JPH09150049A - Stirring of powder, treatment of powder, powder stirring device and powder treating device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To inhibit power from becoming flocculated and sticking to an internal wall and, enable the efficient and uniform stirring of powder to be achieved by storing the powder in a container with a membrane to be vibrated by a sonic wave at the bottom and giving a mechanical vibration to this container to effect a complex stirring action. SOLUTION: Powder 3 is stored in a container 1 and a membrane 2 is vibrated by giving a sonic wave 7 with the help of a speaker 6 installed at the lower part of the container 1 toward the bottom. Simultaneously, a mechanical vibration is applied to the container 1 using a vibrating motor 9 equipped with a balancer 8. In this case, the powder 3 shows such a fluidized state by the vibration of the sonic wave 7 that the powder 3 seems to be boiling up from bottom to top without being blown up, unless the mechanical vibration is applied. Thus it is adjusted so that the surface of a new powder is constantly moved upward. In addition, the powder 3 on a membrane 2 is caused to show a vortex motion heading for the center of the container from the internal wall by adjusting the balancer 8, when the mechanical vibration is given without the vibration by the sonic wave 7. The efficient stirring action is accomplished as described above.

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to a powder stirring method,
The present invention relates to a powder processing method, a powder stirring device, and a powder processing device.

[0002]

2. Description of the Related Art Powders, such as pigments used in paints and inks, have poor surface dispersibility in matrix resins when their surfaces are chemically inactive, resulting in problems in fluidity and storage stability. Occurs. In order to solve these problems, a low temperature plasma treatment of the pigment surface is performed as a physicochemical method. In order to perform these treatments uniformly on the pigment surface, the untreated surface of the pigment must be constantly exposed to an active atmosphere in which plasma treatment is performed.

However, the usual stirring method causes problems such that the fine particles of the pigment are solidified due to the influence of the adsorbed water on the surface of the pigment or the static electricity, so-called granulation, and sticking to the inner wall surface of the container. In order to overcome these problems, various stirring methods have been conventionally used. For example,
A method of treating the pigment surface while stirring the pigment by rotating or rocking a drum containing the pigment, and a method of treating the pigment surface while stirring the pigment with a propeller or a magnetic stirrer are disclosed in JP-A-56. -15563
No. 1, JP-A-57-177342, JP-A-Sho 5
It is described in, for example, JP-A 8-205540 and JP-A-59-145038.

[0004]

However, a method of treating the pigment while stirring the pigment by rotating and rocking the drum,
In the method of treating with stirring with a propeller or magnetic stirrer, granulation or sticking to the inner wall of the container is likely to occur, and efficient stirring cannot be performed, so that uniform treatment cannot be performed on the pigment surface. . As a result, even if the pigments obtained by these treatments were used, an ink or paint having good fluidity and storage stability could not be obtained.

The object of the present invention is to solve the problems of the above-mentioned conventional methods for treating the surface of a pigment, in which powders such as pigments are uniformly agitated and the surface of the new powder is constantly exposed to the external atmosphere. The stirring method of the powder exposed to, the stirring device of the powder used in this stirring method, the powder of the pigment or the like is uniformly stirred,
It is an object of the present invention to provide a powder treatment method for treating an untreated powder surface while always exposing it to an external atmosphere capable of treatment, and a powder treatment apparatus used in this treatment method.

[0006]

Means for Solving the Problems The inventors of the present invention have made extensive studies to solve the above-mentioned problems, and as a result, contained powder in a container having a membrane vibrating by a sound wave at the bottom, and When a powder is agitated using a device that simultaneously provides mechanical vibration and vibration due to sound waves, granulation of the powder and sticking to the inner wall surface of the container are suppressed, and a new powder surface is obtained. The powder is efficiently stirred evenly so that it is continuously exposed to the upper space of the powder, and the powder is efficiently and uniformly stirred. By performing the treatment of 1, the new powder surface is always exposed to the active energy ray irradiation side, so it is possible to perform an efficient and uniform treatment of the powder surface, The present invention has been completed.

That is, according to the present invention, (1) the powder is contained in a container having a membrane vibrating at the bottom by a sound wave, and the powder is agitated by applying mechanical vibration and vibration at the bottom of the container. A method of stirring powder, characterized by
(2) The method for agitating the powder as described in (1) above, wherein the powder is a pigment,

(3) The powder is contained in a container having a film capable of vibrating by a sound wave at the bottom, and mechanical vibration and vibration by a sound wave are applied to the bottom of the container to activate the powder while stirring. A method for treating a powder characterized by irradiating an energy ray, (4) a method for treating a powder according to the above (3), wherein the powder is irradiated with an active energy ray in the presence of gas.
The method for treating powder according to (4) above, wherein the gas is a gas that reacts with the surface of the powder upon irradiation with active energy rays.
(6) The method for treating powder according to the above (3), (4) or (5), wherein the powder is a pigment,

(7) A container having a membrane vibrating at the bottom by sound waves, a mechanism for applying mechanical vibration to the bottom of the container, and a mechanism for applying vibration to the bottom of the container by sound waves. (8) The stirring apparatus according to (7) above, wherein the mechanism for imparting vibration by a sound wave to the bottom of the container is a mechanism using a speaker as an output source of the sound wave. Apparatus, (9) The stirring according to the above (7) or (8), wherein the mechanism for imparting mechanical vibration to the bottom of the container is a mechanism for imparting mechanical vibration to the bottom of the container by a vibration motor equipped with a balancer. apparatus,

(10) A container having a membrane vibrating by a sound wave at the bottom, a mechanism for imparting mechanical vibration to the bottom of the container, and a mechanism for imparting vibration by the sound to the bottom of the container. A powder processing apparatus having a mechanism for irradiating an active energy ray to the bottom of the container, (11) a mechanism for imparting vibration by sound waves to the bottom of the container serves as an output source of sound waves. The processing device according to (10) above, which is a mechanism using a speaker, (12)
The processing device according to (10) or (11) above, wherein the mechanism for applying mechanical vibration to the bottom of the container is a mechanism for applying mechanical vibration to the bottom of the container by a vibration motor equipped with a balancer. The mechanism for irradiating the bottom of the container with active energy rays is an ultraviolet irradiation device (1).
0), (11) or (12) The treatment apparatus according to (12), and (14) The container is any one of the above (10) to (13), which is a container having a gas introduction hole into the container. The above-mentioned powder processing apparatus is provided.

[0011]

BEST MODE FOR CARRYING OUT THE INVENTION The container used in the present invention may be any container having a membrane vibrating by a sound wave at the bottom, and the shape is not limited, but normally the bottom is flat and the center of the bottom is A container that has a membrane that can be vibrated by a sound wave and whose membrane area occupies 80% or more of the bottom area is used. Above all, when the device is a batch type, the bottom is flat,
A container having a circular shape, an elliptic shape, a hexagonal or more polygonal shape, or a shape similar thereto and having a bottom portion entirely made of a film vibrating by a sound wave is preferable because the stirring is performed efficiently and uniformly. The size of the container varies depending on the amount of powder to be processed. The film at the bottom of the container is not particularly limited as long as it vibrates by a sound wave, and for example, a metal film such as stainless steel, copper, or aluminum, Teflon,
A resin film such as silicon can be used. The thickness of the film is preferably as thin as possible so that the vibration of the sound wave can be easily transmitted, but it is preferably about 0.01 to 3.0 mm in order to prevent the film from being broken by the vibration of the sound wave. In addition, in the container,
You may install the lid which can permeate | transmit an active energy ray as needed.

As a mechanism for applying a sound wave to the bottom of the container, any mechanism may be used as long as it has a structure capable of generating a sound wave capable of vibrating the film at the bottom of the container. The one used is general. The number of sound wave output sources is not limited to one, but when using speakers, in a batch-type device,
Usually, the number is one, and in a continuous type apparatus, it largely differs depending on the shape of the container, and usually one or more, preferably 1 to 20. The installation position of the sound wave output source may be at the lower part of the film at the bottom of the container, but when one speaker is used as the sound source, the center of the speaker and the center of the container bottom are perpendicular to the film. It is preferable to install at a position that is on the same line in the direction, and furthermore, due to the vibration of the film by the sound wave generated from the speaker, the powder will not rise and form a fluid state that boils from the bottom up, and a new powder surface It is particularly preferable to adjust the speaker installation position, the output, the frequency of the sound wave, and the like such that the speaker is moved from the center of the container bottom toward the outer inner wall while constantly exposing the speaker to the upper space of the powder. The frequency of the sound wave is usually 10 to 500 Hz, preferably 100 to 500 Hz.
At 300 Hz, the power is typically 0.5-300 W, preferably 3-50 W. In implementing the present invention, the output of the speaker and the frequency of the sound wave may be changed periodically or irregularly as necessary.

The mechanism for imparting mechanical vibration to the bottom of the container may be any mechanism having a structure for imparting mechanical vibration to the bottom of the container. For example, a mechanism for imparting mechanical vibration only to the bottom of the container, the entire container. There is a device that vibrates the bottom of the container by applying mechanical vibration to the inside of the container, but among them, like the mechanism that gives mechanical vibration to the entire container by a vibration motor equipped with a balancer, the inside of the container can be adjusted by adjusting the balancer. It is preferable that the movement of the powder can be controlled. Further, as the vibration motor used here, a motor whose balancer is adjusted so that the powder in the container subjected to the vibration moves spirally from the inner wall outside the container toward the center direction is preferable. At this time, the rotation speed of the vibration motor is generally 500 to 10000 rpm, preferably 3000 to 60 rpm.
00 rpm. In implementing the present invention, the rotation speed of the vibration motor may be changed periodically or irregularly as necessary.

Further, as the vibration due to the sound wave and the mechanical vibration, these vibrations are simultaneously applied to the bottom of the container in a complex manner, so that the powder at the bottom of the container vibrates in a state of spreading to the bottom of the container, It is desirable that the surface of the new powder is adjusted so that it is always exposed to the space above the powder.
For example, the powder on the membrane at the bottom of the container does not soar, but forms a fluid state that boils from bottom to top,
While constantly exposing the new powder surface to the upper space of the powder, the vibration by the sound wave is adjusted so that the powder moves from the center of the container bottom toward the outer inner wall, while the powder on the film at the bottom of the container is adjusted. The mechanical vibration is adjusted so as to move from the inner wall outside the container toward the center, preferably in a spiral shape,
It is particularly preferable to adjust the movement of the powder by these two kinds of vibrations so that the powder at the bottom of the container continues to vibrate while spreading to the bottom of the container.

The powder used in the present invention includes metal powder and
It is not particularly limited as long as it is in powder form such as plastic powder, organic pigment, inorganic pigment, etc.
Pigments such as inorganic pigments are preferable, and organic pigments are particularly preferable. Examples of the organic pigment here include azo pigments,
Polycondensed azo pigment, metal complex azo pigment, flavanthrone pigment, phthalocyanine pigment, quinacridone pigment, anthraquinone pigment, anthrapyridine pigment, pyranthrone pigment, dioxazine pigment, perylene pigment, perinone pigment, Isoindolinone pigment, quinophthalone pigment, thioindigo pigment,
Indanthrene-based pigments and the like, and examples of inorganic pigments include zinc white, titanium oxide, antimony white, carbon black, iron black, red iron oxide, mapico yellow, red lead, cadmium yellow, zinc sulfide, lithopone, barium sulfate, and lead sulfate. , Barium carbonate, calcium carbonate, lead white, alumina white and the like.

When a powder having adsorbed water on the surface or a powder having a wide particle size distribution of powder is used, the adsorbed water is removed from the powder by heating drying or vacuum drying in advance. If the particle diameters of the powder are made uniform by sieving or the like, granulation of the powder is less likely to occur during stirring, and stirring can be performed more efficiently, which is preferable.

Examples of the active energy ray used for treating the powder include ultraviolet rays, electron rays, α rays, β rays, γ rays, visible rays, infrared rays, and the like. Among them, ultraviolet rays are generally used and are treated. It is also preferable in terms of efficiency.

The mechanism for irradiating the active energy ray may be any one capable of irradiating the active energy ray on the bottom of the container. For example, an ultrahigh pressure mercury lamp, a high pressure mercury lamp, a low pressure mercury lamp, a metal halide lamp, a chemical lamp, A black light lamp, a mercury-xenon lamp, a short arc lamp, etc. are mentioned, and they are usually mounted on the upper part of the container.

The treatment of the powder by irradiation with active energy rays is carried out in the presence of various gases such as an inert gas or an active gas which reacts with the powder surface at the time of irradiation with active energy rays. You can also When the treatment is carried out in the presence of an inert gas, the powder surface is activated by the etching effect on the powder surface by irradiation with active energy rays. Affinity is high, and paints and inks with excellent dispersion stability and fluidity can be obtained. In addition, when an active energy ray, for example, an ultraviolet ray irradiation treatment is performed in the presence of the active gas, radicals of the active gas are generated by the ultraviolet rays, and the radicals of the active gas react with the powder surface and are directly taken in. At the same time, a synergistic effect is obtained in which the active points generated on the powder surface due to the etching effect on the powder surface by the irradiation of active energy rays and the radicals of the active gas are more easily reacted and taken in. For example, when oxygen or ammonia gas is used as an active gas, ultraviolet rays generate oxygen radicals or ammonia radicals, which react with the powder surface and are taken in, so that carboxyl groups or amino groups are formed on the powder surface. Generate.

The gases used here include helium, argon, nitrogen, oxygen, ammonia, carbon dioxide,
Gases such as hydrogen, fluorine, chlorine and carbon tetrafluoride, organic compounds such as triethylamine, triethanolamine, methanol, ethanol, benzene and toluene, styrene, acrylic acid, methacrylic acid, methyl methacrylate,
Any compound capable of becoming a gas, such as a monomer such as ethyl acrylate, may be used. Further, the gas to be introduced is not limited to one type, and two or more types of gas may be used at the same time.

There is no problem with the flow rate of the gas as long as the powder surface is sufficiently treated, but preferably 5 to 1 per minute.
It is 00 ml.

The treatment time for carrying out the method for treating powder according to the present invention varies greatly depending on the size of the apparatus, the amount of powder, the irradiation amount of active energy rays, etc., but it is usually 1 minute to 24 minutes.
Time, preferably 5 minutes to 10 hours.

FIG. 1 shows an example of a batch-type apparatus for carrying out the powder stirring method and treatment method of the present invention. In FIG. 1, 1 is a container having a membrane vibrating by a sound wave at the bottom, 2 is a membrane vibrating by a sound wave, 3 is a powder, 4 is a gas inlet, 4'is a gas outlet, 5 is an inlet 4 From the outlet 4 ', 6 is a speaker, 7 is a sound wave generated from the speaker 6, 8 is a balancer, and 9 is a vibration motor having a balancer 8.
Reference numeral 0 is a spring that holds the container 1, 11 is an active energy ray irradiation lamp, 12 is an active energy ray emitted from the active energy ray irradiation lamp 11, and 13 is a transparent glass lid.

In FIG. 1, a concrete example of the container 1 is as follows.
A stainless steel sieve with a diameter of 30 cm at the bottom and a height of 8 cm was modified, and a stainless steel screen with a thickness of 0.3 mm was used instead of the screen at the bottom of the sieve.
The container 1 is held by a spring 10, and the bottom of the container 1 can receive the vibration by the speaker 6 and the vibration motor 9 at the lower part of the container and the irradiation of the active energy ray from the active energy ray irradiation lamp at the upper part of the container. It has become.

To carry out the powder stirring method of the present invention,
For example, the powder 3 is housed in the container 1, and the membrane 2 is vibrated by applying a sound wave 7 from a speaker 6 installed below the bottom of the container 1, and the vibration motor 9 having a balancer 8 is used to vibrate the container 1. Mechanical vibration should be applied to. At this time, the vibration caused by the sound wave 7 forms a fluidized state in which the powder 3 does not rise up but boil from the bottom to the top when there is no mechanical vibration, and the new powder surface is always kept above the powder. It is preferably adjusted so as to move from the center of the bottom of the container toward the outer inner wall while being exposed to the space, that is, the side where active energy rays are radiated, and the mechanical vibration is obtained when there is no vibration due to the sound wave 7. The balancer 8 is preferably adjusted so that the upper powder 3 moves spirally from the inner wall toward the center. Furthermore, these 2
It is particularly preferable that the seed vibration is adjusted so that the movement of the powder 3 due to these vibrations is balanced and the powder 3 is continuously subjected to the vibration while maintaining the state of spreading to the bottom of the container. As a result, a uniform stirring state can be obtained without the powder 3 staying in a certain place or causing granulation or adhesion to the inner wall surface of the container. If this balance cannot be achieved, one of the vibrations can be temporarily stopped as necessary, and this can be repeated.

To carry out the method for treating powder according to the present invention,
For example, an active energy ray irradiation lamp is introduced into the powder 3 which is uniformly stirred in the container 1 as described above, while introducing a gas 5 through the introduction hole 4 as needed and flowing out through the outlet 4 ′. The active energy ray 12 may be irradiated from 11 through a glass lid 13. As an example, a container having a bottom diameter of 30 cm and a height of 8 cm was used.
When the processing time when processing 00 g of the organic pigment is shown,
Usually 10 minutes to 8 hours.

FIG. 1 shows a batch type apparatus,
This apparatus is, for example, as shown in FIG. 2, by installing a powder supply port 14 to the center of the container bottom and a powder discharge port 15 from the vicinity of the inner wall surface of the container, thereby providing a continuous apparatus. It becomes possible. At this time, the vibration by the sound wave 7 and the mechanical vibration applied to the powder 3 may be adjusted so that the powder 3 slowly moves from the center of the container 1 toward the inner wall. In this state, irradiation of active energy rays is performed in the presence of a gas as necessary, so that the powder 3 supplied from the powder supply port to the center of the container 1 moves from the center on the film 2 toward the inner wall. The surface treatment is performed when moving to, and the treated powder is discharged from the discharge port of the powder, so that continuous processing can be performed. The device shown in FIG. 1 is provided with an inlet for powder near the inner wall surface of the container and an outlet for powder from the center of the bottom of the container. By adjusting the above two kinds of vibrations so that 3 moves from near the inner wall surface of the container toward the center of the container bottom, continuous processing can be performed.

When the surface treatment of powder is carried out continuously and in large quantities industrially, for example, a container having a membrane vibrating by a sound wave at the bottom is provided with a powder supply port such as a hopper on one side and the other side. A powder discharge port is installed on the bottom, and a material that can be vibrated by a sound wave from a speaker on the bottom, such as stainless steel,
A vibratory feeder for transporting powder, which is provided with a film made of metal such as copper or aluminum, or a film made of resin such as Teflon or silicon can be used. The vibratory feeder is given mechanical vibration of the motor so that the powder on it moves from the powder supply port side to the discharge port side, and by applying sonic vibration from multiple speakers from below, the powder is While moving in the vibrating feeder from the supply port to the discharge port, it is agitated in the up and down direction by the acoustic vibration. An active energy ray irradiation device is installed above the vibration feeder. It is desirable to cover the upper part of the vibrating feeder with glass or the like that transmits the energy beam so that the stirred powder does not adhere to the active energy beam irradiation device. A gas supply port and a gas discharge port for flowing gas can be installed at any position in the vibrating feeder, but a gas supply port is provided near the powder supply port of the vibrating feeder, and a gas supply port is provided near the powder discharge port. It is desirable in terms of processing efficiency to provide an outlet. There is no problem even if the moving speed of the powder is adjusted by inclining the vibrating feeder according to the specific gravity and the particle diameter of the powder.

[0029]

EXAMPLES The present invention will be described more specifically below with reference to Examples and Comparative Examples. The parts and percentages in the examples are on a weight basis.

Example 1 In a container 1 having a diameter of 30 cm and a height of 8 cm, in which a bottom surface shown in FIG. 1 was covered with a stainless steel film having a thickness of 0.3 mm, heat drying was performed at 80 ° C. under reduced pressure for 48 hours. After adding 50 g of quinacridone pigment and replacing the inside of the container 1 with nitrogen gas, 10 minutes per minute
The surface treatment was carried out by irradiating ultraviolet rays while stirring the pigment while mechanically vibrating it with a vibration motor and vibrating a sound wave with a speaker having an inner diameter of 20 cm while flowing ml of oxygen gas. The rotation speed of the vibration motor is 6000 rpm,
The sound wave had a frequency of 150 Hz and an output of 10 W. As the ultraviolet light source, a low-pressure mercury lamp capable of irradiating with ultraviolet light having a wavelength of 184.9 nm and 253.7 nm was used. The irradiation distance to the treated pigment was 10 cm, and the treatment time was 60 minutes.

Under stirring under the above conditions, during the treatment,
There is no rising of pigment, granulation, and sticking to the inner wall of the container.The pigment vibrates in the state that it spreads to the bottom of the container, and the new pigment surface is always exposed to the outside atmosphere. It was

Next, a coating test with an acrylic resin was conducted using the UV-treated quinacridone pigment obtained by the above treatment.

The acrylic resin used was 500 parts of methyl methacrylate, 366 parts of ethyl acrylate, 130 parts of β-hydroxyethyl methacrylate and 4 parts of β-dimethylaminoethyl methacrylate, and perbutyl-O.
3 parts and 2,2'-azobisisobutyronitrile 15
Was used as an initiator in 500 parts of xylene and 500 parts of butyl acetate by the drop-wise polymerization method. The resulting acrylic resin has a solid content of 50%, and the molecular weight measured by GPC is 100 in terms of polystyrene.
00 and a weight average molecular weight of 30,000.

The paint preparation method is as follows. 250m
l Polyethylene bottle with UV treated quinacridone pigment 10
Parts, 3 mmφ glass beads 150 parts, xylene: n-butanol = 3: 1 mixed solvent 32.5 parts and the above acrylic resin 32.5 parts were added and dispersed by a paint conditioner for 120 minutes to prepare a dispersion paste. 97.8 parts of the above acrylic resin and 27.2 parts of melamine resin (manufactured by Dainippon Ink and Chemicals, Inc .: Super Beckamine L-117-60) were further added to this dispersion paste and dispersed for 5 minutes to form a coating material.

A tin plate is flow-coated with the obtained acrylic coating and baked at 120 ° C. for 20 minutes to prepare an acrylic coated plate, and the 20 ° gloss of the coated plate is measured with a haze-gloss reflectometer manufactured by Vic-Gardner Co., Ltd. according to JIS.
It was measured according to K-5400. Further, the paint viscosity was measured with a B-type viscometer. Table 1 shows 20 ° gloss of coated plate,
Paint viscosity at 60 rpm and T.I. I. The values (ratio of viscosity values when the rotation speed of the rotor is 6 rpm and 60 rpm) are shown.

The obtained coating material was excellent in fluidity, and the baking coated plate was a smooth and glossy coated plate.

Example 2 The quinacridone pigment was treated in the same manner as in Example 1 except that the frequency and output of the sound wave were changed to 200 Hz and 4 W. Under stirring under these conditions, there is no rising of the pigment, granulation, or sticking to the inner wall of the container, and the pigment vibrates in the state of spreading to the bottom of the container, ideally the new pigment surface is always exposed to the outside atmosphere. Thus, the stirring state was uniform.

Then, a coating material was obtained in the same manner as in Example 1 except that the obtained UV-treated quinacridone pigment was used.
A paint test was conducted. Table 1 shows 20 ° gloss of coated plate, 60 rp
m paint viscosity and T.M. I. Indicates a value.

The obtained coating material was excellent in fluidity, and the baking coated plate was a smooth and glossy coated plate.

Comparative Example 1 A paint was prepared and a paint test was conducted in the same manner as in Example 1 except that an untreated quinacridone pigment was used in place of the quinacridone pigment which had been subjected to the UV treatment. Table 1 shows 20 coated plates
Gloss, paint viscosity at 60 rpm and T.I. I. Indicates a value.

The paint obtained had poor fluidity, and the baking coated plate had a poor gloss.

Comparative Example 2 The quinacridone pigment was treated with ultraviolet light in the same manner as in Example 1 except that stirring was not performed by sonic vibration. Under stirring under these conditions, the pigment only slides on the bottom of the container, there is no flow state such as boiling up from the bottom, and the new pigment surface is always exposed to the outside atmosphere. There wasn't.

Then, a coating material was obtained in the same manner as in Example 1 except that the obtained UV-treated quinacridone pigment was used.
A paint test was conducted. Table 1 shows 20 ° gloss of coated plate, 60 rp
m paint viscosity and T.M. I. Indicates a value.

The obtained coating composition had poor fluidity and the baking coated plate had a poor gloss.

[0045]

[Table 1]

Example 3 A diaminoanthraquinone pigment was treated in the same manner as in Example 1 except that a diaminoanthraquinone pigment was used instead of the quinacridone pigment and the frequency and output of the sound wave were changed to 230 Hz and the output was 4.5 W. . Under stirring under these conditions, there is no rising of the pigment, granulation, or sticking to the inner wall of the container, and the pigment vibrates in the state of spreading to the bottom of the container, ideally the new pigment surface is always exposed to the outside atmosphere. Thus, the stirring state was uniform.

Then, in the same manner as in Example 1 except that the obtained UV-treated diaminoanthraquinone pigment was used,
A paint was obtained and a paint test was conducted. Table 2 shows the 20 ° gloss of the coated plate, the coating viscosity at 60 rpm and the T.I. I. Indicates a value.

The obtained coating material was excellent in fluidity, and the baking coated plate was a smooth and glossy coated plate.

Comparative Example 3 A paint was prepared and a paint test was conducted in the same manner as in Example 1 except that an untreated diaminoanthraquinone pigment was used in place of the UV-treated diaminoanthraquinone pigment. Table 2 shows the 20 ° gloss of the coated plate, the coating viscosity at 60 rpm and the T.I. I. Indicates a value.

The resulting coating had poor fluidity and the baking coated plate had a poor gloss.

[0051]

[Table 2]

Example 4 The same as Example 1 except that the perylene pigment was used in place of the quinacridone pigment, the ammonia gas was used in place of the oxygen gas, and the frequency and output of the sound wave were changed to 80 Hz and 2.5 W, respectively. To treat the perylene pigment. Under this condition, there is no rising of the pigment, granulation, and sticking to the inner wall of the container, the pigment vibrates in the state of spreading to the bottom of the container, and the new pigment surface is always exposed to the outside atmosphere Ideal and uniform It was in a good stirring state.

Next, a coating test with an acrylic resin was conducted using the obtained ultraviolet-treated perylene pigment. The paint preparation method is as follows.

UV-treated perylene pigment 10 parts, 3 mmφ glass beads 150 parts, acrylic resin (Dainippon Ink and Chemicals Incorporated: Acridic A-801-P) 38.0 parts in a 250 ml polyethylene bottle, xylene: butyl acetate =
25.0 parts of 6: 4 mixed solvent was added and dispersed for 120 minutes by a paint conditioner to prepare a dispersion paste. The acrylic resin 95.
0 part and 32.0 parts of urethane resin (manufactured by Dainippon Ink and Chemicals, Inc .: Barnock DN-980) were added and dispersed for 5 minutes to form a paint.

A tin plate was flow-coated with the obtained acrylic paint and dried at room temperature for 1 week to prepare an acrylic coated plate. Table 3 shows the 20 ° gloss of the coated plate. The coated plate obtained was a smooth and glossy coated plate.

Comparative Example 4 A paint was prepared and a paint test was conducted in the same manner as in Example 4 except that an untreated perylene pigment was used in place of the ultraviolet-treated perylene pigment. Table 3 shows the 20 ° gloss of the coated plate.

The coated plate thus obtained had a poor gloss.

[0058]

[0059]

EFFECTS OF THE INVENTION According to the stirring method of the present invention, granulation of powder and sticking to the inner wall surface of the container are suppressed, and stirring is performed so that the new powder surface is always exposed to the upper space of the powder. Thus, the powder is efficiently and uniformly stirred. When the powder surface is treated by irradiating it with active energy rays while performing this stirring, the new powder surface is treated in a state where it is always exposed to the active energy ray irradiation side, so an efficient and uniform powder is obtained. Body surface treatment can be performed.

[Brief description of the drawings]

FIG. 1 is a schematic diagram showing an example of a batch-type apparatus for carrying out the powder stirring method and treatment method of the present invention.

FIG. 2 is a schematic view showing an example of a continuous apparatus for carrying out the powder stirring method and the powder processing method of the present invention.

[Explanation of symbols]

1 Container having a membrane vibrated by sound waves at the bottom 2 Membrane vibrated by sound waves 3 Powder 4 Gas inlet 4'Gas outlet 5 Gas introduced from inlet 4 Gas 5'Outflow from outlet 4 ' 6 Speaker 7 Sound Wave Generated from Speaker 6 8 Balancer 9 Vibration Motor with Balancer 8 10 Spring Holding Container 1 Active Energy Ray Irradiation Lamp 12 Active Energy Ray Irradiated from Active Energy Ray Irradiation Lamp 13 Transparent Glass Made lid 14 powder supply port 15 powder discharge port

Claims (14)

[Claims] 1. A powder characterized in that the powder is contained in a container having a membrane vibrating at the bottom by a sound wave, and the powder is agitated by applying mechanical vibration and vibration at the bottom of the container. How to stir the body. 2. The method for stirring powder according to claim 1, wherein the powder is a pigment. 3. The powder is contained in a container having a film capable of vibrating by a sound wave at the bottom, and mechanical energy and vibration by a sound wave are applied to the bottom of the container to stir the powder while the active energy is added to the powder. A method for treating powder, which comprises irradiating a ray. 4. The method for treating powder according to claim 3, wherein the powder is irradiated with an active energy ray in the presence of gas. 5. The method for treating powder according to claim 4, wherein the gas is a gas that reacts with the surface of the powder upon irradiation with active energy rays. 6. The method for treating powder according to claim 3, 4 or 5, wherein the powder is a pigment. 7. A container having at its bottom a membrane vibrating by sound waves, a mechanism for imparting mechanical vibration to the bottom of the container, and a mechanism for imparting vibration to the bottom of the container by acoustic waves. A powder agitator characterized by having. 8. The stirrer according to claim 7, wherein the mechanism for imparting vibration by a sound wave to the bottom of the container is a mechanism using a speaker as a sound wave output source. 9. The stirrer according to claim 7, wherein the mechanism for applying mechanical vibration to the bottom of the container is a mechanism for applying mechanical vibration to the bottom of the container by a vibration motor equipped with a balancer. 10. A container having a membrane vibrating at the bottom by sound waves, a mechanism for applying mechanical vibration to the bottom of the container, and a mechanism for applying vibration to the bottom of the container by sound waves. And a mechanism for irradiating the bottom of the container with active energy rays. 11. The processing apparatus according to claim 10, wherein the mechanism for imparting vibration by a sound wave to the bottom of the container is a mechanism using a speaker as an output source of the sound wave. 12. The processing apparatus according to claim 10, wherein the mechanism for applying mechanical vibration to the bottom of the container is a mechanism for applying mechanical vibration to the bottom of the container by a vibration motor equipped with a balancer. 13. The processing apparatus according to claim 10, 11 or 12, wherein the mechanism for irradiating the bottom of the container with active energy rays is an ultraviolet irradiation device. 14. The powder processing apparatus according to claim 10, wherein the container has a gas introduction hole into the container.