WO2019026208A1 - Dispersing machine, method for dispersing particles in slurry and emulsion production method - Google Patents

Abstract

The present invention relates to a dispersing machine, wherein a rotor 8 that has the form of an impeller is disposed inside a cylindrical vessel and by introducing a slurry, in which particles have been mixed into a solvent, into the cylindrical vessel in which beads have been filled and rotating the rotor 8, the particles in the slurry are dispersed and comminuted. In order to increase the dispersion rate and reduce the destruction of primary particles, the length L of the rotor 8 in the axial direction and the diameter D are set such that the ratio L/D for the rotor is 0.3-1.6.

Description

Dispersing machine, method of dispersing particles in slurry, and method of producing emulsion

The present invention relates to a disperser for grinding and dispersing agglomerated particles in a suspension (hereinafter referred to as a slurry) in which solid or liquid particles are dispersed in liquid, and particles in the slurry by the disperser. And a method of producing an emulsion.
The term “dispersion” as used in the present invention means that secondary particles formed by aggregating several to several tens of primary particles consisting of single crystal particles and amorphous particles are separated and separated in a solution. In other words, in the present invention, pulverization refers to the decomposition of a single particle into a plurality of particles.

The conventional dispersing machine performs dispersion, pulverization and bead separation simultaneously in the separator structure, which is divided into a part that performs stirring for dispersion and pulverization, a separator part that separates dispersion and pulverization beads, and a separator structure. was there. As a disperser of the former apparatus division, for example, a wet ball mill shown in Patent Document 1 below is disclosed. In this apparatus, a cylindrical container filled with beads, and a stirring blade and a separator disposed coaxially with the container in the cylindrical container and fixed to a shaft driven by a motor as a driving source, a stirring blade Has a dispersing and crushing function, and the separator is in the form of an impeller consisting of a disc-like disc fixed on the upper and lower sides of the shaft and stirring blades connecting the upper and lower discs at a constant interval in the circumferential direction ing. The slurry is introduced into the container filled with beads for grinding and dispersion, and the stirring blades and the separator are rotationally driven to disperse and grind particles in the slurry to make the particles finer. At this time, the slurry in which the beads are separated by the action of centrifugal force is moved from the outer peripheral end of the separator to the inner peripheral end from the outer peripheral end of the separator and discharged through the hollow shaft of the shaft. Produce a slurry.

Further, Patent Document 2 is a crusher suitable for dispersion / crushing in the prior art, which corresponds to the disperser of the latter device classification. In this device, there is disclosed a crusher in which both the cylindrical container and the separator have large diameters and the axial length L is smaller than the diameter D and the ratio (L / D) thereof is small. Further, Patent Document 3 is a disperser of the former device section, but is structurally similar to the disperser of the latter device section, and is an invention in which a disc of a partition plate is inserted between upper and lower discs. In the lower chamber, dispersion and pulverization by stirring are performed, and in the uppermost stage, beads are separated and dispersed and pulverized.

The dispersing machine also disperses agglomerated particles in the slurry using the shear force generated in the gap between the cylindrical container and the cylindrical member when the cylindrical member in the closed cylindrical container rotates at high speed. There are devices that For example, in the invention disclosed in Patent Document 4 below, there is a stirrer at the bottom of the apparatus, which disperses secondary particles in which primary particles are aggregated. In order to carry out the dispersion efficiently, hard particles (beads) having a diameter of about 0.05 to 0.5 mm are mixed in the slurry. The slurry which has been dispersed is separated into beads by the upper separating device.

Patent Document 5 below discloses a similar dispersing machine, and in this document 5, asperities may be formed entirely or partially on one or both of the inner peripheral surface of the cylindrical container and the outer peripheral surface of the cylindrical member. , Is also described.

Oil emulsions are also used in cosmetic emulsions, food products, etc., in which fine droplets of oil are suspended in water, and the diameter of oil droplets is generally 0.5 to 10 μm. . In order to industrially produce an emulsion of several μm, it is treated with a vacuum stirring vessel etc., but it is a badge type treatment, and it is necessary to carry out a pre-mixing treatment in the previous step, and bubbles are removed from the emulsion after treatment. It was necessary to remove it, and it was necessary to install the storage tank which holds it and the device for liquid transport. As a result, there is a problem that the process becomes complicated and the processing cost and equipment cost increase. Therefore, a device capable of continuous processing with a simple device has been desired.

JP 2008-253928 A Japanese Patent Application Publication No. 2003-144950 JP 2002-143707 A Patent No. 3703148 JP 2008-238005 A

The disperser described in Patent Document 1 has both a stirring blade and a separator, which makes the apparatus complicated and expensive to manufacture. Furthermore, due to the structure, the position of the blade of the separator is close to the rotation axis and is short, there is a problem that the separation performance is deteriorated. In order to cope with this, the installation density of the separator blades is increased, but as a result, there is a problem that the slurry passage cross-sectional area is reduced, the amount of slurry processing decreases and the slurry feeding power increases.

In addition, in the latter type of apparatus section of the type in which both dispersion / crushing and bead separation processes are performed at the separator position, the ratio of the diameter D of the separator to the axial length L as seen in the example of Patent Document 3. When L / D is large, dispersion of bead concentration in the slurry of the container becomes large in the direction of the rotation axis. As a result, the insufficiently dispersed particles and the particles in which the particles are excessively destroyed are mixed, and there is a problem that it is impossible to obtain a slurry in which the particle diameters are uniform and uniformly dispersed. In particular, in the case of a highly viscous slurry, this phenomenon was remarkable.

The final product using particles obtained from such a slurry has the following problems. For example, in the case of a dielectric manufactured by sintering of an oxide, the variation of the crystal particle diameter in the sintered body becomes large, and there is a problem of the local abnormal dielectric constant decrease due to the enlarged particle. Further, in the case of coloring materials such as ink, there is a problem that color uniformity can not be ensured.

Therefore, as described in Patent Document 2, it is effective to make the above L / D small and perform uniform processing over the entire area of the separator. However, this device also has a processing problem. If the diameter of the separator is increased in order to increase the processing amount, the difference between the centrifugal force in the portion near the separator outer periphery and the centrifugal force in the portion near the center becomes too large. In the outer peripheral portion, there is a problem that the partition plate entraps the beads and the bead mixing rate is deteriorated.

For this reason, as in the device described in Patent Document 2, the main object is to agitate the outer peripheral portion of the separator, and a device in which the length of the blade in the separator diameter direction is short is invented. However, as a result, there is a problem that the dispersion effect is reduced and bead separation is insufficient. In addition, therefore, the dispersion was insufficient and the product was contaminated with many beads. Moreover, the blade length of the separator is too short, the bead separation efficiency is poor, and there is a problem that impurities are mixed in the product slurry.

In order to cope with this problem, in the case where the container and the separator are vertically elongated, as disclosed in Patent Document 3, the invention of inserting the disc of the partition plate between the upper and lower discs is made. However, in this apparatus, the slurry is processed by sequentially passing through the chambers divided by the partition plate, and there is an advantage that the residence time is long, but there is a problem that the apparatus becomes large and a problem that excessive pulverization occurs. The In particular, in the case of a highly viscous slurry, the flow of the slurry was complicated and sufficient processing could not be performed.

The disperser of particles in the conventional slurry also has the following problems. In the efficient disperser described in Patent Document 4, since particles are used for stirring, the particle dispersion is good, but there is a problem that the primary particles are crushed together with the dispersion. There is no problem in the processing in which the crushing and the dispersion are simultaneously performed, but in the case of the processing of the raw material for which the crushing of the primary particles is to be minimized, there is a problem that the damage to the primary particles is large. In addition, there is also a problem that fragments of the beads for grinding mix into the product slurry.

On the other hand, the device described in Patent Document 5 is a dispersion device that does not use beads. The idea was to simply disturb the flow of the slurry between the rotor and the cylindrical vessel in order to apply a shear force to the slurry. Therefore, it was not sufficient as a distributed function. Although it was thought that it would be better to add dimple-like irregularities to the surface of the cylindrical container or rotor for this improvement, the appropriate design was not made regarding this, so it is said that it is sufficient to simply apply the irregularities. It is an idea, and sufficient shear force could not be formed. Therefore, although the damage to the primary particles in the dispersing process is small, there is a problem that the dispersing function is small.

Moreover, in such a device, there is also a problem that the slurry is heated by the friction caused by the shear force between the cylindrical container and the rotor. In the device of Patent Document 5, as described above, since the device was not designed to generate a sufficient shear force, the frictional heat was small, and the technical means to cope with the slurry cooling was insufficient. In this device, since it was thought that heat was merely dissipated, the heat dissipation was insufficient, and the peripheral speed of the rotor could not be increased.

The first object of the present invention is to optimize L / D, and to achieve uniform dispersion of secondary particles in the slurry without lowering the productivity by optimizing the installation conditions of the separator blade. It is an object of the present invention to provide a disperser capable of improving product characteristics and a method of treating fine particles in a slurry by the disperser.
Another object of the present invention is to provide a disperser capable of uniformly dispersing secondary particles without destroying primary particles even with highly viscous fluid, a method of dispersing particles in a slurry, and a method of producing an emulsion. It is a thing.

According to the present invention, a rotor fixed to a rotating shaft coaxially installed with the cylindrical container is disposed inside the cylindrical container, and a shear force is generated in a gap formed between the cylindrical container and the rotor. And treating the slurry.

In a preferred embodiment, a hollow shaft 7 having a hollow space for slurry discharge disposed coaxially with the cylindrical container and rotating in the cylindrical container, a shaft 6 coaxial with the hollow shaft 7, and the shaft 6 , And the rotor 8 rotates in a cylindrical vessel including partition plates 9 which are arranged radially or eccentrically at a suitable interval in the circumferential direction, and the It is a dispersing machine which forms a slurry path through which the slurry supplied from the slurry supply port 13 provided is discharged from the hollow portion of the hollow shaft 7 to the outside of the apparatus through the space between the partition plates 9. The ratio L / D, which is the ratio of the diameter D of the circle in contact with the outer peripheral end of the shaft to the axial length L of the rotor 8, is 0.3 to 3.2.

In another preferred embodiment, a rotor 25 having a concavo-convex outer peripheral surface coaxial with the cylindrical container is installed in a cylindrical container consisting of the cylindrical body 22, the upper lid 23 and the lower lid 24. A shear flow generation gap 28 formed between the inner surface and the outer peripheral surface of the rotor 25 forms a slurry passage, and is provided at the raw material slurry inlet 27 provided on one end side of the cylindrical container and the other end side of the cylindrical container. Product slurry outlet 29 and a driving device for driving to rotate any one of the cylindrical container and the rotor 25 to cool the cylindrical body 22 with liquid, and the inner peripheral surface of the cylindrical body 22 and the rotor The unevenness is formed on the outer peripheral surface of 25 and the depth of the depressions of the unevenness is made deeper than 1 mm or 0.5 times smaller than the shear flow generation gap 28 and the shear flow generation gap 28 is 0.6 And 4mm.

In the present invention, by making the configuration of the disperser appropriate, it is possible to obtain a product slurry in which the secondary particles are decomposed and the primary particles are uniformly dispersed in a state in which primary particle breakage in the slurry is small. It is possible to reduce the ratio of beads in the slurry after treatment. In addition, it also becomes possible to disperse fine particles in a highly viscous slurry that could not be processed by conventional dispersers. The disperser of the present invention is effective particularly for a high viscosity slurry of 500 mPa · s or more containing particles of 0.5 micrometer or less. Furthermore, in the present invention, by using the disperser of the preferred embodiment, it is possible to stably realize processing with a high dispersion rate and less primary particle breakage.

By using the dispersing machine of another preferred embodiment, it is possible to efficiently disperse the slurry in which the particle diameter of 1 micrometer or less is suspended, and it is 30 which greatly exceeds the limit viscosity of 200 to 500 mPa · s in the conventional device. Even in the case of a slurry having a viscosity of at least 1,000 mPa · s, particles can be dispersed. Furthermore, in addition to dispersion processing, it can be used for mixing processing of liquids, etc. In the conventional apparatus, mixing processing of highly viscous fluids which can not be processed, and emulsification processing of oil, water and the like become possible.

Since such treatment becomes possible, it becomes possible to manufacture a highly viscous particle dispersion paste which could not be conventionally manufactured by a single treatment. In addition, with highly viscous fluid, only the badge process can be performed, which makes it possible to have a plant where the pretreatment device and the primary storage device of the mixture are unnecessary, or to simplify the plant by continuing the badge type emulsification process. An effect is obtained.

Moreover, in the disperser of another preferable aspect, since dispersion processing can be performed without using beads, it can be used for the slurry processing of particles in which the performance of the final product is degraded when the particles are damaged. In particular, dispersion treatment can be performed without damaging particles such as organic substances and low-strength oxides. Moreover, there is no mixing of bead fragments into the product slurry, and product contamination by bead components can be prevented.

It is sectional drawing of the disperser of this invention. It is the sectional view on the AA line of FIG. FIG. 3 is a dimension drawing of the main part of the rotor shown in FIG. It is the graph which plotted the average particle diameter (D50) which shows the dispersion performance at the time of processing with the apparatus of this invention with respect to L / D. It is the graph which plotted the specific surface area at the time of making D50 disperse | distribute to 0.3 micrometer which shows the extent of particle | grain crushing at the time of processing with the apparatus of this invention with respect to L / D. The schematic sectional drawing of the principal part of the disperser of another aspect. The top view of the rotor which comprises the dispersing machine shown in FIG. The front view of the rotor. FIG. 7 is a plan view of a cylindrical body constituting the disperser shown in FIG. 6; The longitudinal cross-sectional view of the cylindrical body. The enlarged view of the cylindrical container and the principal part of a rotor. The expansion development of the part which shows another example of unevenness.

Hereinafter, a dispersing machine according to an embodiment of the present invention will be described with reference to the drawings. Although the rotation axis of the device is shown in the vertical direction in this figure, it may be installed in other directions such as horizontal.
FIG. 1 shows a cross section of a dispersing machine generally indicated by reference numeral 1, and FIG. 2 shows a cross section taken along the line AA of FIG. A cylindrical container having a closed shape, and a rotor 8 disposed coaxially with the cylindrical container in the cylindrical container and fixed to a shaft 6 rotationally driven by a motor as a driving source, although not shown. The upper portion of the shaft 6 is circular in cross section and the lower portion is substantially square in cross section, and the rotor 8 is non-rotatably fitted to the lower portion of the shaft 6. In addition, the said cylindrical container does not necessarily need to be divided | segmented and comprised by the cylindrical body 2, the upper cover 3, and the lower cover 4, for example, the cylindrical body 2 and the lower cover 4 may be integrated.

The rotor 8 has a pair of disks consisting of an upper disk 10 fixed to the shaft 6 and a lower disk 11 fixed to the shaft 6 with a constant distance from the upper disk 10, circumferentially, etc. Upper and lower ends are respectively connected to the upper disc 10 and the lower disc 11 so as to be spaced from each other, and are constituted of axial partition plates 9. At the time of classification, the rotor 8 is at the outer peripheral end of the partition plates 9 It rotates at a peripheral speed of 3 to 30 m / sec.

The hollow shaft 7 is formed as a hollow shaft 7 having a hollow portion by hollowing the axial center portion above the upper disc 10 of the rotor 8 and the lower end of the hollow shaft 7 is in the partition plate by the through hole 12 in the diametrical direction. The rotor 8 is open inside. In FIG. 1, as slurry supply ports, the lower slurry supply port 13 which is the first slurry supply port installed in the lower lid 4 on the lower side of the cylindrical container, and the upper lid 3 in the upper side of the cylindrical container Two of the upper slurry inlets 14 which are the second slurry inlets described are described, but one may be installed. During processing, the slurry is supplied from either or both of the lower supply port 13 and the upper slurry supply port 14 and flows toward the center of the rotor 8 via the vicinity of the inner peripheral surface of the cylindrical body 2 and then the hollow shaft It is discharged out of the device through the hollow part of 7.

In the cylindrical container, as shown by the arrow in FIG. 1, the cooling water as a refrigerant enters and leaves to cool the cooling water passage 5 from the peripheral side, but the cooling water is also supplied to the upper lid 3 and the lower lid 4 The cylindrical body 2 may be cooled not only from the circumferential side but also from the top and bottom.

Here, in the present invention, when the slurry supply is from only one direction, the relationship between the diameter (D) of the outer peripheral end of the partition plate 9 of the rotor 8 and the length (L) in the rotational axis direction is 0.3 ≦≦. It is assumed that L / D ≦ 1.6. Under this condition, particles in the slurry are properly dispersed and crushed, and bead contamination in the treated slurry is reduced. In particular, in the case of a highly viscous slurry, the effect of processing with an apparatus equipped with the design requirements of the present invention is large.

When L / D is 0.3 or less, the bead mixing ratio increases, and the level becomes a problem when making the slurry into a product raw material. This is because the rotor is too flat, and the beads stacked on the periphery of the cylindrical body 2 are disturbed by the centrifugal force, and the beads flow into the rotor 8 with the slurry.

On the other hand, in the case of L / D ≧ 1.6, since both the cylindrical container and the rotor 8 are vertically long, the bead concentration in the slurry in the circular container varies, especially in the rotational axis direction (longitudinal direction in FIG. In). As a result, in the part where the beads are dense, local shear force rise occurs, the shear stress of the beads becomes large, and in the part where the beads are sparse, the shearing force is insufficient. Furthermore, the dispersion time of the slurry is increased, and particles with short residence time become insufficiently dispersed, while particles with long residence time increase so-called primary particle breakage. As a result, the insufficiently dispersed particles and the particles in which the particles are excessively broken are mixed, which causes a problem that the particle diameter is uniform and the slurry of the uniformly dispersed particles can not be obtained.

On the other hand, supplying the slurry from the lower slurry supply port 13 and the upper slurry supply port 14 corresponding to the upper and lower slurry supply ports and corresponding to the first and second slurry supply ports is also effective in practicing the present invention. desirable. By supplying the slurry from above and below, there is an advantage that the height of the apparatus can be increased and the apparatus can be enlarged. When the slurry supply ports are present at both the upper and lower sides, since the neutral point of the flow is in the center of the cylindrical vessel in the vertical direction of the slurry, there is an advantage that the height can be about twice that of slurry supply from one direction. An intermediate disc may be installed between the upper disc 10 and the lower disc 11 in order to adjust the slurry flow and to facilitate the production. In addition, the middle disc may have an opening.

In the apparatus for supplying the slurry from both the upper and lower sides, L / D can be up to 3.2, which is the upper limit of claim 2. Also, L / D can be a minimum value of 0.3, since the slurry flow is vertically symmetrical and bead separation is as good or better than a single slurry inlet.

When the partition plate 9 is too short in the diameter direction, the bead separation performance is degraded. This is because the partition plate 9 reduces the function of sending the beads to the inside of the cylindrical container. If the partition plate 9 is too long, the flow in the hollow shaft 7 is bent, and if it is attempted to increase the flow rate, there is a problem that the pressure becomes excessive. Therefore, the diameter of the circumference where the inner peripheral end of the partition plate 9 is located is preferably 50 to 85%, preferably 50 to 70% of the diameter of the circumference where the outer peripheral end of the partition plate 9 is located.

As shown in FIG. 3, the partition plate 9 constituting the rotor 8 preferably has an angle α of 5 to 30 degrees with the radius passing through the axis. The reason is to make the flow of the slurry into the rotor 8 by rotation proper by making the angle α proper, and if the angle is proper, the flow of the slurry into the rotor 8 will be the rotor 8. Uniform in the height direction. As a result, it is possible to prevent the decrease of the slurry flow above the cylindrical body 2 due to the excessive flow of the slurry into the rotor 8 at the lower part and the reverse phenomenon.

The spacing of the dividers 9 is an important requirement of the present invention. The partition plate spacing gap at the inner peripheral end of the partition plate and _{G 1,} when the partition plate spacing gap at the outer peripheral edge and _{G 2, G 1} is 1 ~ 7mm, _{G 2} is good 1.5 ~ 10 mm. Also, _{G 2} is even better if in the range of 100 times 20 times the bead diameter. The distance t between the outer peripheral end of the partition plate and the inner peripheral surface of the container is preferably 3 to 30 mm. The separation performance of the beads is improved as the total number n of the partition plates 9 described above is increased, and it is possible to cope with high viscosity of 500 mPa · s or more. In this case, _{G 1} is 1 ~ 5mm, _{G 2} is good 1.5 ~ 7 mm.

The spacing gap ratio between the dividers 9 is also an important design requirement for bead leakage. The following values are used as an index for expressing the gap gap ratio. The circumferential diameter at which the inner circumferential end is located is D ₁ , the circumferential diameter at which the outer circumferential end is located is D ₂ , and the gap at the inner circumferential end of the partition plate on the inner periphery where the diameter is D ₁ is G ₁ , the gap of the partition plate outer circumferential edge on the circumference whose diameter forms a D ₂ and G _2, when the total number of the partition plate 9 is n, the circumference of the sum and the inner peripheral end of the partition plate spacing gap of the inner peripheral edge The ratio to the length is nG ₁ / πD ₁ and the ratio at the outer peripheral edge of the partition plate is nG ₂ / πD ₂ .

In order to carry out the present invention efficiently, when the ratio of the divider gap to the circumferential length at the inner and outer peripheral ends is appropriate, the taper ratio of the divider gap is also important. Because of this, it is further preferable to set the ratio of the gap between the outer peripheral end and the inner peripheral end to the appropriate range, 1.2 ≦ G ₂ / G ₁ ≦ 3. When the gap between the partition plates 9 is excessively narrowed on the inner circumferential side, the beads are present only between the cylindrical body 2 and the partition plates 9, the degree of crushing becomes too large, and the ratio is too small As a result, the slurry flow rate in the interval gap becomes constant, and as a result, the beads enter more inside, resulting in a decrease in the bead separation rate. It is assumed that 0.15 ≦ nG ₁ / πD ₁ ≦ 0.6, and 0.2 ≦ nG ₂ / πD ₂ ≦ 0.8. That is, by setting the ratio of the partition plate gap at the inner peripheral end to 15 to 60% and the ratio of the partition plate gap at the outer peripheral end to 20 to 80%, the partition plates of the cylindrical body 2 and the rotor 8 Both of the dispersion and crushing of the particles by the beads between 9 and 9, and the inflow of the slurry into the rotor 8 can be properly balanced. As a result, there is no bead leakage, and appropriate dispersion and crushing can be performed.

The lower slurry supply port 13 or the upper slurry supply port 14 is provided at the center of the lower lid 4 of the cylindrical container, and the raw material slurry in which particles are mixed in the solvent is pumped by the lower slurry supply port 13 or the upper slurry supply port 14 The slurry is preferably supplied into the cylindrical container, but it is preferable to pre-mix the slurry using, for example, a stirrer, a homogenizer or the like prior to supplying the cylindrical container. In addition, the raw material slurry may be supplied from both the lower slurry supply port 13 and the upper slurry supply port 14.

The raw material slurry supplied into the cylindrical container from the lower slurry supply port 13 or the upper slurry supply port 14 is stirred and mixed in the cylindrical container by the rotation of the beads and the rotor 8 and the agglomerated particles are loosened. The slurry which is dispersed and particles are separated from the outer peripheral end of the partition plate 9 as the separation portion by the action of centrifugal force moves to the inner peripheral side through the slurry path between the partition plates 9 and is hollowed from the opening 12 formed in the hollow shaft 7 The solution is discharged upward through the hollow portion 7 of the shaft 7 and recovered as a product slurry or fed again to the supply port 13 and mixed with the beads in the cylindrical container with stirring.

The beads are supplied into the cylindrical container from the upper side of the cylindrical container from which the upper lid 3 is removed, or, although not shown, the upper lid 3 is provided with a bead supply port, and through the supply port. It can also be done.

It is desirable to operate the device under the following conditions. The peripheral speed of the outer peripheral end of the partition plate 9 is also an important processing condition. The appropriate operating conditions are that the peripheral speed of the outer peripheral end of the partition plate 9 is 3 to 30 m / sec, and the centrifugal force is 8,000 m / s ² or less. When the centrifugal force is small, the bead separation performance is reduced, but the damage to the primary particles is reduced. Conversely, if the centrifugal force is large, the bead separation performance is improved, but the damage to the primary particles is increased. In particular, in the case of a highly viscous slurry of 500 mPa · s or more, the peripheral speed of the outer peripheral end of the partition plate 9 is preferably 5 to 25 m / s, and the centrifugal force is preferably 8,000 m / s ² or less. If the centrifugal force is too weak, bead leakage will occur, so desirably 800 to 8,000 m / s ² . Here, the centrifugal force is a value calculated by G = 2v ² / D (m / s ² ) from the peripheral velocity v of the outer peripheral end of the partition plate 9 and the diameter D of the outer peripheral end of the partition plate 9.

The shear (shearing force) acting on the slurry in the space formed by the outer periphery of the partition plate 9 and the cylindrical body 2 is also an important processing condition. In the present invention, the shear rate (s) in the space formed by the cylindrical body 2 and the outer peripheral end of the partition plate 9 is represented by the peripheral velocity v (m / sec) of the outer peripheral end of the partition plate 9, the outer peripheral end of the partition plate 9 and the cylindrical body 2 When calculated from the interval t (m) of S and using this to calculate S = v / t, S is operated under the condition of 1000 to 8000 (1 / s). If the share ratio S is low, there is a problem that the dispersion decreases, and if it is high, damage to primary particles becomes large.

Beads used in this device are generally oxide particles, metal particles, etc. Specifically, zirconia, titania, glass, alumina, zircon, stainless steel, etc. are used, and their specific gravity is the raw material It is sufficient if it is larger than the slurry, and more preferably, it is twice or more the specific gravity of the slurry. As such beads, those having a particle diameter of about 0.01 to 1 mmφ are used, and those having a spherical shape are desirable. As the slurry solvent, water, an alcohol-based organic substance, toluene, acetone, glycols, a highly viscous paste, or the like is used, and a dispersant may be used to increase the treatment efficiency. The slurry viscosity can be up to 3,000 mPa · s. The particles of the slurry targeted in the present embodiment are oxides such as titanium oxide powder and barium titanate, metal fine particles such as silver and nickel, and fine carbon fibers. Hereinafter, a first example in the present embodiment will be illustrated.

First embodiment

The main dimensions of the disperser described in FIG. 1 are: in the apparatus having a slurry supply port of 1, D is 100 mm, L is 15 mm to 226 mm, and L / D is 0.15 to 2.26. In an apparatus with two slurry supply ports, D is 100 mm and L is 35 mm to 320 mm. Ratio configuration of the partition plate 9, the spacing is 2 ~ 4mm, 3 ~ 6mm in G ₂ in G _1, the outer peripheral diameter D2 is the same as D, D1 is listed in Table 1 for D2 And the angle α was 5 to 30 degrees. Further, in the apparatus in which the slurry supply port is 2, D is 100 mm and L is 30 mm to 280 mm, and the other dimensions and the like are equal to those of the above-described apparatus. As a comparative example, experimental results are shown for a conventional bead mill in which L having a centrifugal bead separation device and eight stirring pins is 100 mm and D is 40 mm. The raw material slurry was barium titanate, and was treated with a primary particle of 300 nm, a secondary particle diameter of 100 μm, and a slurry concentration of 10%. The slurry viscosity was 30 mPa · s. The beads for grinding and dispersion were 50 μm zirconia.

After activating the apparatus, samples were taken from the outlet of the mill every predetermined processing time. For the particle diameter measurement, a laser diffraction / scattering particle size analyzer LA-950 manufactured by Horiba, Ltd. was used. Further, the specific surface area was determined by a BET single point method using FlowSorb II 2300 manufactured by micrometrics, in order to determine primary particle breakage.

The values employed to evaluate the treatment results are the treatment results after treatment for 1 minute 40 seconds for the Comparative Example and Examples 1 to 4 and 6 to 10, and 3 minutes for Example 5. As the evaluation index, the average particle size of secondary particles (D50: particle size of secondary particles below 50%) and the specific surface area when secondary particles are dispersed to an average of 0.3 μm were used. In the former value, the dispersion performance is evaluated. The smaller this value, the better the dispersion performance. The latter value assesses the degree of destruction of primary particles. When particle breakage occurs, the specific surface area increases even if the average secondary particle diameter is the same, and if it is not desirable to destroy primary particles, the smaller the value, the better.

Examples and comparative examples are shown in Table 1 below. First, Comparative Example 1 is an example processed by a testing machine of a bead mill composed of a conventional stirring rotor and a bead separator. The cylindrical container of this apparatus used the same thing as this apparatus, but the rotating body had a stirring rod in the lower part, and used what has a separator in the upper part. As a result, although the dispersion performance is good, primary particle destruction is progressing, and it is unsuitable for the process which wants to reduce particle destruction.

All the embodiments of Table 1 satisfy the device requirements of the present invention, and L / D is within the scope of the invention according to claim 2, and D ₁ / D ₂ and G ₁ / G ₂ are also claimed. It is the scope of the invention concerning 2 and 3. Examples 1 to 7 are examples in the apparatus having one slurry supply port, and Examples 9 to 11 are examples of the apparatus having two slurry supply ports. When the examples were analyzed, in terms of dispersion performance, good dispersion performance was obtained, with a secondary particle diameter (D50) of 0.4 micrometers or less. On the other hand, in Comparative Example 2, since L / D was as small as 0.15, the dispersion performance was poor at 0.46 micrometers. The processing results of the peripheral speed of 12 m / s on the outer periphery of the partition plate of the rotor are organized by L / D and plotted in FIG. As can be seen from this graph, when L / D was 0.3 or less, the dispersion performance was rapidly deteriorating.

Regarding the evaluation results of particle breakage reduction, in Examples 1 to 5 and 7, the specific surface area was 7 m ² / g or less, and particle breakage was a result that was small. In Comparative Example 3, since L / D was as large as 2.26, the specific surface area was 8.8 m ² / g, and it was found that particle destruction was advanced. In Comparative Example 2, the specific surface area could not be evaluated because the average secondary particle diameter did not fall to 3 micrometers or less within a predetermined time. In Comparative Example 3 in which L / D is 2.26, the processing results of the specific surface area of the peripheral speed of 12 m / s on the outer periphery of the partition plate of the rotor are organized into L / D and plotted in FIG. It was found that when L / D exceeds 1.6, the specific surface area of the particles is increased, and particle destruction is likely to proceed. Therefore, the conditions under which both the dispersion performance and primary particle breakage reduction were good were in the L / D range of 0.3 to 1.6. In addition, when D ₁ / D ₂ and G ₁ / G ₂ were also in appropriate ranges, the processing results were better.

It has been found that processing conditions also affect the same example. As shown in Table 1, when the centrifugal force was in the predetermined range and the shear ratio was in the predetermined range, the treatment results were particularly good. On the other hand, in Example 6 which is an example in which the centrifugal force is too strong, the specific surface area is slightly large, and the particle breakage is slightly advanced. In Example 5 in which the centrifugal force is weak, bead leakage is slight but occurs, and in Example 7, minute bead leakage occurs because the partition plate 9 is short and D1 / D2 is 0.85. There were no processing problems with either.

Examples 8 to 10 are the examples of the apparatus in which the slurry was supplied from the upper and lower directions, and the L / D was able to be effectively processed at 0.35, 1.6 and 3.2.

FIG. 6 is a cross-sectional view schematically showing a dispersing machine according to another embodiment, in which the rotation axis is in the vertical direction for convenience, but the direction of the rotation axis may be another angle such as horizontal. The dispersing machine 21 shown in the drawing has a structure in which a rotor 25 is contained in a cylindrical container formed by a cylindrical body 22, an upper lid 23, and a lower lid 24, and thereafter, the cylindrical body 22, the upper lid 23, and the lower lid 24 are used. The structure to be formed is referred to as a cylindrical container. The rotor 25 fixed to the rotating shaft 26 rotates at high speed by the rotating shaft 26. The raw material slurry is supplied from the slurry inlet 27 to the internal space of the disperser 21 and given shear force at the shear flow generation gap 28 between the inner peripheral surface of the cylindrical body 22 and the outer peripheral surface of the rotor 25 to disperse it. After being processed, it is discharged from the slurry outlet 29 out of the apparatus as a product slurry.

The cylindrical body 22, the upper lid 23, and the lower lid 24 each have a cooling water passage 30 therein, and a cooling water is allowed to flow here to cool the slurry inside the dispersing machine 21. The upper cover 23 or the lower cover 24 may not have the cooling channel 30. The material of the structure between the cooling water passage 30 and the internal space of the cylindrical container adopts a material having a good thermal conductivity and is applied with an appropriate thickness. In FIG. 6, the rotating shaft 26 is installed in the direction of the slurry outlet 29, but may be installed in the direction of the slurry inlet 27.

In the apparatus of the present invention, when the rotor 25 is rotated, a shear force is exerted on the slurry of the shear flow generation gap 28 to disperse the agglomerated particles (secondary particles) in the slurry, thereby separating single particles (primary particles). The particles are dispersed in the liquid. However, as in the prior art, in a device constituted by a cylindrical inner circumferential surface and a rotor outer circumferential surface which are constituted by a smooth surface or provided with only a simple asperity, the shear force generated by the rotation of the rotor 25 Even if the circumferential velocity is 10 m / s or more and the gap is 1 to 3 mm, it is impossible to properly disperse secondary particles composed of particles having a primary particle diameter of 1 micrometer or less in the slurry.

On the other hand, in the device of the present invention, the shear force can be sufficiently increased if the structure of the cylindrical container and the rotor 25 having the concavities and convexities constructed under appropriate design conditions is used. In the apparatus according to the present invention, the slurry density is significantly increased by repeating the penetration of the slurry into the recess on the outer peripheral surface of the cylindrical container after the slurry enters the recess on the inner peripheral surface of the cylindrical container with the rotation of the rotor 25. , The shear force of the slurry increases. As a result, the effect of dispersing the particle group (secondary particles) collected in the slurry is increased.

Here, the shape and size of the unevenness in the device of the present invention will be described. 7 is a plan view of the rotor 25, FIG. 8 is a front view of the rotor 25, FIG. 9 is a plan view of the cylindrical body 22, and FIG. 10 is a longitudinal sectional view of the cylindrical body 22. 7 to 10 show an example in which the grooves 31 and the ridges 32 are alternately formed at equal intervals in the circumferential direction. The projections and depressions provided on the cylindrical body 22 and the rotor 25 can be of any shape other than the above-mentioned concave groove 31 and convex stripe 32 or the dimple 33 shown in FIG. For example, although the grooves 31 and the ridges 32 shown in FIG. 11 have the same width and the same pitch in the axial direction, the widths may be different, and the pitch may be changed to be random. Alternatively, without forming in the axial direction, the inclination angle with respect to the axial center of the cylindrical body 22 and the rotor 25 may be inclined at 10 degrees or less. The grooves 31 and the ridges 32 may also be formed, for example, in a bent, zigzag or curved manner. In this case, it is not necessary to stick to an angle of 10 degrees. FIG. 11 is a view showing the meshing of the rotor 25 and the cylindrical body 22. As shown in FIG.

Further, in FIG. 12, as another example of the asperities, those of discontinuous recesses (dimples 33) are shown. The circular dimples 33 are formed in a form in which the concave portions are independent of one another, and the portions other than the dimples 33 become convex portions. The dimples 33 may be grooves formed of ovals, ovals, polygonal or irregular grooves, or a combination thereof. Also, the surface of the rotor 25 may be an uneven groove, and the inner surface of the cylindrical body 22 may be configured with discontinuous recesses, or vice versa.

According to the studies of the present inventors, the following has been found. It was found that installing the asperities in the rotational direction of the rotation axis of the cylindrical container and the rotor 25 most contributes to the improvement of the shear force. . The grooves 31 and the ridges 32 are formed in the cylindrical container and the rotor 25. If the inclination angle of the recessed groove 31 with respect to the axis of the rotor is large, it is important that the angle is within 10 degrees because it impedes the flow of the slurry upward in FIG. Moreover, the unevenness may be an unevenness formed of recesses which are discontinuous and formed independently of each other. However, in any case, the unevenness is characterized by the following.

About the effect of the present invention, it has been found that the depth of the unevenness has a great influence on the shear force. When the shear flow generation gap 28 is small, sufficient effects can not be recognized when the depth h of the concave and convex portion is 1 mm or less. When the gap is large, it is necessary to have a depth of 0.5 times or more the gap distance. On the other hand, even if the depth of the recess is excessively large, there is no particular increase in the effect, and on the contrary, as a result of the presence of a slurry not receiving shear force at the back of the recess, there is a problem that the dispersion efficiency decreases. Therefore, the depth of the recess is preferably 8 mm or less.

The width of the shear flow generation gap 28 is also an important design factor. In order to make the shear flow generation gap 28 not more than 0.6 mm, high precision is required for the production of the cylindrical container and the rotor 25, which makes production difficult There is also a problem that heat generated by shearing tends to be accumulated in a narrow volume. On the other hand, if the width is larger than 4 mm, the shear force is significantly reduced in a liquid of ordinary viscosity (300 cP or less). Therefore, when the shear flow generation gap 28 is 0.6 to 4 mm, the dispersion performance can be improved without causing difficulty in manufacturing the cylindrical container and the rotor 25. Here, the width of the shear flow generation gap 28 refers to the distance between the circumferences where the projections of the concave and convex portions provided on the cylindrical body 22 and the rotor 25 represented by t in FIG.

Furthermore, the present inventors have found that the dispersion effect of the particles in the slurry is small regardless of whether the width of the recess is wide or narrow. The optimum width is 0.8 to 6 times the shear flow generation gap 28. Here, in the case where the convex portion is constituted by a curved surface, in the case of the concave and convex portions, the maximum width of a position 1/10 lower than the concave portion depth from the apex of the convex portion is referred to. It is also a design requirement that the width of the recess is 0.8 to 6 times the width t of the shear flow generation gap 28. In the case where the width t of the recess is narrow, there is a problem that the slurry gets in and out of the recess and the dispersion becomes worse. On the other hand, when the width t of the recess is too large, although the slurry comes in and out, the number of asperities decreases, so the dispersion also decreases. Furthermore, when the area of the recess is 30% or more and 80% or less of the entire peripheral surface, the slurry flows into and out of the recess on the inner surface of the cylindrical container and the outer periphery of the rotor 5 becomes active, and particle dispersion becomes good. Further, in the case of the groove-like unevenness, when the width of the convex portion is long, the same performance as that of the smooth shape is obtained, and the effect of making the slurry into a turbulent state is lowered, so the dispersion performance is lowered. Therefore, such a problem can be solved by setting the width of the convex portion to five times or less of the width t of the shear flow generation gap 28.

In the device of the present invention, a strong shear force acts on the slurry in the gap between the cylindrical body 22 and the rotor 25 (the shear flow generation gap 28), and this generates a large amount of heat. Therefore, strong cooling is required to prevent deterioration of particles in the slurry and boiling of the liquid due to heat generation. In the device of the present invention, it is necessary to strongly cool this portion, and it is preferable to cool 100% or more of the portion of the cylindrical body 22 facing the rotor 25 with a liquid such as water.

In particular, in the case of processing in which the slurry temperature approaches the boiling point inside the shear flow generation gap 28, cooling in the upper lid 23 part is also important. Since the inside of the apparatus of the present invention is a positive pressure, even if the slurry temperature rises to near the boiling point, it does not boil, but there is a possibility of boiling because it becomes atmospheric pressure or negative pressure at the position where it leaves the apparatus. Out. Therefore, in such a case, cooling between the shear flow generation gap 28 and the product slurry outlet becomes important. Therefore, the upper lid 23 is cooled with a liquid such as water. It is preferable to cool 50% or more of the upper lid 23.

Cooling of the shear flow generation gap 28 which is a portion facing the side surface of the cylindrical body 22, particularly the rotor 25, is performed under the following conditions. Metals, ceramics, and hard resins are used as the material of the cooling portion, and it is preferable that the thermal conductivity (λ) is high, and the thermal conductivity is preferably 15 W / mK or more. The thermal conductivity is more preferably 25 W / mK or more. As the metal, copper or copper alloy (λ: 300 to 430 W / mK), aluminum or aluminum alloy (λ: about 110 W / mK), iron (λ: about 50 W / mK) or the like is preferable. For ceramics, high density alumina (including additives) (λ: 15 to 30 W / mK), aluminum nitride (λ: 100 W / mK or more), silicon nitride (λ: 15 to 30 W / mK), silicon carbide ([Lambda]: about 200 W / mK) is good. Here, the thermal conductivity refers to a value at 0 ° C. or 20 ° C.

The thickness of the material of this part is also an important technical condition. In order to satisfy the cooling condition of the present invention, it is important that the heat transfer resistance of the material portion is small. Since the heat transfer resistance is proportional to the thickness and inversely proportional to the heat conductivity, T / λ is 0.0005 K when the heat transfer resistance is represented by (thickness: T m) / (heat conductivity: λ W / m K) It is important that it is less than / W. However, when the shear flow generation gap 28 with a larger shear force is 2 mm or less or the circumferential speed of the rotor 25 is large, T / λ is preferably 0.00035 K / W or less. For example, when alumina of λ = 17 is used, it is a design condition that T <8.5 mm in the former condition and T <5.95 mm in the latter condition. Similar conditions are desirable for cooling the top cover 23 of the apparatus. When the structure includes a plurality of layers, ΣTn / λn is equal to or less than 0.0005 K / W or 0.00035 K / W. Here, λ n is the thermal conductivity of the n-th material layer from the inside, and T n is the thickness of the n-th material layer from the inside.

The ratio of the axial length L to the diameter D of the rotor 25 is also an important indicator for device design. When L / D is large, the longitudinal length of the shear flow generation gap 28 which is a heat generation region becomes long, and the area ratio of the upper surface to the side surface of the cylindrical container decreases. As a result, the cooling effect of the upper lid 23 is reduced.

The cooling capacity per area is larger in the shear flow generation gap 28. This is because the turbulent flow density at the intervals of the shear flow generation gap 28 is high, so the heat conduction on the liquid side is good. On the other hand, in the portion of the upper lid 23, since the slurry flow velocity is low, the heat conduction on the liquid side is low. In the device of the present invention, the cooling capacity per area is about 0.4 at the portion of the upper lid 23 when the portion of the shear flow generation gap 28 is 1. In order to prevent the slurry heated to a temperature close to the boiling point in the shear flow generation gap 28 from boiling when it comes out of the apparatus, it is necessary to cool the upper lid 23 by 5 ° C. or higher, preferably 10 ° C. The reason why the temperature is lower than the boiling point is that a negative pressure is generated locally due to the flow inside the piping outside the apparatus, and boiling easily occurs.

In the apparatus according to the present invention, under the operating conditions close to the boiling point, the shear flow generation gap 28 cools the temperature rise by 60 to 70 ° C. It is necessary to have a cooling capacity of 7-8% or more for the portion of the flow generation gap 28. Considering the ratio of the cooling capacity per area at the upper lid 23 of 0.4, the area between cooling of the upper lid 23 is preferably about 18% or more of the cooling area of the cylindrical body 22. Therefore, L / D needs to be 1.2 or less in order to satisfy this condition in area. Preferably, the ratio of the area of the upper lid 23 to the area of the shear flow generation gap 28 is 25% or more by setting L / D to 1 or less. However, if L / D is too small, productivity per size of the device is reduced. Therefore, it is desirable that L / D be larger than 0.2, which is the limit L / D at which the device becomes larger in an accelerated manner.

The operating method of the device of the present invention is as follows. The raw material slurry supplied into the container contains particles aggregated in the solvent, and examples of the solvent include water, alcohol-based solutions, toluene-based solutions, acetone, glycols, etc. It is not something to be done. Prior to supplying the raw material slurry to the dispersing machine 1, it is desirable to add, for example, a powder, a dispersing agent and the like, and to pre-mix the raw material slurry using a stirrer, a homogenizer and the like. The applicable viscosity of the slurry is in a wide range of 10 to 40,000 mPa · s, and it is particularly suitable for the treatment of a highly viscous slurry of 500 mPa · s or more which can not be handled by the conventional apparatus.

It is desirable that the dispersing machine of this embodiment operate under the following conditions.
The peripheral speed of the outer periphery of the rotor 25 is 10 to 80 m / sec. The shear fraction in the shear flow generation gap 28 of the particles in the slurry is increased, and the secondary particles in the slurry are decomposed by the shear force to disperse the independent primary particles. The shear ratio is represented by S = v / t, where v is the circumferential speed of the outer periphery of the rotor 25 and t is the radial width of the shear flow generation gap 28. In the device of the invention, a narrower range is appropriate. The proper range in the device of the present invention is 8,000 to 70,000 (1 / s). When the share ratio S is 8,000 or less, dispersion with an average particle size of 1 micrometer or less can not be performed. On the other hand, when it is high shear rate, there is a problem that slurry temperature rises. In the cooling capacity of the apparatus of the present invention, when the shear ratio S is 70,000 (1 / s) or more, the heat generation becomes excessive and the cooling capacity is insufficient. Therefore, it is preferable to set the maximum value to this value.

The apparatus of the present invention can be used for fluid mixing and emulsification as well as dispersion of particles in a slurry. In the conventional apparatus, even a highly viscous fluid having a viscosity of 40,000 mPa · s or more can be processed, and therefore, it is possible to mix two or more kinds of highly viscous fluids, for which continuous processing was difficult. The two or more fluids are premixed and supplied to the apparatus of the present invention by a slurry pump. If this is processed at a share ratio S of 8,000 (1 / s) or more, a mixture with extremely high uniformity is formed. For example, it can be used to mix food pastes, high viscosity electrode material pastes, and the like. In addition, when water and oils (vegetal, animal, mineral) are mixed with a surfactant and treated with a shear ratio S of 15,000 (1 / s) or more, an oil emulsion of about 10 micrometers or less It is possible to produce an emulsion consisting of In addition, in the present apparatus, as the maximum value, if the share ratio is 70,000 (1 / s), particles of about 1 μm can be formed, and for general processing, processing is performed with this share ratio or less. It is economical because it can minimize power loss. The second example of the present embodiment will be illustrated below.

Second embodiment

The device specifications and operating conditions of the dispersing machine used in this example are shown below. The dispersing machine has the structure shown in FIG. 7, and the main specifications are as shown in Table 2 below, the diameter (D) of the rotor 5 is 93 mm, and the length (L) is 90 mm and 25 mm. The width t of the shear flow generation gap 28 is 0.8 to 4 mm, and in the example, it was processed at 1 mm and 2 mm. The circumferential speed of the rotor 25 is a device capable of operating under the condition of 10 to 50 m / sec. Among the cylindrical containers of the apparatus, the cylindrical body 22, the upper lid 23, and the lower lid 24 are cooled. The structure of the cooling unit is as shown in Table 2. The results of dispersing the raw material slurry described in Table 3 using this apparatus are shown in Table 4. The sample was taken from the outlet of the disperser at predetermined time intervals after the disperser was started. A laser diffraction / scattering particle size analyzer LA-950 manufactured by Horiba, Ltd. was used to measure the particle diameter in the slurry after treatment.

As an index for evaluating dispersion, an average particle diameter (D50: a numerical value indicating that a 50% by mass particle has a particle diameter equal to or less than this value) and a particle ratio of 1 μm or more are used. The comparative example 4 is an example of processing in a device having neither unevenness in the cylindrical body 22 nor in the rotor 25. Other treatment conditions are within the range of the present invention, but when there is no unevenness like this, the average particle diameter is only reduced to 2.96 μm, and the particle ratio of 1 μm or more is as high as 72%. . The comparative example 5 is an example of the process which gave unevenness only to the rotor 25. Thus, the average particle diameter of 2.18 μm and the particle ratio of not less than 1 μm were 69%, which is insufficient if only one side was uneven.

On the other hand, in Example 11 to Example 15, which is a processing example in which both the rotor 25 and the cylindrical body 22 are provided with irregularities, the dispersion is strengthened such that the average particle diameter is 0.15 to 0.22 μm, and 1 μm. The particle ratio was also good at 21 to 41%. In addition, the temperature rise of the slurry was also suppressed within 30 ° C., and the result was also good in terms of slurry cooling. In addition, the device 22 with a higher cooling area ratio had a smaller rise in slurry temperature.

In addition, experiments were conducted to confirm the possibility of processing with a high viscosity slurry. Carboxymethylcellulose was treated using real equipment 1-3 in Table 5 below. When the peripheral speed of the rotor 25 was processed at 20 m / sec, as shown in Table 5, the motor power increased as the slurry viscosity increased, but the mixing process could be performed up to 37,000 mPa · s slurry. As described above, even with a highly viscous fluid, dispersion and mixing processing can be performed by using the device of the present invention.

Water and oil were subjected to emulsification treatment using a machine having the concavo-convex structure of the dispersion treatment example 14 in a real machine 1-3 shown in Table 2. As a oil, coconut oil was used to process a raw material liquid to which a surfactant was added at a water: oil ratio of 6: 2. As a result of processing by setting the width of the shear flow generation interval 28 of the device 21 to 1 mm and setting the peripheral speed of the rotor 25 to 10 to 30 m / sec, as shown in Table 6, the average diameter of the oil emulsion is the rotor 25 The circumferential speed was 16 μm at 10 m / s, 8.2 μm at 15 m / s, 5.3 μm at 20 m / s, and 3.9 μm at 30 m / s, and the oil was suspended. As a result of leaving these emulsions to stand for 2 days, oil separation did not occur by treatment at 15 m / sec or more. Thus, emulsification was able to be implemented continuously by processing with the circumferential speed of 15 m / sec or more with the apparatus 21. The share ratio at a circumferential velocity of 15 m / s was 15,000 (1 / s).

The disperser of the present invention and the method of dispersing particles in a slurry are applied to a slurry containing fine particles. The slurry is carbon powder, ceramic powder, organic powder, etc. For example, for dispersion and pulverization of particles of ceramic pigment, ink, paint, dielectric material, magnetic material, pharmaceutical material, food material, fine metal powder material Is suitable.

1, 21 · · Dispersing machine 2 · 22 · · Cylindrical body 3, 23 · · Upper cover 4 · · · Lower cover 5 · · Cooling channel 6 · · Shaft 7 · · Hollow shaft 8 · 25 · · Rotor 9 · · · · Partition plate 10 · · Upper disk 11 · · · Lower disk 12 · · Through hole 13 · · · Slurry supply port 26 · · Rotating shaft 26a · · Rotating shaft stop 27 · · Slurry inlet 28 · · Shear flow Occurrence gap 29 · · · Slurry outlet 30 · · · cooling channel 31 · · concave groove 32 · · convex streak 33 · · · dimple

Claims (17)

1. A rotor fixed to a rotary shaft coaxially installed with the cylindrical container is disposed inside the cylindrical container, and a shear force is generated in a gap formed between the cylindrical container and the rotor to produce a slurry. Dispersing machine characterized by processing.
2. The hollow shaft 7 is provided with a hollow space for discharging the slurry, which is disposed coaxially with the cylindrical container and rotates in the cylindrical container, the shaft 6 coaxial with the hollow shaft 7, and fixed to the shaft 6 A rotor 8 is disposed, and the rotor includes a plurality of partitions 9 radially or eccentrically arranged at appropriate intervals in a circumferential direction, and rotates in a cylindrical container, and a slurry supply provided to the cylindrical container It is a dispersing machine which forms a slurry path through which the slurry supplied from the port 13 is discharged from the hollow portion of the hollow shaft 7 to the outside of the apparatus through the space between the partition plates 9, and the outer peripheral end of the partition plate 9 is The disperser according to claim 1, wherein L / D which is a ratio of the diameter D of the contacting circle to the axial length L of the rotor 8 is 0.3 to 3.2.
3. The slurry supply port includes a first slurry supply port 13 provided on one side of the cylindrical container and both slurry supply ports of a second slurry supply port 14 provided on the other side of the cylindrical container. The disperser according to claim 2.
4. The dispersion according to claim 2 or 3, wherein the diameter of the circumference where the inner peripheral end of the partition plate 9 is located is 50 to 85% of the diameter of the circumference where the outer peripheral end of the partition plate 9 is located. Machine.
5. Either the ratio of the gap spacing of the partition plate 9 at the inner peripheral end and outer peripheral end _(G 2 / G ₁₎ is _1.2 <a G 2 _{/ G} 1 <claims 2 to 4, characterized in that the 3 Disperser as described in.
6. The angle between the partition plate 9 and the diametrical line from the center of the cylindrical container to the side surface of the cylindrical container is 5 to 30 degrees in the rotational direction, as described in any one of claims 2 to 5. Disperser.
7. The slurry containing fine particles is treated by the dispersion machine according to any one of claims 2 to 5 in which the centrifugal force at the outer peripheral end of the partition plate 9 constituting the rotor 8 is 8,000 m / s ² or less A method of treating fine particles in a slurry, comprising:
8. The slurry containing fine particles is used at the outer peripheral end of the partition plate 9 at the interval between the outer peripheral end of the partition plate 9 constituting the rotor 8 and the cylindrical body 2 using the disperser according to any one of claims 2 to 5 A method of treating fine particles in a slurry, wherein the processing is carried out at a shear rate of 1000 to 8000 1 / s, which is calculated based on the circumferential speed of the roller and the interval.
9. A rotor 25 coaxial with the cylindrical container and having an outer peripheral surface formed in a concavo-convex shape is installed in a cylindrical container consisting of the cylindrical body 22, the upper lid 23 and the lower lid 24. A shear flow generation gap 28 formed with the outer peripheral surface forms a slurry passage, and a raw material slurry inlet 27 provided on one end side of the cylindrical container and a product slurry outlet 29 provided on the other end side of the cylindrical container In a dispersing machine including a driving device that rotationally drives one of the cylindrical container and the rotor 25, the cylindrical body 22 is cooled with a liquid, and the inner circumferential surface of the cylindrical body 22 and the outer circumferential surface of the rotor 25 are uneven. To make the depth of the concave portion of the unevenness 1 mm or 0.5 times smaller than the shear flow generation gap 8, which is smaller, and to set the shear flow generation gap 28 to 0.6 to 4 mm. Feature Disperser according to claim 1.
10. The cylindrical body 22 and the rotor 25 are composed of concavo-convex grooves, and the concavo-convex grooves are straight concavo-convex grooves having an inclination angle of 10 degrees or less with respect to the axial center of the rotor 25 or refracted concavo-convex grooves. 10. The disperser according to claim 9, wherein the width of the recess is 0.8 to 6 times the shear flow generation gap.
11. The unevenness formed on the cylindrical container and the rotor 25 is discontinuous and formed of recesses formed independently of each other, and the width of the recesses is 0.8 to 6 times the shear flow generation gap 28 The disperser according to claim 9, characterized in that
12. One of the cylindrical body 22 and the rotor 25 is composed of a concavo-convex groove, and the concavo-convex groove is a linear concavo-convex groove having an inclination angle of 10 degrees or less with respect to the axial center of the rotor 25 or a concavo-convex groove refracted. And the concavities and convexities formed on the other of the cylindrical container and the rotor 25 are discontinuous and are constituted of concave parts formed independently of each other, and the width of the concave parts is 0.8 to 6 times the shear flow generation gap 28 The disperser according to claim 9, characterized in that:
13. In the structure between the cooling water passage 30 installed in the cylindrical body 22 and the inner surface of the cylindrical body 22, the relationship between the thermal conductivity (λ) and the thickness (T) is T / λ <0.0005 K / W The disperser according to any one of claims 9 to 12, characterized in that:
14. Of the total inner surface area of the cylindrical body 22, the area cooled by the liquid is 100% or more of the area of the portion where the inner surface of the cylindrical body 22 faces the rotor 25, and the upper lid 23 is cooled by the liquid The disperser according to claim 13, characterized in that.
15. The disperser according to claim 14, wherein the relationship between the diameter D of the rotor 25 and the height L of the rotor 25 is L / D <1.2.
16. An outer peripheral circumferential velocity (v) of a rotor 25 and a cylindrical body using a disperser according to any one of claims 7 to 12, wherein a slurry formed by dispersing particles having an average particle diameter of 1 micrometer or less is used. The shear ratio s represented by the equation s = v / t is 8,000 to 70,000 (1 / s) from the radial width (t) of the shear flow generation gap which is the distance between the rotor 22 and the rotor 25. The disperser according to any one of claims 9 to 15, which is a method of dispersing and treating particles in a slurry, which is treated in the range of
17. The emulsion manufacturing method characterized by processing a shear ratio with 15,000 (1 / s) or more using 2 or more types of liquids which do not melt | dissolve mutually using the dispersing machine in any one of Claims 9-16.

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