nd Embodiment is demonstrated using FIG.
In the description of the second embodiment, the description of the parts common to the first embodiment will be omitted, and different parts will be mainly described.

«Method of processing liquid to be processed by solution processing apparatus according to second embodiment»
<About the holding means and the second gas-liquid contact means>
In the first gas-liquid contact means 3a, the liquid liquid L1 having a high content of high-boiling organic solvent flows down in the first gas-liquid contact means 3a and is supplied to the holding means 14. Then, a part of the liquid L1 to be treated supplied to the holding means 14 is supplied to the second heating means 6b through the pipe t21 and the pipe t22 by the pump P2 that operates. In the second heating means 6b, heat exchange is performed between the supplied liquid L1 to be distilled and the distilled vapor L3, the liquid L1 to be partially evaporated, and the distillate vapor L3 is condensed. And the to-be-processed vapor | steam which became gaseous by being heated because the to-be-processed liquid L1 which heated up by the 2nd heating means 6b and was partially evaporated returns to the inside of the processing tower 2 through piping t23. L1 rises to the tower top side (the first gas-liquid contact means 3a side) of the treatment tower 2, and the liquid L1 to be treated that remains liquid is supplied to and held by the holding means 14.

And if the to-be-processed liquid L1 hold | maintained in the holding | maintenance means 14 exceeds predetermined amount, the to-be-processed liquid L1 exceeding the said predetermined amount will be supplied to the 2nd gas-liquid contact means 3b via the piping t26.
The liquid to be processed L1 supplied to the second gas-liquid contact means 3b comes into contact with the vapor to be processed L1 rising from the tower bottom side of the processing tower 2. As a result, the to-be-processed vapor | steam L1 with little content of a high boiling point organic solvent passes through the holding means 14, and rises to the tower top side of the processing tower 2. On the other hand, the liquid L1 to be processed having a high content of high-boiling organic solvent flows down in the second gas-liquid contact means 3b and is supplied to the bottom of the processing tower 2.
That is, according to the solution processing apparatus 1b according to the second embodiment, since two gas-liquid contact means are provided in the processing tower 2, compared with the solution processing apparatus 1a according to the first embodiment, the concentrated liquid. It becomes possible to further increase the content of the high-boiling organic solvent in L2.

<Regulator valves and condensers>
A part of the distillate vapor L3 from which liquid droplets have been removed in the gas-liquid separation means 7 is supplied to the condenser 16 through the control valve 15 and the pipe t24.
Specifically, the control valve 15 that has received a signal that the pressure inside the solution processing apparatus 1b has become high causes the piping t6 and the piping t24 to be in communication with each other, thereby causing excess distillation in the processing tower 2. The vapor L3 is sucked (vacuum) by a vacuum pump (not shown) through the pipe t10, the cooler 13, the holding can 12, the pipe t25, the condenser 16, and the pipe t24. Furthermore, the distillate vapor L3 supplied to the condenser 16 is condensed by the cooling water W to become a distillate L3, passes through the pipe t25, and is stored on the bottom side of the holding can 12. Thereby, by providing the 1st heating means 6a and the 2nd heating means 6b, the whole pressure of the solution processing apparatus 1b in which the pressure in an apparatus tends to become high is made into a desired pressure reduction state.

  The configuration of the solution processing apparatus and the processing method according to the present embodiment are as described above. However, other configurations that are not clearly shown may be any conventionally known ones, and can be obtained by the above configuration. Needless to say, there is no limitation as long as the effect is achieved.

Next, the liquid treatment apparatus according to the present invention will be specifically described with reference to examples.
<< Example 1 corresponding to the first embodiment >>
Example 1 corresponding to the first embodiment will be described with reference to FIG.

<Conditions>
As the liquid to be treated L1, wastewater having an NMP content of 5 wt% was used. This waste water was supplied to the solution treatment apparatus 1a (specifically, the concentrated liquid heat exchanger 10) at 100 kg / h.

The pressure at the top of the treatment tower 2 was maintained at 53.3 kPa, and the temperature was 83 ° C. The pressure at the bottom of the treatment tower 2 was kept at 53.5 kPa, and the temperature was 88 ° C.
In order to maintain the pressure and temperature inside the processing tower 2 (top and bottom), the compression means 8 is a suction pressure of 53.3 kPa (83 ° C.) and a discharge pressure of 93.9 kPa (98 ° C.). Roots blower was used. The shaft power of the roots blower was 8.1 kW. Further, the steam S supplied to the first heating auxiliary means 9 was 5 kg / h in a steady state.

The first gas-liquid contact means 3a used a high-performance ordered packing, and the layer height was 600 mm.
As for the bed height of the high-performance ordered packing, when simulated from the vapor-liquid equilibrium relationship of water and NMP, 5 wt% NMP is concentrated to 60 wt% in the first stage of the theoretical stage, and the concentration of the distillate distilled further. Since a simulation result of 0.5 wt% was obtained, the layer height was set to 600 mm as the filling height corresponding to one theoretical plate.

The first heating means 6a was a saddle-type cannulated downflow heat exchanger (heat transfer area 7.8 m ² ).
Other various conditions are as described in the configuration and processing method described as the first embodiment.

<Result>
The amount of the recovered distillate L3 (specifically, the amount flowing out of the distillate heat exchanger 11) was 92.13 kg / h, and the NMP content was 0.3 wt%. Further, the amount of the concentrated liquid L2 recovered (specifically, the amount flowing out of the concentrated liquid heat exchanger 10) was 7.87 kg / h, and the NMP content was 60 wt%.
Here, when trying to obtain a result similar to the above result using a single-column normal distillation column operated at a reflux ratio of 0.2, the steam is 113 kg / h (≈92.13 (kg / h) × 1. 2 × 551/539) is required. In the above formula, “551” is the value of the latent heat of vaporization (kcal / kg) of the liquid to be treated at 83 ° C., and “539” is the latent heat of vaporization of steam at 100 ° C. (kcal / kg). Value.
Therefore, according to the solution processing apparatus 1a according to the present invention, the required steam (energy) is about 4.4% (≈5 ( kg / h) / 113 (kg / h) × 100).

<< Example 2 corresponding to 2nd Embodiment >>
Example 2 corresponding to the second embodiment will be described with reference to FIG.
<Conditions>
Various conditions different from Example 1 corresponding to the first embodiment are as follows.
The pressure in the vicinity of the holding means 14 of the processing tower 2 was kept at 53.5 kPa, and the temperature was 88 ° C. The pressure at the bottom of the treatment tower 2 was kept at 53.7 kPa, and the temperature was 95 ° C.
In addition, the steam S supplied to the 1st heating means 6a was 10 kg / h in the steady state.

The second gas-liquid contact means 3b used a high-performance ordered packing, and the layer height was 600 mm.
Note that the layer height of the high-performance ordered packing was determined for the same reason as in Example 1.
The second heating means 6b was a saddle-type cannulated downflow heat exchanger (heat transfer area 7.8 m ² ).
Other various conditions are as described in the configuration and processing method described as the second embodiment.

<Result>
The amount of the recovered distillate L3 (specifically, the amount flowing out from the distillate heat exchanger 11) was 94.10 kg / h, and the NMP content was 0.3 wt%. The amount of the concentrated liquid L2 recovered (specifically, the amount flowing out of the concentrated liquid heat exchanger 10) was 5.90 kg / h, and the NMP content was 80 wt%.
Therefore, according to the solution processing apparatus 1b of the present invention, the required steam (energy) is about 8.7% (≈10 (kg) compared with the single-column normal distillation column operated at a reflux ratio of 0.2. / H) / 115 (kg / h) × 100).

1a Solution processing apparatus (solution processing apparatus) according to the first embodiment
1b Solution processing apparatus (solution processing apparatus) according to the second embodiment
2 treatment tower 3a first gas-liquid contact means 3b second gas-liquid contact means 4 supply means 5 gas-liquid separator 6a first heating means 6b second heating means 7 gas-liquid separation means 8 compression means 9 first heating auxiliary means 10 Condensate heat exchanger 11 Distillate liquid heat exchanger 12 Holding can 13 Cooler 14 Holding means 14a Chimney tray 15 Control valve 16 Condenser L1 Liquid to be treated, steam to be treated L2 Concentrated liquid L3 Distillate, distillate steam t1 -T30 piping P1-P4 pump

Claims (9)

A solution treatment apparatus for separating a liquid to be treated containing a high-boiling organic solvent into a concentrated liquid having a high content of high-boiling organic solvent and a distillate having a low content of high-boiling organic solvent,
A treatment tower for separating the liquid to be treated into a concentrated liquid and a distillate vapor to be a distillate, distilling the distillate vapor from the top of the tower, and taking out the concentrate from the bottom of the tower;
A first heating means for heating the liquid to be treated supplied to the bottom of the treatment tower;
A first gas-liquid contact means that is installed inside the processing tower and contacts the liquid to be processed and the vapor to be processed that has become gaseous by being heated;
Supply means for supplying a liquid to be processed into the processing tower from above the first gas-liquid contact means;
A solution processing apparatus comprising:   2. The apparatus according to claim 1, further comprising a reflux unit that condenses the distillate distilled from the top of the treatment tower to form a distillate and returns the distillate to the inside of the treatment tower. Solution processing equipment.   3. The solution processing apparatus according to claim 1, wherein the liquid to be processed supplied from the supply unit has a high boiling point organic solvent content of 10.0 wt% or less.   4. The gas-liquid separation unit according to claim 1, further comprising a gas-liquid separation unit that separates droplets accompanying distillate distilled from the top of the processing tower and returns the liquid to the inside of the processing tower. The solution processing apparatus according to item. Comprising compression means for compressing and raising the temperature of distillate distilled from the top of the treatment tower;
5. The solution processing apparatus according to claim 1, wherein a distillate vapor that has been compressed by the compression unit and raised in temperature is used as a heating source of the first heating unit. 6.   The compression means compresses and raises the temperature of distillate distilled from the top of the treatment tower so that the temperature is 2 ° C. or higher than the liquid to be treated at the bottom of the treatment tower. The solution processing apparatus according to claim 5. Second gas-liquid contact means that is installed inside the processing tower and below the first gas-liquid contact means and that contacts the liquid to be processed and the vapor to be processed that has become gaseous by being heated. When,
Installed between the first gas-liquid contact means and the second gas-liquid contact means inside the processing tower and holds a predetermined amount of liquid to be treated supplied from the first gas-liquid contact means And holding means for supplying the liquid to be treated exceeding the predetermined amount to the second gas-liquid contact means,
Compression means for compressing and raising the temperature of distillate distilled from the top of the treatment tower;
Second heating means for heating the liquid to be treated held in the holding means;
With
The distillate vapor that has been compressed by the compression means and heated up is used as a heating source for at least one of the first heating means and the second heating means. Item 2. The solution processing apparatus according to item 1.   The high boiling point organic solvent of the liquid to be treated supplied from the supply means is a solvent having a boiling point higher than that of water, completely dissolved in water, and not azeotropic with water. N-methylpyrrolidone, N-ethyl-2-pyrrolidone N, N-dimethylformamide, N, N-dimethylacetamide, dimethyl sulfoxide, ethylene glycol, diethylene glycol, triethylene glycol, propylene glycol, butyl diglycol, 1,4-butanediol, monoethanolamine, diethylene glycol monomethyl ether, 1 The solution processing apparatus according to claim 1, which is one or more solvents selected from the group consisting of 1,3-dimethyl-2-imidazolidinone. . The high boiling point organic solvent of the liquid to be treated supplied from the supply means is N-methylpyrrolidone,
The distillate distilled from the top of the treatment tower has a high-boiling organic solvent content of 0.5 wt% or less,
The solution according to any one of claims 1 to 7, wherein the concentrated liquid discharged from the bottom of the treatment tower has a high-boiling organic solvent content of 60.0 wt% or more. Processing equipment.

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