JP6457832B2 - Flushing method and apparatus - Google Patents

Description

  In the present invention, water in a water filtration cake (filter cake, water-containing cake, press cake, etc., particles containing about 50 to 80 percent water) containing an organic pigment, which is a solid / liquid processing material, is subjected to a flushing method. The present invention relates to a flushing method and apparatus for producing a colorant having excellent dispersibility by replacing with a lipophilic resin or an organic solvent solution thereof.

  Conventionally, when producing a printing ink, it has been required to enhance the coloring effect of the pigment by dispersing the pigment in an organic medium such as an oil varnish. As a method for dispersing the pigment, after drying the pigment in advance, a dry method in which the dry powder pigment is dispersed in an organic medium, a water-containing cake containing pigment particles and an oily varnish are charged into a flasher, and the mixture is kneaded to form an aqueous phase. There is known a flushing method in which water-based pigments are transferred (flushed) to oil-based pigments to separate and remove water. The basic process of flushing is to move the water phase pigment to the oil phase system and separate the water, so that the vehicle is oily and that the pigment particle surface is lipophilic. is necessary.

In the above dry method using dry powder pigment, the pigment containing nearly 50% air in the dry state causes strong agglomeration during the drying process, so that it is replaced with an oil-based vehicle to wet the particle surface. However, it is difficult to make the pigment particles sufficiently fine in spite of consuming a large amount of energy in the dispersion process.
On the other hand, in the flushing method, since there is no aggregation of particles due to drying of the pigment, if the pigment particles in the water-containing cake are converted into ink as they are, energy for crushing the particles becomes unnecessary, and organic ink such as printing ink, which is very small particles. It is suitably used for the production of colorants such as pigments and developing toners for copying machines.

  As described above, in the case of ink production by the flushing method, the drying-grinding process of the final process in the pigment production process can be omitted, and no manual labor is required in the kneading process during the ink production process, saving labor and energy. It is regarded as important as an ink manufacturing method. Generally, as a flasher used in the flushing method, a kneader type flasher such as a heating vacuum kneader is used (see, for example, Patent Document 1). The kneader is equipped with two blades such as a Σ (sigma) blade that extends in the horizontal direction in a trough (trough shell, kneading tank) that can be tilted, and these two blades rotate around a horizontal axis. So that the material thrown into the trough is kneaded by applying shear stress between the blade and the bottom of the trough, etc., so that water generated from the treatment material accompanying kneading is removed from the upper opening by tilting the trough It is configured. The two blades must be rotatably supported by four shaft sealing devices provided at both ends on the side wall of the trough, so that contamination caused by the treatment material coming into contact with the shaft sealing portion The problem cannot be avoided. Therefore, there is a tendency to install a dedicated machine for each color of pigment to prevent contamination, and to process it in a mass production method. Necessary power to drive was needed. Based on the above, it is also said that kneader type flashers are not suitable for producing printing ink with a small turn. Furthermore, the kneader has a problem that it takes a long processing time because there are few opportunities to apply a shear stress to the processing material in the trough.

JP-A-9-188846 (Summary, paragraph 0004)

  The problem to be solved by the present invention is that it can be applied to the production of printing inks and the like having a small turning size and a small lot size as described above, there is no risk of contamination, and solid / liquid processing materials and oleophilic resins or organic materials thereof. It is an object of the present invention to provide a flushing method capable of uniformly kneading a solvent solution with high viscosity and transferring an aqueous medium to an oil medium in a short time and an apparatus used therefor.

  As described above, in the case of a kneader type flasher, two blades are provided horizontally in the trough and both ends are supported by a shaft sealing portion provided in the trough, resulting in a problem of liquid contact at the shaft sealing location. ing. Therefore, in order to prevent such a problem from occurring, a blade (can, container, stirring tank) for storing the processing material and the blade are separated from each other, and a blade that prevents the processing material from coming into contact with the shaft seal portion is used. By using a so-called change can system that replaces the tank each time it is used for processing, the shaft seal problem is solved. Further, in order to efficiently perform the kneading action by the blades, the plurality of blades may be moved uniformly throughout the tank so as to be kneaded.

  In view of the above, according to the present invention, a flushing method in which a solid / liquid processing material and a lipophilic resin or an organic solvent solution thereof are kneaded and the processing material is transferred from an aqueous phase system to an oil phase system to separate water. , The processing material and the lipophilic resin or its organic solvent solution are put into a tank, and a plurality of frame-type stirring blades rotating and revolving in the tank are lowered from above the tank, and the frame-type stirring blades are moved in a planetary motion. A flushing method is provided, characterized by kneading and collecting the kneaded material into a columnar shape in the tank, and when separated water is generated, the frame type stirring blade is raised from the tank, and the tank is tilted to drain the separated water. Preferably, the flushing method is characterized in that the frame type stirring blades are three torsional frame type stirring blades that perform planetary motion in directions in which the rotation direction and the revolution direction are different.

  In the flushing method of the present invention, an oily varnish is placed in a tank as an organic solvent solution, a water-containing cake containing 20-30% of an organic pigment is added as a solid / liquid processing material, and a frame-type stirring blade is rotated in the tank. When revolving and kneading, water precipitates as described above and gradually becomes clear. At this point, the agitating blade is pulled up to discharge water from the tank.According to the present invention, the tank is slightly inclined by providing drainage valves (insert plugs) on the middle side surface and bottom side surface of the tank. There is provided a flushing method in which water can be drained simply by doing so.

After draining as described above, the frame-type stirring blade is lowered into the tank, kneaded to separate the water, and the operation of draining is repeated. Next, oil varnish is added, the tank is covered with a closed hood, the inside of the tank is decompressed and heated around the tank with a jacket, the temperature of the kneaded product is raised to 60 ° C. Drain the water to finish the oil-based ink. At this time, the gas condenses will water droplets due to the temperature difference between the outside air to the inner surface of the closed hood, also adhering moisture also condensed to the rotor outer surface of the stirring blade located within the sealed hood becomes water droplets, into the tank There is a risk of falling. When such water is generated, the processing time is prolonged. Therefore, according to the present invention, a heating device such as a band heater is provided on the outer surface of the sealed hood so as not to cause the gas condensation in the sealed hood. The flushing method is provided in which the inside of the hood is heated. Further, according to the present invention, a flushing device having the above-described configuration for use in the flushing method is provided.

  The present invention is configured as described above, in a flushing method in which a solid / liquid processing material and a lipophilic resin or an organic solvent solution thereof are kneaded and the processing material is transferred from an aqueous phase system to an oil phase system to separate water. The processing material and the lipophilic resin or its organic solvent solution are put into a tank, and a plurality of frame type stirring blades rotating and revolving in the tank are lowered from above the tank, preferably three twisted frame type stirring blades The kneaded mixture is moved in a planetary direction in a direction different from the rotation direction and the revolution direction, and the kneaded material is combined into a columnar shape in the tank. When separated water is generated, the frame-type stirring blade is raised from the tank, and the tank is tilted to drain the separated water. As a result, there is no shaft seal that causes a liquid contact problem around the tank, and there is no contamination problem as in the conventional flushing method using a kneader type flasher. . Further, since it is sufficient to replace the tank for each process, it is possible to suitably cope with production of printing ink with a small lot size. In addition, since a plurality of frame-type stirring blades move in a planetary motion within the tank, the processing material is repeatedly subjected to shear stress between each stirring blade and the edge of the stirring blade and between the edge of the stirring blade and the inner wall of the tank, thereby reliably kneading. This kneading action is performed uniformly in the tank as a whole by rotation and revolution, so that kneading can be carried out in a shorter time compared to conventional kneader-type flashers, and flushing can be performed at an early stage.

  Further, by providing drainage valves (insert plugs) on the middle side surface and bottom side surface of the tank, the tilt angle of the tank when draining water can be reduced, and workability is good. In addition, if a heating device such as a band heater is provided on the outer surface of the sealed hood, the inner surface of the sealed hood itself and the outer surface of the rotor of the stirring blade located in the sealed hood can be heated so that the gas in the hood does not condense. The dripping of water can be prevented and flushing can be completed early.

The front view which shows one Example of this invention and shows a tank part in cross section. Explanatory drawing which shows the state which the stirring blade rotated and revolved in the direction which is different in a tank. Expansive explanatory drawing of the drain valve part.

  The present invention kneads a solid / liquid processing material and an oleophilic resin or an organic solvent solution thereof, separates water from the aqueous phase processing material and moves to an oil phase system to add a colorant such as ink or toner. Although it can be applied suitably to the flushing operation to manufacture, the flushing method in the manufacturing process of the printing ink which manufactures oil-based ink by isolate | separating water from the water-containing cake containing an easily dispersible organic pigment is demonstrated below.

  FIG. 1 shows an apparatus used in the flushing method of the present invention, which basically has a configuration in which a planetary mixer has a flasher function. In FIG. 1, the main body 1 includes a stirring head 3 that moves up and down by a lifting cylinder 2 and a tank (container, stirring tank) 4 that is positioned below the stirring head 3. In the figure, the agitation head 3 is configured to move up and down. However, the agitation head 3 may be fixed and the tank 4 may be moved up and down so as to be relatively close and disengaged (not shown). . The agitation head 3 is provided with a plurality of agitation shafts 7 extending in the tank direction in communication with a drive shaft 6 driven by a drive means 5 such as a drive motor. The agitation shaft rotates and revolves by a planetary motion mechanism provided in the rotor 8, and the frame-type agitation blade 9 attached to the lower end of the agitation shaft 7 performs a planetary motion in the tank 4 as a whole. In FIG. 1, two twisted frame type stirring blades are illustrated as stirring blades so as not to complicate the drawing, but this number can be two, three, or a plurality of others. As shown in FIG. 2, an apparatus having three stirring blades can be suitably used. As the frame type stirring blade, a twisted frame type stirring blade having a shape in which the vertical side is twisted so that the positions of the upper side and the lower side are located in different directions is used, but a simple frame type stirring blade can also be used. As shown in the figure, the planetary motion mechanism can be variously configured. In the case of a three-axis mixer having a locus in which rotation and revolution rotate in different directions, as shown in the figure, the three stirring shafts 7 revolved by the drive shaft 6 A planetary gear (not shown) is provided at each upper end, and a sun gear (not shown) having an internal gear is provided on the outer periphery of the planetary gear so as to mesh with the planetary gear so that the stirring blades rotate in the direction opposite to the revolution direction. The internal gear (internal gear) system. In the internal gear system, since the gear meshing portion with the sun gear is located outside the planetary gear provided on the stirring shaft, the planetary gear and the sun gear provided on the stirring shaft can be enlarged and kneading with high horsepower is possible. Machine, thereby making it easier to knead the processing material.

  Around the tank 4 is provided a heating jacket 10 through which a temperature adjusting medium such as hot water flows, and a drain valve 13 is provided on the side surface of the tank 4 or the bottom side surface, preferably on both side surfaces. It is. In the embodiment shown in the figure, as shown in FIG. 3, a drain port 11 having one end opened in the tank 4 and extending through the jacket 10 is formed, and a plug 12 is detachably fitted into the drain port 11. It is attached as a drain valve 13 but can have other appropriate configurations. It is preferable that the length of the plug is such that when the drain port 11 is inserted, the inner end thereof reaches the tank inner surface and becomes substantially the same surface. The valve is closed by inserting a gasket 16 between the flange 14 of the insertion plug 12 and the flange 15 of the drain port 11 and fastening the periphery with a clamp 17. The clamp 17 is removed and the insertion plug 12 is removed. It is opened by extracting

  A sealing hood 18 is provided below the stirring head 3 so as to be in contact with the upper edge of the tank 4 so as to seal the inside of the tank. The sealing hood 18 communicates with a vacuum source to vacuum and decompress the tank. A vacuum port 19 is formed. A heating device 20 such as a band heater is provided on the outer periphery of the hermetic hood 18, and the heating device 20 heats the inner surface of the hermetic hood 18 and the periphery of the outer surface of the rotor 8 to prevent gas condensation. It is.

  When the water-containing cake of oil varnish and lipophilic pigment is put into the above apparatus, the frame type stirring blade is lowered, inserted into the tank and rotated planetarily, the frame type stirring blade rotates, so that the edges of the stirring blades are separated. When approaching, and when the edge portion is close to the inner wall of the tank, a shearing stress acts on the processing material and can be kneaded. At this time, in the case of three frame type stirring blades, there are more opportunities to apply shear stress compared to two stirring blades, and the revolution and rotation are made different directions using a twisted frame type stirring blade. Thus, the processing material can be reliably kneaded and kneaded.

By the kneading action, water in the water-containing cake of the lipophilic pigment is discharged, the surface of the pigment is replaced with the oily varnish, and water is gradually precipitated by continuing kneading, and this water gradually becomes clear. In the change can type flushing method, if there is little oil varnish, it becomes whip-like (foam), so if you add a small amount of oil varnish, as shown schematically in FIG. In the case of the two twisted frame type stirring blades, for example, there are six twisted frame type stirring blades that are twisted between the front part of the rotation direction of each twisted frame type stirring blade and the tank wall and between each revolving twisted frame type stirring blade. There is a tendency that the kneaded material 21 is gathered in a substantially columnar body. At this time, when the stirring blade is raised from the tank, the plug is removed, the drain valve is opened, and the tank is tilted slightly, the separated water separated from the water-containing cake can be discharged from the drain valve as described above. . At this time, an appropriate handle or handle may be provided on the outer surface of the tank so that the tank can be easily tilted, or an appropriate tilting device (not shown) that can tilt while holding the tank may be provided. .

  Thereafter, the plug is inserted, the drain valve is closed, the tank is returned to an upright state, the frame type stirring blade is lowered into the tank, and the above kneading and draining operations are repeated. After draining to a certain extent, adding oil-based varnish, heating with a jacket, raising the ink flesh temperature to 60 ° C., and depressurizing operation, the remaining 10-20% water can be extracted, and the sharpness is good Ink can be produced. Further, by heating the interior to 60 ° C. with a heating device provided on the outer surface of the sealed hood, gas condensation can be prevented, and there is no gas condensation on the outer surface of the rotor in the sealed hood, thereby shortening the flushing time. it can.

  According to the present invention, the treatment material is kneaded by the planetary mixer type flashing apparatus as described above, but the rotation speed of the stirring blade is about 50% so that the characteristics of the kneaded material (paste) do not deteriorate due to heat generation during kneading. It is preferable to operate under conditions of 0.2 to 0.5 m / sec and the temperature of the kneaded product (paste) of about 70 ° C. or less. This is because heating at 0.6 m / sec or more increases heat generation, and it is difficult to keep the material temperature at 70 ° C. or less due to material characteristics.

(Example 1)
A tank having a capacity of 15 liters was used, and three torsional frame type stirring blades as shown in FIGS. 1 and 2 were used as stirring blades. Flushing was performed using a three-axis planetary mixer having different revolution and rotation directions. Put a water-containing cake with pigment content of 20-30% and oil varnish in the tank, lower the twisted frame type stirring blade into the tank, heat the tank to 70 ° C with a warm water jacket, raise the ink meat temperature to 60 ° C Kneaded. The precipitated water was drained by raising the stirring blade and tilting the tank. When the above operation was repeated under reduced pressure kneading operation, flushing was possible in 4 hours.

(Example 2)
In addition to the same conditions as in Example 1, a band heater was attached to the outer surface of the sealed hood and heated to 60 ° C. for operation. Although a small amount of condensation was observed outside the rotor, there was no dripping, and there was little condensation of gas adhering to the inner surface of the sealed hood. When three torsional frame type stirring blades are planetarily moved in different directions of revolution and rotation, and kneaded, the treated material becomes whip-like (foam-like), and when a small amount of oily varnish is added there, It was organized in a columnar shape. Then, the drive part was raised, the plug was removed, the drain valve was opened, the tank was slightly tilted and drained. And the tank was returned, the drain valve was closed, the said kneading | mixing was continued, and water was drained in several times. Thereafter, an additional oil varnish was charged, and dehydration finish kneading was performed by heating under reduced pressure under a vacuum of -0.08 to -0.09 MPa (Pe). Finally, oily varnish was added and finish kneaded. In this way, oil ink with good sharpness could be obtained after driving for 2.5 hours.

Comparative example

  The same oily varnish and water-containing cake as in Example 1 were put into a kneader-type flasher, and the two blades were rotated in the trough as in the past, and flushing was performed. The gland packing composed of the five rings constituting the sealing part was contaminated, and even if it was operated for 5 hours and flushing was completed due to the influence, the sharpness of the oil-based ink was insufficient. Further, when the colorants having different colors are processed with the same trough, it is necessary to replace all the gland packings of the shaft seal portion of the blade, which requires cost for parts and takes time for the replacement work.

  As described above, a plurality of frame-type stirring blades, in particular, three frame-type stirring blades rotate and revolve in different directions in the tank to obtain a water-containing cake containing an organic pigment as a solid / liquid processing material and an oily varnish. When kneaded, the problem of contamination due to liquid contact such as a conventional kneader-type flasher is solved, and processing can be performed in a short time. If a drainage valve is provided in the tank, the tank can be drained by tilting the tank slightly when draining, and a heating device such as a band heater is provided on the outer surface of the sealed hood to heat the hood or the outer surface of the rotor of the stirring shaft. The gas is less condensed and can be flushed in a shorter time without the need for drainage.

DESCRIPTION OF SYMBOLS 1 Main body 2 Lifting cylinder 3 Stirring head 4 Tank 8 Rotor 9 Stirring blade 10 Jacket 11 Drain port 12 Plug plug 13 Drain valve 18 Sealing hood 19 Vacuum port 20 Heating device 21 Kneaded material

Claims (6)

In a flushing method in which a solid / liquid processing material and a lipophilic resin or an organic solvent solution thereof are kneaded to transfer the processing material from an aqueous phase system to an oil phase system to separate water , a tank having a jacket, A sealed hood that is hermetically sealed under reduced pressure, and a heating device provided on the outer periphery of the sealed hood to heat the inside of the sealed hood, are charged with a treatment material and a lipophilic resin or an organic solvent solution thereof, The frame-type stirring blades that rotate and revolve in the tank are lowered, the tank is heated with a jacket and sealed with a sealed hood, the inside of the sealed hood is heated, and the frame-type stirring blades are planetarily moved and kneaded. Then, the kneaded material is collected in a columnar shape in the tank, and when separated water is generated, the frame type stirring blade is lifted from the tank, the tank is tilted to drain the separated water, and then the decompression operation is performed .   2. The flushing method according to claim 1, wherein the frame type stirring blades are three twisted frame type stirring blades, and perform planetary movement in directions different in rotation direction and revolution direction.   The flushing method according to claim 1 or 2, wherein a drain valve is provided on a side surface of the tank. A stirring head and a tank provided so as to be relatively close to and away from each other are provided. The stirring head is provided with a plurality of stirring blades that revolve and rotate in the tank, and a heating jacket and a tank in the tank are provided on the side of the tank. A drainage valve for draining water is formed, and a sealing hood having a vacuum port connected to a vacuum source is provided below the stirring head and in contact with the upper edge of the tank so as to seal the inside of the tank under reduced pressure. A flushing device characterized in that a heating device for heating the inside of the hood is provided.   The flushing device according to claim 4, wherein the stirring blades are three torsion frame type stirring blades, and the revolution and rotation make planetary motions in different directions. The drain valve has one end includes a drainage port which opens into the tank, the attachment plug tip is inserted into the exhaust water outlet reaches the inner surface of the tank, the claims are provided in the intermediate portion side surface and or bottom side of the tank 5. The flushing device according to 4 .

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