JPH1133304A - Method and apparatus for separating and recovering hydrophilic solvent - Google Patents

Abstract

PROBLEM TO BE SOLVED: To improve the heat efficiency, miniaturize the apparatus, improve the recovery efficiency, and improve the durability. SOLUTION: A raw liquid, which is a hydrophilic solvent containing water, is supplied to the hollow part of a cylindrical body 2 made of inorganic fibers and the raw liquid is adsorbed by an adsorbent 3 having water-absorptive function and with which the outer circumferential part of the cylindrical body 2 made of inorganic fibers is filled while being passed through the cylindrical body 2 made of inorganic fibers. In this case, the adsorbent 3 is directly heated by an electric heating wire heater 4 to desorb water adsorbed in the adsorbent 3.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION The present invention relates to various alcohols such as isopropyl alcohol, ketones such as acetone, and hydrophilic solvents such as carboxylic acids such as propic acid and acetic acid. The present invention relates to a method for recovering a solvent by separating and removing water and a recovery apparatus for the same.

[0002]

2. Description of the Related Art In related fields such as liquid crystal glass, semiconductors, ultra-precision equipment, and optical communication fibers, extremely high cleanliness is required for the products themselves and the surrounding environment. For this reason, for example, articles that are extremely resistant to contamination, such as wafers, are washed with pure water. However, since washing with pure water is inferior in drying property, water is replaced with isopropyl alcohol (hereinafter simply referred to as IPA) after washing to increase the drying rate. The IPA containing water used for washing is regenerated and recovered, and used repeatedly. Thus, the concentration of regenerated IPA is at least 99.5 watts.
It is considered that it is desirably t% or more.

The recovery of IPA by removing water from the above-mentioned IPA containing water (hereinafter referred to as a stock solution) is roughly classified into the following known methods of distillation, membrane separation and adsorption. Three types of separation methods have been employed. Here, the distillation method is suitable for separating and recovering a solvent and a solute having a large difference in boiling point, and is a general separation method. The membrane separation method is a method in which a solution is flowed through a primary channel through a polymer membrane or a hollow fiber (fiber) having an affinity for a solute, and the solute is vaporized by depressurizing a secondary channel. This is a separation method in which the resin is separated from the solvent by permeating through a polymer membrane or the like. In the adsorption method, a solution is brought into contact with an adsorbent having high adsorption performance for the solute to cause the solute to be adsorbed to the adsorbent, and the solute adsorbed to the adsorbent is removed by heating in the regeneration step. In order to bring the solution into uniform contact with the adsorbent, the adsorbent is previously formed into granules or spheres.

[0004]

However, when IPA is to be separated and regenerated by distillation from the above-mentioned stock solution, an azeotropic phenomenon occurs between IPA and water. It is impossible to obtain IPA above the concentration. Therefore, it is conceivable to employ an extractive distillation method, but this extractive distillation method is inefficient in terms of thermal energy, and it is difficult to reduce the size of the apparatus.

In the above-mentioned membrane separation method, the temperature in the system is lowered due to latent heat of evaporation of water, so that the permeation rate to the polymer membrane is lowered. If the water content is large, the required membrane area must be increased. Not get. Furthermore, in order to secure a constant transmission speed, the size of the vacuum device needs to be increased, and there is a problem in durability of the polymer film.

On the other hand, in the above-mentioned adsorption method, the shape of the adsorbent is formed into a granular shape or a spherical shape in order to uniformly contact the solution with the adsorbent as described above. Then, the mixed liquid is brought into contact with the adsorbent in a liquid state or in a vaporized state. However, when the adsorbent is formed into the above-mentioned shape and the mixed liquid is adsorbed, the shape of the adsorbent is easily broken, the powder is easily formed, or the particles are easily formed into particles. Performance will be significantly reduced. In the regeneration step, when removing the water adsorbed by the adsorbent, the gas is warmed and brought into contact with the adsorbent. When a gas is used indirectly as a heat medium in this way, a large amount of gas is required, the thermal efficiency becomes extremely low, and when air is used as the heating gas, the risk of explosion or ignition increases. Special equipment is required for the prevention, and if an inert gas such as nitrogen is used in order to avoid the above danger, there are many factors that lead to high costs such as gas purchase cost and recovery equipment.

The present invention has been made to solve various problems of the above-mentioned conventional separation / regeneration method, and specifically, (1) improvement of thermal efficiency, (2) realization of miniaturization,
It is an object of the present invention to provide a method and apparatus for separating and recovering a hydrophilic solvent which can achieve (3) an improved recovery and (4) an improved durability.

[0008]

SUMMARY OF THE INVENTION The object of the present invention is to provide a method for regenerating a solvent by separating water from a stock solution of a hydrophilic solvent containing water according to the present invention. Separating and contacting the stock solution directly through a liquid permeable member, and directly heating the adsorbent to desorb water adsorbed on the adsorbent by evaporation, thereby separating and recovering a hydrophilic solvent. Achieved by the method.

As described above, in the case of the adsorption method, in order to desorb water from the adsorbent, heated air or a heated inert gas is brought into contact with the adsorbent and evaporated for regeneration. Since a gas having a small heat capacity is used as a heat catalyst, a large amount of gas is required, which is economically disadvantageous when the heat efficiency is low and an inert gas such as nitrogen is used.

Therefore, the present inventor examined thermal efficiency for desorption of water, initial cost and running cost. It was found that direct heating of an adsorbent having excellent water adsorbability and adsorbing a large amount of water required direct thermal efficiency. Came to the conclusion that it was the most advantageous. As a means for the direct heating, the use of a heating wire makes it easy to control the heating temperature and makes it possible to make the whole apparatus compact, and other pumps and heat exchangers other than a small liquid transfer pump are unnecessary. Therefore, it was considered to be extremely advantageous. Therefore, in the present invention, the adsorbent such as zeolite, which has adsorbed a large amount of water during regeneration, is directly heated by a heating wire heater or the like, and desorption of water from the absorbed adsorbent by heat conduction is performed. The hydrophilic solvent is hardly adsorbed by the adsorbent and is collected in a liquid state before desorption of water. Further, a part of the solvent adsorbed by the adsorbent is desorbed from the adsorbent by a method described later.

If the adsorbent and the stock solution can be brought into direct and uniform contact with each other in a liquid state, the apparatus can be made compact, and the adsorption humidity is dispersed to be relatively low, so that the adsorption efficiency is increased. However, when the form of the adsorbent is in powder form, it is usually impossible to make almost uniform contact, and it is naturally impossible only by the gravity of the undiluted solution. Even it does not occur and cannot pass through the adsorption layer.

In the case of the usual adsorption method, as described above, in order to enhance the contact with the stock solution, the adsorbent is formed into a spherical shape, a columnar shape, or a crushed granule, and the formed adsorbent is filled in a packed bed to be treated. (1) Even if the undiluted solution permeates,
Often, drift occurs, and it is necessary to further improve the contact efficiency. (2) Since the adsorbent is formed in the above-mentioned form, it is partially broken and easily powdered, and the powder is Because it is extremely finer and easier to form particles than the relatively large-sized raw material powder that has been crystallized before molding, it can be reused as it is for high-speed cleaning of precision products that require a large amount of water and require high cleanliness. It is not possible.

Based on this premise, the following experiment was also conducted on the adsorption characteristics based on the form of the adsorbent. As the adsorbent, a zeolite made of the above-mentioned raw material powder which was not formed and a zeolite formed into a spherical shape for comparison were used. FIG. 1 schematically shows the experimental apparatus.

FIG. 1A shows an example in which an adsorbent 3 'made of a spherical body is filled in a glass cylinder 1 and a stock solution is allowed to flow down from above. FIG. FIG. 3C shows an example in which the glass cylinder is filled with the adsorbent 3 made of the raw material powder and the stock solution is allowed to flow down from above, and FIG. A fiber cylinder 2 is arranged, and an adsorbent 3 made of raw material powder is filled between the fiber cylinder 2 and the glass cylinder 1 in the upper half of FIG. In the lower half of FIG. 3 (c), an adsorbent 3 ″ made of finer powder than the raw material powder is filled between the fiber cylinder 2 and the glass cylinder 1, and the hollow of the fiber cylinder 2 is filled. 5 shows an example in which a stock solution is supplied into the unit.

As can be understood from these figures, in the case of the spherically shaped adsorbent 3 'according to the example, there is a portion that does not come into contact with the undiluted solution, and without any intervening material as in the example. When the adsorbent 3 in the form of a raw material powder is brought into direct contact with the stock solution, 1 cm from the contact interface to 3 cm.
It was found that the contact was uniform within minutes, but the contact volume did not increase at any height higher than that. Also, FIG.
As can be understood from the above, in the example, when the adsorbent 3 in the form of the raw material powder is filled, the undiluted solution permeates through the inside of the fiber cylinder, diffuses into the adsorbent, and immediately contacts the whole. I was able to.

According to this experiment, regardless of the form of the adsorbent, it is understood that an increase in the contact area cannot be expected even if the stock solution is directly supplied to the adsorbent, and that a fiber cylinder is interposed. It is considered that the supply region of the stock solution is thereby extended so as to cover the entire adsorbent, and the permeation region is greatly increased and the permeation speed is also increased. Moreover, it can be understood that the form of the adsorbent is desirably in the state of the raw material powder before molding.

Based on the above experimental results, further investigation was made on the effect of interposing a permeable member such as a permeable membrane between the supply path of the undiluted solution and the adsorbent placement portion. When a conventional film is used, it cannot be adopted because of poor heat resistance during reproduction.

Therefore, as a result of an experiment conducted on a permeable member made of various materials permeable to the undiluted solution, the polymer was eluted into the undiluted solution with the permeable member made of a polymer material, and the adsorbent was adsorbed by the foreign matter. It has been concluded that it is impossible to put it to practical use because the performance is lowered and a mechanism for removing those foreign substances is required.

On the other hand, in the case of using a permeable member made of a sintered body of various ceramics, it has been found that if the permeation speed is appropriate, it is extremely effective in improving the contact with the adsorbent. Generally, the porosity of the sintered body is small and the permeation speed of the stock solution is small, so the regeneration efficiency is difficult.If the porosity of the sintered body is increased in order to increase the permeation speed, then molding is performed.
In many cases, the brittleness is increased and it is easily broken, which is not suitable for practical use, and it is difficult to adopt it. Further, since the ceramic sintered body has a high transmission resistance, it is difficult to adopt it.

Therefore, the present inventor uses a tubular braid obtained from inorganic fibers as in the above experiment, and is less likely to form particles around it and has excellent adsorption performance. However, when the stock solution is directly immersed, the contact area is limited. When an adsorbent composed of the above-mentioned non-molded raw material powder was arranged and the undiluted solution was supplied to the adsorbent through the gap of the braid, it was found that extremely uniform contact was obtained. As the material of the inorganic fiber, alumina, silica, carbon, glass, a mixture of alumina-silica, and the like can be used, and the fibrous structure may be a mere sheet, and may not necessarily be used in the above-described braid. It will be appreciated that the fabric is not limited and may be knitted or woven from inorganic fibers at the required density.

However, in this case, the fiber structure should satisfy the following characteristics. (1) The voids of the fibrous structure are smaller than the raw material powder of the adsorbent, and the adsorbent should not pass through the fibrous structure. (2) Heat resistance. (3) There should be no outflow of ions or particles in the stock solution.

From the above results, in the method of the present invention, the liquid permeable member is a tubular cylindrical body made of a heat-resistant material having a large number of fine communication holes between the inner and outer wall surfaces, and the adsorbent is It is preferable to supply the undiluted solution to the hollow portion of the cylindrical body while filling the outer circumferential space of the cylindrical body, and more preferably, the liquid-permeable member is formed of a woven or knitted fabric or a braid obtained from inorganic fibers. And using non-molded raw material powder as the adsorbent. FIG. 2 is an explanatory view of a separation mechanism of a hydrophilic solvent and water according to the method of the present invention. The device shown in FIG.
Although substantially the same as that shown in (c), the heating wire heater 4 is spirally wound independently on the inner peripheral surface of the glass cylindrical body 1 and the outer peripheral surface of the inorganic fiber cylindrical body 2, respectively. I have.

In FIG. 1A, the undiluted solution is supplied to the hollow portion of the inorganic fiber cylinder 2 without being heated by the heating wire heater 4.
In this state, the undiluted solution permeates through the inorganic fiber cylinder 2, and a part of water and IPA is adsorbed by the hydrophilic adsorbent 3 made of the raw material powder, and does not permeate through the inorganic fiber cylinder 2. IPA
Is collected outside the system.

Here, as shown in FIG. 2B, a heating wire heater disposed on the inner peripheral surface of the glass tube 1 is energized to heat the adsorbent 3 to a temperature higher than the IPA evaporation temperature (about 83 ° C.). Then, the dehydrated IPA is evaporated and collected. Alternatively, dehydrated IPA below the evaporation temperature may be recovered in a liquid state. Note that the molecular weight of water is smaller than the molecular weight of IPA, and water enters the pores (4 °) of the adsorbent, but IPA does not enter the pores of the adsorbent. That is, although water is adsorbed by the adsorbent, IPA
Is not adsorbed by the adsorbent and only exists around the adsorbent. Therefore, the IPA evaporates by heating to the evaporating temperature, and the water adsorbed by the adsorbent is desorbed by heating to the desorption temperature or higher.

When the recovery of the IPA is completed, as shown in FIG. 4C, the heating wire 4 disposed on the outer peripheral surface of the inorganic fibrous tubular body 2 is also energized to desorb the adsorbent 3 from the periphery. Heat to above temperature (250-350 ° C). By this direct heating, all of the water adsorbed on the adsorbent 3 is quickly desorbed and discharged out of the system.

Thus, the high regeneration efficiency as described above is achieved even when the undiluted solution is permeated through the fibrous structure, but when the undiluted solution is directly heated and permeated in a gaseous state, the regeneration efficiency is further increased. Knew that it would increase. However, since alcohols and ketones to be regenerated have low boiling points and are flammable, direct heating with a heating wire or the like is considered to be dangerous.

Therefore, in order to put the present invention into practical use, various experiments were conducted on direct heating by a heating wire in consideration of safety.

FIG. 3 schematically shows a schematic view of the experimental apparatus and the results at that time. The experiment was conducted by incorporating a heating wire heater 4 into a cylindrical braid 2 having an inner diameter of 12 mm and using alumina fiber as a raw material. Is installed, and the lower end of the braid 1 moistened with IPA is immersed in the IPA tank.

In this state, the following two experiments were performed. (1) When the ignition portion of the ignition device 5 installed in the internal space of the braid 2 was energized and glowed for 30 seconds, no ignition was recognized. (2) Similarly, when the heating wire heater 4 incorporated in the braid was energized and glowed red, the outer peripheral surface of the braid burned. However, when observed from above during the experiments (1) and (2),
It was found that no flame was generated in the internal space of the braid 2 and no combustion occurred on the inner wall of the tubular braid 2.

From the above experimental results, in order to improve the regeneration efficiency in the method of the present invention, it is desirable to directly heat the stock solution supplied to the hollow portion of the liquid permeable member in the hollow portion. Since ignition does not occur in the hollow portion of the fibrous structure, safety is sufficiently ensured.

When the undiluted solution in the hollow portion is directly heated as described above, the heating temperature of the adsorbent is set to the evaporation temperature of the solvent when the solvent is recovered, and a predetermined time elapses. The water-affinity solvent thus obtained is evaporated and collected. When the collection is completed, the heating temperature is raised to the zeolite water desorption temperature to desorb water from the adsorbent.

In order to carry out the method of the present invention, the apparatus of the present invention for regenerating a solvent by separating water from a stock solution of a hydrophilic solvent containing water comprises a casing and a casing. One or more liquid permeable members housed and having the undiluted liquid supply space and having a large number of fine communication holes, an adsorbent filled in an outer space of the liquid permeable member and having excellent water adsorption performance; It is characterized by comprising heating means for directly heating the agent, and an evaporation outlet for the solvent formed in the casing.

The casing is further provided with a water evaporation outlet. When the solvent is recovered, the water evaporation outlet is closed and the solvent recovery port is opened, and when the water is discharged out of the casing, the water evaporation port is opened and the solvent recovery port is opened. Close.

The liquid permeable member is a tubular cylindrical body made of a heat-resistant material having a large number of fine communication holes communicating between the inner and outer wall surfaces, and the adsorbent is filled in an outer peripheral space of the cylindrical body. The casing has a stock solution supply means for supplying the stock solution to the hollow portion of the cylindrical body, and preferably, the liquid permeable member is made of an inorganic fiber made of a woven or knitted fabric or a braid obtained from an inorganic fiber. The heating means is a heating wire disposed along an outer peripheral surface of the tube body.

Further, the liquid permeable member is a tube made of two or more woven or knitted fabrics or braids obtained from inorganic fibers and having different diameters. The adsorbent and the heating wire may be deformed so as to be accommodated in the gap space therebetween.

In the case where the undiluted solution is allowed to pass through the body-penetrating member in a vaporized state, a heating means for directly heating the undiluted liquid supply hollow portion of the liquid-penetrating member may be further provided. Controlling the temperature and time for evaporating and recovering the solvent after elapse of a predetermined time by setting the temperature to the evaporating temperature of the solvent and elevating the heating temperature of the adsorbent to the desorption temperature of moisture after the elapse of the same time Means.

[0037]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Preferred embodiments of the present invention will be specifically described below with reference to the accompanying drawings by way of typical examples.

(Example 1) A device similar to the device shown in FIG.
A braid 2 made of inorganic fibers is concentrically arranged inside a glass cylinder 1 having an inner diameter of 12 mm, and the glass cylinder 1
The space formed between the braid and the braid 2 was filled with an adsorbent made of zeolite having various forms shown below. A heating wire heater 4 for reproduction was spirally wound around the inner peripheral surface of the glass cylinder 1 and the outer peripheral surface of the braid 2, respectively.

The form of the zeolite may be a raw material powder (150 μm to 10 μm) in a form before molding, a spherical molded product (10 μm).
１５15 mesh), a columnar molded product (diameter 1.5 mm, length 5.0 mm), and a crushed product (14 to 30 mesh).

The zeolite having such a form was subjected to comparison between the amount of the stock solution treated per volume and the amount of water after the dehydration treatment. The results are shown in Table 1. However, the regenerating power per operation was fixed at (0.5 kwh / kg), and the pore diameter of the adsorbent was all 4 mm. As another common experimental condition, the water content of the stock solution was 30
%.

[0041]

[Table 1]

As is apparent from Table 1, as the form of the adsorbent, the raw material powder having a high degree of crystallinity has the smallest charge amount per fixed volume and the largest amount of the liquid to be treated per fixed time. In addition, it can be understood that particle-free processing is possible without powdering. This means that the use of the braid made of inorganic fibers shown in FIG. 1 and described above has ensured the compactness of the apparatus of the present invention, the cleanness of the processing environment, and the durability.

(Embodiment 2) FIG. 4 schematically shows an embodiment in which the apparatus for separating and recovering a hydrophilic solvent according to the present invention is modularized. The apparatus of the embodiment includes a closed chamber 10 having a stock solution supply port 11, a hydrophilic solvent outlet 12, a steam outlet 13, and a nitrogen gas inlet 14, and a ceiling portion in the chamber 10 which communicates with the stock solution supply port 11. An undiluted solution storage tank 15, a large number of tubular braids 16 made of alumina fiber in the chamber 10 erected in the lower space of the undiluted solution storage tank 15, and a gap space between the braids 16. A zeolite raw material powder 17 filled in the portion, and a heating wire heater 18 spirally arranged continuously around the outer periphery of a number of braids are provided.

At the bottom of the undiluted solution storage tank 15, the same number of under-drain nozzles 15a are provided at the upper open ends of the large number of tubular braids 16, and the undiluted solution stored in the undiluted solution storage tank 15 is The liquid is dripped into the hollow portion of each braid 16 through the submerged nozzle 15a.

The hydrophilic solvent outlet 12 and the steam outlet 1
Numerals 3 each have a valve, and when the solvent is recovered, the hydrophilic solvent outlet 12 is opened and the steam outlet 13 is closed. When moisture is desorbed, the steam outlet 13 is opened and the hydrophilic solvent outlet 12 is closed. The nitrogen gas inlet 14
Are formed below the stock solution storage tank 15 at two places, a side wall above the braid 16 and a bottom wall, and both inlets are connected to the same nitrogen gas supply source via a switching valve 19. . Further, the heating wire heater 18 is connected to an external power supply 20, and a heating temperature and a heating time are controlled by a command from a control device 21. The control device 21 is connected to a hydraulic circuit (not shown), and automatically operates the shutters of the hydrophilic solvent outlet 12 and the steam outlet 13 and the switching valve 19 disposed in the nitrogen gas supply passage. Issue an operation command.

The performance and the like of the module according to the present embodiment having the above-mentioned configuration and the conventional indirect adsorption type and pervaporation membrane type separation devices were compared under the following conditions. The results are shown in Table 2. Implementation conditions other than those shown in Table 2 are as follows:
The raw material powder of zeolite used in Example 1 was used as an adsorbent, and a stock solution was a mixed solution of IPA-water. here,
"Indirect adsorption type" refers to a method of adsorbing only water in a state where two substances such as alcohol and water are present as gases.

[0047]

[Table 2]

As can be understood from Table 2, according to the separation / recovery apparatus for a hydrophilic solvent according to the present invention, the volume of the apparatus is small and compact as compared with a similar apparatus of the related art.
The device volume per time processing capacity (L / (L / h)) is 4
Despite being the smallest value of 0, the recovery concentration of the solvent is as high as 99.9% even when the amount of water contained in the undiluted solution is large compared to the others, and the amount of electric power for regeneration is remarkably small.

Table 3 shows the results of analysis of the metal components in the IPA by ICP emission spectroscopy with respect to the remaining amount of the metal contained in the stock solution by the above-mentioned module in the regenerated and recovered liquid.

[0050]

[Table 3]

From Table 3, it can be seen that when zeolite is used, IPA
It can be understood that almost all of the metal contained in is removed by adsorption.

(Embodiment 3) FIG. 5 shows a third embodiment of the present invention. According to this embodiment, two tubular braids 16a and 16b having different diameters are arranged concentrically, and both braids are arranged. 16a, 16
b and the outer peripheral side of the large-diameter braid 16a are filled with the adsorbent 17 made of zeolite raw material powder, and the inner peripheral surface of the large-diameter braid 16a and the outer peripheral surface of the small-diameter braid 16b, respectively. The heating wire heaters 18a and 18b are spirally wound.

In this state, the undiluted solution was supplied to the hollow portion of the small-diameter braid 16b under the same conditions as in the first embodiment, and at the same time, the heating wires 18a and 18b were energized to directly heat the adsorbent 17. The concentration of water contained in the IPA after the treatment is 0.0
It did not exceed 6 wt%.

(Embodiment 4) Under the same conditions as in the third embodiment, thin tape-shaped electric heating tapes 18c and 18d are used in place of the heating wire heaters 18a and 18b, as shown in FIG. The stock solution was processed by spirally winding at the same pitch. As a result, the amount of water contained in the treated IPA was 0.05 wt% or less.

From the above results, it can be seen that as the area of the heater for heating the adsorbent per unit weight increases, the heating distribution to the adsorbent 17 becomes more uniform, and the amount of water in the IPA after the treatment decreases.

Example 5 Using the same apparatus as in Example 1,
100 g of adsorbent consisting of zeolite raw material powder is used without replacement, and 60 g of undiluted solution is supplied to supply IP.
After recovering A, a drying treatment was performed at 250 ° C. for 3 hours, and an operation of desorbing water adsorbed on the adsorbent was performed five times, and a difference in water absorption / desorption characteristics in each time was examined. Table 4 shows the results. The undiluted solution is an IPA mixed solution having a water content of 30% by weight, and the power for regeneration and dehydration of the adsorbent is all 0.5 (kw).
h / kg).

[0057]

[Table 4]

As shown in Table 4, according to the separation and recovery apparatus of the present invention, even if the operation of absorbing and desorbing water is repeated,
It can be seen that the desorption function has not been reduced.

Example 6 A heating wire heater for directly heating the hollow portion of the inorganic fibrous braid 2 is further provided in the apparatus shown in FIG. Was transmitted. As a result, the permeation speed was about twice as high as that in the case where the permeation was performed in a liquid state, and at the same time, the adsorbent 3 was uniformly and quickly adsorbed. This is because when adsorbed in liquid form, only the upper adsorbent adsorbs and saturates, and the lower adsorbent is adsorbed by diffusion from the upper part, resulting in a lower adsorption speed. it is conceivable that.

[Brief description of the drawings]

FIG. 1 is an explanatory view of a separation mechanism of a hydrophilic solvent and water according to the present invention.

FIG. 2 is an explanatory diagram showing one embodiment of a procedure for separating a hydrophilic solvent and water according to the present invention.

FIG. 3 is an explanatory diagram of an ignition experiment of the device of the present invention.

FIG. 4 is a schematic configuration diagram showing a typical example of a reproducing apparatus in which the present invention is modularized.

FIG. 5 is a schematic sectional view of a main part showing another embodiment of the device of the present invention.

FIG. 6 is a schematic configuration diagram of a main part showing still another embodiment of the apparatus of the present invention.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Glass cylinder 2, 16 Inorganic fiber braid 3, 17 Adsorbent 4, 18 Heating wire heater 5 Ignition device 10 Chamber 11 Stock solution supply port 12 Hydrophilic solvent outlet 13 Steam outlet 14 Nitrogen gas inlet 15 Stock solution storage tank 19 Switching valve 20 external power supply 21 controller

Claims (16)

[Claims] 1. A method for recovering a solvent by separating water from a stock solution of a hydrophilic solvent containing water, wherein the stock solution is directly contacted with an adsorbent having excellent water adsorption performance via a liquid permeable member. And directly heating the adsorbent to desorb water adsorbed on the adsorbent. 2. The liquid permeable member is a tubular cylindrical body made of a heat-resistant material having a large number of fine communication holes between inner and outer wall surfaces, and the adsorbent is filled in an outer peripheral space of the cylindrical body. ,
And supplying the undiluted solution to a hollow portion of the cylindrical body. 3. The method for regenerating a hydrophilic solvent according to claim 2, wherein the liquid permeable member is a tube formed of a woven or knitted fabric obtained from inorganic fibers or a braid. 4. The method for separating and recovering a hydrophilic solvent according to claim 2, further comprising using unformed raw material powder as the adsorbent. 5. The method according to claim 2, further comprising directly heating the stock solution supplied to the hollow portion of the liquid permeable member in the hollow portion.
Or the method for separating and recovering a hydrophilic solvent according to 3. 6. The method for regenerating a hydrophilic solvent according to claim 1, wherein the heating is direct heating by a heating wire. 7. The method according to claim 7, further comprising: setting the heating temperature to the evaporating temperature of the solvent for a predetermined time, and increasing the heating temperature of the adsorbent to the desorption temperature of moisture after the elapse of the same time. 7. The method for separating and recovering a hydrophilic solvent according to 1 to 6. 8. The method according to claim 1, wherein the solvent is selected from alcohols, ketones or carboxylic acids, and the adsorbent is zeolite. 9. An apparatus for separating and recovering a solvent by separating water from a stock solution of a hydrophilic solvent containing water, comprising: a casing having a supply section for the stock solution; One or more liquid permeable members having a supply space and a large number of fine communication holes, an adsorbent filled with an outer space of the liquid permeable member and having excellent water adsorption performance, and directly heating the adsorbent A hydrophilic solvent separation / recovery device comprising: a heating means; and a recovery port for the solvent formed in the casing. 10. The apparatus for separating and recovering a hydrophilic solvent according to claim 9, further comprising an outlet for evaporating moisture in the casing. 11. The liquid-permeable member is a tubular cylindrical body made of a heat-resistant material having a large number of fine communication holes communicating between inner and outer wall surfaces, and the adsorbent is filled in an outer peripheral space of the cylindrical body. The hydrophilic solvent separation / recovery device according to claim 9 or 10, further comprising a stock solution supply means for supplying the stock solution to a hollow portion of the cylindrical body inside the casing. 12. The liquid permeating member is a tube made of a woven or knitted fabric or a braid obtained from inorganic fibers, and the heating means is an electric heater disposed along the outer peripheral surface of the tube. 12. The apparatus for separating and collecting a hydrophilic solvent according to any one of claims 11 to 11. 13. A tube body in which the liquid-permeable member is made of two or more woven or knitted fabrics or braids having different diameters obtained from inorganic fibers. The hydrophilic solvent separation / recovery device according to claim 11 or 12, wherein the adsorbent and the heating wire are accommodated in a gap space between the bodies. 14. The apparatus according to claim 11, further comprising heating means for directly heating the raw liquid supply hollow portion of said liquid permeable member.
The hydrophilic solvent separation and recovery device according to any one of the above. 15. The apparatus for separating and recovering a hydrophilic solvent according to claim 9, wherein the solvent is an alcohol, a ketone or a carboxylic acid, and the adsorbent is a zeolite composed of unformed raw material powder. . 16. The method according to claim 16, wherein the heating temperature is set to an evaporation temperature of the solvent, and the solvent is evaporated and recovered after a lapse of a predetermined time, and after the lapse of the same time, the heating temperature of the adsorbent is increased to a desorption temperature of moisture. 15. The apparatus for separating and recovering a hydrophilic solvent according to claim 14, further comprising control means for controlling temperature and time for desorbing moisture.