JP4898358B2 - Distillation method and distillation apparatus - Google Patents

Description

  The present invention relates to a distillation method, and more particularly to a distillation method and a distillation apparatus suitable for distillation of distilled spirits such as shochu, whiskey, and brandy.

  "Continuous distillation" as a method of distillation such as moromi to produce distilled liquor, by continuously supplying raw materials to the distillation apparatus and continuously removing the distillate and the bottom liquid (bottom liquid) of the distillation apparatus In addition, there is “batch distillation” in which a raw material is put into a distillation apparatus for each distillation and distillation is performed. In addition, from the viewpoint of separation ability, there are “rectification” that performs high-level separation by reflux and “single distillation” that does not perform reflux, and single distillation equipment is usually used for the production of authentic shochu, whiskey, brandy, etc. A batch rectifier is used in part. Due to differences in distillation methods, the liquor tax law defines shochu produced by the continuous distillation method as `` continuous distillation shochu '' and shochu produced by methods other than the continuous distillation method as `` single distillation shochu ''. Of the “distilled shochu”, those that satisfy certain conditions are called “real shochu”.

  As shown in FIG. 5, the conventional “single distillation shochu” manufacturing method uses a distillation apparatus (100) having a distillation section (A) and a cooling section (B), and uses the distillation section (A). Filling liquid such as mash is heated and heated by a heating device to generate steam, and the steam is passed through (16) and introduced into the cooling section (B) where heat is exchanged with cooling water to condense the steam. The obtained condensate is recovered in the distillate tank (21). In addition, the flavor of the distillate in the distillate tank (21) varies depending on the amount of alcohol, acid, and other components contained.

  When producing a full-blown shochu by such a single distillation method, if the mash that has been fermented is distilled at normal pressure, a burnt odor may appear in the distillate at the end of the distillation and then gradually become stronger. The characteristics of the incense are called “end-smelling odor”, “post-scent odor”, and the like, and are regarded as defects that occur at the end of distillation in the atmospheric distillation method. In addition, at the end of distillation, the acid concentration increases and the taste of the distillate becomes heavy. At present, furfurals such as furfural, oxymethylfurfural, and methylfurfural are known as substances having a burning odor. In shochu, oxymethylfurfural is the main component, and during distillation, the carbohydrates in the mash are also decomposed by heating. It is thought to generate.

As a method for preventing the generation of furfural and producing a savory shochu, there is a method for producing a shochu characterized by instantaneously heating a shochu raw material (moromi) and evaporating it instantaneously (patent document) 1). The invention described in Patent Document 1 has a long heating time in the conventional production method and causes the generation of furfural, which is a quality-decreasing component. Therefore, the mash is instantly heated and instantly evaporated, and the evaporated component is distilled to form a component of shochu. Extract what you need. When the alcohol content in the mash is evaporated using a continuous instantaneous heating type evaporator under conditions where the degree of vacuum is from 700 Torr to 100 Torr and the heating temperature is from 183 ° C. to 100 ° C. In addition to preventing the thermal decomposition of the product, the generation of furfural, a component that degrades the quality, is reduced, and a good shochu with a good flavor can be achieved.
JP-A-8-84581

  However, in the instantaneous heating and instantaneous evaporation method described in Patent Document 1, since the heated raw material is instantly evaporated, it can be used in a continuous distillation apparatus, but batch distillation can use all the raw material at once. Cannot be performed because it cannot be sprayed.

  In addition, if the taste of shochu, whiskey, brandy, etc. can be adjusted, a product that better matches the taste of the consumer can be manufactured.

  Therefore, an object of the present invention is to provide a distillation method and a distillation apparatus for producing a distilled liquor that prevents the generation of furfural as a causative odor causative substance and that has a low acid concentration and has a good flavor.

  The present inventor has studied in detail how to shorten the heating time of the feed liquid in order to prevent the generation of furfural when producing distilled spirits such as shochu, whiskey, brandy, etc. As a result, the steam was cooled in the distillation apparatus. If the collected condensate is collected separately without mixing it in the feed liquid, the heating time of the feed liquid can be shortened, and the occurrence of furfural can be reduced. Distillation reduces the occurrence of furfural without reducing the yield, and the condensate has a low concentration of high-boiling components such as volatile acids. The inventors have found out what can be done and have completed the present invention.

  The distillation apparatus of the present invention is a distillation apparatus suitable for the production of distilled liquor, particularly shochu, and has a charging part and a condensate storage part in the distillation part, and is more efficient than a case where two distillation columns are provided. The furfural can be reduced easily and easily.

  The distillation apparatus of the present invention has a charging part and a condensate storage part in the distillation part, and when the condensate stored in the condensate storage part is distilled, the concentration of high-boiling components such as volatile acids is reduced. A distilled liquor having a lower acidity than the distillate of the charged solution can be produced.

The first of the present invention is a distillation apparatus having a distillation part and a cooling part for cooling the steam generated in the distillation part, wherein the distillation part is formed by partitioning the inside of the distillation part with a partition wall. And a condensate reservoir that communicates with the cooling unit and is a part other than the charging unit, and condenses vapor generated by heating the charging solution at the upper end of the charging unit. A communication part to be introduced into the liquid storage part is formed, the condensate storage part stores condensate obtained by introducing and condensing the steam, and the condensate is provided at the upper end part of the communication part. The distillation apparatus is provided with a backflow prevention mechanism that prevents the steam and / or condensate in the liquid storage part from flowing back to the charging part.

It said backflow prevention mechanism is a check valve or may be I placed on the bell-shaped lid der an upper end portion of the communicating portion.

The feed portion is provided with a heating device for heating the charge liquid, wherein the condensate reservoir, the condensate heating device for heating is provided to, and wherein the out of the distillation unit cuts the steam cooling section recirculation device may be provided for recirculating part or all of the condensate produced is introduced into the condensate reservoir in. Hereinafter, the present invention will be described with reference to the drawings showing preferred embodiments of the present invention.

(I) Distillation apparatus The distillation apparatus (100) of this invention has a distillation part (A) and a cooling part (B), as shown in FIG. 1, and the said distillation part (A) is a preparation liquid (3). ) And the condensate storage part (A2) communicating with the preparation part (A1), and the distillation part (A) is generated in the condensate storage part (A2). A lid (8) is provided as a backflow prevention mechanism that prevents the condensate from flowing back to the charging section (A1). Note that “Watari (16)”, which is a transition part of the steam generated in the charging part (A1) or the condensate storage part (A2) to the cooling part (B), is a part of the distillation part (A) and is condensed. A part of the liquid reservoir (A2) shall be configured.

(1) Preparation part and condensate storage part In the present invention, the preparation part (A1) and the condensate storage part (A2) can be formed by partitioning the inside of the distillation part (A) with a partition wall, At that time, at least a part of the communication part (C) is provided so that the vapor generated from the charged liquid (3) can be introduced into the condensate storage part (A2). For example, as shown in FIG. 1, a cylindrical partition may be provided inside the distillation section (A), the inside of the distillation section (A) may be the charging section (A1), and the outer periphery thereof may be the condensate storage section (A2). As shown in FIG. 3, the distillation part (A) may be divided into upper and lower stages, the lower part may be a charging part (A1), and the upper part may be a condensate storage part (A2).

In the present invention, the volume of the condensate storage part (A2) relative to the preparation part (A1) is 180 to 350, if the volume of the preparation part (A1) is 100. Preferably it is 200-320. Moreover, you may comprise so that the vapor | steam of a preparation part (A1) may be introduce | transduced into a condensate storage part (A2) through a vapor | steam channel | path (6), as shown in FIG. At this time, the upper end portion of the steam passage (6) serves as a communication portion (C) with the condensate storage portion (A2). The number of steam passages (6) is not limited to one, and a plurality of steam passages (6) may be provided, and the total cross-sectional area is 5 to 25%, preferably 10 to 15% of the charged portion cross-sectional area other than the steam passage (6). is there. If it is less than 5%, the pressure in the charging part may increase, and if it exceeds 25%, the effective bottom area of the condensate reservoir (A2) is small and may not be sufficient for condensate storage. However, as shown in FIG. 2, the condensate storage limit of the condensate storage part (A2) depends on the height of the steam passage (6), and therefore the lowest position of the one or more steam passages (6). It is preferable to adjust the height and volume of the steam passage so that the volume of the condensate storage part (A2) up to 80% to 120% of the volume of the charging part (A1). In addition, as shown to FIG. 13, FIG. 14, when a vapor | steam channel | path (6) is a type arrange | positioned in a condensate with a cover part, it is not limited to this.

  In the present invention, the charging unit (A1) is provided with a heating device (11) for heating the charging solution (3), and the condensate storage unit (A2) is provided with a heating device (13) for heating the condensate. In addition, as shown to FIGS. 1-3, in order to cool a preparation liquid (3), a cooling pipe (10) is accelerated | stimulated at a preparation part (A1), and distillation of a condensate is accelerated | stimulated at a condensate storage part (A2). A sub-heating device (14) may be provided. By disposing the cooling pipe (10) and the auxiliary heating device (14), the heating temperature of the charged liquid in the charging section (A1) and the condensate liquid in the condensate storage section (A2) can be quickly adjusted. . In addition, there is no restriction | limiting in particular as a heating apparatus (11, 13) or a subheating apparatus (14), The thing suitable for distillation of mash can be selected suitably, and can be used. For example, as a method for heating the mash in the shochu distiller, there are a method in which steam is blown directly into the mash (direct heating method) and a method in which steam is heated through a steam pipe or a jett (indirect heating method). According to the direct heating method, steam is blown into the crumb, so that the amount of the charged liquid (3) increases. However, in the indirect heating method, when the distillation proceeds, the charged liquid (3) decreases and the viscosity increases. , May burn. In the case of moromi with high viscosity such as potato shochu, the direct heating method and the indirect heating method are preferably used in combination, and can be appropriately selected depending on the properties of the feed liquid (3). Therefore, any of the heating devices (11, 13) and the auxiliary heating device (14) may be a direct heating type or an indirect heating method, or may be heated by other methods. Such a heating device and sub-heating device are not limited to 1, and a plurality of heating devices and sub-heating devices may be provided. In the present invention, a heating device for distilling the condensate in the condensate reservoir (A2) may be arranged in the preparation part (A1). For example, as shown in FIG. 13 and FIG. 14, steam heated by a steam injector (12) provided at the lower part of the steam passage (6) is introduced, and the condensate (5) is heated and evaporated. Can do. In addition, although not shown in figure, you may use together the heating jacket for heating a preparation part (A1) or a condensate storage part (A2).

(2) Backflow prevention mechanism and steam introduction mechanism In this invention, the vapor | steam which generate | occur | produced in the preparation part (A1) is introduce | transduced into a condensate storage part (A2) through a communication part (C). This steam passes through the condensate storage part (A2) and then moves to the cooling part (B), but a part of the steam comes into contact with the inner wall of the condensate storage part (A2) to become a condensate and the condensate storage part. Descent the wall of (A2). When the condensate is mixed into the charging liquid (3) of the charging part (A1), the heating time in the charging part (A1) may be extended due to an increase in the amount of the charging liquid, and furfural may be generated. Moreover, also when the vapor | steam in a condensate storage part (A2) flows back into a preparation part (A1), the amount of preparation liquids (3) of a preparation part (A1) increases. Therefore, in the present invention, in order to prevent the backflow of the condensate and steam to the charging section (A1), a condensate and / or steam backflow prevention mechanism is provided at the upper end of the communication section of the distillation section (A). Arrange.

(2-1) Lid (shallow type)
As such a backflow prevention mechanism, as shown in FIG. 1, there is a lid portion (8) provided at the upper end portion of the communicating portion . When the charging liquid (3) is heated by the heating device (11) provided in the charging section (A1) to generate steam, the lid (8) is lifted upward by the vapor pressure, and the steam is discharged from the charging section (A1). It moves to a condensate storage part (A2). On the other hand, if the heating in the charging section (A1) is stopped, the generation of vapor pressure stops, and the lid becomes liquid-tight with the top of the charging section (A1) due to the weight of the lid (8), and the condensate storage section ( The backflow of the condensate and vapor generated in A2) can be prevented. In addition, if such a cover part (8) has the tolerance with respect to the vapor pressure, temperature, and distillate in a preparation part (A1) or a condensate storage part (A2), it will be made of metals, such as SUS and aluminum. In addition, it can be prepared with glass, synthetic resin or the like. Moreover, you may prepare by the same or different member as the member which comprises the distillation part (A). The lid portion (8) in FIG. 1 is composed of an upper surface (8a) and a side surface (8b), and is therefore a shallow lid portion (8) with a short side surface (8b). For example, a “valve” may be configured by fixing only a part of the upper surface (8a) to the upper part of the communication part (C) with a hinge or the like.

(2-2) Bell-shaped lid As another backflow prevention mechanism, for example, a bell-shaped lid (7) shown in FIG. 2 can be used. The distillation apparatus (100) illustrated in FIG. 2 has a steam passage (6), and the bell-shaped lid (7) is placed on the upper portion of the steam passage (6). The lid (7) has a longer side surface (7b) than the lid (8) of FIG. 1, and the end of the side surface (7b) reaches the condensate stored at the bottom of the condensate reservoir (A2). To do. For this reason, the steam generated in the charging section (A1) flows into the steam passage (6) and then passes through the gap formed by the steam passage (6) and the side surface (7b) in the condensate storage section (A2). It is introduced into the condensate (5) stored at the bottom. Thus, if the vapor | steam from a preparation part (A1) is introduce | transduced into the condensate of a condensate storage part (A2), and it ensures as a condensate, the backflow of a vapor | steam can be prevented easily.

  Moreover, the float (9) may be arrange | positioned at the said side surface (7b) of the said bell-shaped cover part (7). If the bell-shaped lid (7) floats in the condensate via the float (9), the bell-shaped lid (7) floats according to the liquid level of the condensate, and from the charging section (A1) The vapor pressure of the vapor introduced into the condensate reservoir (A2) can be adjusted to be constant.

  The bell-shaped lid (7) can prevent the backflow of steam, but the condensate is charged from the gap formed by the steam passage (6) and the side surface (7b) (A1). ) May flow backward. For this reason, according to the amount of condensate in the condensate reservoir (A2), for example, as shown in FIG. 2, steam is introduced from a steam injector (12) provided at the lower portion of the steam passage (6). By using this apparatus together, it is possible to prevent not only the vapor but also the back flow of the condensate.

(2-3)
As another backflow prevention mechanism, there is a lid portion (63) shown in FIG. The upper part of the lower steam passage (6) is provided with a cover part (63) only on the upper surface, but the weight is adjusted so that the cover part (63) does not rise even when immersed in the condensate (5). Or a part thereof is fixed to the steam passage (6). Although this lid part (63) can introduce the vapor generated in the charging part (A1) into the condensate storage part (A2), it can prevent back flow to the charging part (A1) due to the pressure of the condensate. This is referred to as “mold lid”. The valve-type lid (63) prevents the condensate (5) from flowing backward, and also has an effect of introducing and bubbling the vapor generated in the charging section (A1) into the condensate (5).

  The valve-type lid portion (63) can prevent the backflow of steam, but since the lid portion is composed only of the upper surface, the gap between the lid portion (63) and the steam passage (6). There is a possibility that the condensate flows back to the charging part (A1).

  In addition, the valve-type lid portion may be a shallow valve-type lid portion (60) as shown in FIG. Similar to the lid portion (63) shown in FIG. 13, a shallow lid portion is provided at the upper end of the low steam passage (6), and the lid portion (60) even if submerged in the condensate (5). The weight is adjusted so as not to float, or as shown in FIG. 14, it is fixed to the steam passage (6) with a weak spring (61) or the like. Although this lid part can also introduce the vapor | steam which generate | occur | produces in a preparation part (A1) into a condensate storage part (A2), the backflow to a preparation part (A1) can be prevented with the pressure of a condensate. That is, when the steam is generated in the charging part (A1), the valve-type lid part (60) blows the steam from the steam passage (6) into the condensate in the condensate storage part (A2). When the temperature of (A1) decreases and the pressure of the charging part (A1) decreases, it adheres closely to the upper part of the charging part (A1) and does not cause the condensate (5) to flow back to the charging part (A1). . According to this valve-type lid part (60), it is possible to prevent the backflow of both condensate and steam.

  In order to ensure liquid tightness, a packing material such as elastomer may be used for the contact portion between the lid portions (60, 63) and the steam passage (6).

(2-4) Backflow prevention valve As another backflow prevention mechanism, there is a backflow prevention valve shown in FIG. In the present invention, the shape of the steam passage (6) is not particularly limited. For example, the top of the steam passage (6) constituting the communication portion (C) is deformed into a U shape toward the condensate (5). It may be. In this case, when the outlet of the steam passage (6) is inserted into the condensate (5) and the above-described valve-type lid (60, 63) is disposed at the outlet as shown in FIG. The backflow of liquid and vapor can be prevented.

(2-5) Steam Introducing Mechanism In the distillation apparatus of the present invention, it is preferable to provide a steam introducing mechanism such as a steam injector (12) in the distillation section (A), particularly the charging section (A1 ) . If steam is introduced by a steam introduction mechanism such as a steam injector (12) provided in the charging section (A1) , the condensate (5) can be heated and distilled. When the steam generated in the charging section (A1) contains a plurality of components, the solubility of each component in the condensate (5) varies depending on the vapor pressure. It is because it can introduce | transduce and can change the composition of a condensate by this. As such a steam introduction mechanism, for example, there is the above-described steam injector (12), and “a steam introduction mechanism for introducing the steam generated in the charging section into the condensate (5) in the condensate storage section” in the present invention. It becomes.

  Moreover, the steam generated in the charging section (A1) can be introduced into the condensate in the condensate storage section (A1) by such a steam injector (12). For example, when steam is introduced from the bell-shaped lid (7) of FIG. 2 by the steam injector (12), the pressure in the charging part (A1) is increased, and the condensate (5) flows back to the charging part (A1). Can be prevented. Therefore, the steam injector (12) can be a backflow prevention mechanism in the present invention. Further, the bell-shaped lid (7) described above can be a steam introduction mechanism simultaneously with the backflow prevention mechanism. When the steam or steam generated in the charging part (A1) is introduced into the condensate and heated and evaporated, the bell-shaped lid part (7) is placed on the upper part of the steam passage (6). The steam generated in A1) is introduced into the condensate (5) stored in the bottom of the condensate storage part (A2) through a gap formed by the steam passage (6) and the side surface (7b). Because.

  Further, the steam passage (6) deformed into a U-shape shown in FIG. 12 described above is also capable of introducing the steam from the charging section (A1) into the condensate (5). At the same time, it becomes a steam introduction mechanism. Accordingly, in the present invention, the backflow prevention mechanism, the steam introduction mechanism, the steam introduction mechanism and the like do not have to exist as separate bodies as long as they have the function, and one member has the function of the other member. Or they may be configured as one piece.

(3) Reflux device The distillation unit (A) is preferably provided with a reflux device that circulates a part of the condensate introduced into the cooling unit (B) to the condensate storage unit (A2). As described above, the composition of the distillate can be adjusted by the amount of the condensate in the condensate reservoir (A2), but the amount of the condensate can be easily adjusted by arranging the reflux device. Because it can.

  A distillation apparatus (100) provided with such a reflux apparatus is shown in FIGS. 2 to 4, 13, and 14. FIG. The inner diameter, length, etc. of the reflux pipe having the condensate discharge port (15) are not particularly limited, as long as the condensate can flow back from the cooling part (B) to the condensate storage part (A2). Good. Further, the reflux device is provided with a cock (20) for refluxing the condensate to the condensate reservoir (A2) and a cock (19) for collecting it outside the system.

(4) Bubbling type distillation apparatus An example of the preferable aspect of the distillation apparatus (100) of this invention is demonstrated with reference to FIG. 2 can bubble the steam generated in the charging section (A1) to the condensate in the condensate reservoir (A2) via the bell-shaped lid, which is referred to as “bubbling type” in the present specification. It is called a “distillation device”.

  The distillation apparatus used in the present invention is provided with a charging section (A1) in the distillation section (A) and a condensate storage section (A2) in the upper stage for condensing steam generated in the charging section (A1). One or a plurality of steam passages (6) leading upward from the liquid reservoir (A2) are provided. The capacity of the charged portion (A1) is at least 150% or more, more preferably 180 to 220% of the planned charged liquid volume. The reason why it is set to 150% or more is that foaming when the charged liquid boils in the charged portion (A1) and an increase due to condensation of steam blown in order to heat are taken into consideration. Further, a heating device (11) for heating the raw material liquid and a cooling pipe (10) are introduced into the bottom of the charging section (A1), and a space on the liquid surface of the planned charging liquid to be put into the charging section (A1). And a steam injector (12). Steam can be generated from the steam injector (12) and introduced into the condensate in the condensate reservoir (A2). The cooling pipe (10) is used to cool the residual liquid in the charging section (A1) through cold water immediately after the distillation of the charging section (A1) is completed. Can be used. If the volume of the condensate reservoir (A2) is 100, the volume of the condensate reservoir (A2) is 180 to 350, more preferably 200 to 320. 180 or more was taken into account that the amount of liquid in the condensate storage part (A2) gradually increases due to the condensation of the vapor in the distillation part (A) and the condensate storage part (A2) and the reflux by the reflux device. It is. In addition, the heating apparatus (13) of a condensate storage part (A2) is arrange | positioned at the bottom part of the condensate storage part (A2). When the condensate in the condensate reservoir (A2) increases too much, the amount of liquid can be adjusted by heating with the heating device (13). The cooling unit (B) is provided with a reflux device for refluxing the condensate to the condensate storage unit (A2), and the condensate in the condensate storage unit (A2) depends on the amount of reflux of the condensate. The amount can be adjusted.

  The upper part of the steam passage (6) is covered with a bell-shaped lid (7), and the bell-shaped lid (7) is provided with a float (9), which moves up and down in the condensate. Can do. When the condensate increases in the condensate reservoir (A2), the bell-shaped lid (7) floats by the float (9), and the lower end of the side surface (7b) of the bell-shaped lid (7) extends from the liquid level. A certain depth can be maintained, and steam can be introduced while bubbling all of the condensate in the condensate reservoir (A2) while keeping the pressure in the charging section (A1) constant. In addition, you may fix to an appropriate depth, without attaching a float (9). When the height of the bell-shaped lid (7) is fixed to an appropriate height, bubbling is started after the condensate in the condensate reservoir (A2) has accumulated at a predetermined height.

  The distillation apparatus shown in FIGS. 2, 4, 13, and 14 is also a bubbling distillation apparatus.

(5) Non-Bubbling Distillation Device An example of another preferred embodiment of the distillation device (100) of the present invention will be described with reference to FIG. In the distillation apparatus of FIG. 3, the steam in the charging section (A1) is transferred to the cooling section (B) without being bubbled into the condensate in the condensate storage section (A2). This is referred to as a “non-bubbling distillation apparatus”.

  The difference from the distillation apparatus shown in FIG. 2 is that a light and shallow lid (8) is disposed at the upper end of the steam passage (6) as a backflow prevention mechanism, and a steam injector (12) is disposed at the charging section. That is not the point. When the shallow lid portion (8) is made of a light material, when steam is generated in the charging portion (A1), the shallow lid portion (8) is lifted by the vapor pressure, and the steam is shallow in the shallow lid portion (8 ) Straightly flows into the condensate storage part (A2) from the lower end, and can further shift to the cooling part (B). In addition, when generation | occurrence | production of the vapor | steam in a preparation part (A1) is stopped and an inside becomes a negative pressure, since a shallow type | mold cover part (8) will closely_contact | adhere to an upper end of a vapor | steam channel | path (6), a vapor | steam does not flow backward, Steam backflow can be prevented.

  If an outside air introduction pipe (17) having a cock (25) is provided at the top of the charging section (A1), and the heating of the charging section (A1) is completed, the cock (25) is opened to communicate with the outside. The inside of (A1) becomes equal to atmospheric pressure, and backflow from the condensate reservoir (A2) can be prevented.

(6) Batch rectifier Further, an example of another embodiment of the present invention will be described with reference to FIG.

The difference between the distillation apparatus shown in FIG. 4 and the distillation apparatus shown in FIG. 3 is that the distillation part (A) has a shelf part (A3) in which a shelf or a filler communicating with the condensate storage part is arranged. Is a point. The lowermost stage (first stage) has a charging part (A1), and the upper part (second stage) has a condensate storage part (A2). The steam passage (6) communicating from the first stage to the second stage has A bell-shaped lid (7) with a float is provided, and in addition, a cooling pipe (10) and a heating device (11) are arranged. A shelf (49, 50, 51) is provided above the third level, and a downcomer (52, 53, 54) is provided on each shelf to keep the amount of liquid constant. Further, a part of the condensate obtained by cooling the vapor coming from the top of the tower by the reflux apparatus by the cooler (B) is refluxed to the uppermost stage. Although various types of shelves can be used, perforated plate trays widely used in rectification towers can be suitably used. If the perforated plate tray is not refluxed, the steam passes through the perforated plate, so that the rectifying effect is low. If refluxed, the rectifying effect is increased, so that various distilled liquors can be produced. In this distillation apparatus, the reflux device has a structure in which the condensate is refluxed from the cooling part (B) to the condensate storage part (A2), and is returned to the shelf part (A3) as shown in FIG. May be. Further, a steam passage (6) for introducing the steam from the charging section (A1) into the condensate storage section (A2) is arranged, and the upper part thereof is covered with a bell-shaped lid section (7).

  In the present invention, the charging unit (A1) in which the raw material is put is kept in a short time by condensing as much as possible, and the generated condensate is not mixed into the charging unit (A1), but the condensate storage unit (A2). In addition to the above, various forms are possible as long as they are allowed to flow into and separately distilled, and these apparatuses can be used for a single distillation apparatus and a batch rectifier in addition to a continuous type.

(II) Distillation method The second of the present invention is a distillation method using the above distillation apparatus, wherein the vapor generated by heating the charged liquid in the charged portion is transferred to the condensate reservoir via the backflow prevention mechanism. Introducing the vapor of the condensate storage unit into the cooling unit, returning a part or all of the condensate generated by cooling the cooling unit to the condensate storage unit, and the condensate And a step of obtaining a distillate by heating the condensate of the steam generated and stored in the condensate reservoir and introducing the generated steam into the cooling section . This is a distillation method. The distillation method of the present invention may be carried out continuously or batchwise. By storing the condensate of vapor generated in the condensate storage part (A2) in the storage part, the condensate is prevented from flowing back to the preparation part (A1), and the amount of preparation liquid is prevented from increasing. Time can be shortened and the occurrence of furfural can be prevented.

(1) Non-Bubbling Distillation Method The steam from the charging section (A1) is not bubbled into the condensate (5) of the condensate storage section (A2), and constitutes a part of the condensate storage section (A2). In order to transfer to the cooling part (B) as it is via (16), this distillation method is referred to as “non-bubbling distillation method” in the present specification.

  The non-bubbling distillation method of the present invention will be described with reference to FIG. In addition, this apparatus is the distillation apparatus (100) by which the condensate storage part (A2) was arrange | positioned in the outer periphery of the preparation part (A1).

  The charging unit (A1) is provided in the distillation apparatus (100), the upper part of the communication part (C) with the condensate storage part (A2) is covered with a shallow lid part (8), and the inside of the charging part (A1) is also melted. When the charged liquid (3) is heated by the charging device (11), the generated steam pushes the lid portion (8) covering the communicating portion (C) upward with vapor pressure, and then the lid It is introduced straight into the condensate reservoir (A2) through the side of the section (8). In the condensate storage part (A2), the steam further rises, passes through (16), reaches the cooling part (B), cools and condenses, and is introduced into the distillate tank (21). On the other hand, a part of the vapor in the condensate reservoir (A2) is cooled and condensed on the inner wall of the condensate reservoir (A2), flows down the inner wall, and is stored in the bottom of the condensate reservoir (A2).

  In the present invention, when charging liquid is continuously supplied from a raw material supply port (not shown), the condensate in the condensate reservoir (A2) is heated by the heating device (13), and the condensate is distilled. In addition, the distillation can be continuously carried out by the above method.

  On the other hand, when the batch distillation is carried out using the apparatus, the charged liquid (3) is heated by a heating apparatus (11) or the like, and the alcohol concentration of the vapor generated in the charged part (A1) by the progress of distillation is previously determined. When it becomes a predetermined value, for example, 10% (v / v) or less, or the alcohol content of the charging liquid (3) in the charging section (A1) becomes a predetermined value, for example, 1% (v / v) or less. The heating of the charging part (A1) liquid is stopped. The furfural once distilled from the charging section (A1) is likely to evaporate and easily shift to a product, and therefore the heating stop timing of the charging section (A1) is important. It is certain that the vapor generated in the charging section (A1) is collected and the alcohol concentration is analyzed and determined, but the residual liquid in the charging section (A1) is collected and analyzed for alcohol concentration. From this, the alcohol concentration of the steam may be estimated to determine the heating stop timing of the charging section (A1). In the distillation of authentic shochu, it is common to stop collecting the distillate when the alcohol concentration of the distillate drops to about 10 to 15% (v / v).

  Next, the condensate in the condensate reservoir (A2) is distilled by heating with the heating device (13), and the alcohol concentration of the distillate recovered in the distillate tank (21) is lower than a predetermined value. When the distillation is complete, the distillation is terminated. A part of the steam is cooled and condensed in the condensate storage part (A2) and stored in the bottom of the condensate storage part (A2), but this condensate has finished distillation of the charging part (A1) Then, it may be distilled, or it may be distilled together with distillation of the charging part (A1). If distillation is performed at the same time, the distillation time can be shortened. When heating the condensate storage part (A2), in order to suppress the boiling of the residual liquid in the charging part (A1), a cooling pipe (10) or the like is used to keep the residual liquid in the charging part (A1). It is preferable to suppress boiling of the residual liquid. This is to prevent evaporation of furfural due to boiling.

  The non-bubbling distillation method of the present invention can also be carried out with an apparatus in which the charging section (A1) and the condensate storage section (A2) are arranged one above the other. For example, FIG. 3 shows a distillation apparatus (100) in which a charging section (A1) and a condensate storage section (A2) are arranged up and down. According to the apparatus of FIG. 3, since the preparation part (A1) and the condensate storage part (A2) are arranged one above the other, the area of the condensate storage part (A2) can be secured widely, When the condensate storage unit (A2) is passed from the cooling unit (B) through the reflux device, the degree of freedom of disposing the reflux device is improved. When the charging liquid (3) is poured into the charging section (A1) of the distillation apparatus (100) and heated, the steam generated in the charging section (A1) rises through the steam passage (6), and the steam path (6 ) Through the side of the lid (8) covering the upper part of the condensate storage part (A2) and further rises straight, and most of the steam flows to (16) as it is. The heating stop conditions in the charging section (A1) are the same as those in the apparatus of FIG.

  In the method of the present invention, when the condensation of the steam generated in the charging section (A1) is suppressed, the heating time in the charging section (A1) is shortened and the amount of furfural generated is further reduced. For example, the charging part (A1) and the communication part (C) and the cover part (31) are sufficiently insulated from the outside by covering the outer periphery of the charging part (A1) with a heat insulating material, and the like in the charging part (A1). It is preferable to carry out the distillation operation while keeping the temperature uniform. Note that, when the heating in the charging section (A1) is stopped and the residual liquid is cooled, the pressure in the charging section (A1) is reduced, and an air flow from the condensate storage section (A2) to the charging section (A1) is generated. However, the backflow prevention mechanism of the lid (8) provided at the upper end of the steam passage (6) can prevent the condensate from entering the charging part (A1).

  In the non-bubbling distillation method of the present invention, the condensed liquid can be refluxed. For example, when the apparatus shown in FIG. 3 is used, the liquid amount in the condensate storage part (A2) is stored to a predetermined amount by reflux immediately after the start of the distillation operation, for example, 10% of the charged liquid volume, and then cooled. You may collect | recover the condensate of a part (B) with a distillation tank (21). Thereby, stabilization of the distillate component can be achieved.

  In the present invention, it has been found that the composition of the distillate can be adjusted by controlling the amount of the condensate accumulated in the condensate reservoir (A2) (see Examples). That is, according to the non-bubbling distillation method, most of the steam rising from the charging section (A1) passes through the condensate storage section (A2) and flows into the cooling section (B). A type of distilled liquor close to the apparatus can be produced. On the other hand, if the heating time of the charging section (A1) and / or the condensate storage section (A2) is lengthened to increase the evaporation amount, the taste of the distillate can be concentrated. Further, the amount of the reflux liquid can be reduced, and the flavor of the distillate can be increased. On the contrary, if the heating time of the charging part (A1) and / or the condensate storage part (A2) is shortened to reduce the evaporation amount, the taste of the distillate can be made lighter and the reflux liquid amount is increased. The flavor can be lightened. For example, the distillate is fully refluxed until the alcohol concentration in the charging section (A1) decreases to a predetermined value, for example, 1.0% (v / v) as the distillation proceeds, and the condensate storage section (A2). If the condensate is stored in the tank, and then the distillation of the charging part (A1) is stopped and the condensate storage part (A2) is distilled, the whole amount of the condensate is distilled, and the acidity is low. Sake is obtained. As described above, according to the distillation method of the present invention, not only the production amount of furfural can be reduced, but also from a conventional flavor to a low-acidity, light liquor-type distilled liquor. it can.

  The above distillation method can be used not only for the atmospheric distillation apparatus but also for the vacuum distillation apparatus.

(2) Bubbling-type distillation method The distillation method which introduce | transduces the vapor | steam from a preparation part (A1) into a condensate storage part (A2), bubbling is called a "bubbling-type distillation method."

  The composition of the distillate recovered in the distillate tank (21) changes depending on the amount of the condensate in the condensate reservoir (A2), and also in the condensate reservoir (A2). It also changes with changes in the composition of the condensate. When steam is introduced into the condensate in the condensate reservoir (A2), the composition of the condensate can be adjusted. This distillation method will be described with reference to FIG.

  In the apparatus of FIG. 2, the charging section (A1) and the condensate storage section (A2) are arranged one above the other, and a bell-shaped lid section (7) is provided above the steam passage (6) functioning as the communication section (C). ) And a reflux device for returning the condensate in the cooling part (B) to the condensate storage part (A2) is provided, and a steam injector (12) is provided in the charging part (A1). Yes.

  The bubbling type distillation method using the distillation apparatus (100) is carried out batchwise. When the charging section (A1) is heated, the generated steam rises through the steam passage (6), and the condensate storage section (A2) of the condensate storage section (A2) is formed from the side of the bell-shaped lid section (7) by the bell-shaped lid section (7). Steam is blown into the bottom and becomes a condensate. If a predetermined amount of condensate is present, the steam introduced thereafter is blown into the condensate and heat exchanged with the condensate, condensing the high-boiling components in the steam, and evaporating the low-boiling components in the condensate. Is done. In the present invention, in order to effectively introduce the heat exchange and the vapor component into the condensate, a part of the condensate is recirculated to the condensate reservoir (A2) by the reflux device to adjust the amount of the condensate. . Further, after the heating of the charging section (A1) is stopped, steam is supplied from the steam injector (12), and steam is blown into the bottom of the condensate storage section (A2) from the side of the bell-shaped lid section (7). The heating stop conditions in the charging section (A1) are the same as in the non-bubbling distillation method.

  In the bubbling type distillation method, the condensate in the cooling part (B) is returned to the condensate storage part (A2) at the start of distillation, and a certain amount of condensate is stored in the condensate storage part (A2). The amount of condensate in the condensate reservoir (A2) gradually increases due to the condensation of the vapor in (A2). However, the concentration of furfural in the condensate is low, and even if it takes time to heat-distill the condensate, no new furfural is generated, so that the transition of the furfural to the distillate can be reduced. In addition, if a predetermined amount of water, a part of the target distillate, and the like are put in the condensate storage unit (A2) in advance and the distillation operation is started, the time for storing the reflux liquid can be shortened.

  According to the bubbling type distillation method described above, since there is a rectification effect corresponding to one stage of a normal distillation column, a distillate having a higher alcohol concentration can be obtained.

  In addition, according to the bubbling distillation method, the alcohol concentration of the distillate decreases as the amount of the condensate in the condensate reservoir (A2) at the start of distillation decreases, but in the non-bubbling distillation method described above, Since only the liquid stored in the condensate storage part (A2) is distilled later, the more the condensate storage part (A2) liquid amount, the more the flavor of the distillate such as distilled liquor recovered in the distillate tank. It becomes pale. In the present invention, as described above, distilled liquors having different flavors can be produced by the two methods of the bubbling distillation method and the non-bubbling distillation method.

(3) Distillation method with shelf part The third aspect of the present invention uses a distillation apparatus in which a shelf or packing having a rectifying function is arranged in the condensate storage part, and the feed liquid of the preparation part When the alcohol concentration of the steam in the charging section generated by the heating or the alcohol concentration of the charging liquid falls below a predetermined value, the heating of the charging section is stopped, and then the condensation in the condensate storage section The distillation method is characterized in that the liquid is heated and the generated steam is introduced into the cooling section to obtain a distillate. In this method, a shelf portion is further added to the bubbling distillation method described above.

A distillation apparatus suitable for this distillation method is shown in FIG. In the apparatus of FIG. 4, the charging part (A1) and the condensate storage part (A2) are arranged vertically, and the charging part (A1) and the condensate storage part (A2) communicate with each other through the steam passage (6). Furthermore, a shelf step (A3) in which a shelf or a filler is disposed is arranged above the condensate reservoir (A2). The shelf (A3) is connected to the condensate reservoir (A2), and a reflux device that recirculates part or all of the condensate generated in the cooling unit (B) to the condensate reservoir. It is arranged. Further, a steam passage (6) for introducing the steam from the charging section (A1) into the condensate storage section (A2) is arranged, and the upper part thereof is covered with a bell-shaped lid section (7). Note that a steam injector (12) is provided in the charging section (A1).

In the distillation method of the present invention, first, the charging liquid (3) is put into the charging section (A1) and heated, and the resulting steam is passed through the bell-shaped lid section (7) at the top of the steam passage (6). was introduced into the condensate reservoir (A2), then through the condensate reservoir and (A2) were introduced into trays portion (A3), generated in the condensate reservoir (A2) and tray portion (A3), flow down The condensate to be accumulated is stored in the condensate reservoir (A2). At this time, a part or all of the condensate produced in the cooling section (B) is returned to the shelf section (A3) by the reflux device. When the alcohol concentration of the steam generated in the charging section (A1) or the alcohol concentration of the charging section (A1) becomes a predetermined value, for example, 1.0% (v / v) or less due to the progress of distillation, the charging is performed. The heating of the part (A1) is stopped, the residual liquid in the charging part (A1) is immediately cooled by the cooling pipe (10) to suppress boiling, and thereafter the steam injector (12 provided above the charging part (A1)) ), And steam is distilled while refluxing with a reflux device, and a part of the condensate is distilled to the distillate tank (21) by opening the valve (19). When the alcohol concentration of the distillate collected in the distillate tank (21) becomes lower than a predetermined value, the distillation is terminated.

  That is, the vapor from the charging unit (A1) is introduced into the entire condensate storage unit (A2) and stored as condensate. After the distillation of the charging unit (A1) is finished, the condensate in the condensate storage unit (A2) is removed. Distill. When heating of the charging section (A1) is stopped, furfural is not generated, and therefore the amount of furfural in the condensate storage section (A2) and rectification section (A3) does not increase, so it is purified through the rectification section (A3). Thus, furfural can be separated efficiently.

  According to the above distillation method, the condensation is minimized in the charging section (A1) and distilled in a short time, and the distillate is rectified in the upper rectifying section. Therefore, the amount of furfural produced in the charging section (A1) And the amount of furfural distillate can be reduced.

  In the distillation method of the present invention, the predetermined amount of alcohol can be appropriately selected according to the distillation conditions and the flavor of the target distillate.

  EXAMPLES Next, although an Example is given and this invention is demonstrated concretely, these Examples do not restrict | limit this invention at all.

Example 1 (Bubbling type)
(1) The distillation apparatus shown in FIG. 2 was used. The charging part (A1) is cylindrical and has a glass separable flask with a capacity of 2,000 ml. The condensate storage part (A2) is cylindrical and is made of glass with a capacity of 1,400 ml. The inner diameter is 15 mm, the outer diameter is 35 mm, and the height is high. One steam passage (6) having a length of 85 mm is provided, and an aluminum bell-shaped lid portion having a depth of 100 mm and a radius of 50 mm, in which a glass float (9) is provided at the upper end of the steam passage (6). 7) is coated. A heating jacket (not shown) is provided outside the charging section (A1).

  (2) 500 ml of fermented moromi mash (brown sugar shochu mash, alcohol 16.2% (v / v), acidity 6.1) is placed in the charging section (A1) and gently heated from the outside with a heating jacket. After reaching 70 ° C., the mashing temperature was heated to 99 ° C. even when steam was blown from the heating device (11). The cock 20 is opened and the cock 19 is closed until 50 ml of condensate has accumulated in the condensate reservoir (A2), the condensate is returned to the condensate reservoir (A2) from the condensate outlet, and then the cock 19 is opened. As a result, the distillate was collected in the distillate tank (21). The distillate was collected in 12.5 ml portions. Further, 5 ml of mash of the preparation part (A1) was sampled and the alcohol concentration thereof was measured.

  When the mash's alcohol concentration in the charging part (A1) becomes 0.7% (v / v) (17.5% of the charged raw material is distilled), from the heating device (11) to the charging part (A1) Then, steam was blown from the steam injector (12) at a rate of 5 g / min and distilled while bubbling the condensate in the condensate reservoir (A2).

  As a control, a cylindrical separable flask having a volume of 2,000 ml shown in FIG. 5 was used. 500 ml of the same mash was put in the charging portion, and gently heated by a heating jacket (not shown). After heating to 0 ° C., steam was blown from the heating device (11) and the mash temperature was heated and distilled to 99 ° C., and 12.5 ml of distillate was sampled from the distillate tank (21).

  (3) In the example (bubbling type) and the control, fractionation was performed up to the first section where the alcohol concentration of the distillate was lower than 10.0% (v / v). The relevant fraction in the bubbling type is Category 1 to 10 (alcohol content 83.0 to 9.5% (v / v)), and the control is Category 1 to 13 (alcohol content 77.0 to 9.55% ( v / v)).

  Bubbling-type sections 1 to 10 and control sections 1 to 13 were mixed in a fixed amount to obtain a “mixed sample”. Further, the alcohol concentration of the mixed sample was adjusted to 25% (v / v) with distilled water to obtain an alcohol concentration adjusted sample.

  (4) The alcohol concentration of the mixed sample was measured. Further, the acidity, 275 nm ultraviolet absorption, and furfural concentration of the alcohol concentration adjusted sample were measured.

i) Alcohol Alcohol was measured with Alcomate (Riken Keiki AL-2 type).

i) Acidity One to two drops of phenolphthalein indicator was added to 5 ml of a sample, titrated with an N / 100 sodium hydroxide solution, and the value obtained by multiplying the titration constant by 2 was defined as acidity.

ii) Furfural Freshly distilled aniline 9.0 was mixed with 5.7 ml of glacial acetic acid, and ethyl alcohol was added to 3 ml of the mixed solution to make 100 ml to obtain an aniline acetic acid solution. Also, 1 g of freshly distilled furfural was dissolved in 100 ml of ethyl alcohol, and 1 ml of this was dissolved in 100 ml of 50% (v / v) alcohol. Since this liquid has a furfural content of 0.1 mg / ml, it was appropriately diluted with water to form a furfural standard solution series containing 0.01 to 0.2 mg of furfural in 5 ml.

  Take 5 ml of furfural standard solution, add 15 ml of aniline acetic acid solution, shake well and leave at 18 ° C. for 1 hour, then measure the absorbance at 505 nm to prepare a calibration curve. Similarly, take 5 ml of sample and add 15 ml of aniline acetic acid solution. The mixture was shaken well and allowed to stand at 18 ° C. for 1 hour, and then the absorbance was measured at 505 nm. The concentration of furfural was obtained from a calibration curve, and the value was multiplied by 20 to obtain the amount of furfural (mg) in 100 ml of the sample.

iii) 275 nm UV absorption Since the furfural concentration correlates with the UV absorption at 275 nm, the sample was filtered with a membrane run filter (Millipore 0.45 μm), and then a spectrophotometer (Hitachi U-2001 type) was used. ), The ultraviolet absorption at 275 nm was measured.

(5) Results (i) Concentration of alcohol The alcohol concentration of the charged solution of the charging portion (A1) and the distillate collected separately is shown in FIG. The alcohol concentration of the distillate was higher than that of the control, and the alcohol concentration rapidly decreased after stopping the steam blowing from the heating device (11) to the charging section (A1).

(Ii) UV absorption (275 nm)
As shown in FIG. 7, from the start of distillation to the stop of steam, the bubbling type and the control showed substantially the same ultraviolet absorption (275 nm). However, in the bubbling type, after the steam supply from the heating device (11) was stopped at the charging unit (A1), the ultraviolet absorption (275 nm) in the distillate rapidly decreased from the 8 fractions of distillate, The control increased rapidly.

(Iii) Acidity of the distillate The measurement results of the acidity are shown in FIG. The acidity of the distillate in the bubbling type was lower than that of the control from the beginning, and the acidity further decreased after stopping the blowing of steam from the heating device (11) in the charging section (A1).

(Iv) Composition of collected sample Table 1 shows the measurement results of alcohol concentration, acidity, furfural, and ultraviolet absorption (275 nm) of the mixed sample in the bubbling type and the control.

  The bubbling-type alcohol concentration-adjusted sample had a significantly higher alcohol concentration of 13.6 points than the control, and the alcohol recovery rate was 3 points lower than the control. The furfural and ultraviolet absorption (275 nm) of the bubbling type was significantly lower than that of the control, and the acidity of the bubbling type was significantly lower than that of the control. From the above, the bubbling type distillation method was effective in reducing furfural and acidity as compared with the conventional single-type distiller.

実施例２（非バブリング型）
（１） 図３に示す蒸留装置を使用した。仕込み部（Ａ１）は円筒状で、容量２，０００ｍｌのガラス製セパラブルフラスコ、凝縮液貯留部（Ａ２）は円筒状で容量１，４００ｍｌのガラス製であり、内径１５ｍｍ、外径３３ｍｍ、高さ８５ｍｍの蒸気通路（６）が１つ設けられ、前記蒸気通路（６）の上部に、ガラス製の浅い蓋部（８）が被覆されている。実施例１と同様に、仕込み部（Ａ１）の外部には、図示しない加熱ジャケットが設けられている。

Example 2 (non-bubbling type)
(1) The distillation apparatus shown in FIG. 3 was used. The charging part (A1) is cylindrical and has a glass separable flask with a capacity of 2,000 ml. The condensate storage part (A2) is cylindrical and is made of glass with a capacity of 1,400 ml. The inner diameter is 15 mm, the outer diameter is 33 mm, and the height is high. One steam passage (6) having a length of 85 mm is provided, and a shallow lid portion (8) made of glass is covered on the upper portion of the steam passage (6). Similar to the first embodiment, a heating jacket (not shown) is provided outside the charging section (A1).

  (2) 400 ml of moromi mash that has been fermented in the charging section (A1) (brown sugar shochu mash, alcohol 16.3% (v / v), acidity 6.6) is slowly heated from the outside with a heating jacket, After reaching 70 ° C., steam was blown from the heating device (11) and the mash temperature was heated and distilled to 99 ° C., and 10 ml of the distillate was sampled from the distillate tank (21). As in Example 1, steam was blown from the heating device (11) into the charging section (A1) until the amount of the distillate reached 17.5% (Section 7) of the charged raw material, and thereafter, Steam was blown into the condensate (5) in the condensate reservoir (A2) from the heating device (14) and distilled.

  As a control, a cylindrical separable flask having a volume of 2,000 ml shown in FIG. 5 was used, and 400 ml of the same mash as above was placed in the charging portion, and gently heated by a heating jacket (not shown). After heating to ° C., steam was blown from the heating device (11) and the mash temperature was heated to 99 ° C. and distilled, and 10 ml of distillate was sampled from the distillate tank (21).

  (3) Sorted samples were collected up to the first section where the alcohol concentration was below 10.0% (v / v). The fraction in the non-bubbling type is Category 1-12 (alcohol content 80.00-8.45% (v / v)) and the control is Category 1-13 (alcohol content 79.50-10.00% (V / v)).

  Non-bubbling sections 1 to 12 and control sections 1 to 13 were mixed in a fixed amount to form a “mixed sample”. Further, the alcohol concentration of the mixed sample was adjusted to 25% (v / v) with distilled water to obtain an alcohol concentration adjusted sample. This sample was analyzed in the same manner as in Example 1.

(4) Results (i) Concentration of alcohol The transition of the concentration of alcohol is shown in FIG. The alcohol concentration at the beginning of the non-bubbling distillation (sections 1 to 4) was almost the same as that of the control, but the alcohol concentrations of sections 5 to 7 were lower than those of the control. In addition, after stopping the steam blowing from the heating device (11), the alcohol concentration immediately after starting the distillation of the condensate in the condensate reservoir (A2) was 12.5 points higher than the control.

(Ii) UV absorption (275 nm)
As shown in FIG. 10, in the non-bubbling type, the ultraviolet absorption (275 nm) of the distillate rapidly decreased after the stop of steam blowing from the heating device (11).

(Iii) Acidity of the distillate The measurement results of the acidity are shown in FIG. In the non-bubbling type, after stopping the steam blowing from the heating device (11), the acidity also decreased sharply compared to the control. 8 and 11, the bubbling type has a lower acidity than the non-bubbling type because the condensate is distilled from the beginning unlike the non-bubbling type.

(Iv) Composition of collected sample Table 2 shows the measurement results of alcohol concentration, acidity, furfural, and ultraviolet absorption (275 nm) of the mixed sample in the non-bubbling type and the control.

  The non-bubbling type alcohol concentration-adjusted sample had significantly lower furfural concentration, ultraviolet absorption (275 nm) and acidity than the control. On the other hand, there was no big difference in the alcohol recovery rate and the alcohol concentration of the mixed sample. From the above, the non-bubbling distillation method was effective in reducing furfural and acidity.

It is a figure which shows the batch distillation apparatus which shows the principle of this invention. It is a figure which shows the bubbling type | mold batch distillation apparatus which shows embodiment of this invention. It is a figure which shows the non-bubbling type | mold batch distillation apparatus which shows embodiment of this invention. It is a figure which shows the distillation apparatus which arrange | positioned the shelf which shows embodiment of this invention. It is a figure which shows the conventional single distillation apparatus for full scale shochu manufacture. It is a figure which shows the density | concentration of the alcohol of the preparation part (A1) liquid in Example 1, and the distillate collected by division | segmentation. It is a figure which shows the ultraviolet part absorption (275 nm) of the distillate collected by division in Example 1. It is a figure which shows the acidity of the distillate collected by division | segmentation in Example 1. FIG. It is a figure which shows the alcohol density | concentration of the distillate collected in Example 2 by division | segmentation. It is a figure which shows the ultraviolet part absorption (275 nm) of the distillate collected by division in Example 2. It is a figure which shows the acidity of the distillate collected by division | segmentation in Example 2. FIG. It is a figure which shows the aspect of a steam introduction mechanism. It is a figure which shows an example of the bubbling type | mold batch distillation apparatus which shows embodiment of this invention. It is a figure which shows an example of the bubbling type | mold batch distillation apparatus which shows embodiment of this invention.

Explanation of symbols

A: Distillation part,
A1 ... Preparation section,
A2 ... Condensate reservoir,
A3 ... shelf step ,
B ... Cooling unit,
C: Communication part
3 ... Feeding liquid,
5 ... Condensate,
6 ... steam passage,
7: Lid (bell type),
8: Lid (shallow type),
9 ... float,
10 ... cooling pipe,
11, 13 ... heating device,
14 ... Sub-heating device 12 ... Steam injector,
15 ... reflux outlet,
16 ...
17 ... Tube for introducing outside air,
19, 20, 25 ... valve,
21 ... Distillate tank,
49, 50, 51 ... shelf,
52, 53, 54 ... Downcomer,
60, 63 ... Valve-type lid,
61 ... spring,
100: distillation apparatus.

Claims (9)

A distillation apparatus having a distillation section and a cooling section for cooling the steam generated in the distillation section,
The distillation unit is composed of a charging liquid charging unit formed by partitioning the inside of the distillation unit with a partition, and a condensate storage unit that is a part other than the charging unit and communicates with the cooling unit,
At the upper end of the charging part, a communication part for introducing steam generated by heating the charging liquid into the condensate storage part is formed,
The condensate storage unit stores a condensate formed by the vapor being introduced and condensed,
And an upper end portion of the communicating portion, characterized in that steam and / or condensate to not flow back into the charging unit backflow prevention mechanism of the condensate in the reservoir is disposed, the distillation apparatus. The distillation apparatus according to claim 1, wherein the backflow prevention mechanism is a backflow prevention valve or a bell-shaped lid portion placed on an upper end portion of the communication portion .   The distillation apparatus according to claim 1 or 2, wherein the distillation section is provided with a steam introduction mechanism for introducing the steam generated in the charging section into the condensate storage section.   The charging unit is provided with a heating device for heating the charged liquid, the condensate storage unit is provided with a heating device for heating the condensate, and the steam distilled from the distillation unit is supplied to the cooling unit. The distillation apparatus according to any one of claims 1 to 3, further comprising a reflux device configured to recirculate a part or all of the condensate produced by introducing into the condensate reservoir.   The distillation apparatus according to any one of claims 1 to 4, wherein the condensate storage unit is provided with a shelf or a packing having a rectifying function. A distillation method using the distillation apparatus according to claim 1,
Introducing the steam generated by heating the charging liquid of the charging unit into the condensate storage unit via the backflow prevention mechanism;
Steam of the condensate storage part is introduced into the cooling part, and part or all of the condensate generated by cooling the cooling part is returned to the condensate storage part, and the remainder of the condensate is distilled off. Obtaining as a liquid;
Heating the condensate of the steam generated and stored in the condensate storage part, and introducing the generated steam into the cooling part to obtain a distillate.   The said charging liquid is a distillation method of Claim 6 which is 67% or less of the said charging part capacity | capacitance.   The distillation method according to claim 6 or 7, wherein the heating of the charging liquid in the charging unit is performed by introducing steam by a steam introduction mechanism arranged at a lower part of the charging unit.   The charging liquid in the charging section is heated, and the heating of the charging section is stopped when the alcohol concentration of the steam in the charging section generated by the heating or the alcohol concentration of the charging liquid is equal to or lower than a predetermined value. The distillation method according to any one of claims 6 to 8, wherein the condensate in a liquid storage part is heated, and the generated steam is introduced into the cooling part to obtain a distillate.

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