JP4360194B2 - Method and apparatus for concentrating water-soluble organic substances - Google Patents

Description

  The present invention relates to a water-soluble organic substance concentration method and concentration apparatus, and more specifically, it can suppress thermal energy required for concentration, and can obtain a high-concentration water-soluble organic substance using a separation membrane having a limited membrane area. The present invention relates to a water-soluble organic substance concentration method and concentration apparatus.

  As a method for concentrating a mixed solution of a water-soluble organic substance and water, one of the most widely used techniques is a distillation method. However, when concentrating a liquid mixture of a relatively low concentration water-soluble organic substance and water, the distillation method requires a large amount of heat energy because a large amount of water is evaporated and separated. For example, in the production of ethanol by fermentation, fermentation productivity of methods using biotechnology such as continuous fermentation and immobilized enzyme method is remarkably high. Nevertheless, since the ethanol concentration in the fermentation broth is lower than that in the conventional batch fermentation method, it is said that the concentration / separation energy by the distillation method is increased and the ethanol production cost is rather disadvantageous. In addition, in the manufacturing process of the chemical industry, a mixed solution of water-soluble organic matter and water having a low concentration is often generated, but it is too expensive to concentrate and separate by a distillation method alone.

  For this reason, a mixed liquid of low-concentration water-soluble organic substance and water is supplied to the primary side of the pervaporation separation module having an organic liquid permselective pervaporation membrane, and a carrier gas composed of an inert gas is allowed to flow on the secondary side. A vapor rich in organic liquid components that permeate through the membrane, and subsequently introduce a carrier gas containing the organic liquid component into the primary side of the vapor permeation separation module having a moisture permselective vapor permeable membrane, A dry inert gas is allowed to flow to the secondary side of the vapor permeation separation module to remove moisture contained in the carrier gas through the membrane, and then the primary side carrier gas is introduced into the condenser to be cooled, and organic A method for producing a concentrated liquid of an organic liquid aqueous solution in which a liquid component is taken out as a condensate has been proposed (see Patent Document 1).

  In addition, an apparatus for producing a concentrated liquid of an organic liquid aqueous solution using a pervaporation separation module having a separation membrane that preferentially permeates an organic liquid and a permeation vaporization separation module having a separation membrane that preferentially permeates water. It has been proposed (see Patent Document 2).

  Although the techniques described in Patent Documents 1 and 2 can greatly reduce the thermal energy cost required for separation, an enormous amount is required for the membrane area of the separation membrane to be used, and a large capital investment is required.

On the other hand, when water-soluble organics pre-concentrated in a distillation column are further concentrated using a moisture selective permeable membrane, the vapor at the top of the distillation column is led to a vapor permeable membrane to separate the water vapor (vapor transmission Method: Vapor Permeation method) and a method of separating water by introducing a distillate from a distillation column to a pervaporation membrane (pervaporation method: PerVaporation method) have been studied. In any of the methods using a moisture selective permeable membrane, the membrane permeation of water molecules is caused by a partial pressure difference of water existing through the membrane as a driving force, and the side of the permeated vapor is reduced in pressure. There is a need to operate with the partial pressure of the water to be concentrated or the water in the liquid being greater than the partial pressure of the water of the permeate side steam.
Japanese Patent No. 2765032 Japanese Patent No. 2780323

  As a result of studies on the combination of the vapor permeation method and the pervaporation method using the moisture selective permeable membrane with the distillation method, the present inventor conducted the following as described in detail in Comparative Examples 1 and 2 below. It turns out that there is a serious drawback.

  In the case of the vapor permeation method, heat energy for membrane separation is unnecessary and energy saving can be achieved. However, when attempting to highly concentrate the organic liquid in the top vapor of the distillation column operated near atmospheric pressure, Since the partial pressure of water in the concentrated steam is low, permeation does not occur unless the permeate steam side is at a high vacuum. Further, it has been found that since the driving force of water permeation at the portion where concentration has progressed, that is, the partial pressure difference of water, is small, a large membrane area is required for concentration.

  On the other hand, in the case of the osmotic vaporization method, the partial pressure of water in the mixture of water-soluble organic substances increases by increasing the operating temperature. Therefore, in order to ensure the driving force, pressurization is performed so that the liquid does not boil. Then, the temperature of the supply liquid (mixture of water-soluble organic substance and water) may be increased by heating. However, in the case of osmotic vaporization, the permeated water vaporizes, so the amount of heat necessary for water evaporation must be added. Therefore, it has been found that the more heat in the supply liquid (mixture of water-soluble organic matter and water), the more heat energy is required.

  Therefore, an object of the present invention is to provide a water-soluble organic substance concentration method and concentration apparatus that can suppress thermal energy required for concentration and can obtain a high-concentration water-soluble organic substance using a separation membrane having a limited membrane area. Is to provide.

The said subject of this invention has the following structure.
1. A combination of a vapor permeation method using a vapor permeation separation module and an osmosis vaporization method using an osmosis vapor separation module to obtain a high-concentration water-soluble organic substance by concentrating a mixed solution of the water-soluble organic substance and water. In the concentration method,
Obtaining a first concentrated steam in which organic matter is concentrated by distillation of a mixture of the water-soluble organic matter and water,
Thereafter, the first concentrated vapor is concentrated by a vapor permeation method using the vapor permeation separation module to obtain a second concentrated vapor,
Next, the second concentrated vapor is liquefied and concentrated by an osmotic vaporization method using the osmosis vapor separation module to obtain a high-concentration water-soluble organic substance.

2. A water-soluble organic substance that obtains a high-concentration water-soluble organic substance by concentrating a liquid mixture of a water-soluble organic substance and water by combining a vapor permeation method using a vapor permeation separation module and an osmosis vaporization method using an osmosis vapor separation module. In the concentration method of
The vapor permeation separation module has a moisture permselective vapor permeable membrane that selectively permeates water vapor from the vapor supplied to the primary side to the secondary side,
The pervaporation separation module has a moisture permeation type pervaporation membrane that selectively permeates moisture from the solution supplied to the primary side to the secondary side,
The pressure on the secondary side of each membrane has a low have pressure than the primary side,
Concentrating the liquid mixture of the water-soluble organic substance and water by distillation to obtain a first concentrated vapor,
Thereafter, the first concentrated vapor is supplied to the moisture selective permeable vapor permeable membrane and concentrated by selectively allowing moisture to pass through to obtain a second concentrated vapor.
Next, the secondary concentrated vapor is liquefied to produce a liquefied concentrated water-soluble organic substance,
After pressurizing and heating the heated liquefied concentrated water-soluble organic matter,
A method for concentrating a water-soluble organic substance, characterized in that it is supplied to the moisture permselective pervaporation membrane and selectively permeated to obtain a high-concentration water-soluble organic substance.

3. The concentration of the water-soluble organic substance in the mixed liquid of the water-soluble organic substance and water is 3% by mass to 50% by mass,
The concentration of the water-soluble organic substance in the first concentrated steam is 30% by mass to 95% by mass,
The concentration of the water-soluble organic substance in the secondary concentrated steam is 90% by mass to 99% by mass,
3. The method for concentrating a water-soluble organic material according to 1 or 2 above, wherein the concentration of the water-soluble organic material in the high-concentration water-soluble organic material is 95% by mass to 99.9% by mass.

4). In a water-soluble organic substance concentration apparatus that obtains a high-concentration water-soluble organic substance by concentrating a mixture of a water-soluble organic substance and water,
A distillation column for concentrating the liquid mixture of the water-soluble organic substance and water by distillation to obtain a first concentrated vapor;
A vapor permeation separation module that supplies the first concentrated vapor to a moisture selective permeation type vapor permeable membrane and selectively permeates moisture to obtain a second concentrated vapor;
A concentrated steam condenser for liquefying the secondary concentrated steam to produce a liquefied concentrated water-soluble organic substance;
A pressure pump for pressurizing the produced liquefied concentrated water-soluble organic matter;
A pervaporation heater for heating and heating the pressurized liquefied concentrated water-soluble organic matter;
A permeable vapor separation module that supplies the pressurized and heated liquefied concentrated water-soluble organic matter to a moisture selective permeation type pervaporation membrane and selectively permeates the moisture to obtain a high concentration water-soluble organic matter. An apparatus for concentrating water-soluble organic substances.

5. The concentration of the water-soluble organic substance in the mixed liquid of the water-soluble organic substance and water is 3% by mass to 50% by mass,
The concentration of the water-soluble organic substance in the first concentrated steam is 30% by mass to 95% by mass,
The concentration of the water-soluble organic substance in the secondary concentrated steam is 90% by mass to 99% by mass,
5. The water-soluble organic substance concentrating device according to 4 above, wherein the concentration of the water-soluble organic substance in the high-concentration water-soluble organic substance is 95% by mass to 99.9% by mass.

  The present invention was invented in order to concentrate a water-soluble organic substance pre-concentrated in a distillation column to a higher concentration using a moisture selective permeable separation membrane. After the top distillate is supplied in a vapor state to a moisture selective permeable vapor permeable membrane, the moisture is permeated to concentrate the organic liquid, and then the vapor formed by liquefying the vapor concentrated in the organic liquid is pressurized. Heating temperature is raised and supplied to a moisture permselective pervaporation membrane, allowing moisture to permeate, so that the heat energy required for concentration can be suppressed, and a high concentration water-solubility can be achieved using a separation membrane with a limited membrane area Organic matter can be obtained.

  A method of concentrating a 10% by mass ethanol aqueous solution by the concentration method of the present invention using the concentration apparatus shown in FIG. 1 will be described, but the present invention is not limited to this. 1, 4, and 5, among the paths connecting the members constituting the concentrator, the path indicated by a solid line indicates a liquid flow path, and the path indicated by a dotted line indicates a vapor flow. Showing the road.

  1 is a distillation column 10 for distilling the ethanol fermentation liquid 1 (in this embodiment, a first distillation column 101 and a second distillation column 111 for distilling ethanol concentrated by the first distillation column 101). And a vapor permeation separation module 20 for separating the vapor from the top of the distillation column 10, and an ethanol liquid condensed after being concentrated by the vapor permeation separation module 20 The pervaporation separation module 30 is provided.

  The distillation column 10 is not particularly limited as long as it is suitable for distillation operation, such as a plate type or a packed column. A middle part of the first distillation column 101 has a supply unit for supplying an ethanol liquid (fermented liquid) 1. A part of the liquid at the bottom of each of the distillation columns 101 and 111 is heated by the reboilers 102 and 112 to become vapor, and rises in the column while exchanging heat and materials with the liquid flowing down the column. For this reason, most of the components of the vapor are water at the bottom of the tower, but the ethanol concentration increases near the top of the tower. In addition, the remainder of the liquid taken out from the tower bottom is taken out as a bottomed liquid 11.

  The vapor distilled from the top of the second distillation column 111 is sent to the vapor permeation separation module 20, and a part thereof is condensed by the top condenser 12 and is refluxed to the top of the second distillation column 111.

  The operating pressure of each distillation column 101, 111 is preferably 50 to 150 kPa. If the operating pressure exceeds 150 kPa, (1) the construction cost of the distillation towers 101 and 111 becomes high, (2) the temperature at the bottom of the tower needs to be raised, and the energy cost becomes high, (3) against water There are problems such as a low relative volatility of ethanol. On the other hand, if the operating pressure is less than 50 kPa, the condensation temperature of the steam distilled from the top of the tower is too low, so that the top steam cannot be condensed with normal cooling water. The reboilers 102 and 112 are supplied with steam from the outside and heated by the condensation heat.

  Vapor distilled from the second distiller 111 is introduced into the vapor permeation separation module 20, and water vapor out of the introduced vapor is taken out as a permeation component, and the remaining components are non-permeation components. And then sent to the concentrated vapor condenser 21.

  The concentrated vapor condenser 21 condenses the non-permeate component of the vapor flowing out from the vapor permeation separation module 20 to generate a condensate, and the condensate tank 22 stores the condensate.

  The pressurizing pump 23 pressurizes the condensate stored in the condensate tank 22 to a predetermined pressure and sends it to the pervaporation separation module 30.

  The pervaporation heat exchanger 31 preheats the condensate sent out by the pressurization pump 23 and the concentrated ethanol discharged from the pervaporation separation module 30 so as to increase the temperature of the condensate. It has become.

  The pervaporation heater 32 heats the ethanol liquid sent out by the pressurizing pump 23 and the ethanol liquid flowing out from the pervaporation separation module 30 to a predetermined temperature by heating steam introduced from the outside. Yes.

  The pervaporation separation module 30 is configured to separate water from the ethanol liquid pressurized by the pressurizing pump 23 and heated by the pervaporation heat exchanger 31 and the pervaporation heater 32.

  The vapor permeation separation module 20 has a moisture selective permeation type vapor permeable membrane, and includes a vacuum pump 24 that depressurizes the permeation side of the separation membrane, and a condenser that cools and condenses the permeated vapor with cooling water. 25, the pressure is reduced.

  Each of the pervaporation / separation modules 30 has a moisture permeation type pervaporation membrane, and includes a vacuum pump 34 that depressurizes the permeation side of the separation membrane, and a condenser 35 that cools and condenses permeated water with cooling water. The pressure is reduced through.

  As the vapor permeation separation module 20 and the pervaporation separation module 30, a shell and tube type module including a tubular separation membrane in which a separation membrane is formed on a porous tubular support is preferable. Since both modules have the same structure, the vapor permeation separation module will be described first, and then, only the differences from the vapor permeation separation module will be described for the pervaporation separation module.

FIG. 2 shows an example of a vapor permeation separation module 20 that can be used in the concentration method of the present invention. However, the “primary or secondary concentrated steam” in the present invention is simply referred to as steam.
The vapor permeation separation module 20 includes a cylindrical shell 41, support plates 42a and 42b fixed to both ends of the shell 41, and a plurality of outer plates supported by the support plates 42a and 42b and extending in the longitudinal direction of the shell 41. A tube 43, a tubular separation membrane 44 provided in the longitudinal direction of the outer tube 43, and channels 45a and 45b attached to the shell 41 so as to cover the support plates 42a and 42b are provided. An inlet 46 of the steam F1 protrudes from the channel 45a, and an outlet 47 of the non-permeated steam F3 protrudes outward from the shell 41. The steam outlet 47 is provided at a position close to the support plate 42b. The channel 45b is provided with an outlet 48 for the membrane-permeated vapor F2. The flanges of the channels 45a and 45b are airtightly engaged with the support plates 42a and 42b.

  Each support plate 42 a, 42 b has a plurality of openings 421 a, 421 b, and each opening 421 a and opening 421 b are accurately positioned so as to face each other in the longitudinal direction of the shell 41. The front end 431 of the outer tube 43 is fixed to each opening 421a, and the rear end 432 of the same outer tube 43 is engaged with the opening 421b opposite to the opening 421a. Thus, each outer tube 43 has a support plate 42a. , 42b. A steam passage port 433 is formed in each outer tube 43 at a position close to the support plate 42b.

  FIG. 3 shows the detailed structure of the outer tube 43 and the tubular separation membrane 44 supported by the support plates 42a and 42b. The front end (channel 45a side) of the tubular separation membrane 44 is a sealed end 441, and the rear end (channel 45b side) is an open end 442. The sealing end 441 is sealed with a sealing member 49. The open end 442 engages with the support member 410, and the support member 410 is screwed into the rear end portion 432 of the outer tube 43. The outer tube 43 has a plurality of pin portions 434 projecting from the inner surface at a position close to the support plate 42 a, and the tip of the pin portion 434 supports the tubular separation membrane 44 by contacting the sealing member 49. Yes.

  As shown in FIGS. 2 and 3, when the steam F <b> 1 is supplied from the steam inlet 46 to the shell 41, the permeated steam F <b> 2 permeates the tubular separation membrane 44 and flows out from the membrane permeated steam outlet 48. The remaining steam F3 (non-permeated steam) that does not permeate the tubular separation membrane 44 passes through the gap between the outer tube 43 and the tubular separation membrane 44 and flows out from the passage port 433. Next, the non-permeate vapor F <b> 3 passes outside the outer tube 43 and flows out from the vapor outlet 47.

  The separation membrane 44 is not particularly limited and may be made of polymer PVA, polyimide or the like, but is preferably made of an inorganic material such as zeolite or zirconia, and more preferably made of zeolite. For example, a tubular support made of porous alumina having a zeolite thin film formed thereon can be used particularly preferably. The zeolite is not particularly limited, and can be appropriately selected depending on the water-soluble organic substance to be concentrated from ZSM-5 type, A type, Y type and the like.

  The pervaporation separation module has basically the same structure as the vapor permeation separation module, and differs in the following points.

  That is, in the vapor permeation separation module, the vapor of the solution to be concentrated is introduced from the vapor inlet (in this case, the solution inlet) 46, but in the pervaporation separation module, the solution to be concentrated is a liquid. Is introduced. Where the introduced solution comes into contact with the tubular separation membrane 44, the vapor mainly composed of water passes through the tubular separation membrane 44 and flows out from the membrane permeation vapor outlet 48. The solution from which moisture has been removed by the tubular separation membrane 44 passes through the gap between the outer tube 43 and the tubular separation membrane 44, flows out from the passage port 433, and flows out from the vapor outlet (in this case, the solution outlet) 47. The point to do is different.

  The water-soluble organic substance to be concentrated by the concentration method of the present invention is not particularly limited, such as ethanol, methanol, i-propyl alcohol, acetone, dioxane, DMF, but is preferably an alcohol, and preferably ethanol or i-propyl alcohol. More preferred.

Examples of the present invention are shown below.
(Example 1)
In Example 1, the concentration apparatus shown in FIG. 1 was used to concentrate ethanol from a fermentation solution of 8% by mass of ethanol to 90% by mass, and then water was separated by the method of the present invention. The Example which obtained is shown.

  Ethanol in the fermentation liquid was distilled in the first distillation column 101 and the second distillation column 111 and concentrated to 90% by mass at the top of the second distillation column 111.

The second distillation column 111 is operated at a pressure at the top of the column of 110 kPa (primary side pressure), which is approximately atmospheric pressure, and the vapor at the top of the column is partially condensed and refluxed to maintain the ethanol concentration at 90% by mass, 8.9 kg / h was led to the vapor permeation separation module 20. In this separation module 20, water was separated by a vapor permeation method and ethanol was concentrated. The element of the separation membrane constituting the module 20 used is obtained by forming A-type zeolite in the form of a membrane on the outer surface of a tubular alumina support, and inside the tubes of the tubular membrane element group included in the module 20. The (secondary side) was depressurized to 8.5 kPa by the vacuum pump 24, so that water of 0.52 kg / h permeated the membrane. As a result, the vapor at the outlet of the separation module 20 increased in ethanol concentration to 95.6% by mass. The surface area of the membrane contained in module 20 was 0.36 m ² . The water that permeated through the separation membrane was condensed by cooling with cooling water using the condenser 25, and the ethanol contained in the condensed liquid was 0.3% by mass.

Next, 95.6% by mass of the ethanol vapor exiting the separation module 20 is cooled and liquefied by the concentrated vapor condenser 21 and stored in the condensate tank 22, and the stored condensate is 700 kPa ( The pressure was increased to (primary side pressure) and then heated to 135 ° C. by the pervaporation superheater 32 to perform ethanol concentration by permeation vaporization. The separation module 30 used for pervaporation is composed of an A-type zeolite tubular membrane element, similar to vapor permeation, but in the case of pervaporation, the moisture in the solution is vaporized through the membrane, so the latent heat generates the module. The temperature of the liquid drops inside. For this reason, it was set as the apparatus structure by which the temperature rise by the pervaporation heater 32 and the water separation by the pervaporation separation module 30 are performed alternately, and the temperature of the solution in the pervaporation separation module 30 was maintained at 130-135 degreeC. Using a membrane having a membrane area of 0.3 m ² and reducing the pressure on the permeate side (secondary side) to 1.5 kPa by the vacuum pump 34, 0.346 kg / h of moisture permeates the membrane and 99.7 masses. % Ethanol 8.03 kg / h was obtained. The permeated vapor was cooled and condensed in the condenser 35 using a 1 ° C. refrigerant, but ethanol contained in the condensed liquid was 1% by mass. The amount of heat for pervaporation was 221 kcal / h. The difference in partial pressure of water inside and outside the membrane, which is the driving force for moisture permeation, was 4.05 kPa at the module outlet.

  At this time, the condensate sent to the pervaporation superheater 32 was preheated by the pressurization pump 23 using the pervaporation heat exchanger 31.

In Example 1 of the present invention, the heat energy required to concentrate 90% by mass of ethanol solution to 99.7% by mass is 221 kcal, and the membrane area of the separation modules 20 and 30 used is 0.66 m in total. ² .

(Comparative Example 1)
The block diagram shown in FIG. 4 is an apparatus configuration used in an experimental example for reducing the water content of the vapor at the top of a distillation column containing 90% by mass of ethanol only by the vapor permeation method. The same members are the same.

First, 8.9 kg / h of the top vapor was obtained in the same manner as in Example 1 above, and this was led to the 0.36 m ² first separation module 201 and concentrated until the ethanol concentration was 95.6% by mass.

Next, this concentrated vapor was guided to the second separation module 211 and further concentrated by the vapor permeation method. The permeation side of the second separation module 211 was depressurized to 1.5 kPa as in the method of Example 1 above. In this case, since it is vapor permeable, it is not necessary to apply heat energy for the operation of the second separation module 211. In the second separation module 211, the ethanol concentration reached when the membrane area is 0.3 m ² is 98.7% by mass. If the membrane area is increased to 1 m ^2, ethanol will be concentrated to 99.4% by mass. At this concentration, the partial pressure difference between the inside and outside of the membrane, which becomes the driving force for moisture permeation, is only 0.04 kPa. Even when the area was increased, water permeation did not progress and ethanol was not concentrated.

  That is, in this method, it is not necessary to add heat energy for membrane separation, but the concentration of ethanol that can be reached is low. In FIG. 4, 241 and 242 indicate the same vacuum pump as the vacuum pump 24 in the first embodiment, 251 and 252 indicate the same condenser as the condenser 25 in the first embodiment, and 26 indicates the condensation. The pump which takes out concentrated ethanol from the liquid tank 22 is shown.

(Comparative Example 2)
The block diagram shown in FIG. 5 is an apparatus configuration used in an experimental example in which the vapor at the top of the distillation column containing 90% by mass of ethanol is cooled and liquefied, and then the moisture content is reduced only by the pervaporation method. The members denoted by the same reference numerals as those in FIG.

  First, similarly to the method of Example 1 above, 8.9 kg / h of the top vapor containing 90% by mass of ethanol is obtained, and this is condensed by the top condenser 12 and stored in the condensate tank 22. After the pressure of the condensed liquid was increased to 700 kPa with the pressurizing pump 23, the condensed liquid was heated to 135 ° C. using the pervaporation heater 32 and supplied to the pervaporation separation module 30 of the zeolite membrane. Since the temperature of the solution in the module 30 decreases due to the vaporization of water through the membrane, the operation of taking out the liquid from the module 30 once, reheating it by the pervaporation heater 32 and sending it to the next module 30 was repeated.

  At this time, the condensate sent to the pervaporation heater 32 was preheated by the pressurizing pump 23 using the pervaporation heat exchanger 31.

The pervaporation and the heating of the liquid were repeated so that the temperature of the solution in the module was maintained at 130 to 135 ° C. If the pressure on the permeate side of the module 30 is kept at 8.5 kPa until the ethanol concentration reaches 95.6% by mass, and 1.5 kPa at higher concentrations, the separation module with a total membrane area of 0.6 m ² The concentration could be increased to 99.7% by mass.

  However, in this case, the thermal energy required for membrane separation is 495 kcal / h, which is much more than the method of Example 1. In FIG. Reference numerals 341 and 342 denote the same vacuum pump as the vacuum pump 24 in the first embodiment, and reference numerals 351 and 352 denote the same condenser as the condenser 25 in the first embodiment.

It is a block diagram explaining the schematic structure of the concentration apparatus of this invention. It is sectional drawing which shows an example of a vapor permeable separation module. It is an expanded sectional view which shows the tubular separation membrane and outer tube | pipe of a vapor permeable separation module. It is a block diagram explaining the schematic structure of the concentration apparatus using only a vapor permeation method. It is a block diagram explaining the schematic structure of the concentration apparatus using only the pervaporation method.

Explanation of symbols

1 Ethanol solution (fermented solution)
DESCRIPTION OF SYMBOLS 10 Distillation tower 11 Bottom liquid 12 Top condenser 20 Steam transmission separation module 21 Condensation steam condenser 22 Condensate tank 23 Pressure pump 24 Vacuum pump 25 Condenser 26 Pump 30 Pervaporation separation module 31 Pervaporation heat exchanger 32 Pervaporation heater 34 Vacuum pump 35 Condenser 101 First distillation column 102 Reboiler 111 Second distillation column 112 Reboiler 201 Steam permeation separation module 211 Steam permeation separation module 241 Vacuum pump 242 Vacuum pump 251 Condenser 252 Condenser 341 Vacuum pump 342 Vacuum pump 351 Condenser 352 Condenser

Claims (5)

A combination of a vapor permeation method using a vapor permeation separation module and an osmosis vaporization method using an osmosis vapor separation module to obtain a high concentration water-soluble organic substance by concentrating a mixture of the water-soluble organic substance and water. In the concentration method,
Obtaining a first concentrated steam in which organic matter is concentrated by distillation of a mixture of the water-soluble organic matter and water,
Thereafter, the first concentrated vapor is concentrated by a vapor permeation method using the vapor permeation separation module to obtain a second concentrated vapor,
Next, the second concentrated vapor is liquefied and concentrated by an osmotic vaporization method using the osmosis vapor separation module to obtain a high-concentration water-soluble organic substance. A water-soluble organic substance that obtains a high-concentration water-soluble organic substance by concentrating a liquid mixture of a water-soluble organic substance and water by combining a vapor permeation method using a vapor permeation separation module and an osmosis vaporization method using an osmosis vapor separation module. In the concentration method of
The vapor permeation separation module has a moisture permselective vapor permeable membrane that selectively permeates water vapor from the vapor supplied to the primary side to the secondary side,
The pervaporation separation module has a moisture permeation type pervaporation membrane that selectively permeates moisture from the solution supplied to the primary side to the secondary side,
The pressure on the secondary side of each membrane has a low have pressure than the primary side,
Concentrating the liquid mixture of the water-soluble organic substance and water by distillation to obtain a first concentrated vapor,
Thereafter, the first concentrated vapor is supplied to the moisture selective permeable vapor permeable membrane and concentrated by selectively allowing moisture to pass through to obtain a second concentrated vapor.
Next, the secondary concentrated vapor is liquefied to produce a liquefied concentrated water-soluble organic substance,
After pressurizing and heating the heated liquefied concentrated water-soluble organic matter,
A method for concentrating a water-soluble organic substance, characterized in that it is supplied to the moisture permselective pervaporation membrane and selectively permeated to obtain a high-concentration water-soluble organic substance. The concentration of the water-soluble organic substance in the mixed liquid of the water-soluble organic substance and water is 3% by mass to 50% by mass,
The concentration of the water-soluble organic substance in the first concentrated steam is 30% by mass to 95% by mass,
The concentration of the water-soluble organic substance in the secondary concentrated steam is 90% by mass to 99% by mass,
The concentration method of the water-soluble organic substance according to claim 1 or 2, wherein the concentration of the water-soluble organic substance in the high-concentration water-soluble organic substance is 95 mass% to 99.9 mass%. In a water-soluble organic substance concentration apparatus that obtains a high-concentration water-soluble organic substance by concentrating a mixture of a water-soluble organic substance and water,
A distillation column for concentrating the liquid mixture of the water-soluble organic substance and water by distillation to obtain a first concentrated vapor;
A vapor permeation separation module that supplies the first concentrated vapor to a moisture selective permeation type vapor permeable membrane and selectively permeates moisture to obtain a second concentrated vapor;
A concentrated steam condenser for liquefying the secondary concentrated steam to produce a liquefied concentrated water-soluble organic substance;
A pressure pump for pressurizing the produced liquefied concentrated water-soluble organic matter;
A pervaporation heater for heating and heating the pressurized liquefied concentrated water-soluble organic matter;
A permeable vapor separation module that supplies the pressurized and heated liquefied concentrated water-soluble organic substance to a moisture selective permeation type pervaporation membrane and selectively permeates the moisture to obtain a high-concentration water-soluble organic substance. An apparatus for concentrating water-soluble organic substances. The concentration of the water-soluble organic substance in the mixed liquid of the water-soluble organic substance and water is 3% by mass to 50% by mass,
The concentration of the water-soluble organic substance in the first concentrated steam is 30% by mass to 95% by mass,
The concentration of the water-soluble organic substance in the secondary concentrated steam is 90% by mass to 99% by mass,
The concentration device of the water-soluble organic substance in the high-concentration water-soluble organic substance is 95% by mass to 99.9% by mass.

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