JP2906141B1 - High-speed stirring method and high-speed stirring device - Google Patents

Abstract

Abstract: PROBLEM TO BE SOLVED: To emulsify a liquid by mixing and stirring at a high speed.
A method for easily predicting the particle size of a finely divided liquid. A rotating blade (12) having an outer diameter (φ) slightly smaller than the inner diameter (A) of a container is provided at the center of a cylindrical container (2), and is rotated at a high speed while maintaining a small gap (S). The mixture is stirred while being rotated at a high speed in the form of a film along, and the product is taken out from the outflow pipe 7. Although the film thickness t is determined by the inner diameter of the weir plate 3, it can be batch-processed by enclosing an amount of the liquid to be treated to form an arbitrary film thickness using a lid-like weir plate. It is taken out from the raw material supply pipes 5, 6. If the pressure P generated by the rotation of the liquid is detected by the pressure transmitter 10 and the rotating blades are rotated so as to generate the preset pressure P, a product in which the desired particle diameter is uniformly formed can be obtained in a short time.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION The present invention relates to a liquid and a liquid or a mixture of a liquid and a powder, which are used as raw materials for medicines, cosmetics, foods, etc., as a liquid to be treated, and the components of the liquid to be treated are highly refined. The present invention relates to a stirring method and a stirring device for dispersing and emulsifying.

[0002]

2. Description of the Related Art In a cylindrical container, a rotating blade slightly smaller in diameter than the container is rotated at a high speed, and the liquid to be treated is stirred while being rotated in a film shape along the inner surface of the container, whereby the components of the liquid to be treated are agitated. A technique for miniaturizing is known, for example, from the invention described in Japanese Patent Application Laid-Open No. 9-75698 filed by the present applicant.

According to the means of the present invention, not only can the liquid to be treated be made into particles having a very small diameter of about 0.2 to 3 μm, but also the stirring time is extremely short. The stirring time varies depending on the peripheral speed of the impeller. If the peripheral speed is high, the stirring time is within 1 minute, but if the peripheral speed is low, about 5 minutes are required.

However, if there is such a difference in the particle size and the stirring time, the particle size is measured during the stirring, or the stirring time is set to be uniformly long regardless of the type of the liquid and the type of the rotating blade. It is necessary to work and there is a disadvantage that the work becomes inefficient.

[0005]

SUMMARY OF THE INVENTION According to the present invention, when a liquid to be treated is stirred and emulsified and mixed, a stirring speed at which components of the liquid to be treated can be atomized is set in advance, and the stirring speed is set to a short time. It is an object to stir.

[0006]

According to the present invention, as a result of experiments using various liquids to be treated and rotating blades, the liquid to be treated is rotated in the form of a cylindrical film, and high-speed rotation is performed with the average peripheral speed kept constant. It is discovered that the particle diameter of the component of the liquid to be treated becomes substantially constant upon stirring, and if the pressure of the liquid to be treated calculated from the peripheral speed and the film thickness of the liquid is maintained, the liquid amount and the rotating blade The inventors have discovered that a substantially constant particle diameter can be obtained regardless of the outer diameter, and have made the present invention based on these findings. The method is, as described in claim 1, a cylindrical shape containing a liquid to be treated. In the container, the rotating blade having an outer diameter slightly smaller than the inner diameter of the container is rotated at a high speed, and the liquid to be treated is pressed along the inner surface of the container by the rotational force and the centrifugal force generated in the liquid to be treated, and the cylindrical film is formed. A high-speed stirring method that produces fine particles by stirring while rotating The peripheral speed of the liquid to be treated corresponding to the desired particle diameter of the liquid to be treated is preset, the pressure on the peripheral surface of the liquid to be treated is detected, the inner diameter of the container, the film thickness and the specific gravity of the liquid to be treated, and An average peripheral speed of the liquid to be treated is calculated from the pressure and the pressure, and the rotational speeds of the different types of rotating blades are adjusted so as to generate a pressure at which the set peripheral speed is generated.

According to a third aspect of the present invention, there is provided an apparatus for rotating a container having an outer diameter slightly smaller than the inner diameter of the container in a cylindrical container containing the liquid to be treated. In a high-speed stirring device that rotates the blades at high speed and agitates while rotating the liquid to be processed in a cylindrical film along the inner surface of the container with the rotational force and centrifugal force generated in the liquid to be processed to generate fine particles, the side wall of the container Is provided with a pressure detector for detecting the pressure on the outer peripheral surface of the liquid to be treated, a speed change means is provided in the drive section of the rotary blade, and the pressure of the liquid to be treated at which a desired particle diameter is generated is preset, and the rotation at which the pressure is generated is set. The rotating blades are driven at a speed.

[0008]

Embodiments of the present invention will be described below with reference to the drawings. In FIG. 1, 1 is a high-speed stirring device for carrying out the present invention, 2 is a cylindrical stirring vessel, and an upper vessel 2 is provided on a top of the vessel 2 via a ring-shaped weir plate 3.
a is connected and closed by the lid 4. Material supply pipes 5 and 6 for supplying a material of the liquid to be treated L are provided at the bottom of the container 2.
Are connected, and valves 5a and 6a are provided in the respective tubes 5 and 6. Further, an outflow pipe 7 for taking out the processed product is connected to the upper container 2a.

The above-mentioned ring-shaped weir plate 3 is provided with a liquid L to be treated.
Is used for continuous processing, and for batch processing, the product is taken out from the raw material supply pipe 5 or 6 using a lid-shaped dam plate 3a (FIG. 2) having almost no gap between the rotary shaft.

Cooling chambers 8 and 9 are provided outside the containers 2 and 2a to cool frictional heat generated by stirring, and the cooling chamber 8 is connected to an inlet pipe 8a and an outlet pipe 8b of cooling water. A tube (not shown) branched from the tubes 8a and 8b is connected to the other cooling chamber 9. One or more pressure transmitters 10 for detecting the pressure on the outer peripheral surface of the processing liquid are attached to the side surface of the container 2, and the signal transmission circuit 10a is connected to a display unit or a control unit (not shown). Is done.

The rotating shaft 11 is provided through the lid 4 in an airtight manner. A rotating blade 12 is fixed to a lower end of the rotating shaft 11, and a motor 13 capable of variable speed rotation is connected to an upper end of the rotating shaft.

FIG. 2 shows an apparatus used in the experiment of the present invention. The inner diameter A of the container 2 is 156 mm, and two kinds of rotating blades having different outer diameters φ are used as the rotating blades 12. φ is 152 mm and 150 mm. Therefore, the gap S between the inner circumference of the container and the outer circumference of the rotary blade is 2 mm or 3 mm. Further, as the weir plate 3, a lid-like weir plate 3a is used.
Is used, and the liquid to be treated has a thickness t
_1, t ₂ ... is 9 mm, and supplying an amount to be 18mm or 35mm to batch processing, product after treatment was taken out from the raw material supply pipe.

As the rotating blades 12, a type shown in FIG. 3 is used. In the drawing, W is a wire type in which a large number of wires are fixed radially and is shown in FIG. D is a blade type in which a stirring blade is cut and raised around the periphery, M is a milling type in which gear-shaped teeth are provided around the periphery, and C is a cylinder type having a smooth cylindrical surface on the outer periphery. When such a rotary blade is rotated at a high speed, the liquid to be treated L and the air inside the container are rotated at a high speed by receiving the swirling force of the rotating blade, and the liquid to be treated L is stirred by the centrifugal force generated by the rotation of the container 2. Is pressed into a cylindrical film shape on the inner surface thereof, and a pressure P is applied to the inner surface.
The pressure is detected by the pressure transmitter 10.

Table 1 shows that water, liquid paraffin, and emulsifier
By mixing at a ratio of 0: 30: 1, the rotating blades 12 are rotated at a peripheral speed of 47.
The data shows the data when an emulsion having a specific gravity of 0.96 was produced by spinning at 60 m / s for 60 seconds, and the symbols and numerical values described in the column of the type of the blade were 152 mm in outer diameter and 150 mm in outer diameter.
m, two wire-type rotating blades φ152W, φ150W
And a blade-shaped rotary blade φ15 having an outer diameter of 152 mm each.
2D, a milling type rotary blade φ152D and a cylinder type rotary blade φ152C are shown, and these rotary blades are rotated in the container 2 having an inner diameter of 156 mm.

[0015]

[Table 1]

In the apparatus shown in FIG.
The pressure P of the liquid detected at 0 changes according to the film thickness as described in the column of the maximum pressure in Table 1, and from the pressure, the liquid amount and the film thickness, a well-known formula is used.

[0017]

(Equation 1)

The liquid peripheral speed V calculated in the above is, as described in the column of the liquid peripheral speed converted value in Table 1, a peripheral speed converted value substantially approximated for each type of rotary blade indicated by W, D, M, and C. Becomes φ15
In the case of 2W and φ150W, the outer diameters of the rotating blades are different, and therefore, even if the gap S is different, the converted values of the pressure and the liquid peripheral speed are approximate values.

When the diameter D μm of the emulsified particles of paraffin in the liquid to be treated taken out after the stirring is measured, the particle diameter is approximated by the type of the rotating blade as described in the column of the average particle diameter. That is, for the wire type W, 1
~ 2μm, 2μm latter half for blade type D, 2μm for milling type
The first half of μm is 3 μm in the cylinder type. From the above data, when it is desired to stir to a desired particle size, the numerical value of the film thickness t and the peripheral speed of the liquid to be treated are set according to the type of the rotating blade used, and the pressure at which the peripheral speed occurs is calculated. Then, the speed of the rotating shaft 11 may be controlled so that the pressure can be detected by the pressure transmitter.

The diameter of each particle is within the order of 3 μm, regardless of the type of rotating blade used. Therefore, when the particle size in this range is sufficient, any rotating blade may be used, and it is desired to be on the order of 1 μm. Sometimes a wire type is used.

Next, Table 2 shows that the operating time of the apparatus of FIG.
The data are shown for seconds, 30 seconds, and 60 seconds. The particle size at 60 seconds is the same as that in Table 1.
However, atomization on the order of 1 μm to 5 μm has occurred even when operated for only 15 seconds or 30 seconds.

[0022]

[Table 2]

The particle size distribution is calculated as follows: distribution ratio = (D ₉₀ -D
₁₀₎ / D is shown as _50, the D _90, D ₁₀ is 90%, counting from the smallest particle size distribution, particle diameter corresponding to 10% th, D ₅₀ is the median particle diameter of the particle size distribution, distribution The smaller the ratio is, the more homogeneous it is, most of which is in the range of 0.4 to 0.75.

4 and the following are graphs of the data of Tables 1 and 2, wherein φ152W and the like in the upper column in FIGS. 4 to 8 indicate the outer diameter and model of the rotating blade, and 47 indicates the peripheral speed of the rotating blade m /.
s, (9, 18, 35) or (18, 35) is the film thickness m
m, (15, 30, 60) indicates the second of the operation time. In each figure, the graph on the left shows the relationship between the average particle size and the operation time, and the graph on the right shows the relationship between the average particle size and the distribution ratio at each measurement.

As is clear from these graphs, the average particle size becomes extremely small after 15 seconds of stirring time, and the curves showing the changes in the average particle size have small slopes, respectively. Horizontal, particle size is mostly 3μ
m or less. In addition, since the distribution ratio curve also changes in the vertical direction and there is little change in left and right, it can be seen that uniform fine particles are produced in an extremely short time.

FIG. 9 shows the relationship between the average particle diameter and the peripheral speed conversion value after operating for 60 seconds at a film thickness of 18 mm and 35 mm. Obviously, they will be the same size. The frame shown in the figure shows the shape and outer diameter of the rotating blade used. For example, in a frame showing a cylinder type φ152C, the particle diameter is almost the same regardless of the thickness of the film thickness. Similarly, blade type φ152D, milling type φ15
2M, wire type φ150W and φ152W also have the same tendency, and the average particle diameter is almost the same regardless of the film thickness. However, as for the size of the average particle diameter, the type of the rotary blade becomes smaller in the order of the cylinder type C, the blade type D, the milling type M, and the wire type W.

Therefore, it can be seen that, when the stirring is performed within 60 seconds under the pressure P at which a constant peripheral speed conversion value is generated, the average particle diameter is determined by the type of the rotating blade.

FIG. 10 is a graph showing the unit energy (E / cc) and the numerical value of the converted value of the peripheral speed V shown in Table 1. The curve 1 connecting the data is almost a quadratic curve, and the motion Since the energy is proportional to the square of the speed, it is understood that the energy corresponding to the peripheral speed converted value V of the liquid to be treated is consumed irrespective of the outer diameter and the type of the rotary blade.

Although the example in which the rotating blades are driven at 47 m / see has been described above, the same tendency was observed at 40 m / see and other cases.

[0030]

As described above, according to the present invention, the particle diameter of the fine particles to be emulsified is determined by the type of the rotary blade and the average peripheral speed of the liquid to be treated. It is determined by the specific gravity and the pressure, so that the type of the rotary blade is determined, the pressure of the liquid to be treated is set, and a liquid amount is supplied so that the film thickness becomes a predetermined size. It is effective in a short time.

[Brief description of the drawings]

FIG. 1 is a longitudinal sectional view showing one embodiment of a stirring device for carrying out the present invention.

FIG. 2 is a longitudinal sectional view of another embodiment.

FIG. 3 is a perspective view of a rotating blade.

FIG. 4 is a graph of data obtained by a wire type rotating blade.

FIG. 5 is a graph of data obtained by using another wire type rotating blade.

FIG. 6 is a graph of data from a milling type rotating blade.

FIG. 7 is a graph of data from a blade-type rotating blade.

FIG. 8 is a graph of data from a cylinder type rotating blade.

FIG. 9 is a graph showing a relationship between an average particle diameter and a liquid peripheral velocity.

FIG. 10 is a graph showing a relationship between driving energy and liquid peripheral speed.

[Explanation of symbols]

2 Container 3, 3a Weir plate 5, 6 Raw material supply pipe 7 Product outflow pipe 8, 9, Cooling chamber 10 Pressure transmitter 11 Rotary shaft 12 Rotary blade W Wire type rotary blade M Milling type rotary blade D Blade type rotary blade C Cylinder type rotary blade A container inner diameter φ rotary vane outside diameter A pressure L liquid to be treated t _1, t _2, t ₃ thickness

──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Yasuko Waka 8-16-43 Ebie, Fukushima-ku, Osaka-shi, Osaka, Japan (56) References JP-A-9-75698 (JP, A) ( 58) Fields surveyed (Int.Cl. ⁶ , DB name) B01F 3/00-3/22 B01F 7/00-7/32

Claims (3)

(57) [Claims] 1. In a cylindrical container containing a liquid to be treated,
The rotating blade having an outer diameter slightly smaller than the inner diameter of the container is rotated at a high speed, and the liquid to be treated is pressed against the inner surface of the container by the rotational force and the centrifugal force generated in the liquid to be treated while rotating in a cylindrical film shape. In the high-speed stirring method of generating fine particles by stirring, the peripheral speed of the liquid to be treated corresponding to the desired particle diameter of the liquid to be treated is set in advance, the pressure on the peripheral surface of the liquid to be treated is detected, The inner peripheral diameter of the liquid to be treated is calculated from the thickness and the specific gravity of the liquid to be treated, and the pressure, and the pressure at which the set peripheral velocity is generated is generated. A high-speed stirring method characterized by adjusting each rotation speed. 2. The method according to claim 1, wherein the pressure on the surface of the liquid to be treated is P, the inner diameter of the container is R, and the thickness of the liquid to be treated in the form of a cylindrical film is t.
When the specific gravity of the liquid is ρ, the average peripheral velocity v is given by the following equation: A high-speed stirring method, wherein the speed of the rotating blades is adjusted so as to generate the pressure P determined by the above method. 3. In a cylindrical container containing a liquid to be treated,
The rotating blade having an outer diameter slightly smaller than the inner diameter of the container is rotated at a high speed, and the liquid to be treated is agitated while being rotated in a cylindrical film shape along the inner surface of the container by the rotational force and centrifugal force generated in the liquid to be treated. In a high-speed stirring device that generates fine particles, a pressure detector that detects the pressure of the outer peripheral surface of the liquid to be treated is provided on the side wall of the container, and a speed change unit is provided in the driving unit of the rotating blade, and a desired particle diameter is generated. A high-speed stirring device wherein a pressure of a liquid is set in advance, and a rotating blade is driven at a rotation speed at which the pressure is generated.