JP2008142617A - Method for cleaning powder, and method for cleaning and drying therefor - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method which enables the easy cleaning of powder with high productivity. <P>SOLUTION: The method is for cleaning powder by using a vibrating and fluidizing apparatus M provided with a filtering perforated plate 36 in a treating vessel 28, a vibrating means 30 vibrating the filtering perforated plate 36 and an air feeding means 24. In the method, a cleaning process is repeated required times which consists of (1) a first step of forming on the filtering perforated plate 36, a layer F of powder containing liquid containing powder in a cleaning liquid, feeding air from the lower part of the filtering perforated plate 36 and cleaning the powder by vibrating the filtering perforated plate 36, (2) a second step of partially removing the liquid through the filtering perforated plate 36 after the first step, and (3) a third step of replenishing a cleaning liquid to the residual liquid after the second step when the first step is performed again. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention relates to a novel powder washing method and washing / drying method, and in particular, adheres to synthetic fine particles (for example, organic pigments and synthetic metal oxides) dispersed in a suspension after a synthesis reaction (polymerization). The present invention relates to a fine powder cleaning method and a cleaning drying method suitable for removing impurities (not only unreacted substances but also acids, alkalis, solvents, etc.).

  The particle size of the powder to be cleaned (target) of the present invention is usually less than about 2 mm, but can be applied to powders of 2 mm or more as long as the effects of the present invention are achieved.

  The cleaning method of the present invention has a surface energy of 100 mesh (147 μm) or less, which is referred to as a fine powder having a large surface energy and is easy to agglomerate, in particular, approximately 200 mesh (74 μm), referred to as an ultrafine powder. In the following, the effect is exerted on those having a thickness of 10 μm or less.

  Here, the case where the synthetic fine powder (average particle diameter of 1 to 10 μm) in the suspension after the synthesis reaction is washed and dried will be mainly described as an example. The present invention is not limited to this case, and the present invention can be applied to various inorganic (ceramic, metal oxide, metal) and organic (compound, polymer) powders as long as the effects of the present invention are exhibited.

  Conventionally, synthetic fine particles (for example, organic pigments) dispersed in the reaction solution (suspension: slurry) after the synthesis reaction as described above are not synthesized as impurities (unreacted substances (reactive compounds, waxes)). , Pigments, etc.) and interfacial lubricants). If it is dried while attached, the required performance cannot be maintained. For this reason, normally, the synthetic fine particles dispersed and contained in the suspension have been washed and dried as follows using a filtration conveyor device 12 as shown in FIG.

  The filtration conveyor device 12 includes a plurality of suction chambers 16 connected to the lower surface of the transport zone Z in a conveyor belt 14 made of filter cloth (perforated plate) disposed endlessly. A shower 18 for supplying cleaning water is provided at an intermediate position above, and a doctor knife 20 is provided at the reverse start position of the belt 14 on the end side in the transport zone Z of the belt 14.

  Then, the synthesized fine particle-containing liquid (suspended, slurry: object to be treated) S after synthesis is supplied onto the belt 14, and suction filtration is performed by operating the suction chamber 16 on the raw material supply side of the conveyor 14. . Thus, the filter cake (powder layer or particle layer) formed on the conveyor 14 is washed with shower 18 of washing water, and after washing, the liquid is again drained by using suction means on the outlet side. To do. The filter cake (cake) c thus produced is scraped and collected from the conveyor 14 with a doctor knife 22 or the like.

  And this cake c is thrown into a stirring tank etc. with washing | cleaning water, is stirred and washed, is again supplied to the said filtration conveyor apparatus 12, and slurry supply filtration and washing | cleaning dehydration are repeated. If the particles are washed cleanly, the cake discharged from the filtration conveyor device 12 is further put into a suitable crushing / drying device to obtain a product.

  However, in this cleaning method, the cleaning efficiency is not good, and a large amount of cleaning water is required. In addition, the number of man-hours for washing or washing / drying was increased, and the productivity of washing or washing / drying was not good.

  Although it does not affect the patentability of the present invention, for example, Patent Documents 1 and 2 exist as prior art documents related to the present invention (related to the application of the same applicant as the present applicant).

  In addition, Patent Document 1 only describes a method of filtering and drying a solid-liquid mixture using a filtration drying apparatus having the same configuration as that of the vibration flow treatment apparatus similar to that used in the present invention. The cleaning process is not scheduled as in the present invention.

In addition, Patent Document 2 describes a method in which a bead body (micro body) is fluidly contacted using a vibration flow treatment apparatus similar to that used in the present invention. It is not intended to clean powder that tends to harden when it is vibrated and fluidized.
JP 2002-320803 A JP 2006-263468 A

  In view of the above, an object of the present invention is to provide a method (problem) in which powders can be easily washed or dried with good productivity.

  In order to solve the above-mentioned problems, the present inventors can efficiently wash the organic fine powder after the synthesis as described above by using the vibration flow treatment apparatus manufactured and sold by the applicant of the present application. Furthermore, after knowing that drying can be performed, the inventors have devised a washing method or washing / drying method for fine powder having the following constitution.

(1) Use a vibration flow treatment apparatus provided with a perforated plate in a treatment tank, and provided with a vibrating means for vibrating the perforated plate and an air feeding means capable of sending air from below the perforated plate. A method for washing powder,
1) A powder-containing liquid in which a powder is contained in a cleaning liquid is formed on a perforated perforated plate, and air is fed from below the perforated porous plate and the perforated plate is vibrated to perform powder cleaning. Step 2) After the first step, after the first step, the second step of partially draining through the filter perforated plate, and 3) When the first step is performed again, the remaining liquid after the second step (hereinafter “after draining”) It is characterized in that the cleaning process comprising the third step of replenishing the cleaning liquid with the “residual liquid”) is repeated a required number of times.

  In the case of the above-described cleaning method, even if the amount of the cleaning liquid (mainly water) is small, it can be cleaned cleanly, and the man-hour (time) for clean water cleaning can be significantly reduced. The reason is estimated as follows. Furthermore, bubbling (foaming) of the cleaning liquid (cleaning water) by air supply and liquid fluidization by vibration occur. The bubbling and liquid fluidization are synergistically performed, and the mixing between the powder particles is performed stronger than the mixing and stirring of the powder and the cleaning liquid by bubbling. As a result, the surface impurities of the powder particles (particle size is smaller than that of the fine powder fluid) are peeled off and discharged out of the cleaning system together with the cleaning liquid at the time of liquid removal.

  Here, the powder-containing liquid is usually a slurry (suspension), but it is not always necessary that the powder is uniformly dispersed in the cleaning liquid. In addition, a slant dispersion whose powder concentration changes in the direction of gravity is also included.

  As the cleaning liquid, when the object to be cleaned is an organic powder as described above, cleaning water (pure water) is usually used. However, a cleaning auxiliary such as a surfactant is added purely, alcohol or the like. It may be mixed with a hydrophilic solvent. Furthermore, when the object to be cleaned is inorganic, organic solvents such as hydrocarbons can be used as appropriate.

  (2) In the above configuration, after the powder is supplied from below the perforated plate and while vibrating the perforated plate, the cleaning liquid is supplied while continuing the air supply and vibration. May be.

  Usually, it is difficult to diffuse naturally just by putting a fine powder (less than 1 mm: μm order) into a tank together with a cleaning liquid (cleaning water). In particular, in the case of organic fine particles, the specific gravity is usually about 1 or less, and a floating layer is formed by floating. Furthermore, when the powder becomes a fine powder (particularly, an ultrafine powder of 10 μm or less), it tends to aggregate and harden. In these states, it is difficult to obtain a suspension (uniform dispersion system) in which fine particles are uniformly dispersed without being associated with each other with a normal stirring blade, and it is difficult to sufficiently wash the particles. It is presumed that the shower filtration cleaning that allows the cleaning liquid to pass through the interstices and the stirring cleaning whose main purpose is crushing were repeatedly performed.

  On the other hand, in the method of the present invention, the powder layer (dried state) deposited on the filter perforated plate is fed from the lower surface (aeration), and if necessary, the powder layer is fluidized while being vibrated. The cleaning liquid can be poured in a state of being converted. For this reason, uniform dispersion (suspension) is easily promoted by mixing and stirring.

  (3) When the present invention is applied to the washing of the synthetic fine powder contained in the suspension containing the synthetic fine powder after the synthetic reaction after the synthetic reaction, the constitution is as follows.

Using a vibration flow treatment apparatus provided with a perforated plate in the treatment tank, and provided with a vibrating means for vibrating the perforated plate and an air feeding means capable of feeding air from below the perforated plate, A method for washing the body,
The powder is a synthetic fine powder contained in a reaction liquid containing the synthetic fine powder after the synthetic reaction,
After the reaction liquid is put into the treatment tank, it is partially drained through a filter perforated plate, and the residual liquid after the partial liquid removal is supplemented with a cleaning liquid to form a powder-containing liquid layer. 1) Filtration A first step of supplying air from below the perforated plate and oscillating and washing the perforated plate; 2) a second step of partially draining through the perforated plate after the first step; and 3) again. In the case of performing the first step, the cleaning includes the third step of forming a powder-containing liquid layer by replenishing the remaining liquid after the second step (hereinafter referred to as “residual liquid after deliquidation”) with a cleaning liquid. The method is characterized in that the process is repeated as many times as necessary.

  (4) In each of the above-described configurations, air may be intermittently supplied from below the perforated plate during partial liquid removal in the second step. It is possible to prevent clogging of the perforated plate generated during partial liquid removal.

  (5) Residual liquid after dehydration should be fluidized by vibration of the perforated plate and be as high as possible and fluidized after replenishing the cleaning liquid. It is preferable to carry out this process. It becomes easy to uniformly mix the remaining liquid and the cleaning liquid after the liquid removal.

  (6) The vibration flow treatment apparatus used in each configuration is a treatment tank having a discharge port whose lower end is positioned below the upper surface of the filtration porous plate, and the attachment site of the filtration porous plate is removable from the treatment tank body. The structure which makes a division body is preferable.

  With this configuration, the filtration porous plate can be easily replaced, and the lower end of the discharge port is positioned below the upper surface of the filtration porous plate, so that the entire amount of powder after cleaning (treatment) can be easily discharged. A discharge stirrer may be disposed on the filter perforated plate in order to facilitate discharge of the washed (processed) powder from the discharge port.

  (7) The cleaned product (slurry) that has undergone each of the cleaning methods having the above-described configurations is subjected to final drying by vibration fluidized drying after preliminary drying or liquid removal. Although not particularly limited, the preliminary drying is performed by, for example, an air dryer or a vacuum drum dryer, and the liquid removal is performed by, for example, a centrifugal separator or a filter press. In addition, vibration fluidized drying is suitable for final drying because it can obtain a product (powder) with a low water content, but is not limited to vibration fluidized drying as long as a product (powder) with a low water content can be obtained. .

  Next, the powder washing method or washing / drying method of the present invention will be described mainly in the case where the powder is organic fine particles contained in the reaction liquid (suspension) after synthesis of the organic pigment. Explained. In the following description, “moisture content” means “dry moisture content”. “%” Indicating “concentration” or the like means “mass (weight)%” unless otherwise specified.

  FIG. 2 shows an example of a flowchart of a cleaning apparatus used in the method for cleaning organic fine particles (powder) of the present invention.

  The washing / drying apparatus M basically includes a washing machine 22, an air supply (aeration) pipe 24 connected to the washing machine (vibration flow processing apparatus) 22, and an exhaust pipe 26. .

  The cleaning machine 22 includes a sealable (sealed) cleaning tank (processing tank) 28 and a vibration motor (vibration means: oscillator) 30 that vibrates (vibrates) the cleaning tank 28. The cleaning tank 28 is supported on a gantry (base) 32 through a compression coil spring (elastic support) 34 so as to vibrate. The vibration motor 30 is attached to both sides of the bottom of the cleaning tank 28 so that the cleaning tank 28 can be vibrated.

  The cleaning tank 28 is provided with a filter perforated plate (rectifying plate or dispersion plate) 36 that forms the bottom of the cleaning zone (fluidized bed) F in the middle. Further, an object to be cleaned (raw material) / cleaning liquid (cleaning water) inlet 38 and an exhaust port 39 are provided on the ceiling side of the cleaning tank 28 (above the filter porous 36), and a position directly above the filter porous plate 36 on the peripheral wall. Is provided with a product (washed powder) outlet 30. Further, on the bottom side of the washing tank (below the filter porous plate 36), there are a drain port 42, a gas inlet 43 for air supply (in a position directly below the filter porous plate 36), and a suction pipe (not shown). A connected suction port 45 is provided. In addition, the bottom part shape in which the drain outlet 42 of the washing tank 8 was formed is formed in the taper shape so that drainage is easy.

  The filtration porous plate 36 is usually a metal or ceramic porous plate (for example, a punching plate) or a wire mesh. The filtration porous plate 36 may be a composite filtration porous plate in which a filter cloth is held on both sides by a wire mesh or a grit plate (lattice frame plate), or a plastic filtration porous plate formed of porous FRP or the like.

  The unit aperture diameter / opening ratio of the filter porous plate 36 is such that the powder does not pass through and the cleaning liquid can pass through, the gas resistance is as small as possible, and the powder containing powder formed on the filter porous plate 36 is contained. The diameter should be equal to or larger than the diameter at which an air (gas) flow rate capable of generating bubbling that contributes to powder cleaning in the liquid can be obtained. For example, when the average particle diameter of the powder is 4 μm, the unit opening diameter is 5 ± 5 μm, although it varies depending on the characteristics of the powder and the processing concentration.

  Here, the inlet 38 for the powder to be cleaned (raw material) and the cleaning water (cleaning liquid) is shared, but may be provided separately.

  Further, the drainage port 42 is provided with a drainage valve 44, and a drainage tube 48 with a tip outlet facing the drainage receiving tank 46 is connected.

  Further, the product take-out port 40 may be provided with a chute or the like in the product receiving tank 42 so that it can be dropped and collected.

  Although not necessary, the peripheral wall of the cleaning tank 28 is covered with a temperature control jacket 52. The temperature adjustment jacket 52 can pass temperature adjustment water (cold water to hot water) so that the temperature of the cleaning zone (fluidized bed) F can be adjusted.

  In this embodiment, the vibration means (oscillation device) is the vibration motor 30 that is an oscillation device using the rotation of an unbalanced weight. However, the vibration means is not limited to this, and when the cleaning tank 28 is small and lightweight, an electromagnetic type is used. It may be an oscillation device.

  The air supply pipe (gas inlet pipe) 24 includes a blower (gas transporter) 48 on the gas (air) intake side and a temperature controller (heat exchanger) 50 in the middle. In addition, although the temperature controller 50 is a switching system of cold water / hot water (or steam) as one heat medium, a heater and a cooler may be provided separately. The gas intake side can be connected to an inert gas tank (not shown). This is effective when the powder to be processed is subject to air oxidation.

  The exhaust pipe 26 is connected to an exhaust port 39 formed on the ceiling side of the cleaning tank 28 (above the perforated porous plate 36), and can be exhausted by a vacuum pump 56 via a condenser 54. Yes. The condenser 54 is provided with a liquid recovery tank 58. A bag filter 40 is attached to the exhaust port 39.

  In this embodiment, although not necessarily, the attachment part of the filtration porous plate 36 is removable from the washing / drying tank main body 28a, and the discharge port 40 having the lower end located below the upper surface of the filtration porous plate 36 is provided. The processing tank division body (short cylinder whose upper and lower ends can be connected to a flange) 28b. A piston-type product take-out valve 60 is attached to the discharge port 40.

  In this embodiment, the discharge port 40 of the cleaning tank 28 is connected to a raw material input port 64 of an airflow drying device (preliminary dryer) 62 through a slurry pipe 66 so as to be input (supplied). An inlet of a drying pipe (spiral winding pipe) 68 of the airflow drying device 62 is connected to a hot air pipe 74 having a blower 70 at the base and a heating device 72 in the middle. Naturally, the outside of the drying pipe 68 is surrounded by a jacket or a heat insulating material, although not shown, and is kept warm.

  The pre-dried product outlet 76 of the air flow drying device 62 is connected to a cyclone type pre-dried product collecting device 80 via a pre-dried product pipe 78. In addition, 82 is a cyclone and 84 is a collection tank. The gas outlet side of the cyclone 82 of the pre-dried product collection device 80 is connected to a suction pipe 90 having a wind exhauster 88 at the tip via a dust collector 86.

  Furthermore, in this embodiment, a vibration drying device 92 as a preliminary drying device as shown in FIG. 3 is prepared. The vibration drying device 92 includes a hot air pipe 100 having a blower 96 in the middle and a heater 98 in the middle so that hot air can be fed into the treatment tank 94, and an exhaust fan 102 at the tip of the exhaust port 101. In the middle, a suction pipe 108 having a condenser 106 with a liquid recovery tank 104 is provided. A bag filter 112 is attached to the exhaust port 101 of the vibration drying device 92.

  Next, a method for cleaning organic fine particles contained in a suspension after synthesizing organic fine particles using a powder cleaning / drying plant comprising the above-described cleaning device, preliminary drying device and drying device, and a subsequent drying method will be described. .

A: Washing step (1) First, with the drainage valve (drainage valve) 44 and the product outlet 40 of the drainage port 42 closed, the reaction solution (suspension: object to be treated) is washed in the washing tank ( (Treatment tank) 28. At this time, although not necessary, the reaction solution may be charged while air is supplied from below the filtration porous plate 36 and the filtration porous plate 36 is vibrated (vibrated). By this air supply and vibration, the homogeneity of the suspension is easily maintained. At this time, the amount of supplied air and the amplitude of vibration vary depending on the type of the object to be treated (suspension) and the input amount. For example, when the input amount is 500 L, 50 L / min, amplitude: 8 mm or less, frequency ( Rotational speed): 500 to 2000 min ⁻¹ . The same applies hereinafter.

  (2) Next, the above air supply and vibration are stopped, and partial liquid removal is performed through the perforated filter plate 36. This liquid removal is usually performed by differential pressure. That is, if the lower surface side chamber of the filter porous plate 36 is decompressed through the suction port 45 by the suction pipe, the suction and drainage can be performed. Naturally, the upper chamber (the cleaning zone F side) of the perforated filtration plate 36 of the cleaning tank (processing tank) 28 may be pressurized. At this time, air supply may be intermittently performed. The powder in the suspension is pulled downward by the differential pressure, and clogging of the perforated filter plate 36 is less likely to occur.

  Then, partial liquid removal is performed until the residual liquid is in a state that can be fluidized by vibration (vibration) of the perforated plate and is in a state where the concentration is as high as possible. The solid content concentration at this time varies depending on the type (material, particle size, etc.) of the powder material. For example, in the case of toner (organic pigment), it is about 5 to 40%, preferably 25 to 30%.

  (3) Next, the third step of forming the powder-containing liquid layer F by replenishing the cleaning tank 28 with cleaning water (cleaning liquid) while blowing and vibrating again is performed. This is for uniformly mixing the washing water and the residual liquid. At this time, the addition amount of the washing water with respect to the remaining liquid amount varies depending on the type of powder, but is usually 1 to 4 times the volume.

  (4) Subsequently, the flow cleaning in the first step is performed by continuing the air blowing and the vibration. The cleaning time at this time is, for example, several minutes to 60 minutes.

  (5) After the fluid cleaning in the first step, the partial drainage in the second step is performed again. The steps (3) replenishing the cleaning solution (third step), (4) cleaning (first step), and (5) partial liquid removal (second step) are repeated the required number of times (usually 2 to 5 times). After confirming the completion of cleaning based on electrical conductivity (unreacted deposits or the like usually have electrical conductivity), etc., partial liquid removal is performed to obtain a cleaned powder-containing liquid (slurry). The solid content concentration of the washed slurry is also about 5 to 40%, preferably 25 to 30%, as described above.

  This washed slurry (suspension) may be used as it is as a drug, industrial material, or product depending on the type of powder.

B: Drying step In this drying step, final drying (secondary drying) using a vibration fluidized drying apparatus is usually performed after preliminary drying (primary drying). When trying to obtain a target dry product (final dry product) with a predetermined moisture content or less in only one stage using a vibration fluidized drying device, there is a lot of moisture, so the powders are closely packed by vibrational flow and difficult to disintegrate. This is because a clay-like mass is formed. In addition, in the case of vibration fluidized drying, when a lump (lumps) due to vibration condensation is not formed, a preliminary drying step is not necessary. Furthermore, vibration fluidized drying is suitable for products with a low moisture content (dried products). If a product with a low moisture content is not required, use a general-purpose drying device for preliminary drying. A dry product may be obtained.

(1) Pre-drying (primary drying):
The washed liquid (slurry) is opened in the valve 60 of the product outlet 40 and hot air is fed into the air feed port 68 while being continuously fed into the feed port 64 of the predrying device 62. Then, dry the water-containing powder while winding it up with an air stream. The pre-dried product that has been pre-dried by the airflow is sucked by the air exhaust device 88, transported through the dry product transport duct 90, collected by the cyclone 82 of the pre-dried product recovery device 80, and collected in the pre-dried product recovery tank 84. The The water content of the pre-dried product at this time varies depending on the type of powder, but in the case of toner (organic pigment), it is about 30% or less, preferably about 20% or less.

(2) Final drying (secondary drying):
The preliminary dried product (primary dried product) is further subjected to final drying using a vibration drying device 92. This final drying may be performed using the washer 22 while changing the operating conditions.

  After supplying the pre-dried product into the treatment tank 94 of the vibration drying device 92, hot air is fed through the hot air pipe 100, and the pre-dried product is put into the processing tank 94 under reduced pressure by the suction pipe 108. At this time, the hot air temperature and the degree of reduced pressure vary depending on the type of the powder, but do not affect the powder and vary depending on the required dryness, for example, 30 to 100 ° C. and 5 to 50 Pa.

  Thus, by operating the vibration drying apparatus 92 for a required time (for example, 2 to 4 hours), the moisture content is about 5% or less, preferably about 0.5% or less.

  Here, instead of the vibration drying device 92, the vibration flow treatment device M used as a cleaning device may be used.

  Furthermore, depending on the type (material / diameter) of the powder, the cake obtained by eliminating the pre-drying and directly drying or dehydrating with a dehydrator (filter press, centrifuge, etc.) instead of the pre-drying. May be finally dried.

Next, examples carried out for confirming the effects of the present invention will be described. In addition, each Example was performed on a pilot machine with a pilot machine, and when applied to an actual machine, the operating conditions may vary.

<Example 1>
The object to be cleaned (object to be treated) of this example was a synthetic organic pigment-containing liquid (solid content concentration of about 20%) having an average particle diameter of 4 μm. The purpose of washing in this embodiment is mainly to remove impurities such as unreacted substances adhering to the synthetic organic pigment.

  As the cleaning device and fluidized drying device used, a vibration fluidizing device “UVA type” manufactured by Chuo Kakoki Co., Ltd. having the following specifications was used.

Filtration perforated plate 36: Material Sintered stainless steel, thickness 15mmt, unit pore diameter 5μm,
Air flow rate 10L / (min · cm ² ) (200mmH ₂ O)
Washing tank 28: inner diameter 210 mmφ × filtration perforated plate height 600 mm
Vibration motor 30: output 0.2kW × 2 units, blower 48: output 0.75kW,
Ventilator 58: Output 0.75 kW
1) 2.5 kg of the object to be cleaned (slurry) was put into the cleaning tank 28. At this time, normal air supply and vibration were omitted.

  2) After charging, the drain valve 34 is opened, the exhaust port 39 is used as a pressurizing port, and a partial drainage is performed using a compressor (not shown) for 60 minutes at a pressure of 98 kPa (drainage amount: 1.2 kg). Went. At this time, the air supply usually performed intermittently was also omitted.

3) About 1.2 kg of cleaning water (pure water) is added to the remaining liquid after partial drainage, air supply conditions: normal temperature, air flow rate 50 L / min, vibration conditions: amplitude 2 mm, frequency 1500 min. Washing for 60 min (fluid) was performed under the condition of ^-1 . And the partial liquid removal was carried out by pressurization of the upper processing chamber under the same conditions as above (liquid removal amount: 1.2 kg). This was repeated three times, followed by dehydration to finish the washing step (treatment), and a slurry (water content 100%) as a washed product was prepared.

  4) The slurry is continuously charged (0.5 kg / h) into a drum dryer having the following specifications, preliminarily dried under the conditions of a drum temperature of 40 ° C. and a vacuum degree of 50 torr, and a moisture content of about 2%. A pre-dried product was obtained.

<Vacuum drum dryer>
Drum: Cylindrical (200mmφ × 200mmL) × 2, Body motor: 0.4kW, Vacuum pump: 0.75kW
5) Using the vibration-flow treatment device ("UVA type") of the same specification that used the pre-dried product (water content about 2%) for cleaning, air supply: hot air temperature 40 ° C, hot air volume 240L / min, Excitation: Amplification 2 mm, frequency 1500 min ⁻¹ , bath heating: jacket temperature 40 ° C., drying was performed for about 60 min. As a result, a final dry product of about 0.27% was obtained.

<Example 2>
In this example, the object to be treated was a metal oxide (copper oxide, average particle size 4 μm) produced by chemical synthesis. The purpose of cleaning in this embodiment is mainly to remove the acid adhering to the synthetic metal oxide.

  In the cleaning method of Example 1, a mixture of 2 kg of cleaning water with respect to 0.5 kg of the object to be treated is put into the cleaning tank 22, and after washing under the same conditions, the steps of partial liquid removal and cleaning water replenishment are repeated. A slurry (water content 97.5%) was obtained. At the time of this charging, as in Example 1, air supply and vibration were omitted.

The slurry thus obtained is directly passed through the washing tank (treatment tank) 28 without being subjected to a preliminary drying step. Air supply: hot air temperature 130 ° C., hot air volume 50-100 L / min, vibration: amplitude 2 mm, vibration Drying was carried out for about 120 minutes under the conditions of several 1500 min ⁻¹ , bath heating: jacket temperature 130 ° C. As a result, about 5% of the final dried product was obtained.

<Example 3>
The object to be cleaned (object to be treated) of this example was a synthetic organic pigment-containing liquid (solid content concentration of about 20%) having an average particle diameter of 5 μm. The purpose of cleaning in this example is to remove impurities such as unreacted substances adhering to the synthetic organic pigment, as in Example 1.

  Using the same vibration flow treatment apparatus as in Example 1, washing treatment was performed under the same conditions to obtain a washed product (slurry) (water content 70%).

The washed product was preliminarily dried using an air dryer (pipe diameter: 160 mmφ) under the conditions of hot air temperature: 80 ° C., hot air volume: 192 m ³ / min, jacket temperature: 80 ° C. As a result, the moisture content of the pre-dried product was 10.18%.

  The preliminary dried product (water content at the start of treatment: 16.8%) was subjected to final drying for 230 minutes under the same conditions using the same vibration flow treatment apparatus as in Example 1. The reason why the moisture content at the start of the treatment of the pre-dried product is high is that after pre-drying, water was absorbed (moisture absorption) for standing in the air.

  As a result, a final dry product of about 0.23% was obtained. For reference, the water content / drying time relationship in the final drying treatment is shown in FIG.

It is a flowchart which shows an example in the past of the washing | cleaning method of the powder (organic pigment) contained in the reaction liquid (suspension) after organic pigment synthesis. It is a flowchart which combined the washing | cleaning apparatus and pre-drying apparatus which are used for the washing | cleaning and drying method of this invention. It is the schematic which shows an example of the vibration fluidized drying apparatus used for the secondary drying of the washing | cleaning and drying method of this invention. 6 is a graph showing the relationship of moisture content / drying time in the final drying process of Example 3. FIG.

Explanation of symbols

22 Washing machine (liquid processing machine)
24 Aeration piping 26 Exhaust piping 28 Cleaning tank (treatment tank)
30 Vibration motor (vibration means, oscillator)
36 Filtration perforated plate (dispersion plate)
38 Object to be cleaned (raw material) / cleaning liquid (cleaning water) inlet M Cleaning device (vibration flow treatment device)

Claims (7)

Powder is obtained using an oscillating flow treatment apparatus comprising a perforated plate in a treatment tank, a vibration means for vibrating the perforated plate, and an air feeding means capable of feeding air from below the perforated plate. A method of cleaning,
1) A powder-containing liquid layer containing the powder in a cleaning liquid is formed on a filtration porous plate, and air is fed from below the filtration porous plate and the filtration porous plate is vibrated to obtain a powder. A first step for cleaning, 2) a second step for partially draining through the filter perforated plate after the first step, and 3) when the first step is performed again, after the second step. A powder characterized in that a cleaning process comprising a third step of replenishing a residual liquid (hereinafter referred to as “residual liquid after deliquidation”) to form the powder-containing liquid is repeated a required number of times. How to wash your body.   The powder is fed from below the perforated plate and while the perforated plate is vibrated, and then the cleaning liquid is fed while continuing the air and vibration. The method for cleaning powder according to claim 1. Using a vibration flow treatment apparatus provided with a perforated plate in the treatment tank, and provided with a vibrating means for vibrating the perforated plate and an air feeding means capable of feeding air from below the perforated plate, A method for washing the body,
The powder is a synthetic fine powder contained in a reaction liquid containing a synthetic fine powder after a synthetic reaction,
After the reaction solution is put into the treatment tank, it is partially drained through the perforated plate, and a washing liquid is supplemented to the residual liquid after the partial drainage to form a powder-containing liquid layer. 1) A first step in which air is fed from below the perforated plate and the perforated plate is vibrated and washed. 2) After the first step, a second liquid is partially drained through the perforated plate. Step 3) When the first step is performed again, the residual liquid after the second step (hereinafter referred to as “residual liquid after draining”) is supplemented with a cleaning liquid to form the powder-containing liquid layer. A method for cleaning powder, characterized in that the cleaning step comprising the third step is a method of repeating the required number of times.   The method for washing powder according to claim 1, 2, or 3, wherein, in the partial liquid removal in the second step, air is intermittently fed from below the perforated plate.   The residual liquid after the liquid removal is in a state that can be fluidized by vibration of the perforated plate and has a concentration as high as possible, and replenishment of the cleaning liquid in the third step is performed. The method for washing powder according to any one of claims 1 to 4, wherein the after-residue is fluidized.   The attachment part of the filtration porous plate is removable from the treatment tank main body, and is a treatment tank divided body provided with a discharge port whose lower end is located below the upper surface of the filtration porous plate. Item 6. The method for washing powder according to any one of Items 1 to 5.   Washing and drying of a powder, wherein the washed powder-containing liquid obtained by the washing method according to any one of claims 1 to 6 is subjected to preliminary drying by fluidized drying treatment after preliminary drying or liquid removal Method.

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