WO2023203974A1 - 粉粒体の乾燥方法、乾燥装置及び製造方法 - Google Patents
粉粒体の乾燥方法、乾燥装置及び製造方法 Download PDFInfo
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Images
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B17/00—Machines or apparatus for drying materials in loose, plastic, or fluidised form, e.g. granules, staple fibres, with progressive movement
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B17/00—Machines or apparatus for drying materials in loose, plastic, or fluidised form, e.g. granules, staple fibres, with progressive movement
- F26B17/18—Machines or apparatus for drying materials in loose, plastic, or fluidised form, e.g. granules, staple fibres, with progressive movement with movement performed by rotating helical blades or other rotary conveyors which may be heated moving materials in stationary chambers, e.g. troughs
- F26B17/20—Machines or apparatus for drying materials in loose, plastic, or fluidised form, e.g. granules, staple fibres, with progressive movement with movement performed by rotating helical blades or other rotary conveyors which may be heated moving materials in stationary chambers, e.g. troughs the axis of rotation being horizontal or slightly inclined
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/06—Controlling, e.g. regulating, parameters of gas supply
- F26B21/10—Temperature; Pressure
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B3/00—Drying solid materials or objects by processes involving the application of heat
- F26B3/18—Drying solid materials or objects by processes involving the application of heat by conduction, i.e. the heat is conveyed from the heat source, e.g. gas flame, to the materials or objects to be dried by direct contact
- F26B3/22—Drying solid materials or objects by processes involving the application of heat by conduction, i.e. the heat is conveyed from the heat source, e.g. gas flame, to the materials or objects to be dried by direct contact the heat source and the materials or objects to be dried being in relative motion, e.g. of vibration
- F26B3/24—Drying solid materials or objects by processes involving the application of heat by conduction, i.e. the heat is conveyed from the heat source, e.g. gas flame, to the materials or objects to be dried by direct contact the heat source and the materials or objects to be dried being in relative motion, e.g. of vibration the movement being rotation
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
Definitions
- the present invention relates to a method and apparatus for drying powder and granular material, and in particular, to a method and apparatus for drying powder and granular material that perform continuous processing under reduced pressure, and more particularly to a method for producing powder and granular material with a specific degree of dryness. It is.
- the drying operation can be roughly classified by the heat transfer method and the method of contact with the object to be treated, and there are various methods depending on the combination of these methods and the method of transporting the object to be treated.
- Heat transfer methods include direct heating, indirect heating, and heating by electromagnetic waves.
- Methods for contacting the object to be treated include a stationary type, an airflow type, a stirring type, a fluidized bed type, etc.
- solvents residual moisture in the processing target and general liquids used as solvents and dispersion media in the manufacturing process, hereinafter simply referred to as "solvents").
- solvents solvents
- Efforts are being made to add heat energy.
- various studies are being conducted, such as reducing the pressure to lower the boiling point of the solvent.
- drying operation since the drying operation is located in the final step in manufacturing materials for industrial products, it has a great impact on the quality of the product. Therefore, it is not enough to simply pursue drying efficiency; for example, it is also required to reduce the content of volatile components such as volatile organic compounds (hereinafter referred to as "VOC") as much as possible. Meeting these strict requirements will contribute to increasing the commercial value of industrial products produced from treated powder.
- VOC volatile organic compounds
- drying systems have been studied in order to improve drying efficiency and increase the commercial value of processed materials.
- a drying system used for materials for industrial products is a fluidized bed drying system.
- a fluidized bed drying system blows hot air up from a dispersion plate such as a perforated plate to fluidize the granular raw material, thereby ensuring efficient contact with the hot air and movement of evaporated matter, thereby eliminating VOCs, etc. It also becomes easy to remove volatile components. It also has the advantage that there are no moving parts in the device body, making maintenance easy. Furthermore, in a fluidized bed drying system, for example, the equipment is divided into multiple drying chambers, and the treated powder is supplied in a fixed amount to the first drying chamber, and then transferred to the next drying chamber through the gap under the partition plate, and then It is possible to continuously process a large amount of treated powder by a method such as overflowing and discharging from a drying chamber.
- problems with fluidized bed drying systems include that the equipment becomes larger and that a large amount of exhaust gas is generated.
- the drying system A regenerative combustion type deodorizing device (hereinafter referred to as "RTO") capable of removing VOCs is introduced in the exhaust process of
- RTO regenerative combustion type deodorizing device
- Drying at high temperatures is not suitable for drying substances with a low thermal decomposition point, low softening temperature, or low melting point.
- Another example of a drying system used to dry such treated powder is a reduced pressure drying system that performs drying under vacuum or reduced pressure.
- the vacuum drying system can evaporate and dry the solvent in the treated powder without raising the temperature of the treated powder, and easily removes components that tend to remain, such as VOC. It has the advantage that it can be reduced to On the other hand, under reduced pressure, it is difficult to efficiently transfer a high amount of heat only by heating with hot air. Drying is in progress. Further, the vacuum drying system has the problem that it is difficult to continuously introduce and discharge treated powder, and therefore it is not suitable for large-scale processing.
- One of the most efficient heat transfer methods that can handle large quantities of heat is to use hot air, such as in a fluidized bed drying system, but applying reduced pressure to the fluidized bed drying system mentioned above means Fluidization and heat transfer are incompatible with a vacuum or reduced pressure environment.
- fluidized bed drying systems have high drying efficiency, are capable of continuous processing of large quantities of processed materials, and can obtain high-quality processed materials with volatile components such as VOCs removed.
- the problem is that they are large and have a large environmental impact.
- vacuum drying systems are an effective means for processing materials that are not suitable for drying at high temperatures, and are also suitable for removing volatile components such as VOCs, but they are difficult to perform continuous processing and are not suitable for large-scale processing. The problem is that it is unsuitable.
- Patent Document 1 granular material placed in a vacuum state in a preliminary vacuum chamber is continuously fed into a rotating drum rotating in the vacuum chamber, and the granular material is transported along a ribbon-shaped screw provided on the inner surface of the rotating drum.
- a method for continuous vacuum drying of granules is disclosed in which the granules are dried by moving the granules, and then the granules are taken out after returning to normal pressure in a vacuum release chamber.
- Patent Document 2 discloses a dryer main body portion in which a water-containing material is supplied into an interior under reduced pressure, and transports the water-containing material in a fixed direction while heating the dryer main body portion, and a dryer main body portion that transports the water-containing material in a fixed direction.
- a storage hopper section that is provided downstream along the line so that its interior communicates with the interior of the dryer main body section, and that has an opening/closing mechanism that can airtightly close and open an outlet for discharging the water-containing material;
- a water-containing material drying apparatus is disclosed.
- Patent Document 3 and Patent Document 4 are cited as drying systems that focus on fluidization of the processed material for the purpose of increasing heat transfer efficiency.
- Patent Document 3 discloses that the interior of a closed drying chamber having a heating jacket and stirring blades capable of fluidizing the material to be dried is maintained in a reduced pressure state, and the moisture content of the material to be dried is maintained within a range that can be fluidized.
- a method for drying high moisture content materials is disclosed that operates as follows. However, although Patent Document 3 explains that fluidization improves the heat transfer coefficient, ⁇ When drying by the method of the present invention, the properties of the material to be dried change during drying, We investigated the relationship between moisture and properties, especially when the material to be dried was strongly stirred in the drying chamber.The results showed that when the moisture content was approximately 40% or less, the material to be dried began to flow due to strong stirring.
- Patent Document 4 describes at least 3,9-bis(1,1-dimethyl-2-hydroxyethyl)-2,4,8,10-tetraoxaspiro[5,5]undecane (hereinafter referred to as Using a dryer having an inlet for powder (referred to as "SPG"), an outlet for dried SPG powder, fluidizing means for the wet powder, and a jacket on the outer wall of the dryer, A method for producing dry SPG is disclosed in which the wet powder is indirectly heated by passing a heating medium in the temperature range from the boiling point of 190° C. to 190° C. through a jacket.
- SPG inlet for powder
- a heating medium in the temperature range from the boiling point of 190° C. to 190° C.
- Patent Document 4 states, ⁇ The means for fluidizing the powder may be a stirring blade that rotates around an axis, the dryer itself may rotate, or the dryer itself may vibrate.
- stirring blades include paddle blades, anchor blades, ribbon blades, etc.'', and ⁇ fluidization'' in Patent Document 4 refers to stirring force, rotational force, etc. This has a technical meaning in that the treated powder is stirred and flows by the action.
- Patent Document 4 states, ⁇ The temperature of the heating medium is preferably 15°C or more higher than the boiling point of the solvent, and by setting the temperature of the heating medium 15°C or more higher than the boiling point of the solvent, the amount of solvent is 0.5% by weight or less.
- the drying method disclosed in Patent Document 1 or Patent Document 2 mentioned above merely enables continuous processing under reduced pressure, and no improvement has been made in the heat transfer mechanism. Therefore, the drying system did not have a practical level of drying ability capable of mass processing.
- the fluidization of the treated material disclosed in Patent Document 3 and Patent Document 4 is a state in which stirring force or rotational force is applied to the treated material, in other words, a state in which the treated material is scattered due to movement, which will be described in detail later. This method does not achieve the ideal fluidization of the processed material. Therefore, it was not possible to expect a dramatic improvement in heat transfer efficiency.
- the present invention has been made in view of the problems of the above-mentioned background technology, and its purpose is to realize an ideal fluidized state of the processed material and perform continuous processing under reduced pressure to obtain high drying efficiency. It is an object of the present invention to provide a method and apparatus for drying powder and granular material, and furthermore, a method for efficiently producing powder and granular material having a specific degree of dryness.
- the present invention provides a method and apparatus for drying a granular material, as well as a method for producing a granular material, as described in the following [1] to [5].
- a powder drying method in which powder and granule raw materials are continuously supplied, a heating medium is supplied to a stirring means under reduced pressure, and the powder and granule raw materials are dried by heating while stirring.
- the median diameter (D50) of the granular raw material is in the range of 1 ⁇ m to 1000 ⁇ m, and is 15 to 120% lower than the boiling point of the solvent in the granular raw material under reduced pressure at an absolute pressure of 4 to 30 kPa.
- a method for drying powder or granular material characterized in that the powder or granular material is fluidized and dried by heating with a heating medium at a temperature as high as 0.degree. C.
- a discharge port provided at a lower part of the casing, the casing is connected to a pressure reducing means so as to be able to reduce the pressure inside the casing, a hollow shaft is rotatably spanned within the casing, and a hollow stirring means is connected to the hollow shaft.
- Powder and granule material is arranged at a predetermined interval and is configured to heat the powder and granule raw material while stirring it under reduced pressure by supplying a heating medium to the hollow shaft and the hollow stirring means. drying equipment.
- a valve casing in which the supply port and the discharge port of the casing are provided with an inlet opening on the upper side and an outlet opening on the lower side, a position in the valve casing that closes the inlet and the outlet.
- a method for producing a powder or granule material which comprises producing a powder or granule material having a moisture content of 1.0% by mass or less by the drying method for a powder or granule material according to [1] or [2] above.
- FIG. 2 is a diagram conceptually showing a method for measuring the powder surface inclination angle ( ⁇ ) of a powder surface in a fluidized state.
- 1 is a partially cutaway side view showing an embodiment of a drying device used in the drying method of the present invention.
- 4 is an enlarged cross-sectional view of a portion taken along line XX in FIG. 3.
- FIG. It is a conceptual block diagram of an air lock valve. It is a figure showing the process of feeding the processed material of the air lock valve. It is a perspective view of a stirring means.
- FIG. 3 is a perspective view showing a state in which stirring means is arranged on the shaft.
- the present inventors have completed the present invention not only by making continuous processing possible in vacuum drying, but also by fundamentally reviewing the heat transfer mechanism in vacuum drying.
- the feature of the present invention is that the median diameter (D50) of the powder and granular material to be treated is in the range of 1 ⁇ m to 1000 ⁇ m, and the powder and granular material is processed under reduced pressure of 4 to 30 kPa absolute pressure.
- Channeling and bubbling are examples of phenomena associated with fluidization in a broad sense.
- Channeling refers to a phenomenon in which gas generated or supplied is not uniformly dispersed throughout the powder layer, but intermittently blows through a portion of the layer.
- Bubbling refers to a phenomenon in which gas generated or supplied in the lower part of the powder bed or in the powder bed rises in the layer as bubbles.
- the ideal fluidization state in a fluidized bed drying system is that the gas is in the powder bed in terms of contact with hot air and movement of evaporated matter. It can be said that it is in a state where it is uniformly dispersed. At this time, depending on the amount of gas generated or supplied, the powder layer assumes a relatively smooth powder surface state.
- the fluidization disclosed in Patent Document 3 and Patent Document 4 mentioned in the background art is a state in which stirring force or rotational force is applied to a powder or granule, in other words, a state in which the powder or granule is scattered due to movement. This is different from the above-mentioned ideal fluidized state in which the gas and the treated powder are uniformly dispersed.
- Patent Document 4 discloses that in a conductive heat transfer type dryer in which a heating medium is passed through a stirring means, the heat transfer efficiency is improved by fluidizing the processed material by stirring.
- the treated powder becomes scattered due to movement, which increases the number of times of contact between the treated powder and the heat transfer surface, making heat exchange more efficient. Possible effects include the effect of oxidation, and the effect of making it easier for the solvent to evaporate smoothly.
- fluidization by stirring as described above is not only insufficient as a fluidization state, but also causes the powder layer to oscillate as a result of stirring, resulting in poor heat transfer. It was found that the exposure of the surface and the generation of large cavities inside the powder layer lead to a reduction in the heat transfer surface that comes into contact with the powder, and that this method is not a fundamental solution to improving heat transfer efficiency.
- FIG. 1(A) conceptually shows the relationship between the stirring means in the dryer and the powder surface.
- the stirring means is shown as a perfect circular disk for ease of understanding, but even when using an asymmetrically shaped stirring means, the trajectory of the outermost periphery when rotating around the rotation axis is It can be assumed that it shows a perfect circle.
- the stirring means is divided into regions a to d in the upper, lower, right, and left directions, in the vicinity of region b on the upstream side of the rotation, the processed powder is lifted as the stirring means rotates, and the powder surface is lifted by force.
- the heat transfer surface will be exposed in region c. Moreover, large cavities are generated instantaneously and continuously inside the powder layer, and the heat transfer surface cannot come into contact with the treated powder at the portion where the cavities are generated. If the rotational speed of the stirring means is significantly lowered in order to suppress the occurrence of this shifting and shaking, the heat exchange efficiency between the treated powder and the heat transfer surface is reduced, and the heat transfer efficiency is lowered. Further, even if the powder surface is raised by increasing the amount of processed powder input without changing the rotational speed of the stirring means, the powder surface will shift or oscillate. Furthermore, in this case, the number of times the treated powder contacts the heat transfer surface per unit time and per unit weight decreases, and the heat transfer efficiency decreases. This reduction in heat transfer efficiency was more noticeable in the conduction heat transfer dryer having a single shaft than in the conduction heat transfer dryer having a plurality of shafts of stirring means.
- the present invention fundamentally improves the above problem by creating a state in which the treated powder spontaneously fluidizes without the application of kinetic energy such as stirring force or rotational force.
- the fluidized state in the present invention is characterized in that the powder layer rises uniformly and becomes fluidized, the powder surface is flat without shaking even when stirred, and there is little inclination of the powder surface due to stirring.
- the fluctuation of the powder surface is suppressed and the powder surface is flat, and at the same time, the angle of inclination of the powder surface is small.
- the fluidized state of the present invention refers to a state in which the powder surface is ranked 5 or 4 during operation of the dryer.
- the powder surface inclination angle ( ⁇ ) in the table is within a perfect circle formed by the locus of the outermost periphery of the stirring means when the stirring means is rotated in the drying operation of the treated powder, and within the upstream of the rotation. This is the angle between the horizontal plane and a straight line connecting the part ( ⁇ ) where the powder surface on the side is raised the most and the part ( ⁇ ) where the powder surface is the most depressed on the downstream side of the rotation (see FIG. 2).
- the powder surface inclination angle ( ⁇ ) For the powder surface inclination angle ( ⁇ ), if the powder surface is not stable and is shaking violently, record a video, calculate the powder surface inclination angle ( ⁇ ) for each frame, and calculate the maximum value. This is the plane inclination angle.
- the rotation conditions of the stirring means are 0.03 to 0.8 m/s, preferably 0.25 to 0.63 m/s at the linear velocity at the outermost periphery, but the powder surface inclination angle ( ⁇ ) is defined not only by the rotation conditions but also by the state of the powder surface during operation of the dryer.
- the treated powder when the treated powder is heat-treated under reduced pressure of an absolute pressure of 30 kPa or less by passing a heating medium at a temperature 15° C. or more higher than the boiling point of the solvent in the treated material under the reduced pressure through a stirring means, the powder becomes It was confirmed that the liquid inside the layer evaporated instantaneously, gas was generated, and the powder layer was in a fluidized state of rank 4 or 5.
- This fluidized state allows the generated gas to move easily even under reduced pressure, and the treated powder is not only in motion but also maintains contact with the heating means.
- heat transfer efficiency increases dramatically, providing processing capacity that cannot be achieved with conventional vacuum dryers.
- the effect of improving throughput due to the above-mentioned fluidized state is noticeable, and it is suitable from the viewpoint of making the device more compact.
- Drying has traditionally been carried out using a combination of reduced pressure and heating, but the technical intention was to lower the boiling point of the solvent by reducing pressure, thereby allowing efficient drying even at lower temperatures. Therefore, even though an excessive amount of heat may be added at normal pressure, when the pressure is reduced to a certain level or below, processing is performed at a temperature close to the boiling point of the solvent, and considering the purpose of drying at a lower temperature. It can be said that there are inhibiting factors that cannot be selected when excessive heating is performed after reducing the pressure.
- Fluidization in a broad sense occurs due to boiling of the solvent even at normal pressure depending on the temperature, but gas generation due to evaporation is uneven and involves intermittent channeling, so it remains at rank 1 in the above fluidization ranking, and the present invention This was different from the fluidized state of .
- the upper limit of the heating temperature needs to take into consideration the decomposition point and melting point of the material to be treated, but in the examples, the difference ( ⁇ T) between the heating medium temperature and the boiling point of the solvent under reduced pressure is up to 120°C.
- the above ⁇ T is preferably in the range of 15 to 100°C, more preferably in the range of 15 to 70°C.
- the temperature is preferably 20°C or higher, and taking this point into account, ⁇ T is preferably in the range of 20 to 100°C, most preferably 20 to 70°C.
- the median diameter (D50) of the granular raw material to be treated is in the range of 1 ⁇ m to 1000 ⁇ m.
- D50 exceeds 1000 ⁇ m, the treated powder becomes too heavy and spontaneous fluidization is difficult to occur even under the above-mentioned heating conditions under reduced pressure.
- D50 is less than 1 ⁇ m, there are many fine powders of about 1 ⁇ m or less, and the cohesiveness is strong, making continuous fluidization difficult to occur.
- the median diameter (D50) of the powder raw material to be treated is preferably in the range of 100 ⁇ m to 800 ⁇ m, more preferably in the range of 150 ⁇ m to 700 ⁇ m.
- the moisture content of the powder raw material to be treated is preferably 10 to 70% by mass, more preferably 20 to 60% by mass, and still more preferably 20 to 50% by mass. . If the moisture content is less than 10% by mass, fluidization ends in a short period of time, and a sufficient effect of improving drying capacity is not observed. When the moisture content exceeds 70% by mass, uniform fluidization becomes difficult to occur.
- the powder or granular raw material to be treated does not have the above-mentioned median diameter or moisture content, it is preferable to perform pretreatment to adjust the powder or granular raw material to the above-described median diameter or moisture content.
- the pretreatment in this case is not limited in any way, and a wide variety of known pulverization methods and moisture adjustment methods can be employed.
- the moisture contained in the treated powder may be moisture remaining in the object to be treated or any liquid used as a solvent or dispersion medium in the manufacturing process, as long as it is generally used as a solvent.
- a solvent for example, water, lower alcohols such as methanol, ethanol, propanol, isopropanol, polyhydric alcohols such as glycerin, ethylene glycol monoethyl ether, propylene glycol, 1,3-butylene glycol, acetone, methyl ethyl ketone, methyl isobutyl ketone, etc.
- any of lower ketones, lower esters such as ethyl acetate and isopropyl acetate, lower ethers such as diethyl ether and diisopropyl ether, or a mixture of two or more of these may be used.
- at least one of the solvents is heated under the above conditions, that is, under reduced pressure with an absolute pressure of 4 to 30 kPa, and at a temperature 15 to 120°C higher than the boiling point of the solvent under the reduced pressure. If the following conditions are satisfied, the fluidized state of the present invention can be obtained.
- an azeotropic mixture is generated, the azeotropic point according to the ratio is used as the standard.
- the heating means for the treated powder is preferably a conduction heat transfer dryer configured to include a hollow shaft and a hollow stirring means, and to indirectly heat the treated powder by circulating a heating medium inside the dryer.
- heating may be performed from the casing.
- a disk-shaped stirring means, a paddle-shaped stirring means, or a screw-shaped stirring means can be used as the stirring means.
- a conduction heat transfer dryer in which stirring means are arranged on multiple axes the effect of improving throughput is noticeable, and from the viewpoint of making the device more compact, a conduction heat transfer dryer in which the stirring means is arranged on a single axis is adopted. It is preferable.
- the fluidized state of the present invention occurs in at least 1/5 or more of the path length in which the heating means and the treated powder come into contact.
- the fluidized state of the present invention does not occur, so a transition occurs to lapse rate drying in a part of the downstream region of the path length, and the constant rate drying of the present invention No fluidization state occurs.
- FIG. 3 is a partially cutaway side view of the drying device
- FIG. 4 is an enlarged sectional view of a portion taken along line XX in FIG. 3.
- reference numeral 1 denotes a casing of a drying device consisting of a relatively horizontally long container.
- the casing 1 is installed in a slightly inclined state by a support base 2.
- a supply port 3 for the material to be treated is provided at the upper front end of the casing 1, and a discharge port 4 for the material to be processed is provided at the bottom of the rear end.
- an exhaust port 5 is provided in the upper part of the casing 1.
- the feed port 3 for the processed material provided in the casing 1 is connected to the raw material hopper 7 via an air lock valve 6 that continuously introduces the processed material.
- the discharge port 4 is connected to a recovery hopper 9 via an air lock valve 8 which also continuously discharges the processed material.
- an exhaust port 5 provided in the casing 1 is connected to an exhaust pressure reduction unit 10.
- the configuration of the air lock valve 6 includes a valve casing 13 having an inlet 11 opened at the top and an outlet 12 opened at the bottom; It consists of a valve 14 that is rotatably provided within the valve casing 13 to a position where the inlet port 11 is closed and a position where the outlet port 12 is closed. Then, in a state where only the outflow port 12 is closed by the valve 14 (the state shown in FIG. 6A), the processed material P is passed from the raw material hopper 7 (or the casing 1 of the drying device) to the valve casing 13 through the inflow port 11. After the valve 14 is rotated to close both the outflow port 12 and the inflow port 11 (the state shown in FIG.
- the exhaust depressurization unit 10 serves to exhaust steam from the inside of the casing 1 of the drying device and to depressurize the inside.
- the exhaust pressure reduction unit 10 includes, for example, dust removal equipment such as a bag filter that removes dust contained in the exhaust gas from the casing 1, a condenser that cools and condenses steam contained in the exhaust gas, and a depressurizer inside the casing 1. It can be configured by depressurizing means to remove the odor contained in the exhaust gas, deodorizing equipment to remove the odor contained in the exhaust gas, etc.
- the pressure reducing means can be a pump, an aspirator, or the like.
- the deodorizing equipment can be a metal catalyst, a filter, activated carbon, etc. It is preferable that the exhaust gas pressure reduction unit 10 is equipped with at least pressure reduction means and deodorization equipment.
- a hollow shaft 20 passes through the front and rear of the casing 1 of the drying device, and is rotatably supported by bearings 21 and 22 provided at the front and rear of the casing 1.
- a sprocket 23 is provided at the front of the hollow shaft 20, and the rotation of the motor 24 is transmitted to the hollow shaft 20 via a chain meshed with the sprocket 23.
- a direct drive in which a motor is directly connected may be used, and a hydraulic motor may also be used as the motor.
- a heating medium supply pipe 26 is connected to the front end of the hollow shaft 20 via a rotary joint 25, and a heating medium discharge pipe 28 is similarly connected to the rear end of the hollow shaft 20 via a rotary joint 27.
- the hollow shaft 20 is provided with a partition plate 29 that partitions the inside into two parts in the axial direction, as shown in FIG.
- the interior of the hollow shaft 20 is divided by the partition plate 29 into a primary chamber 20a and a secondary chamber 20b.
- the primary chamber 20a is communicated with the front part of the hollow shaft 20, and the secondary chamber 20b is communicated with the rear part of the hollow shaft 20.
- the hollow stirring means 30 is formed in the shape of a disk that is thinner than its diameter. More specifically, it has concentric protrusions 31, 31 that are gently curved in the left-right direction when viewed from the side in the center, and openings 32, 32 are formed at the tips of the protrusions 31, 31, respectively. It is formed into a thin, substantially hollow disk shape with both plate surfaces parallel to each other.
- a plurality of scraping blades 33 are attached to the outer periphery of the disk-shaped hollow stirring means 30 at equal intervals.
- the scraping blades 33 are attached to each stirring means 30, but depending on the physical properties of the material to be treated, the scraping blades 33 may be attached between two or more adjacent stirring means 30, 30. It is also possible to have a raking blade (not shown) attached to the blade. On the other hand, it may also have no raking blades.
- a partition plate 34 is attached inside the hollow stirring means 30 as shown in FIGS. 4, 8, and 10, and the internal space 35 of the stirring means 30 is partitioned off by the partition plate 34. Then, the heating medium that has flowed into the internal space 35 of the hollow stirring means 30 from the primary chamber 20a of the hollow shaft 20 described above through the communication hole 36 circulates in the internal space 35 in a fixed direction and passes through the communication hole 37.
- the structure is such that a flow is formed that flows out into the secondary chamber 20b of the hollow shaft 20.
- a large number of the hollow stirring means 30 having the above-mentioned configuration are arranged on the hollow shaft 20 at regular intervals so that the scraping blades 33 thereof are lined up in the same direction. This distance between the stirring means is ensured by the tips of the protrusions 31, 31 of the adjacent stirring means 30, 30 coming into contact with each other when the hollow shaft 20 is inserted into the opening 32 of the stirring means 30.
- the number of hollow shafts 20 is not limited to one, and may be two or more, for example. However, as mentioned above, it is preferable to use only one wire, from the viewpoint of significantly improving the processing capacity and making the device more compact.
- the hollow stirring means 30 disposed on the hollow shaft 20 may be entirely disk-shaped.
- stirring means of other shapes may be appropriately combined and attached to the hollow shaft 20, but at least in the region where the fluidized state of the present invention is formed, As mentioned above, from the viewpoint of ensuring a heat transfer surface, it is preferable to use a disc-shaped stirring means.
- the inside of the casing 1 of the drying device is brought into a predetermined reduced pressure and heated state. Therefore, the hollow shaft 20 is rotated by the motor 24 via the sprocket 23, and a heating medium such as steam or hot water is sent to the hollow shaft 20 from the rotary joint 25.
- the heating medium sent to the hollow shaft 20 flows into the internal space 35 of the hollow stirring means 30 from the primary chamber 20a of the hollow shaft 20, heats the stirring means 30, and passes through the secondary chamber 20b of the hollow shaft 20.
- the heating medium is discharged from a discharge pipe 28 via a rotary joint 27 connected to the rear part of the hollow shaft.
- the exhaust pressure reducing unit 10 is operated to take in air from the exhaust port 5 provided in the casing 1 to bring the inside of the casing 1 into a reduced pressure state.
- the inside of the casing 1 is brought into a reduced pressure state with an absolute pressure of 4 to 30 kPa, and is also heated to a temperature 15 to 120°C higher than the boiling point of the moisture (solvent) in the powder raw material under the reduced pressure. do.
- the granular raw material (which may be powder or granules), which is the processed material, is continuously supplied into the casing 1 from the supply port 3 of the drying device.
- the supplied granular raw material preferably has a median diameter (D50) in the range of 1 ⁇ m to 1000 ⁇ m, and has a moisture content of 10 to 70% by mass. If the granular raw material to be treated does not have the above median diameter or moisture content, it is not possible to pre-process as described above to adjust the granular raw material to the above median diameter or moisture content. preferable.
- the powder raw material supplied into the casing 1 is heated while being stirred by the stirring means 30, and drying progresses.
- the powder raw material is heated under reduced pressure of an absolute pressure of 30 kPa or less at a temperature 15°C or more higher than the boiling point of the solvent under the reduced pressure, so the solvent instantly vaporizes from inside the powder layer. Due to this, gas is generated, and the powder bed becomes a fluidized state of ranks 4 and 5 as described above, and the generated gas is easy to move, and the powder and granules are not only in motion but also in contact with the heating means. Since this is maintained, heat transfer efficiency increases dramatically and efficient drying is performed.
- the granular material charged into the casing 1 gradually flows down inside the casing 1 due to the pressure due to the filling height of the granular material subsequently introduced from the supply port 3 and the inclination of the casing 1, and achieves the efficiency described above. After being subjected to a drying process, it moves to the discharge port 4, is discharged through the air lock valve 8 in an airtight state, and is collected in the collection hopper 9.
- the recovered granular material has a moisture content of 1.0% by mass or less, and is a dry granular material with volatile components such as VOCs reduced as much as possible.
- NVD-3 type uniaxial conduction heat transfer dryer, heat transfer area 3.4 m 2 , volume 150 L
- Fig. 3 and Fig. 4 are shown in Fig. 5.
- the stirring means was disk-shaped, and the diameter of the disk was 300 mm.
- Example 1- Water was added to commercially available polyester ketone (D50: 648 ⁇ m, melting point: 300 to 360° C.) to prepare a wet raw material with a moisture content of 20% by mass.
- Continuous drying treatment was performed using the above drying apparatus according to the following procedure. Steam was used as the heating medium, the temperature was set at 180°C, and the heating medium was circulated. The pressure inside the apparatus was reduced to 20 kPa. The boiling point of water at this time is 60°C, and ⁇ T is 120°C.
- the peripheral speed of the outermost circumference of the disk was set to 0.3 m/s, and the wet raw material was supplied at an input speed of 90 kg/h (based on dry powder), and continuous reduced-pressure drying was started.
- Table 4 shows the results of the drying treatment of each wet raw material.
- Comparative Example 1 the powder surface was disturbed by stirring and was not flat. Further, the product moisture content was 8% by mass, which was very inferior to that of the examples.
- Comparative Examples 2 and 3 intermittent and local gas blow-through (channeling) occurred. The product moisture content was 3% by mass, which was inferior to the Examples.
- Comparative Example 4 intermittent and local gas blow-through (channeling) occurred. The product moisture content was 23% by mass, which was very poor compared to the examples.
- Comparative Example 5 the powder surface was disturbed by stirring and was not flat. The product moisture content was 3% by mass, which was inferior to the Examples.
- the powder drying method, drying device, and production method according to the present invention can be used for drying and producing powder and granule materials in a wide range of fields such as synthetic resins, foods, and chemical products.
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Abstract
Description
一方、減圧乾燥システムは、高温での乾燥が適さない処理物に対しては有効な手段であり、VOC等の揮発成分の除去にも適しているが、連続処理が困難で、大量処理には不向きであるという課題がある。
例えば、特許文献1には、予備真空室で真空状態におかれた粒状物を真空室中で回転する回転ドラム中に連続的に送り、前記回転ドラム内面に設けられたリボン状スクリューに沿って粒状物を移動させることにより乾燥させ、その後真空解除室で常圧に戻した状態で粒状物を取出す粒状物の連続真空乾燥方法が開示されている。
また、特許文献2には、減圧された状態の内部に含水物が供給され、前記含水物を加熱しながら一定方向に搬送する乾燥機本体部と、前記乾燥機本体部の含水物搬送方向に沿って下流側にその内部を前記乾燥機本体部の内部と連通させて設けられるとともに、前記含水物を排出する排出口を気密に閉塞可能であって且つ開放可能な開閉機構を有する貯留ホッパー部と、を備える含水物乾燥装置が開示されている。
また、特許文献3、特許文献4に開示された処理物の流動化は、処理物に撹拌力や回転力を作用させた状態、換言すると処理物が運動により飛び散った状態であり、後に詳述する理想的な処理物の流動化を実現したものではない。そのため、伝熱効率を飛躍的に向上させることを期待できるものではなかった。
〔1)粉粒体原料を連続的に供給し、減圧下において、攪拌手段に加熱媒体を供給し、撹拌しながら加熱することにより粉粒体原料の乾燥処理を行う粉粒体の乾燥方法であって、粉粒体原料のメジアン径(D50)が、1μmから1000μmの範囲であり、絶対圧力4~30kPaの減圧下において、前記減圧下における粉粒体原料中の溶媒の沸点より15~120℃高い温度の加熱媒体で加熱することにより、粉粒体原料を流動化させて乾燥処理を行うことを特徴とする、粉粒体の乾燥方法。
〔2〕上記粉粒体原料の湿分が、10~70質量%であることを特徴とする、上記〔1〕に記載の粉粒体の乾燥方法。
〔3〕上記〔1〕に記載の粉粒体の乾燥方法に用いる乾燥装置であって、ケーシングと、前記ケーシングの一方の端部の上部に設けられた供給口と、ケーシングの他方の端部の下部に設けられた排出口とを有し、前記ケーシングは内部を減圧可能に減圧手段と接続され、前記ケーシング内には中空シャフトが回転可能に架け渡され、前記中空シャフトに中空攪拌手段が所定の間隔を隔てて配置され、前記中空シャフト及び中空攪拌手段に加熱媒体を供給することにより、粉粒体原料を減圧下において撹拌しながら加熱する構成としたことを特徴とする、粉粒体の乾燥装置。
〔4〕上記ケーシングの供給口と排出口に、上側に開口した流入口と下側に開口した流出口を設けたバルブケーシングと、前記バルブケーシング内において上記流入口を閉塞する位置と上記流出口を閉塞する位置とに回動可能に設けられたバルブとからなり、前記バルブを回転することで、粉粒体を気密状態での供給、排出が可能なエアーロックバルブが設けられていことを特徴とする、上記〔3〕に記載の粉粒体の乾燥装置。
〔5〕上記〔1〕又は〔2〕に記載の粉粒体の乾燥方法により、湿分1.0質量%以下の粉粒体を製造することを特徴とする、粉粒体の製造方法。
図示したように攪拌手段を上下左右でa~dの領域に分けると、回転上流側のb領域付近では、攪拌手段の回転に伴って処理粉体が持ち上げられるため、勢いで粉面が持ち上がる。これに対して、回転下流側のc領域付近では、逆に粉面が下方に落ち込んだ形となり、粉面の片寄りが生じる。粉面の片寄りは、回転数を上げると更に増大する。また、攪拌を促進するために、掻き上げ部材等を用いる場合は、粉面の片寄りに加えて、周期的な粉面の揺動を伴う場合も生じる。
なお、攪拌手段の回転条件は、最外周の線速で0.03~0.8m/s、好ましくは、0.25~0.63m/sであるが、本発明の粉面傾斜角(θ)は、前記回転条件に限らず、乾燥機の運転時における粉面の状態によって定義される。
これらの図において1は、比較的横に長い容器からなる乾燥装置のケーシングである。前記ケーシング1は、支持台2によってやや傾斜した状態で設置されている。前記ケーシング1の前端上部には処理物の供給口3が、後端底部には処理物の排出口4がそれぞれ設けられている。また、前記ケーシング1の上部には排気口5が設けられている。
先ず、乾燥装置のケーシング1内を、所定の減圧状態及び加熱状態とする。そのため、中空シャフト20は、モーター24によりスプロケット23を介して回転させ、ロータリージョイント25より中空シャフト20に加熱媒体、例えは蒸気又は熱水等を送る。中空シャフト20に送られた加熱媒体は、中空シャフト20の一次室20aより中空撹拌手段30の内部空間35に流入し、撹拌手段30を加熱し、そして中空シャフト20の二次室20bを経て、中空シャフト後部に接続したロータリージョイント27を介して加熱媒体の排出管28より排出される。また、排気減圧ユニット10を作動させ、ケーシング1に設けられた排気口5より吸気し、ケーシング1内を減圧状態とする。上記の操作により、ケーシング1内を、絶対圧力4~30kPaの減圧状態とするとともに、粉粒体原料中の湿分(溶媒)の前記減圧下における沸点より15~120℃高い温度の加熱状態とする。
攪拌手段はディスク状で、ディスクの直径は300mmであった。
市販のポリエステルケトン(D50:648μm、融点:300~360℃)に水を加え、湿分20質量%の湿潤原料を調製した。
上記乾燥装置を用いて、下記の手順で、連続乾燥処理を行った。
加熱媒体として蒸気を用い、温度を180℃に設定し、加熱媒体を循環した。装置内を減圧し、20kPaとした。このときの水の沸点は60℃であり、ΔTは120℃である。
ディスクの最外周の周速0.3m/sとし、投入速度90kg/h(乾粉基準)で湿潤原料を供給し、連続減圧乾燥を開始した。
乾燥処理が安定した開始から30分後においては、湿潤原料は装置内において流動化しており、粉面は平らで滑らかな状態となっていた。このときの流動化ランクは、表1に示したランクにおいて「ランク5」であった。また、経路長の上流から80%の範囲で「ランク4」以上の流動化が認められた。
開始から30分後、2時間連続乾燥処理を行い、湿分0.3質量%の製品粉体、180kg(乾粉基準)が得られた。
表2に示す湿潤原料を調製し、表3に示す条件で上記乾燥装置を用いて連続乾燥処理を行った。
Claims (5)
- 粉粒体原料を連続的に供給し、減圧下において、攪拌手段に加熱媒体を供給し、撹拌しながら加熱することにより粉粒体原料の乾燥処理を行う粉粒体の乾燥方法であって、粉粒体原料のメジアン径(D50)が、1μmから1000μmの範囲であり、絶対圧力4~30kPaの減圧下において、前記減圧下における粉粒体原料中の溶媒の沸点より15~120℃高い温度の加熱媒体で加熱することにより、粉粒体原料を流動化させて乾燥処理を行うことを特徴とする、粉粒体の乾燥方法。
- 上記粉粒体原料の湿分が、10~70質量%であることを特徴とする、請求項1に記載の粉粒体の乾燥方法。
- 請求項1に記載の粉粒体の乾燥方法に用いる乾燥装置であって、ケーシングと、前記ケーシングの一方の端部の上部に設けられた供給口と、ケーシングの他方の端部の下部に設けられた排出口とを有し、前記ケーシングは内部を減圧可能に減圧手段と接続され、前記ケーシング内には中空シャフトが回転可能に架け渡され、前記中空シャフトに中空攪拌手段が所定の間隔を隔てて配置され、前記中空シャフト及び中空攪拌手段に加熱媒体を供給することにより、粉粒体原料を減圧下において撹拌しながら加熱する構成としたことを特徴とする、粉粒体の乾燥装置。
- 上記ケーシングの供給口と排出口に、上側に開口した流入口と下側に開口した流出口を設けたバルブケーシングと、前記バルブケーシング内において上記流入口を閉塞する位置と上記流出口を閉塞する位置とに回動可能に設けられたバルブとからなり、前記バルブを回転することで、粉粒体を気密状態での供給、排出が可能なエアーロックバルブが設けられていことを特徴とする、請求項3に記載の粉粒体の乾燥装置。
- 請求項1又は2に記載の粉粒体の乾燥方法により、湿分1.0質量%以下の粉粒体を製造することを特徴とする、粉粒体の製造方法。
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PCT/JP2023/012478 WO2023203974A1 (ja) | 2022-04-22 | 2023-03-28 | 粉粒体の乾燥方法、乾燥装置及び製造方法 |
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EP (1) | EP4431851A1 (ja) |
JP (1) | JPWO2023203974A1 (ja) |
WO (1) | WO2023203974A1 (ja) |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS56127168A (en) | 1980-03-13 | 1981-10-05 | Nikku Ind Co | Method of and apparatus for continuous vacuum drying of particulate matter |
JPH01217176A (ja) * | 1988-02-26 | 1989-08-30 | Okawara Mfg Co Ltd | 固体に含まれた溶剤の除去方法 |
JPH0650659B2 (ja) | 1990-08-27 | 1994-06-29 | 株式会社ニチフ端子工業 | 電線端部識別片取付装置 |
JP2001091157A (ja) * | 1999-09-21 | 2001-04-06 | Mizusawa Ind Chem Ltd | 粉体乾燥装置におけるシール機構 |
JP2003055383A (ja) | 2001-05-09 | 2003-02-26 | Sumitomo Chem Co Ltd | 乾燥3,9−ビス(1,1−ジメチル−2−ヒドロキシエチル)−2,4,8,10−テトラオキサスピロ[5,5]ウンデカンの製造方法 |
JP2011163602A (ja) | 2010-02-05 | 2011-08-25 | Mitsubishi Heavy Industries Environmental & Chemical Engineering Co Ltd | 含水物乾燥装置 |
-
2023
- 2023-03-28 EP EP23791627.5A patent/EP4431851A1/en active Pending
- 2023-03-28 JP JP2024516152A patent/JPWO2023203974A1/ja active Pending
- 2023-03-28 WO PCT/JP2023/012478 patent/WO2023203974A1/ja active Application Filing
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS56127168A (en) | 1980-03-13 | 1981-10-05 | Nikku Ind Co | Method of and apparatus for continuous vacuum drying of particulate matter |
JPH01217176A (ja) * | 1988-02-26 | 1989-08-30 | Okawara Mfg Co Ltd | 固体に含まれた溶剤の除去方法 |
JPH0650659B2 (ja) | 1990-08-27 | 1994-06-29 | 株式会社ニチフ端子工業 | 電線端部識別片取付装置 |
JP2001091157A (ja) * | 1999-09-21 | 2001-04-06 | Mizusawa Ind Chem Ltd | 粉体乾燥装置におけるシール機構 |
JP2003055383A (ja) | 2001-05-09 | 2003-02-26 | Sumitomo Chem Co Ltd | 乾燥3,9−ビス(1,1−ジメチル−2−ヒドロキシエチル)−2,4,8,10−テトラオキサスピロ[5,5]ウンデカンの製造方法 |
JP2011163602A (ja) | 2010-02-05 | 2011-08-25 | Mitsubishi Heavy Industries Environmental & Chemical Engineering Co Ltd | 含水物乾燥装置 |
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EP4431851A1 (en) | 2024-09-18 |
JPWO2023203974A1 (ja) | 2023-10-26 |
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