JP2009148751A - Organic matter dehydration concentration apparatus and organic matter dehydration concentration method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an organic matter dehydration concentration apparatus and an organic matter dehydration concentration method which can prevent impurities from attaching and depositing at a separation membrane even when impurities are included in a liquid to be treated that is evaporated at an evaporator and which can also restrain the accumulation, deterioration and polymerization of impurities by which dehydration concentration performance can be favorably sustained. <P>SOLUTION: The organic matter dehydration concentration apparatus 1 is provided with the evaporator 2 which vaporizes the liquid to be treated that includes a water-soluble organic matter and water and generates the vapor of liquid to be treated and a membrane separation apparatus 4 which has a separation membrane 3 which selectively permeates steam. It is also provided with a vapor of a liquid to be treated condensation device 23 which generates a condensation liquid by condensing a part of the vapor of the liquid to be treated that is sent from the evaporator 2 to the membrane separation apparatus 4, bubble cap trays 15, 16 which stagnates the condensation liquid from the vapor of a liquid to be treated condensation device 23 so that the vapor of the liquid to be treated can go through and permeate and which are provided in the flow path of the vapor of the liquid to be treated inside of the evaporator 2, and favorably, and preferably, is provided with a flow amount control valve 10 for discharging the stagnating substance at the bottom part of the evaporator 2. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to an organic dehydration concentration apparatus and an organic dehydration concentration method for dehydrating and concentrating a liquid to be treated containing a water-soluble organic substance and water using an evaporator and a separation membrane.

  Conventionally, a distillation apparatus has been widely used as an apparatus for dehydrating and concentrating a liquid to be treated containing a water-soluble organic substance and water. However, many water-soluble organic substances form an azeotropic mixture with water. For example, ethanol, propanol, ethyl acetate, methyl ethyl ketone and the like. For the distillation of these azeotropes, extractive distillation with the addition of a third component is applied, but there are disadvantages that the number of apparatuses is increased, the operation is complicated, and the energy required for separation is also increased. As a solution to such a drawback, there is a dehydration concentration method using a separation membrane as proposed in Patent Document 1, for example.

Japanese Patent No. 3764894

  In the organic matter dehydrating and concentrating apparatus for realizing the dehydrating and concentrating method according to Patent Document 1, a liquid to be treated containing a water-soluble organic substance and water is distilled in a distillation column with an operating pressure of 50 to 150 kPa, and the top of the distillation column or The condensate obtained by condensing the fraction taken out from the concentration stage is supplied to the evaporator and heated to form a vapor having a pressure higher than the operating pressure of the distillation column, and this high-pressure vapor is supplied to the separation membrane. It is dehydrated by selectively permeating water vapor to obtain highly concentrated water-soluble organic matter.

  By the way, when impurities are mixed in the liquid to be treated containing water-soluble organic substances and water, the impurities accumulate in the evaporator and reach the membrane separation device along with the liquid to be processed and adhere to the separation membrane (adsorption). As a result, the separation performance of the separation membrane may be deteriorated. Further, when the impurities react to polymerize, it becomes a viscous liquid or solid and accumulates at the bottom of the evaporator. The viscous liquid or solid accumulated in the bottom of the evaporator rises toward the liquid surface together with the vapor bubbles, and becomes splashy impurities as the vapor bubbles burst on the liquid surface. The impurities are accompanied by the liquid vapor generated in the evaporator and are sent out from the evaporator, reach the membrane separation device, and adhere (adsorb) to the separation membrane, which may deteriorate the separation performance of the separation membrane.

  That is, in the conventional dehydration and concentration apparatus, when impurities to be processed are evaporated in the evaporator, the impurities are accompanied by the liquid to be processed and reach the membrane separation apparatus, and are separated into the separation membrane. There is a problem in that impurities adhere and accumulate, which causes a decrease in the performance of the separation membrane, resulting in poor dehydration concentration performance.

  The present invention has been made to solve such problems, and even when impurities are contained in the liquid to be processed which is evaporated by the evaporator, the impurities are adhered and deposited on the separation film. It is an object of the present invention to provide an organic matter dewatering and concentration apparatus and an organic matter dewatering and concentration method that can be prevented and thereby maintain good dehydration and concentration performance.

In order to achieve the above object, an organic matter dehydration concentration apparatus according to the first invention comprises:
An evaporator for evaporating a liquid to be treated containing a water-soluble organic substance and water; and a membrane separation apparatus having a separation membrane for selectively allowing water vapor to pass through the evaporator. In the organic matter dehydrating and concentrating apparatus for introducing the liquid vapor to be processed generated in the process into the membrane separator and separating the water vapor from the liquid vapor to be processed,
A liquid vapor condensing means to be processed for condensing a part of the liquid vapor to be processed which is vaporized by the evaporator and sent to the membrane separation device;
Provided in the middle of the flow path of the liquid vapor to be treated in the evaporator, and a condensate retention means for retaining the condensate from the liquid vapor condensation means to be treated,
The condensate retention means is configured such that the liquid vapor to be treated passes through the condensate retained in the condensate retention means.

In the present invention, the evaporator not only generates steam by heating the liquid to be treated with steam or a heating medium, but also includes a vapor condensing means for liquid to be treated and a condensate retaining means, and particularly a post-process. A function of removing impurities harmful to the separation membrane from the liquid vapor to be processed is provided.
Here, the to-be-processed vapor condensing means has a role of generating a condensate that is retained in the condensate retaining means, so that only a part of the to-be-treated liquid vapor is partially condensed and sent to the condensate retaining means. Composed. The ratio of the condensed amount to the evaporated amount is sufficient if the condensate to be retained in the condensate retaining means is secured, and is preferably less than 10% by mass, more preferably less than 5% by mass, and particularly less than 3% by mass.

  Further, the liquid vapor to be treated passes through the condensate retained in the condensate liquid retention means, so that impurities accompanying the liquid vapor to be treated are removed. Therefore, “the liquid to be treated is configured to pass through the condensate retained in the condensate retaining means” is sufficient contact to be able to perform the function of removing impurities. In terms of area, this means that the liquid vapor to be treated and the condensate come into gas-liquid contact, but preferably it penetrates through extremely fine holes formed by the condensate retained in the condensate retention means. It means that the liquid vapor to be treated passes through the liquid layer of the condensate liquid retained in the condensate liquid retention means, more finely bubbled through the condensate liquid layer.

  In the present invention, the condensate retention means is either a bubble cap tray or a sheave tray in which a vent member through which the liquid vapor to be processed passes is provided in a tray member provided in the middle of the flow path of the liquid vapor to be processed. It is preferable (second invention).

  For example, the condensate staying means passes the liquid vapor to be processed through a tray member provided in the middle of the flow path of the liquid vapor to be processed inside the evaporator (partitioned so as to divide the flow direction of the liquid vapor to be processed). It is preferable that the bubble cap tray is provided with a vent hole and a cap member provided so as to block the flow of the liquid vapor to be processed after passing through the vent hole. The bubble cap tray is preferably provided with a condensate overflow means for causing the condensate to overflow from the bubble cap tray when the depth of the condensate staying in excess of a predetermined depth.

  Further, the condensate retaining means is, for example, a sheave tray (partitioned so as to divide the flow direction of the liquid vapor to be processed) in the middle of the flow path of the liquid vapor to be processed inside the evaporator (a large number of holes in the disc). Are preferred. Also here, it is preferable to provide a condensate overflow means for allowing the condensate to overflow from the sheave tray when the liquid depth of the condensate staying exceeds a predetermined depth. There is no member that blocks the flow of the steam to be processed unlike the bubble cap tray, but the bubble rises in the liquid that stays and the upper liquid level of the bubble blocks the flow, and the sieve tray is a tray that conforms to the bubble cap tray. .

  That is, the impurities accompanying the liquid vapor to be treated are removed by the condensate liquid retention means, but the condensate liquid condensate is supplied to the condensate liquid retention means, and the condensate liquid overflow means is lowered to the lower stage. Since the condensate is overflowing, the condensate in the condensate retention means is always replaced, and impurities are not concentrated.

  In the present invention, the condensate retention means is, for example, a packing (layer) that is disposed in the middle of the flow path of the liquid vapor to be processed inside the evaporator and allows the liquid vapor to be processed and the condensate to come into gas-liquid contact. There may be an embodiment in which a condensate dispersion means for dispersing the condensate is provided for the filler (layer) (third invention).

  In the present invention, since impurities in the liquid to be processed are retained at a high concentration at the bottom of the evaporator, an extraction port for discharging the impurities is provided at the bottom of the evaporator as necessary, and the impurities accumulated in the bottom of the evaporator It is preferable to extract the bottom liquid containing. In particular, when the impurities contained in the liquid to be treated are likely to react and polymerize, and when they are scattered to the separation membrane, the membrane is clogged, the evaporator is treated with water-soluble organic matter and water. The liquid is supplied to a position where there is at least one stagnant stage in the upper part and no stagnant stage in the lower part, and a part of the bottom liquid can be withdrawn. It is preferable to be able to extract every period (fourth invention).

In the present invention, a plurality of condensate residence stages may be provided in the evaporator. In that case, the evaporator has a plurality of stages of condensate retention means, and the liquid to be treated containing water-soluble organic matter and water is at least one stage in the upper part and at least one stage in the lower part. In order to prevent impurities from scattering and adhering / depositing on the separation membrane, a part of the bottom liquid can be extracted, and the bottom of the evaporator It is preferable to reduce the amount of water-soluble organic components entrained when the bottom liquid is discharged (fifth invention).
Even when a plurality of condensate residence stages are provided in the evaporator, it is suitable that the number of stages is 5 or less, preferably 3 or less, and more preferably 2 stages. If a large number of condensate stay stages are provided, the function as an evaporator (evaporation function) becomes inefficient.

  The organic matter dehydration concentration apparatus of the present invention is particularly useful when the liquid to be treated containing a water-soluble organic substance and water is a treatment liquid further containing impurities harmful to the separation membrane (the sixth invention).

Next, the organic matter dehydration concentration method according to the seventh invention is:
An evaporator for evaporating the liquid to be processed to generate a liquid to be processed and a membrane separation device having a separation membrane that selectively permeates water vapor, and the liquid vapor to be processed generated by the evaporator Organic substance for dehydrating and concentrating organic substances from the liquid to be treated containing water-soluble organic substances, water and other impurities, using an organic substance dehydrating and concentrating apparatus for separating water vapor from the liquid vapor to be treated In the dehydration and concentration method,
Supplying a liquid to be processed containing a water-soluble organic substance, water and other impurities to the evaporator to generate a liquid to be processed;
The liquid vapor to be treated is condensed by the liquid vapor condensation means to be treated, and condensed from the liquid vapor condensation means to the condensate retention means provided in the middle of the flow path of the liquid vapor to be treated in the evaporator. A step of retaining the liquid,
A step of allowing the liquid to be treated to pass through the condensate retained in the condensate retaining means; and supplying the liquid vapor to be treated from the evaporator to the membrane separation device, The method includes a step of selectively separating water vapor from liquid vapor.
This organic matter dehydration and concentration method can suitably suppress degradation of the dehydration and concentration performance of the separation membrane due to the harmful impurities when the impurities in the liquid to be treated are harmful impurities to the separation membrane.

  In the present invention, the impurities contained in the liquid to be treated are harmful to the separation membrane (eighth invention).

  According to the present invention, when the liquid vapor to be processed generated in the evaporator passes through the condensate liquid retention means, the impurities accompanying the liquid vapor to be processed are condensed by the condensate retained in the condensate liquid retention means. Since it is trapped, it is possible to prevent impurities from adhering and depositing on the separation membrane, and to maintain good dehydration concentration performance.

  In particular, by adopting a bubble cap tray or a sieve tray as the condensate retention means, the vapor-liquid contact area can be increased when the liquid vapor to be processed passes through the condensate in the tray. Impurities accompanying the vapor can be captured more effectively. Further, by providing the condensate overflow means on the bubble cap tray, the liquid depth of the condensate retained in the bubble cap tray is kept constant, which is preferable because the pressure loss can be kept constant. is there.

  On the other hand, by using a filling material as the condensate retention means, it is possible to capture impurity-containing droplets accompanying the liquid to be treated while suppressing pressure loss. In particular, by providing a condensate dispersion means for dispersing the condensate with respect to the packing, when the liquid to be processed passes through the condensate of the packing through the gas, the gas between the liquid to be processed and the condensate is removed. By increasing the liquid contact area, impurities accompanying the liquid vapor to be processed can be captured more effectively.

  Further, by extracting a part of the bottom liquid staying at the bottom periodically as required by the liquid outlet at the bottom of the evaporator, it is possible to suppress an increase in the concentration of impurities or increase in the polymer.

  The liquid to be treated is supplied to a position where at least one condensate staying stage exists at the upper part, and impurities are collected at the upper condensate staying stage, and then flow down to the lower stage and discharged from the bottom of the evaporator. The When the liquid to be treated is supplied to a position where one or more condensate residence stages exist in the lower part, the concentration of impurities is increased at the bottom of the evaporator, and the amount of the accompanying impurities increases. Impurities can be effectively removed because the impurities are diluted in the stage and the amount of impurities entrained in the upper condensate residence stage can be suppressed. In addition, compared to the case where the impurities are supplied to the bottom of the evaporator, the residence time distribution from the start of the introduction of the impurities to the discharge can be narrowed, and when the impurities are easily polymerized, the polymerization can be suppressed.

  Next, specific embodiments of an organic matter dehydration concentration apparatus and an organic matter dehydration concentration method according to the present invention will be described with reference to the drawings.

[First Embodiment]
FIG. 1 shows a schematic system configuration diagram of the organic matter dehydration concentration apparatus according to the first embodiment of the present invention. In addition, in the organic matter dehydrating and concentrating apparatus described below, the liquid to be treated for dehydrating and concentrating treatment is a recovered product of water-soluble organic matter after use for a certain purpose or a recovered product of water-soluble organic matter from a certain process. Yes, it contains impurities in addition to water-soluble organic substances and water.

  An organic dehydration concentration apparatus 1 shown in FIG. 1 includes an evaporator 2 that evaporates a liquid to be processed to generate a liquid to be processed and a membrane separation apparatus 4 that includes a separation membrane 3 that selectively permeates water vapor. The liquid vapor to be processed generated in the evaporator 2 is introduced into the membrane separation device 4 to separate the water vapor from the liquid vapor to be processed. Here, the non-permeate vapor that has not passed through the separation membrane 3 is condensed by the non-permeate vapor condenser 5, and the condensate obtained by the condensation action by the non-permeate vapor condenser 5 is stored in the dehydrated concentrate tank 6. The On the other hand, the permeate vapor that has passed through the separation membrane 3 is condensed by the permeate vapor condenser 7, and the condensate obtained by the condensing action by the permeate vapor condenser 7 is stored in the permeate receiver 8. In addition, what is shown with the code | symbol "9" in FIG. 1 is a vacuum pump. In addition, when there are many impurities in the liquid to be treated, or when the impurities are easily polymerized, it is necessary (usually at regular intervals (intermittently) or continuously in a very small amount). A part of the bottom liquid at the bottom of the evaporator can be extracted using the flow control valve 10.

  Next, a more specific structure of the evaporator 2 will be described below with reference to the structure explanatory diagram of FIG.

  The evaporator 2 includes an evaporator body 11 in which an upper lid body 11a, an intermediate cylinder body 11b, and a lower lid body 11c are integrally joined, and a liquid to be processed supplied into the evaporator body 11 by steam or a heat medium. A jacket type heater 12 mounted on the lower outer surface of the evaporator main body 11 for indirect heating and evaporation, and a liquid vapor generated in the evaporator main body 11 directed to the membrane separation device 4 In order to send out, the liquid vapor | steam delivery pipe | tube 13 to be processed connected to the upper side cover body 11a is provided.

  An upper stage bubble cap tray 15 and a lower stage bubble cap tray 16 are disposed in the upper space in the intermediate cylinder 11b of the evaporator main body 11 with a predetermined interval in the vertical direction. Each of the bubble cap trays 15 and 16 includes a tray member 17 that divides the upper space in the intermediate cylinder 11b so as to divide the upper space in the flow direction of the liquid vapor to be processed. The outer peripheral edge of the tray member 17 is fixed to the inner wall surface of the intermediate cylinder 11b over the entire circumference. The tray member 17 is provided with necessary vent holes 18 for allowing the liquid vapor to be processed to pass therethrough, and a cap member 19 is provided so as to block the flow of the liquid vapor to be processed after passing through each vent hole 18. It is attached. Each of the bubble cap trays 15 and 16 corresponds to the “condensate retention means” in the present invention.

  In the tray member 17 in the upper bubble cap tray 15, the upper side overflow of a required length so as to penetrate vertically on the one side (left side in FIG. 2) portion with respect to the center line O of the intermediate cylinder 11 b. A flow tube 21 is fitted. On the other hand, in the tray member 17 in the lower bubble cap tray 16, the lower side of the required length so as to penetrate vertically on the other side (right side in FIG. 2) with respect to the center line O of the intermediate cylinder 11 b. A side overflow tube 22 is fitted.

  On the outer surface of the liquid vapor delivery pipe 13 to be processed, a jacket-type liquid vapor condenser (a liquid vapor to be processed of the present invention) that condenses the liquid vapor flowing through the pipe indirectly by cooling with cooling water. Corresponds to "condensing means"). In this way, a part of the liquid vapor to be processed sent out from the evaporator body 11 toward the membrane separation device 4 is condensed. And the condensate produced | generated by the condensing effect | action by this to-be-processed liquid vapor | steam condenser 23 is dripped from the to-be-processed liquid vapor | steam delivery pipe | tube 13, or goes along the inner wall of the upper side cover body 11a from the to-be-processed liquid vapor | steam delivery pipe | tube 13. And is stored in the upper bubble cap tray 15.

When the liquid depth of the upper stage bubble cap tray 15 to the reservoir is condensate exceeds a predetermined depth D _1, the condensate is overflowed from the upper side bubble cap tray 15 through the upper side downcomers 21. Thus, liquid depth of the condensate that is collected in the upper stage bubble cap tray 15 is adapted to be kept constant at a sufficient depth D _1. The condensate overflowed from the upper stage side bubble cap tray 15 through the upper stage side overflow pipe 21 is stored in the lower stage side bubble cap tray 16. When the liquid depth of the condensate that is collected in the lower stage bubble cap tray 16 has exceeded a predetermined depth D _2, the condensate is overflowed from the lower side bubble cap tray 16 through the lower side downcomers 22. Thus, liquid depth of the condensate that is collected in the lower stage bubble cap tray 16 is adapted to be kept constant at a sufficient depth D _2.

  Below the lower bubble cap tray 16, in order to collect the condensate overflowing from the lower bubble cap tray 16 through the lower overflow tube 22, the intermediate cylinder 11 b extends from the inner wall of the intermediate cylinder 11 b. An overflow liquid receiver 24 having a required volume is provided integrally with the intermediate cylinder 11b so as to project toward the center line O. The condensate overflowing from the overflow liquid receiver 24 is heated and evaporated again by the heater 12 together with the liquid to be treated stored in the lower part of the evaporator body 11.

When the liquid depth of the condensate that is collected in the overflow liquid receiver 24 is in the maximum depth D _3, as the lower end of the lower side downcomers 22 immersed in the condensate, of the lower side downcomers 22 A lower end position is defined. This prevents the liquid to be processed generated in the lower part of the evaporator main body 11 from leaking through the lower overflow pipe 22 without going through the condensate stored in the lower bubble cap tray 16. Have been to. Therefore, the liquid vapor to be processed generated in the lower part of the evaporator main body 11 passes through the gaps between the tray member 17 and the cap members 19 from the vent holes 18 of the tray member 17 in the lower bubble cap tray 16. Then, the condensate stored in the lower bubble cap tray 16 passes through and flows to the upper bubble cap tray 15.

When the liquid depth of the lower-side bubble cap tray 16 to the reservoir is condensate is at a predetermined depth D _2, as the lower end of the upper side downcomers 21 immersed in the condensate, the upper side downcomers 21 A lower end position is defined. As a result, the liquid vapor to be treated that has passed through the condensate on the lower bubble cap tray 16 passes through the upper overflow pipe 21 without passing through the condensate stored in the upper bubble cap tray 15. To prevent leakage. Therefore, the liquid vapor to be processed that has passed through the condensate stored in the lower bubble cap tray 16 passes through the vent holes 18 of the tray member 17 in the upper bubble cap tray 15 and the tray member 17 and each cap. The condensate stored in the upper bubble cap tray 15 passes through the gap between the members 19 and flows into the liquid vapor delivery pipe 13 to be processed.

  In the organic matter dehydrating and concentrating apparatus 1 configured as described above, the liquid to be processed generated in the lower part of the evaporator main body 11 passes through the vent holes 18 of the tray member 17 in the lower bubble cap tray 16. The condensate stored in the lower bubble cap tray 16 passes through the gap between the tray member 17 and each cap member 19 and flows into the upper bubble cap tray 15, and further flows into the upper bubble cap tray. 15 through each air hole 18 of the tray member 17 through the gap between the tray member 17 and each cap member 19, the condensate stored in the upper-stage bubble cap tray 15 passes through, and the liquid vapor to be processed It is made to flow to the delivery pipe 13. Accordingly, when the liquid vapor to be processed passes through the condensate on the lower bubble cap tray 16, most of the impurity-containing droplets accompanying the liquid vapor to be processed are caused by the condensate on the lower bubble cap tray 16. Be captured. Further, when the liquid vapor to be processed passes through the condensate on the upper bubble cap tray 15, remaining impurity-containing droplets accompanying the liquid vapor to be processed are captured by the condensate on the upper bubble cap tray 15. The Note that the bubble cap tray may be one stage as long as the trapping ability of the impurity-containing droplets is high. There may also be an embodiment in which three or more bubble cap trays are provided.

According to the organic dehydration concentration apparatus 1 of the present embodiment, the following effects (1) to (3) can be obtained.
(1) Impurities accompanying the liquid to be treated are trapped by the condensate retained in the bubble cap trays 15 and 16, so that the impurities can be prevented from adhering and depositing on the separation membrane 3. The dehydration concentration performance can be maintained well.
(2) The vapor to be treated passes through the gap between the tray member 17 and each cap member 19 in each bubble cap tray 15, 16 and passes through the condensate on each bubble cap tray 15, 16. Therefore, when the liquid vapor to be treated is bubbled through the condensate, it can be bubbled to further increase the gas-liquid contact area, and more effectively capture the impurity-containing droplets accompanying the liquid vapor to be treated. be able to.
(3) together with the liquid depth of the condensate to be retained on the upper side bubble cap tray 15 by the upper side downcomers 21 are provided on the upper side bubble cap tray 15 is kept constant at a predetermined depth D _1, By providing the lower side overflow cap 22 in the lower stage bubble cap tray 16, the depth of the condensate retained in the lower stage bubble cap tray 16 is kept constant at a predetermined depth D _2. The desired droplet trapping performance can be stably maintained while keeping the pressure constant.

  In the present embodiment, the liquid vapor condenser 23 to be processed is mounted on the outer surface of the liquid vapor delivery pipe 13 to be processed, and the condensate generated by the condensation action by the liquid vapor condenser 23 to be processed is processed. A condenser that condenses a part of the liquid vapor to be treated sent from the evaporator main body 11 toward the membrane separation device 4 is supplied from the liquid vapor delivery pipe 13 to the upper bubble cap tray 15. Separately from the evaporator 2, a condensate supply pipe for supplying the condensate to the upper bubble cap tray 15 is provided in the evaporator main body 11 separately from the liquid vapor delivery pipe 13 to be processed. Alternatively, the condensate generated by a condenser installed separately may be supplied to the upper stage bubble cap tray 15 through the condensate supply pipe.

  When there are many impurities in the liquid to be processed to be supplied, or when impurities are easily polymerized, the liquid can be quantitatively extracted from the flow control valve 10 to suppress accumulation of impurities or polymerization. Furthermore, when the liquid to be treated is supplied to a position where one or more condensate stay stages exist at the bottom, the residence time from the start of the introduction of impurities to the discharge is compared with the case where it is supplied to the bottom of the evaporator. When the distribution can be narrowed and the impurities are easily polymerized, the polymerization can be suppressed.

[Second Embodiment]
FIG. 3 shows a structural explanatory diagram of an evaporator applied in the organic matter dehydration concentration apparatus according to the second embodiment of the present invention. In the present embodiment, the same or similar parts as those in the first embodiment will be denoted by the same reference numerals in the drawings, and detailed description thereof will be omitted. The following points are different from those in the first embodiment. (The same applies to the third embodiment described later).

This embodiment relates to an example using an evaporator 2A to which an upper sheave tray 15A and a lower sheave tray 16A are applied in place of the upper bubble cap tray 15 and the lower bubble cap tray 16 in the first embodiment. Is. Here, each of the sheave trays 15A and 16A is simply provided with a required air hole 18A for allowing the liquid vapor to be processed to pass through the tray member 17A that divides the inside of the evaporator main body 11 in the flow direction of the liquid vapor to be processed. It is only what has been done. Each sheave tray 15A, 16A corresponds to the “condensate retention means” in the present invention. Further, in this embodiment, instead of the upper-stage overflow pipe 21 and the lower-stage overflow pipe 22 in the first embodiment, the upper-stage overflow plate 21A and the lower-stage overflow plate 22A are applied, and the upper stage with liquid depth of the condensate to be retained on the upper side sieve tray 15A by the side overflow plate 21A is kept constant at a predetermined depth D _1, condensate is accumulated in the lower stage sieve tray 16A by the lower side overflow plate 22A liquid depth of is to be kept constant at a predetermined depth D _2.
Also according to the present embodiment, basically the same effects as those of the first embodiment can be obtained.

  In the first and second embodiments, the overflow members 21 and 22 or the overflow plates 21A and 22A are provided on the tray member 17; 17A. , 22 or overflow plates 21A, 22A may not be provided. In this case, from the amount of vapor generated in the evaporator body 11, the amount of condensate supplied from the liquid vapor condenser to be treated 23, and the opening area of the vent hole 18; 18A formed in the tray member 17; 17A. The liquid depth of the condensate on the tray member is determined.

[Third Embodiment]
FIG. 4 is an explanatory view of the structure of an evaporator applied in the organic matter dehydration concentration apparatus according to the third embodiment of the present invention.

In this embodiment, instead of the respective bubble cap trays 15 and 16 in the first embodiment, the filling material is filled in the evaporator main body 11 so that the liquid vapor to be treated and the condensate can come into gas-liquid contact. This relates to an example using the evaporator 2B in which the (layer) 25 is arranged. Here, as the filler 25, either a regular filler in which a large number of filler materials such as metal plates or wire meshes are regularly arranged, or an irregular filler such as a Raschig ring or a pole ring is used. It may be adopted.
Further, in the present embodiment, a dispersion plate that disperses the condensate dropped from the liquid vapor delivery pipe 13 to be processed in a position directly below the liquid vapor delivery pipe 13 to be processed and over the filling 25. 26 is provided. The dispersion plate 26 is formed of a plate-like member having a large number of holes such as punching metal. The dispersion plate 26 corresponds to “condensate dispersion means” in the present invention.

  Also according to the present embodiment, basically the same effects as those of the first embodiment can be obtained. Furthermore, since the filling material 25 is employed as the condensate retention means, it is possible to capture the impurity-containing droplets accompanying the liquid to be treated while keeping the pressure loss low. Further, since the dispersion plate 26 for dispersing the condensate with respect to the filling 25 is provided, the gas-liquid contact between the liquid to be treated and the condensate is performed in the filling 25 more favorably, Impurities accompanying the liquid vapor can be captured more effectively.

  In addition, when impurities in the liquid to be processed chemically change at the temperature of the evaporator heating wall surface, but do not change chemically at a temperature lower by 10 to 30 ° C. than that temperature, the liquid to be processed is condensed on the upper part of the evaporator. You may supply to the uppermost stage of a liquid retention part. As shown in FIG. 4, when the filler 25 is used, a dispersion plate 26 is provided, but the liquid to be treated may be supplied to the dispersion plate 26. An appropriate number of spray nozzles may be attached on the surface of the dispersion plate 26 to improve the contact between the liquid to be sprayed and the vapor.

  As mentioned above, although the organic substance dehydration concentration apparatus of this invention was demonstrated based on several embodiment, this invention is not limited to the structure described in the said embodiment, The structure described in each embodiment is combined suitably. The configuration can be changed as appropriate without departing from the spirit of the invention.

The organic matter dehydrating and concentrating method of the present invention relates to an organic matter dehydrating and concentrating method that is suitably used with the organic matter dehydrating and concentrating device of the present invention. As a representative example, a method for dehydrating and concentrating organic matter that is preferably used with the organic matter dehydrating and concentrating device 1 according to the first embodiment will be described below.
That is, the organic matter dehydration concentration method of the present invention comprises:
An evaporator 2 for evaporating the liquid to be treated to generate a liquid to be treated and a membrane separation device 4 having a separation membrane 3 that selectively permeates water vapor are provided. An organic substance is removed from a liquid to be treated containing a water-soluble organic substance, water, and other impurities using the organic substance dehydrating and concentrating apparatus 1 for introducing the liquid vapor into the membrane separation device 4 and separating the water vapor from the liquid vapor to be treated. In the organic matter dehydration concentration method for dehydration concentration,
Supplying a liquid to be processed containing a water-soluble organic substance, water and other impurities to the evaporator 2 to generate a liquid to be processed;
The liquid vapor to be treated is condensed by the liquid vapor condensing means 23 to be treated, and the liquid vapor condensing means 23 to be treated is added to the condensate retention means 15 and 16 provided in the flow path of the liquid vapor to be treated inside the evaporator 2. A step of retaining the condensate from
The process liquid vapor passes through the condensate retained in the condensate retention means 15, 16 and the process liquid vapor from the evaporator 2 is supplied to the membrane separation device 4, and the liquid to be processed The method includes a step of selectively separating water vapor from the steam.

  The evaporator 2 is heated using steam, a heating medium, or the like so as to evaporate the liquid to be processed and generate a liquid to be processed. Such an operation is an operation performed in a normal evaporator, and is not particularly limited, but can be suitably performed at an operating pressure of 50 to 700 kPaG, preferably 50 to 400 kPaG, more preferably 50 to 200 kPaG. The to-be-processed vapor condensing means 23 partially condenses only a part of the to-be-processed liquid vapor, and is suitably provided in the course of the to-be-processed liquid vapor sent from the evaporator 2 to the membrane separation device 4. However, you may prepare in the middle of the flow path | route of the to-be-processed liquid vapor | steam in the evaporator 2. FIG. Condensation can be suitably performed with normal cooling water. The total amount of the condensate is preferably sent to the condensate retention means 15, 16 of the evaporator 2. In addition, the temperature and amount of the cooling water can be controlled so that the ratio of the condensation amount to the evaporation amount is preferably less than 10% by mass, more preferably less than 5% by mass, and particularly less than 3% by mass. It is preferable that

  The separation membrane 3 is not particularly limited as long as it can selectively permeate water vapor from the liquid vapor to be treated. It may be made of a polymer such as polyimide, polyetherimide, polycarbonate, polysulfone or high molecular weight polyvinyl alcohol, or may be made of an inorganic material such as zeolite or zirconia. And the form of the membrane separation apparatus 4 is also a shell and tube type module including a hollow fiber separation membrane module made of, for example, an asymmetric polyimide hollow fiber membrane, and a tubular separation membrane element in which a zeolite is formed on a porous tubular support. A conventionally well-known thing etc. can be used suitably. Examples of these include, but are not limited to, Japanese Patent Application Laid-Open No. 2003-93844 using a zeolite membrane, such as Japanese Patent Application Laid-Open No. 2000-262838 and Japanese Patent Application Laid-Open No. 2001-62257 using a polyimide hollow fiber membrane. Those described in JP-A-2006-263574, JP-A-2007-203210 and the like can be preferably exemplified.

The permeation performance of the separation membrane 3 is preferably such that the water vapor transmission rate (P ′ _{H 2 O 2} ) is 0.5 × 10 ⁻³ cm ³ (STP) / cm ² · sec · cm Hg or more, more preferably 1. 0 × 10 ⁻³ cm ³ (STP) / cm ² · sec · cmHg or more, and the ratio of the permeation rate between water vapor and water-soluble organic vapor is preferably 50 or more, more preferably 100 or more. is there.

  The liquid to be treated discharged from the evaporator 2 is preferably supplied to the membrane separation device 4 after being heated to about 5 to 20 ° C. As the operating conditions of the membrane separation apparatus 4, known conditions that are usually performed in the employed membrane separation apparatus can be used as they are. For example, when a polyimide hollow fiber membrane is used, Japanese Patent Application Laid-Open Nos. 2000-262838 and 2001-62257, and when a zeolite membrane is used, Japanese Patent Application Laid-Open Nos. 2003-93844 and 2006 are disclosed. Specific apparatuses and methods described in JP-A No. 263574 and JP-A No. 2007-203210 can be suitably employed.

In the present invention, the liquid to be treated contains a water-soluble organic substance, water, and other impurities. For example, parts may be washed with water-soluble organic substances such as alcohols in the semiconductor manufacturing process, but the water-soluble organic substances after use include water-soluble organic substances, water, and other impurities. . In order to purify and reuse this water-soluble organic material, it is necessary to dehydrate and concentrate the water-soluble organic material while removing impurities contained therein.
In addition, for example, when purifying and dehydrating a fermented alcohol aqueous solution to obtain a high-purity alcohol, the fermented alcohol aqueous solution contains insoluble components such as cellulose based on the fermentation raw materials and fermentation conditions even after being treated in the mash tower or distillation tower. Since chemical substances by-produced by fermentation such as metal ions, salts and aldehydes derived from raw materials are mixed, it is necessary to dehydrate and concentrate alcohols while removing impurities contained therein.
Furthermore, in chemical processes, liquids that contain water-soluble organic substances, water, and other impurities are often generated. In such cases, it is necessary to dehydrate and concentrate the water-soluble organic substances while removing the contained impurities. There is.
The dehydration concentration method of the present invention can suitably dehydrate and concentrate such a treatment liquid.

  The water-soluble organic substance is not particularly limited, but is a water-soluble organic compound having a boiling point of 50 to 250 ° C., preferably 60 to 220 ° C., for example, alcohols such as methanol, ethanol, propanol, and butanol, acetone, methyl ethyl ketone, Ketones such as methyl butyl ketone and ethyl ethyl ketone, ethers such as diethyl ether and dipropyl ether, esters such as ethyl acetate, butyl acetate and butyl formate, hydrocarbons such as hexane, and alicyclic hydrocarbons such as cyclohexane And the like.

  In the present invention, everything other than the target water-soluble organic substance and water is an impurity, but as impurities harmful to the separation membrane, pyridines such as pyridine, phenols such as phenol, aldehydes such as acetaldehyde, Metal ions such as calcium ion, sodium ion and iron ion, ionic compounds such as salts such as sodium chloride and magnesium chloride, organic or inorganic acid compounds, organic or inorganic alkali compounds, JP-A-9-103633 Halogen compounds, ammonia, ozone, silane, tungsten hexafluoride, etc., as well as high molecular weight materials such as aldehydes, and inorganic or organic substances such as cellulose derived from raw materials There are insoluble or non-volatile impurities. If these adhere and deposit on the separation membrane 3, the performance of the separation membrane 3 is reduced, and the dehydration concentration performance is deteriorated.

  In the method for dehydrating and concentrating water-soluble organic matter of the present invention, water-soluble organic matter can be suitably dehydrated and concentrated from a liquid to be treated containing water-soluble organic matter, water and other impurities. When it is harmful, it is particularly preferable because it can suppress a decrease in performance of the separation membrane 3.

Schematic system configuration diagram of the organic matter dehydration concentration apparatus according to the first embodiment of the present invention Structure explanatory drawing of the evaporator applied with the organic substance dehydration concentration apparatus which concerns on 1st Embodiment Structure explanatory drawing of the evaporator applied with the organic substance dehydration concentration apparatus which concerns on 2nd Embodiment Structure explanatory drawing of the evaporator applied with the organic substance dehydration concentration apparatus which concerns on 3rd Embodiment

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Organic substance dehydration concentration apparatus 2,2A, 2B Evaporator 3 Separation membrane 4 Membrane separation apparatus 10 Flow control valve 15 Upper stage bubble cap tray (condensate retention means)
15A Upper sheave tray (condensate retention means)
16 Lower bubble cap tray (condensate retention means)
16A Lower sheave tray (condensate retention means)
17, 17A Tray member 18, 18A Ventilation hole 19 Cap member 21 Upper stage overflow pipe (condensate overflow means)
21A Upper stage overflow plate (condensate overflow means)
22 Lower overflow pipe (condensate overflow means)
22A Lower overflow plate (condensate overflow means)
23 Processed liquid vapor condenser (Processed liquid vapor condensing means)
25 Packing (condensate retention means)
26 Dispersion plate (condensate dispersion means)

Claims (8)

An evaporator for evaporating a liquid to be treated containing a water-soluble organic substance and water; and a membrane separation apparatus having a separation membrane for selectively allowing water vapor to pass through the evaporator. In the organic matter dehydrating and concentrating apparatus for introducing the liquid vapor to be processed generated in the process into the membrane separator and separating the water vapor from the liquid vapor to be processed,
A liquid vapor condensing means to be processed for condensing a part of the liquid vapor to be processed which is vaporized by the evaporator and sent to the membrane separation device;
Provided in the middle of the flow path of the liquid vapor to be treated in the evaporator, and a condensate retention means for retaining the condensate from the liquid vapor condensation means to be treated,
The condensate retention means is configured so that the liquid to be treated passes through the condensate retained in the condensate retention means.   The condensate retention means is either a bubble cap tray or a sheave tray in which a vent member through which a liquid vapor to be processed passes is provided in a tray member provided in the middle of a flow path of the liquid vapor to be processed. The organic substance dehydration concentration apparatus as described. The condensate retention means is a packing that is disposed in the middle of the flow path of the liquid vapor to be processed, and allows the liquid vapor and the condensate to come into gas-liquid contact,
The organic matter dehydrating and concentrating apparatus according to claim 1, further comprising a condensate dispersion means for dispersing the condensate with respect to the filling.   The evaporator supplies a liquid to be treated containing a water-soluble organic substance and water to a position where at least one or more residence stages exist in the upper part and no residence stage exists in the lower part, and a part of the bottom liquid The organic matter dewatering and concentrating apparatus according to claim 1, wherein the organic substance dehydrating and concentrating apparatus is configured to be able to extract water.   The evaporator has a plurality of stages of condensate retention means, and a stage in which at least one stage of the liquid to be treated containing water-soluble organic matter and water is present in the upper part and at least one stage in the lower part is present. The organic matter dehydration and concentration apparatus according to claim 1, wherein the organic matter dehydration and concentration apparatus is configured so that a part of the bottom liquid can be extracted while being supplied to a position between the two stages.   Furthermore, the organic substance dehydration concentration apparatus of Claim 1 used in order to spin-dry | dehydrate and concentrate the said water-soluble organic substance from the to-be-processed liquid containing a harmful | toxic impurity in a separation membrane. An evaporator for evaporating the liquid to be processed to generate a liquid to be processed and a membrane separation device having a separation membrane that selectively permeates water vapor, and the liquid vapor to be processed generated by the evaporator Organic substance for dehydrating and concentrating organic substances from the liquid to be treated containing water-soluble organic substances, water and other impurities, using an organic substance dehydrating and concentrating apparatus for separating water vapor from the liquid vapor to be treated In the dehydration and concentration method,
Supplying a liquid to be processed containing a water-soluble organic substance, water and other impurities to the evaporator to generate a liquid to be processed;
The liquid vapor to be treated is condensed by the liquid vapor condensation means to be treated, and condensed from the liquid vapor condensation means to the condensate retention means provided in the middle of the flow path of the liquid vapor to be treated in the evaporator. A step of retaining the liquid,
A step of allowing the liquid to be treated to pass through the condensate retained in the condensate retaining means; and supplying the liquid vapor to be treated from the evaporator to the membrane separation device, An organic dehydration concentration method comprising a step of selectively separating water vapor from liquid vapor.   The method of claim 7, wherein the impurities contained in the liquid to be treated are harmful to the separation membrane.

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