JP5531262B2 - Freeze concentrator - Google Patents

Description

The present invention also relates apples, citrus, pomelos, juice or the like ginger, bonito soup, alcohols such as bio-ethanol, the freeze concentration equipment for freeze concentration of unconcentrated liquid such as milk.

  Conventionally, methods for concentrating a non-concentrated liquid are roughly classified into an evaporation concentration method and a freeze concentration method. The evaporative concentration method is a method in which the non-concentrated liquid is concentrated by heating and boiling the non-concentrated liquid and evaporating the water in the non-concentrated liquid. The non-concentrated liquid contains a substance that is easily denatured by heating such as protein. If there is, there is a risk of losing the flavor. On the other hand, the freeze concentration method is capable of high-quality concentration of foods, pharmaceuticals, and the like, and is preferable as a method for concentration of thermally unstable substances.

  Examples of the freeze concentration apparatus used in the freeze concentration method include an ice making machine, a vertically-bottomed cylindrical draining tower, and a transfer pipe connected from the ice making machine to the lower part of the draining tower. The thing is known (refer patent document 1). In the freeze concentration apparatus of Patent Document 1, ice slurry made of ice particles and concentrated liquid produced by an ice making machine is transferred to the lower part of the draining tower through a transfer pipe.

  The ice slurry transferred to the lower part of the draining tower is transported upward with the ice particles having a specific gravity lighter than that of the concentrate, and the concentrated liquid having a higher specific gravity than the ice particles stays at the lower part of the draining tower. Separated into liquid. The separated concentrated liquid is collected through a pipe piece provided in the draining tower.

  However, in the freeze concentration apparatus of Patent Document 1, if an attempt is made to increase the concentration rate by increasing the proportion of ice particles produced by the ice maker, an excessive load is applied to the ice maker or pump due to the increased ice particles. The transfer pipe will be blocked. For this reason, in the freeze concentration apparatus of Patent Document 1, it is difficult to increase the concentration rate. In particular, in the case of an ice making machine that scrapes off ice particles generated on the inner surface with a scraping blade, if the ice filling rate in the ice making machine is 30% or more, an excessive load is applied to the scraping blade due to the increased ice particles. Therefore, there is a problem that the ice filling rate in the ice making machine cannot be increased to 30% or more and the concentration rate is lowered. In order to concentrate the non-concentrated liquid three times or more, the ice filling rate in the ice making machine needs to be 67% or more.

  Then, what was described in patent document 2 as a freeze concentration apparatus which can raise a concentration rate is known. The freeze concentration apparatus of Patent Document 2 includes a first ice maker and a second ice maker, transfers ice slurry produced by the first ice maker to the second ice maker, and transfers the transferred ice slurry to the second ice maker. The concentration rate is increased by further increasing the proportion of ice particles in the ice slurry with an ice making machine. The concentrated liquid concentrated by the second ice maker is separated from the ice particles and collected by passing through a large number of holes in the inner tank. However, the freeze concentration apparatus of Patent Document 2 can increase the concentration rate without applying an excessive load to the ice making machine or the pump or blocking the piping, but two ice making machines are required. There is a problem that the apparatus becomes complicated and large, and manufacturing costs and running costs are increased.

JP-A-48-77054 Japanese Patent Laid-Open No. 2000-093131

An object of the present invention can be miniaturized with a simple structure, yet to provide a freeze concentration equipment that can increase the no concentration rate by changing the components.

The invention according to claim 1 is made to solve the above-described problems of the prior art, and includes a supply pipe for supplying a non-concentrated liquid and a discharge pipe for discharging the generated concentrated liquid. An outer tube having a space serving as a refrigerant flow path between the inner tube provided and the outer peripheral surface of the inner tube and covering the outer peripheral surface of the inner tube; and a rotating member rotatably disposed inside the inner tube An ice maker that projects radially from the outer peripheral surface of the rotating member and scrapes off the ice particles that are generated on the inner surface of the inner tube. The inner pipe is closed at the bottom, and an opening is formed at the top. Ice particles generated in the inner pipe rise in the inner pipe due to the difference in specific gravity and are discharged from the opening. The concentrated liquid concentrated in the pipe descends in the inner pipe due to the difference in specific gravity, thereby the ice particles. Separated so as to be discharged from the discharge pipe, by connecting a cylindrical ice storage tank to the upper end of the inner tube of the icemaker, the ice particles between the inner tube and the ice storage tank is movable An ice channel is formed above the ice making machine in the ice storage tank, and is provided on a cylindrical portion that rotates about the same axis as the central axis of the ice storage tank, and on the outer peripheral surface of the cylindrical portion. An auger provided with an outer screw extending in the axial direction while being wound in a direction opposite to the rotation direction of the cylindrical portion is provided, and the auger is provided on the inner peripheral surface of the cylindrical portion in a direction opposite to the winding direction of the outer screw. The present invention relates to a freeze concentrating device provided with an inner screw extending in the axial direction while being wound .

According to a second aspect of the present invention, the ice particles discharged from the opening are transferred to a centrifugal separator, and the centrifugal action of the centrifugal separator is exerted on the ice particles, thereby concentrating the ice particles attached to the ice particles. 2. The freeze concentration apparatus according to claim 1, wherein a liquid is separated from the ice particles.

In the present invention, a non-concentrated liquid consisting of an aqueous solution having a low concentration of 0.5 wt% to 13 wt% is cooled, and a predetermined amount of fresh water is frozen from the aqueous solution into ice particles, and the ice particles are removed. A freeze concentration method that can increase the concentration of the non-concentrated liquid by about 3 times or more is used.

  According to the first aspect of the invention, by adopting the above-described configuration, the generated ice particles rise in the inner tube due to the difference in specific gravity, so that the discharge of the ice particles from the opening is promoted. The load due to the ice particles produced in is less likely to be applied to the scraping part. For this reason, even if the ratio of the ice particles produced by the ice making machine is increased, the load applied to the scraping part of the ice making machine is unlikely to be excessive, and the concentration rate can be stably increased. Moreover, since the non-concentrated liquid is not heated, the concentration rate can be increased without changing the components contained in the non-concentrated liquid. Further, the concentrated liquid concentrated in the inner pipe descends in the inner pipe due to the difference in specific gravity, and is separated from the ice particles and discharged from the discharge pipe. Therefore, the discharge pipe is not blocked by the ice particles. Furthermore, since it is not necessary to provide two ice makers in order to increase the concentration rate as in the prior art, the size can be reduced with a simple structure, and the manufacturing cost and running cost can be reduced.

According to the first aspect of the present invention, an ice flow path in which a cylindrical ice storage tank is connected to the upper end of the inner pipe of the ice making machine so that the ice particles can move between the ice storage tank and the inner pipe. By forming the ice particles, since the ice particles are transferred to the ice storage tank, the ice particles can be easily collected.

According to the first aspect of the present invention, the cylindrical portion that rotates about the same axis as the central axis of the ice storage tank and the outer peripheral surface of the cylindrical portion are provided above the ice making machine in the ice storage tank. By providing an auger provided with an outer screw that extends in the axial direction while being wound in a direction opposite to the rotation direction of the cylindrical portion, ice particles in the inner tube are pushed up into the ice storage tank by the feeding action of the outer screw. Therefore, the discharge of ice particles is further promoted. For this reason, the load on the scraping part due to ice particles is less likely to be applied, so that the concentration rate can be further increased.

According to the first aspect of the present invention, the auger is provided on the inner peripheral surface of the tubular portion with the inner screw extending in the axial direction while being wound in the direction opposite to the winding direction of the outer screw. The concentrated liquid adhering to the ice particles can be returned to the ice making machine while preventing the ice particles pushed up by the inner screw from returning to the inner pipe of the ice making machine by the inner screw, so that the concentration rate can be further increased.

According to the second aspect of the present invention, the ice particles discharged from the opening are transferred to a centrifuge, and the centrifugal action of the centrifuge is applied to the ice particles, thereby adhering to the ice particles. When the concentrated liquid is separated from the ice particles, the concentrated liquid is prevented from being discharged in a state of adhering to the ice particles, so that the recovery rate of the concentrated liquid can be increased.

Oite the present invention, the non-concentrated solution of a low concentration aqueous solution of 0.5 wt% to 13 wt% was cooled and frozen to a predetermined amount of fresh water from the aqueous solution into the ice particles, remove the ice particles As a result, the concentration of the non-concentrated liquid can be increased by about 3 times or more, so that a concentrated liquid with a high concentration that has not existed before can be obtained without changing the components.

It is the schematic which shows the freeze concentration apparatus which concerns on this invention. FIG. 2 is a partially enlarged longitudinal sectional view of an ice making machine and an ice storage tank of the freeze concentration apparatus of FIG. 1. It is an expanded longitudinal cross-sectional view which shows the auger of the freeze concentration apparatus which concerns on this invention. It is a front view which shows the auger of the freeze concentration apparatus which concerns on this invention. It is a front view which shows the outer side screw of the auger of the freeze concentration apparatus which concerns on this invention. It is a front view which shows the inner side screw of the auger of the freeze concentration apparatus which concerns on this invention. It is the schematic which shows the modification of the freeze concentration apparatus which concerns on this invention.

  Hereinafter, a preferred embodiment of a freeze concentration apparatus according to the present invention will be described with reference to the drawings. However, the present invention is not limited to the following embodiments.

  As shown in FIG. 1, the freeze concentration apparatus (1) of the first embodiment of the present invention includes a storage tank (2) in which a non-concentrated liquid (a) is stored, and ice particles (from the non-concentrated liquid (a) ( an ice making machine (3) for producing an ice slurry comprising b) and a concentrated liquid (c), an ice storage tank (4) to which ice particles (b) discharged from the ice making machine (3) are transferred, and an ice storage tank ( 4) A centrifuge (5) to which the ice particles (b) are transferred, and a re-storage tank (6) for storing the concentrated liquid (c) separated from the ice particles (b) by the centrifuge (5) And a concentrated liquid recovery tank (7) for recovering the concentrated liquid (c) concentrated in the ice making machine (3), and an ice recovery tank (8) provided below the centrifugal separator (5). The freeze concentrator (1) is operated in a state where it is placed in a cold box (not shown) set to 10 ° C. or lower as a whole. Note that the freeze concentration device (1) can include only the ice maker (3), the ice storage tank (4), and the centrifuge (5) in the cool box, but at least the centrifuge (5) is in the cool box. It is enough if it is included.

  The non-concentrated liquid (a) is not particularly limited as long as it is a liquid containing water, such as an aqueous solution. For example, juice such as apples, eggplant, Buddha, ginger, etc., bonito soup, alcohol such as bioethanol Milk, etc. can be mentioned, Among these, those having a low concentration of 0.5 to 13% by weight such as jujutsu, ginger, bonito soup and bioethanol are particularly preferred. When the concentration of the non-concentrated liquid (a) exceeds 13% by weight, when the non-concentrated liquid (a) is concentrated, the ice slurry produced by the ice making machine (3) becomes a gel and ice particles (b) Can no longer be separated from the concentrated liquid (c), and when the concentration of the non-concentrated liquid (a) is less than 0.5% by weight, the non-concentrated liquid (a) is cooled by the ice making machine (3). The produced ice particles (b) are condensed and the non-concentrated liquid (a) does not become an ice slurry, which is not preferable in any case. The aqueous solution includes a colloidal solution in which the dispersion medium is water.

  As shown in FIGS. 1 and 2, the ice making machine (3) has a space serving as a refrigerant flow path (10) between the inner pipe (9) and the outer peripheral surface of the inner pipe (9). An outer tube (11) covering the outer peripheral surface of (9), a rotating member (12) rotatably disposed inside the inner tube (9), and a radial projection from the outer peripheral surface of the rotating member (12) And a scraping part (13) for performing. The ice making machine (3) is supported such that the central axis of the inner pipe (9) is vertically oriented, the lower end of the inner pipe (9) is closed by the lid member (14a), and the inner pipe (9 ) Is provided with a lid member (14b). The lid member (14b) is formed with an opening (15) penetrating in the vertical direction at a position offset radially outward from the center thereof. The longitudinal direction of the central axis of the inner tube (9) includes an oblique direction inclined from the vertical.

  The inner tube (9) is a cylindrical body and has a space for storing the non-concentrated liquid (a) and freezing it. A supply pipe (16) for supplying the non-concentrated liquid (a) is supplied to the lower left part of the inner pipe (9), and a concentrated liquid (c) is discharged to the lower right part of the inner pipe (9). The discharge pipes (17) are connected to each other. The position of the supply pipe (16) is not limited to the lower part of the inner pipe (9), but may be the upper part or the central part of the inner pipe (9). The position of the discharge pipe (17) is not limited to the lower part of the inner pipe (9) and may be the upper part or the central part of the inner pipe (9). Is preferred.

  The rotating member (12) is a rotating shaft disposed substantially coaxially with the central axis of the inner tube (9) inside the inner tube (9), and is arranged inside the lid member (14a) and inside the lid member (14b). Are supported by bearings (not shown) respectively attached to the. In the lateral direction of the ice making machine (3), a scraping blade electric motor (19) is disposed so that the motor shaft (18) is parallel to the rotation shaft of the rotating member (12). 18) is connected to the rotating shaft of the rotating member (12) via a gear (20). Thereby, a rotation member (12) rotates with rotation of a motor shaft (18).

  A refrigerant inlet (21) is provided near the lower left end of the refrigerant flow path (10), and a refrigerant outlet (22) is provided near the upper right end of the refrigerant channel (10). The refrigerant is supplied from the refrigerant inlet (21). Then, the process of passing through the refrigerant flow path (10) and being discharged from the refrigerant outlet (22) is repeated. Thus, the refrigerant circulates in the refrigerant flow path (10), whereby the non-concentrated liquid (a) inside the inner pipe (9) is cooled and ice particles (b) are generated on the inner surface of the inner pipe (9). Become.

  The lid member (14) can be formed of a metal material such as stainless steel or a synthetic resin.

  The scraping portion (13) is fixedly disposed on the outer peripheral surface of the rotating member (12) and protrudes in the radial direction of the rotating member (12). Further, a scraper (23) for scraping ice particles (b) generated on the inner surface of the inner tube (9) is provided at the radial tip of the scraping portion (13). The scraper (23) is a rectangular plate-like body and is formed so that both ends in the longitudinal direction thereof reach both ends of the inner tube (9).

  The ice storage tank (4) is formed in a cylindrical shape having the same diameter as the inner diameter of the inner pipe (9), and is connected to the upper end of the inner pipe (9) of the ice making machine (3) so that the central axis is vertically oriented. Has been. The vertical orientation of the central axis of the ice storage tank (4) includes an oblique direction inclined from the vertical as in the case of the inner pipe (9). Between the ice storage tank (4) and the inner pipe (9) of the ice making machine (3), an ice channel (24) in which ice particles (b) can move is formed. Examples of the connection means between the ice making machine (3) and the ice storage tank (4) include a fixing member such as a bolt. In addition, a pipe line (25) for transferring ice particles (b) in the ice storage tank (4) to the centrifuge (5) is provided at the upper part of the ice storage tank (4). The pipe line (25) is disposed so as to extend obliquely downward.

  An auger (26) is provided above the ice making machine (3) in the ice storage tank (4). As shown in FIG. 3, the auger (26) includes a cylindrical outer cylindrical portion (27) and a cylindrical inner cylindrical portion (28) whose outer diameter is smaller than the inner diameter of the outer cylindrical portion (27). And have. The outer cylindrical portion (27) is rotatably disposed about the same axis as the central axis of the ice storage tank (4). As shown in FIGS. 4 and 5, the outer cylindrical portion (27) is wound around the outer peripheral surface (27 a) in the direction opposite to the rotation direction of the outer cylindrical portion (27) (see the arrows in FIGS. 1 and 2). However, an outer screw (29) extending in the axial direction is formed from the lower end (27b) to the upper end (27c). The outer screw (29) has an outer diameter side edge (29a) extending to the vicinity of the inner surface of the ice storage tank (4), and a minute amount between the outer diameter direction side edge (29a) and the inner surface of the ice storage tank (4). A gap is formed.

  The inner cylindrical portion (28) is disposed inside the outer cylindrical portion (27) and is rotatable about the same axis as the central axis of the ice storage tank (4). On the outer peripheral surface (28a) of the inner cylindrical portion (28), as shown in FIGS. 3 and 6, an inner screw extending in the axial direction while being wound in a circumferential direction opposite to the winding direction of the outer screw (29). (30) is formed from the lower end (28b) to the upper end (28c). The inner screw (30) is fixed in contact with the inner peripheral surface (27d) of the outer cylindrical portion (27) at its outer diameter side edge (29a) over the entire circumference. Thus, the inner screw (30) is provided on the inner peripheral surface (27d) of the outer cylindrical portion (27).

  The inner cylindrical portion (28) is fitted into a stirring shaft (31) disposed substantially coaxially with the central axis of the ice storage tank (4), and the upper end tap hole (32) and the lower end tap hole (33). ) Is fixed to the stirring shaft (31) by inserting and tightening screws. The stirring shaft (31) is supported by a bearing on the lid member (14b), and is coupled to the motor shaft (35) of the stirring electric motor (34) disposed on the ice storage tank (4) (36). ). Thereby, the auger (26) can rotate substantially coaxially with the central axis of the ice storage tank (4) by the power of the stirring electric motor (34).

  As shown in FIG. 1, the centrifuge (5) includes a motor (37), a rotating body part (39) connected to the motor shaft (38), and an outer side of the rotating body part (39) by centrifugal action. A tank part (40) for recovering the concentrated liquid (c) transferred to the surface, and an ice scraping blade (41) slidable between the inner wall surface (39a) of the rotating body part (39) and the motor shaft (38). And have. The ice scraping blade (41) is a rectangular plate-like body, and is formed so that both ends in the longitudinal direction thereof reach the upper end and the lower end of the rotating body (39), respectively.

  The freeze concentration apparatus (1) configured as described above operates as follows.

  First, the non-concentrated liquid (a) is transferred from the storage tank (2) through the supply pipe (16) into the inner pipe (9) of the ice making machine (3). The non-concentrated liquid (a) transferred into the inner pipe (9) is cooled while exchanging heat with the refrigerant flowing through the refrigerant flow path (10) while rising in the inner pipe (9), so that fresh water is It freezes to become an ice slurry consisting of ice particles (b) and concentrate (c). The ice particles (b) having a lighter specific gravity than the concentrated liquid (c) rise in the inner tube (9) due to the specific gravity difference, and the concentrated liquid (c) having a higher specific gravity than the ice particles (b) is caused by the specific gravity difference. The inside of the inner pipe (9) is lowered. As a result, the ice particles (b) and the concentrated liquid (c) are separated. At this time, the separated ice particles (b) are discharged from the opening (15) to the ice storage tank (4). On the other hand, the separated concentrated liquid (c) is cooled and further concentrated while exchanging heat with the refrigerant while being discharged from the discharge pipe (17), and then concentrated through the discharge pipe (17). ). At this time, since the concentrated liquid (c) is separated from the ice particles (b) and passes through the discharge pipe (17), the discharge pipe (17) is not blocked by the ice particles (b).

  The ice particles (b) discharged to the ice storage tank (4) are fed by the outer screw (29) of the auger (26) by rotating the auger (26) in the circumferential direction shown by the arrows in FIGS. By the action, it is pushed up above the auger (26) in the ice storage tank (4). As a result, the discharge of the ice particles (b) in the inner pipe (9) is promoted. The scraping part (13) of (3) is less likely to be loaded with ice particles (b). For this reason, a concentration rate can be raised by increasing the ratio of the ice particle (b) manufactured with an ice making machine (3).

  The ice particles (b) pushed up above the auger (26) are prevented from falling back into the inner pipe (9) of the ice making machine (3) by the upper surface (30a) of the inner screw (30). . On the other hand, the concentrate (c) adhering to the ice particles (b) moves along the upper surface (30a) of the inner screw (30) and returns into the inner pipe (9) of the ice making machine (3).

  When the ice particles (b) pushed up above the auger (26) reach the upper part of the ice storage tank (4), the ice particles (b) flow into the pipe (25), flow through the pipe (25) by gravity, and descend by a centrifugal separator ( 5) Enter. The ice particles (b) that have entered the centrifuge (5) are subjected to a centrifugal separation action in the rotating body (39), and the attached concentrated liquid (c) is separated. When the ice particles (b) in the rotating body (39) accumulate in the rotating body (39), the ice scraping blade (41) is moved from the inner wall surface (39a) of the rotating body (39) to the motor shaft (38). ) And dropped into an ice collection tank (8) below the centrifuge (5) to be collected.

  On the other hand, the concentrated liquid (c) separated by the centrifugal separation action is collected in the tank section (40) and then stored in the re-storage tank (6) through the pipe line (42). The concentrated liquid (c) stored in the re-storage tank (6) is transferred to the storage tank (2) and stored again in the storage tank (2), and then transferred to the ice making machine (3) for re-concentration. The By this cycle, the concentrated liquid (c) adhering to the ice particles (b) discharged from the opening (15) of the ice making machine (3) is returned again into the inner pipe (9) of the ice making machine (3). Therefore, the recovery rate and concentration rate of the concentrated liquid (c) can be improved.

Next, the freeze concentration apparatus (51) of 2nd Embodiment of this invention is demonstrated.
The freeze concentration apparatus (51) of the second embodiment is obtained by omitting the ice storage tank (4) and the re-storage tank (6) of the freeze concentration apparatus of the first embodiment, than the freeze concentration apparatus of the first embodiment. Is also simplified. In addition, the part corresponding to the freeze concentration apparatus (1) of 1st Embodiment attaches | subjects the code | symbol same as 1st Embodiment, and abbreviate | omits the description.

  As shown in FIG. 7, the freeze concentration apparatus (51) includes a storage tank (2), an ice maker (3), a centrifuge (5), a concentrate recovery tank (7), an ice recovery tank ( 8). This freeze concentrator (51) is operated in a state where it is placed in a cold box (not shown) set to 10 ° C. or lower as in the first embodiment. In addition, the freeze concentrator (51) can put only the ice maker (3) and the centrifuge (5) in the cold box, but at least if the centrifuge (5) is in the cold box. Good. Reference numeral 52 is a concentration measuring device such as a BRIX meter, and reference numerals 53 and 54 are electromagnetic valves.

  In the freeze concentrating device (51) thus configured, the non-concentrated liquid (a) is transferred from the storage tank (2) through the supply pipe (16) into the inner pipe (9) of the ice making machine (3). The The non-concentrated liquid (a) transferred into the inner pipe (9) is cooled while exchanging heat with the refrigerant flowing through the refrigerant flow path (10) while rising in the inner pipe (9), so that fresh water is It freezes to become an ice slurry consisting of ice particles (b) and concentrate (c). The ice particles (b) having a lighter specific gravity than the concentrated liquid (c) rise in the inner tube (9) due to the difference in specific gravity, thereby promoting discharge from the opening (15). Thereby, the ice particles (b) in the inner tube (9) are removed. On the other hand, the concentrated liquid (c) having a higher specific gravity than the ice particles (b) descends in the inner pipe (9) due to the specific gravity difference, is separated from the ice particles (b), and is discharged from the discharge pipe (17). The refrigerant is further cooled and concentrated while exchanging heat with the refrigerant, and then collected through the discharge pipe (17) into the concentrate collection tank (7).

  The ice particles (b) discharged from the opening (15) are transferred manually to the centrifuge (5). The ice particles (b) that have entered the centrifuge (5) are subjected to a centrifugal separation action in the rotating body (39), and the attached concentrated liquid (c) is separated. When the ice particles (b) in the rotating body (39) accumulate in the rotating body (39), the ice scraping blade (41) is moved from the inner wall surface (39a) of the rotating body (39) to the motor shaft (38). ) And dropped into an ice collection tank (8) below the centrifuge (5) to be collected.

  The concentrated liquid (c) separated by the centrifugal separation action is recovered in the tank section (40), and when the concentration reaches the target value, it passes through the electromagnetic valve (53) to the concentrated liquid recovery tank (7). Collected. When the concentration of the concentrate (c) does not reach the target value, the solenoid valve (53, 54) is switched to transfer the concentrate (c) into the inner pipe (9) of the ice making machine (3). The concentration step of cooling again can be repeated.

  Hereinafter, the effect of the present invention will be made clearer by showing examples relating to the freeze concentration apparatus (1, 51) according to the present invention. However, the present invention is not limited to the following examples.

  Bundan juice obtained from Okabayashi Farm Co., Ltd. (Ochi-cho, Takaoka-gun, Kochi Prefecture) was concentrated with the freeze concentration apparatus (1). The concentrated Bundan squeezed juice is concentrated for a predetermined time by the freeze concentration device (1), and the concentrated liquid (c) is taken out from the inner tube (9) of the ice making machine (3). Samples of Examples 1 to 5 were used. The density | concentration of the sample of these Examples 1-5 was calculated | required with the density | concentration analysis method shown below. Moreover, the Bundan squeezed juice before concentration used in the examples was used as a comparative example, and the concentration was also determined by the concentration analysis method shown below. Analyzed items are organic acids (malic acid, citric acid), free sugars (fructose, glucose, sucrose), ascorbic acid, flavanones (naringin, hesperidin), limonoids (limonin), which are the main components of Bundan Juice An amino acid. The concentration of the main component in the Bundan squeezes of Examples 1 to 5 and the comparative example was indicated by the Brix value, which is the concentration by weight of the solid content dissolved in the solution. The results are shown in Tables 1 and 2. In addition, you may show a density | concentration by the weight% density | concentration of the solute dissolved in the solution which is a concept wider than a Brix value. Hereinafter, the concentration analysis method will be described in detail for each component.

(1) Organic acid analysis Bundan juice (sample) filtered through filter paper was diluted 10-fold with ultrapure water (MQ water), passed through a 0.45 μm filter, and then injected into a post-column HPLC apparatus. . The concentration of the organic acid in the sample was calculated by using the peak area value of the chromatogram obtained with the standard organic acid reagent and the value obtained with the sample. HPLC conditions are as follows: Column Shodex Rspak KC-LG + KC-811 (φ8.0 × 300 mm), column temperature 50 ° C., mobile phase 1.0 mM HClO ₄ , mobile phase flow rate 1.0 mL / min, reaction reagent 1/10 ST3-R The reaction reagent flow rate is 0.5 mL / min, the detection wavelength is 430 nm, and the injection volume is 10 μL.

(2) Free sugar analysis Bundan juice (sample) filtered through filter paper was diluted 10-fold with ultrapure water (MQ water), passed through a 0.45 μm filter, and then HPLC apparatus (Delta 600 system manufactured by Waters) Injected into. The concentration of free sugar in the sample was calculated by using the peak area value of the chromatogram obtained with the standard saccharide reagent and the value obtained with the sample. HPLC conditions are a column Shodex Asahipak NH2P-50 4E (φ4.6 × 250 mm), a column temperature of 30 ° C., a mobile phase of 75% acetonitrile, a mobile phase flow rate of 1.0 mL / min, a detector RI, and an injection volume of 10 μL.

(3) Ascorbic acid analysis Bundan squeezed juice (sample) filtered through filter paper was treated with the homocysteine reduction method, passed through a 0.2 μm filter, and then injected into an HPLC apparatus (X-LC system manufactured by JASCO Corporation). did. The total ascorbic acid concentration in the sample was calculated by using the peak area value of the chromatogram obtained with the standard ascorbic acid reagent and the value obtained with the sample. HPLC conditions were as follows: column Phenomenex LUNA NH ₂ (φ3.0 × 50 mm, 3 μm), column temperature 40 ° C., mobile phase 50 mmol / L triethanolamine-phosphate buffer (pH 2.2) / acetonitrile = 15/85 ( v / v), mobile phase flow rate 0.8 mL / min, detection wavelength 240 nm, injection volume 1.0 μL.

(4) Flavanone Analysis Bundan Juice (sample) filtered with filter paper is diluted with 60% acetonitrile at an arbitrary ratio, passed through a 0.2 μm filter, and then HPLC apparatus (X-LC system manufactured by JASCO Corporation) Injected into. Using the peak area value of the chromatogram obtained with the standard reagent and the value obtained with the sample, the concentrations of naringin and hesperidin in the sample were calculated. HPLC conditions were: column COSMOSIL 2.5C ₁₈ -MS-II (φ3.0 × 75 mm, 2.5 μm), column temperature 35 ° C., mobile phase A 10 mmol / L ammonium formate buffer (pH 3.7) / acetonitrile = 9/1 ( v / v), mobile phase B 10 mmol / L ammonium formate buffer (pH 3.7) / acetonitrile = 2/8 (v / v), gradient condition 0% B (0 min) → 50% B (7.0 min) → 100% B (7.55 min) → 100% B (8.0 min), mobile phase flow rate 0.7 mL / min, detection wavelength 285 nm, injection volume 1.0 μL.

(5) Limonoid analysis Bundan juice (sample) filtered through filter paper was applied to a solid-phase extraction cartridge (Excelpak SPE-ENV / 124, 8 mL, 250 mg manufactured by Agilent), washed with 60% methanol, and eluted with 90% methanol. did. The eluate was passed through a 0.2 μm filter and then injected into an HPLC apparatus (X-LC system manufactured by JASCO Corporation). The limonin concentration in the sample was calculated by using the peak area value of the chromatogram obtained with the standard reagent and the value obtained with the sample. HPLC conditions: Column Zorbax Eclipse Plus C18 Rapid Resolution HT 600Bar (φ3.0 × 50mm, 1.8μm), column temperature 30 ° C, mobile phase 60% acetonitrile, mobile phase flow rate 0.4mL / min, detection wavelength 210nm, injection volume 1.0μL It is.

(6) Amino acid analysis Bundan juice (sample) filtered through filter paper was diluted 50-fold with ultrapure water (MQ water) and passed through a 0.2 μm filter. The filtered sample was labeled with a Waters AccQ • Tag Ultra derivatization reagent kit and then injected into an HPLC apparatus (Waters UPLC system). The amino acid concentration in the sample was calculated by using the peak area value of the chromatogram obtained with the standard amino acid and the value obtained with the sample. HPLC conditions are: Column AccQ • Tag ^™ Ultra column (φ2.1 × 100 mm, 1.7 μm), column temperature 60 ° C., mobile phase AccQ • Tag Ultra dedicated solvents A and B, mobile phase flow rate 0.7 mL / min, measurement wavelength 260 nm The injection volume is 1.0 μL.

  As a result of concentrating the Bundan juice in the freeze concentration apparatus (1), as shown in Tables 1 and 2, the Brix value of the Bundan juice was 13.2 (Example 1), 19.0 (Example 2), It became 23.2 (Example 3), 34.9 (Example 4), and 38.7 (Example 5). From this, it can be seen that Bundan Juice was concentrated about 1.2 times to about 3.5 times before the concentration.

  In addition, as shown in Tables 1 and 2, each component in Bunju Juice increases in concentration at almost the same rate as the increase rate of Brix value, so in the range of Brix value, precipitation and It turns out that the component change has not arisen. Therefore, the freeze concentration apparatus (1) does not impair the flavor even if the Bundan juice is concentrated about 3.5 times from the undiluted juice.

  Next, by using the freeze concentration device (1) of the first embodiment and the freeze concentration device (51) of the second embodiment, respectively, the same bundan juice is concentrated, depending on the presence or absence of the auger (26). The change in Brix value of Judan Juice was examined. The Brix value was calculated by the following method. The proportion of ice particles (b) produced by the ice making machine (3) is increased, and the load applied to the scraping part (13) of the ice making machine (3) by the increased ice particles (b) becomes a certain level or more. Then, the operation was stopped, and the concentrated liquid (c) in the inner tube (9) at this time was collected, and the Brix value was calculated by the same concentration analysis method as described above. The calculation of the Brix value is performed when the auger (26) is provided (when the freeze concentration apparatus (1) of the first embodiment is used) and when the auger (26) is not provided (the freeze concentration apparatus (51) of the second embodiment). In the case of use). The results are shown in Table 3. The operation was stopped by operating a thermostat that prevents the motor (19) from seizing when the load applied to the scraper (13) exceeds a certain level.

  As shown in Table 3, it is confirmed that the Brix value increased about 1.13 times in the case with the auger (26) than in the case without the auger (26). Therefore, when the auger (26) is arranged above the ice making machine (3), it can be seen that the concentration of jujuda juice can be further increased. Moreover, it is confirmed that the bunju squeezed juice is about 3.7 times concentrated when there is an auger (26). Therefore, it can be seen that Buntan's squeezed juice can be stably concentrated three times or more without increasing the load on the scraping part (13) of the ice making machine (3). Note that the Brix value is concentrated about 3.3 times even without the auger (26).

  Next, in order to examine the recovery rate of the concentrated liquid (c) concentrated by the ice making machine (3), the following experiment was performed using the freeze concentration apparatus (1). First, the ice particles (b) discharged from the upper end of the inner pipe (9) of the ice making machine (3) are transferred to the centrifuge (5), and the concentrate (c) adhering to the ice particles (b). And ice particles (b) were separated by centrifugation. Next, the Brix value when the separated ice particles (b) are melted is calculated by the same concentration analysis method as described above, and this Brix value is compared with the Brix value of Bundan Juice before the concentration test. The recovery rate was calculated. This operation was performed 7 times. The results are shown in Table 4.

  As shown in Table 4, the ice particles (b) discharged from the upper end of the inner pipe (9) of the ice making machine (3) and the concentrated liquid (c) adhering to the ice particles (b) are centrifuged. It was confirmed that the recovery rate of the concentrated liquid (c) can be 90% or more by separating with the machine (5).

  In the above embodiment, the bunjou juice was concentrated as the non-concentrated liquid (a) by the freeze concentration apparatus (1), but as the non-concentrated liquid (a), juices such as apples, eggplants, ginger, etc. Alcohols such as bioethanol, milk and the like can also be concentrated by the freeze concentration apparatus (1, 51) by the same method as described above. In this case, in any case, it can be concentrated to 3 to 3.5 times the weight% concentration of the non-concentrated liquid (a).

  When bioethanol is used as the non-concentrated liquid (a), the freeze concentration apparatus (1, 51) can drastically reduce the energy required for distillation when used in the pre-process of the bioethanol distillation process. It is preferable because it is possible.

3 ice making machine 4 ice storage tank 5 centrifuge 9 inner pipe 10 refrigerant flow path 11 outer pipe 12 rotating member 13 scraping part 15 opening 16 supply pipe 17 discharge pipe 24 ice flow path 26 auger 27 cylindrical part 27a outer peripheral surface 27d inside Peripheral surface 29 Outer screw 30 Inner screw a Non-concentrated liquid b Ice particle c Concentrated liquid

Claims (2)

An internal pipe having a supply pipe for supplying the non-concentrated liquid and a discharge pipe for discharging the produced concentrated liquid and an outer peripheral surface of the inner pipe having a space serving as a refrigerant flow path An outer tube that covers the outer peripheral surface of the tube, a rotating member that is rotatably disposed inside the inner tube, and scrapes ice particles that protrude radially from the outer peripheral surface of the rotating member and that are generated on the inner surface of the inner tube. Having an ice making machine with a scraping part for removing,
The ice making machine is supported so that the inner pipe is oriented vertically, the lower part of the inner pipe is closed, an opening is formed in the upper part, and the ice particles generated in the inner pipe rise in the inner pipe due to the difference in specific gravity. The concentrated liquid discharged from the opening and concentrated in the inner pipe descends in the inner pipe due to the difference in specific gravity so as to be separated from the ice particles and discharged from the discharge pipe ,
A cylindrical ice storage tank is connected to the upper end of the inner pipe of the ice making machine to form an ice channel through which the ice particles can move between the ice storage tank and the inner pipe.
Above the ice making machine in the ice storage tank, a cylindrical portion that rotates about the same axis as the central axis of the ice storage tank, provided on the outer peripheral surface of the cylindrical portion, and the rotation direction of the cylindrical portion Provides an auger with an outer screw extending in the axial direction while winding in the opposite direction,
The auger is provided with an inner screw that extends in the axial direction while being wound in the direction opposite to the winding direction of the outer screw on the inner peripheral surface of the cylindrical portion.
The freeze concentration apparatus characterized by the above-mentioned. The ice particles discharged from the opening are transferred to a centrifuge, and the concentrated solution adhering to the ice particles is separated from the ice particles by exerting the centrifugal action of the centrifuge on the ice particles. The freeze concentrating apparatus according to claim 1, which is configured as described above.

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