JPH11285630A - Production of hydrophilic grain and production device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To produce hydrophilic grains having a relatively small and uniform diameter with a convenient device and operation in a short time at a low cost without charging the grains. SOLUTION: This device 21 for producing hydrophilic grains is provided with an atomizer 10 for atomizing a soln. 14 made of an acidic soln. dissolving a hydrophobic substance and a mixing part 22b for bringing the liq. grain granulated in the atomizer 10 into contact with steam to form supersaturated steam and to condense water on the liq. grain surface. By dissolving the hydrophobic substance in the acidic soln., the hydrophilic property is provided. When the supersaturated steam is brought into contact with the liq. grain, by condensing the steam making the liq. grain as a nucleus, the steam is mixed with the acidic soln. to dilute the acidic soln. Consequently, the hydrophilic substance (the hydrophobic substance made to hydrophilic) dissolved in the acidic soln. is deposited due to the dilution of the acidic soln. to be the hydrophilic grain.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and an apparatus for producing hydrophilic particles such as a treated pigment in which a hydrophobic substance such as a pigment having a hydrophobic property is provided with a hydrophilic property. More specifically, the present invention relates to a method and apparatus for producing hydrophilic particles from a solution obtained by dissolving a hydrophobic substance in an acidic solution so as to impart hydrophilicity to the hydrophobic substance.

[0002]

2. Description of the Related Art Conventionally, various methods for modifying the properties of various particles have been proposed. More specifically, for example, a modification method for imparting hydrophilicity by forming a film of a modifier on a particle surface by treating particles having hydrophobicity (hydrophobic substance) with a modifier, Various modification methods for coating the surface with a modifier having hydrophilicity have been implemented. As the reforming method, a dry method, a kneading method, a stirring method using a medium (a method of performing surface modification in a liquid phase), a spray drying method, and the like are known.

[0003] For example, "Powder Engineering Handbook" (edited by the Society of Powder Engineering; published by Nikkan Kogyo Shimbun) and "Particle Handbook"
(Edited by Jinpo Genji; published by Asakura Shoten Co., Ltd .; first edition, September 1, 1991, first edition) On pages 383-394, a surface modification method using a kneading and pulverizing method, a spray drying method, etc., is described. ing.

[0004] For example, "Particle Engineering-Fundamentals and Applications of Dispersion-" (edited by the Japan Powder Technology Association; published by Asakura Shoten Co., Ltd .; first edition of the first edition on June 25, 1994) 123
Page to 136 pages, using a high-speed rotary impact pulverizer, a grinding mill, a ball mill, a roll mill, a medium stirring type pulverizer, a dry pulverizer such as a jet mill, the powdery surface to the powdery particles A method for producing a coated composite particle having a modified particle surface property by binding different kinds of components (surface modifier) of the present invention is described.

[0005]

However, in the above-mentioned conventional reforming method, when the particles are treated with the modifying agent, the particles are stirred using a stirring device such as a stirring blade, so that the particles are subject to friction or the like. Will be charged. For this reason, handling of the resulting modified particles (hydrophilic particles) becomes difficult. Also,
In the above-mentioned conventional reforming method, the treatment requires a very long time. Furthermore, the operation when performing the processing is complicated, and
There is a problem that an expensive device must be used.

In addition, in the above-mentioned conventional modifying method, the particle size of the obtained modified particles depends on the particle size before the treatment, and when the particles are treated with the modifying agent, for example, agglomeration of the particles may occur. Therefore, the particle size of the obtained modified particles tends to be large and irregular. Furthermore, when processing submicron-order fine particles, it is difficult to stably perform processing on each individual particle.

Further, since the particles are treated with the modifier by stirring the particles using a stirrer, various chemicals such as the modifier are used in a much larger amount than the theoretical amount required for the treatment of the particles. And post-treatment such as waste liquid treatment is troublesome. Therefore, the above-described conventional method has a problem that the production cost (treatment cost) of the surface-modified particles is increased.

As described above, the conventional reforming method described above, that is,
In the above-mentioned conventional method for producing hydrophilic particles, it is possible to produce the hydrophilic particles having a relatively small and uniform particle size without charging the particles, and with a simple apparatus and operation in a short time and at low cost. Can not. Therefore, a manufacturing method and a manufacturing apparatus capable of manufacturing hydrophilic particles having a relatively small and uniform particle size without charging the particles, and in a short time and at a low cost with a simple device and operation, and It is expected.

The present invention has been made in view of the above-mentioned conventional problems, and an object of the present invention is to make it possible to compare the particle size without charging the particles, with a simple apparatus and operation, in a short time and at low cost. It is an object of the present invention to provide a manufacturing method and a manufacturing apparatus capable of manufacturing relatively small and uniform hydrophilic particles.

[0010]

In order to solve the above-mentioned problems, the method for producing hydrophilic particles according to the present invention is intended to impart hydrophilicity to a hydrophobic substance which is solid at normal temperature and normal pressure. After the solution obtained by dissolving the substance in the acidic liquid is formed into particles, the particles are brought into contact with steam containing water vapor having a temperature higher than the temperature of the particles to form a supersaturated atmosphere of the steam, and the surface of the particles is formed. It is characterized by condensing water.

According to the above method, the hydrophobic substance is imparted with hydrophilicity by dissolving in an acidic solution, and the hydrophobic substance is hydrophilized. Then, the steam containing water vapor forms a supersaturated atmosphere and mixes with the acidic liquid by contacting the particles, thereby diluting the acidic liquid.

For this reason, the hydrophilic substance dissolved in the acidic liquid (that is, the hydrophilized hydrophobic substance) precipitates as the acidic liquid is diluted to become hydrophilic particles. Therefore, unlike the conventional method of stirring particles using a stirring device such as a stirring blade, there is no possibility that the particles are charged by friction or the like.

Further, since an apparatus capable of generating steam containing water vapor is used, the processing can be performed in a short time with a simple apparatus and operation. Furthermore, since the hydrophilic particles are formed by precipitation, the particle size of the obtained hydrophilic particles does not depend on the particle size of the hydrophobic substance used, and
The particle diameter of the hydrophilic particles can be relatively small and uniform.

According to the above method, hydrophilic particles having a relatively small and uniform particle size can be produced in a short time and at low cost with a simple apparatus and operation without charging the particles. .

[0015] In the above method, the supersaturated atmosphere of the vapor is converted to a temperature higher than the temperature of the particles.
The supersaturated atmosphere was formed by contacting with steam containing steam, but the supersaturated atmosphere was cooled after mixing the particles with steam containing steam, or after mixing the particles with steam containing steam. It may be formed by adiabatic expansion.

In the method for producing hydrophilic particles of the present invention, the particles are preferably cooled and then brought into contact with steam. According to the above method, the vapor containing water vapor is more easily condensed with the particles as nuclei. Therefore, in the above method, the hydrophilic particles can be produced in a shorter time.

In the method for producing hydrophilic particles of the present invention, it is preferable that the hydrophobic substance is a pigment. According to the above method, pigment particles having hydrophilicity can be stably and simply produced.

In the method for producing hydrophilic particles of the present invention, the hue of the pigment is preferably red, blue or yellow. According to the above method, pigment particles having hydrophilicity and a hue of red, blue or yellow and suitable for a liquid crystal filter or the like can be stably and simply produced.

In the method for producing hydrophilic particles of the present invention, it is preferable that the acidic liquid further contains chlorosulfonic acid and / or sulfuric acid. According to the above method, hydrophilic particles to which hydrophilicity has been imparted by introducing a sulfonic acid group can be stably and simply produced.

In the method for producing hydrophilic particles of the present invention, it is preferable that the particles are further brought into contact with steam in the presence of an inert gas. According to the above method, for example, by using an inert gas as a carrier for particles, when the hydrophilic particles are formed by precipitation, an undesired reaction or action on the hydrophilic particles due to the carrier is eliminated. can do.

In order to solve the above-mentioned problems, the method for producing hydrophilic particles of the present invention dissolves a hydrophobic substance which is solid at normal temperature and pressure in an acidic liquid so as to impart hydrophilicity to the substance. A first step of forming the solution into particles, and contacting the particles with a vapor containing water vapor having a temperature higher than the temperature of the particles to form a supersaturated atmosphere of the vapor and condensing water on the particle surface And a third step of collecting and washing the hydrophilic particles obtained in the second step with water.

According to the above method, the hydrophobic substance is rendered hydrophilic by dissolving it in an acidic liquid, and the hydrophobic substance is rendered hydrophilic. Then, when a supersaturated atmosphere is formed and the particles come into contact with the particles, the vapor containing the water vapor condenses with the particles as nuclei, thereby mixing with the acidic liquid and diluting the acidic liquid.

For this reason, the hydrophilic substance dissolved in the acidic liquid (that is, the hydrophobic substance which has been hydrophilized) precipitates as the acidic liquid is diluted to become hydrophilic particles. Therefore, unlike the conventional method of stirring particles using a stirring device such as a stirring blade, there is no possibility that the particles are charged by friction or the like.

Further, since a device for generating steam containing water vapor is used, the treatment can be performed in a short time with a simple device and operation. Furthermore, since the hydrophilic particles are formed by precipitation, the particle size of the obtained hydrophilic particles does not depend on the particle size of the hydrophobic substance used, and the particle size of the hydrophilic particles is relatively small and Can be aligned.

Furthermore, since the obtained hydrophilic particles are collected and washed with water, impurities contained in the hydrophilic particles can be removed. Thereby, without charging the particles,
Moreover, with a simple device and operation in a short time and at low cost,
It is possible to produce hydrophilic particles having a relatively small and uniform particle size and from which impurities have been removed.

In the above method, instead of the second step, the particles are mixed with steam containing water vapor and then cooled to form a further supersaturated atmosphere of steam, and water is condensed on the surface of the particles. A step or a step of mixing the particles with steam containing water vapor and then adiabatically expanding to form a supersaturated atmosphere of steam and condensing water on the surface of the particles can be used as the second step.

In order to solve the above-mentioned problems, the apparatus for producing hydrophilic particles of the present invention dissolves a hydrophobic substance which is solid at normal temperature and normal pressure in an acidic liquid so as to impart hydrophilicity to the hydrophobic substance. A granulating device for forming the solution into particles, and a condensing device for bringing the particles granulated by the granulating device into contact with supersaturated steam containing water vapor to condense water on the particle surface. It is characterized by:

According to the above configuration, the solution containing the hydrophilic substance (that is, the hydrophobic substance that has been hydrophilized) is formed into particles by the granulator. The granulated particles are contacted with supersaturated steam containing water vapor in a condenser.

At this time, when the supersaturated vapor containing water vapor comes in contact with the particles, the supersaturated vapor is condensed with the particles as nuclei, mixed with the acidic liquid, and dilutes the acidic liquid. For this reason, the hydrophilic substance dissolved in the acidic liquid precipitates as the acidic liquid is diluted to become hydrophilic particles.

Therefore, unlike the conventional apparatus in which the particles are agitated by using a stirring device such as a stirring blade, there is no possibility that the particles are charged by friction or the like, and the processing can be performed in a short time with a simple apparatus and operation. be able to. Furthermore, since the hydrophilic particles are formed by precipitation, the particle size of the obtained hydrophilic particles does not depend on the particle size of the hydrophobic substance used, and the particle sizes of the hydrophilic particles are relatively small and uniform. be able to.

Thus, without charging the particles,
Moreover, with a simple device and operation in a short time and at low cost,
An apparatus capable of producing hydrophilic particles having a relatively small particle diameter and uniformity can be provided.

The supersaturated vapor may be brought into contact with the particles and a vapor containing water vapor having a temperature higher than the temperature of the particles, preferably saturated vapor, to form a supersaturated atmosphere of the vapor. The mixture with steam may be cooled or adiabatically expanded to form a supersaturated atmosphere of the steam.

The apparatus for producing hydrophilic particles of the present invention may further include a cooling device for cooling the particles granulated by the granulating device. According to the above configuration, since the particles are cooled by the cooling device, it is possible to provide a device that is more easily condensed and can produce hydrophilic particles in a shorter time.

[0034] In the apparatus for producing hydrophilic particles of the present invention, it is preferable that the granulating apparatus is a spraying apparatus for forming the solution into particles by spraying the solution.

According to the above configuration, since the solution is formed into particles by the spraying device, the particle diameter of the particles obtained by granulating the solution containing the hydrophilic substance can be made relatively small.
As a result, the particle size of the obtained hydrophilic particles can be further reduced. Thereby, it is possible to provide an apparatus capable of producing hydrophilic particles having a smaller particle diameter.

In the apparatus for producing hydrophilic particles of the present invention, it is desirable that the spraying apparatus further has a particle diameter adjusting section for adjusting the particle diameter. According to the above configuration, since the particle diameter is adjusted by the particle diameter adjusting unit, the particle diameter of the particles obtained by granulating the solution containing the hydrophilic substance is relatively small, and
It can be even more aligned. As a result, the particle size of the obtained hydrophilic particles can be further reduced and made uniform. This makes it possible to provide an apparatus capable of producing hydrophilic particles having a smaller and uniform particle diameter.

Another apparatus for producing hydrophilic particles of the present invention has a processing space inside, and has a steam generating section for generating a condensing agent vapor, and is connected to the steam generating section to be solid at normal temperature and normal pressure. For particles obtained by dissolving the hydrophobic substance in an acidic liquid to impart hydrophilicity to the hydrophobic substance,
A cooling pipe for condensing the condensing agent vapor, a particle inlet for introducing particles into the processing space of the steam generator, a particle outlet for taking out the processed particles from the cooling pipe, and a steam generator. An adjusting means for changing the temperature in the processing space and the temperature in the cooling pipe is provided.

Another apparatus for producing hydrophilic particles of the present invention has a processing space inside, and a steam generating section for generating a condensing agent vapor, and a processing space of the steam generating section, which is operated at normal temperature.
A particle inlet for introducing particles obtained by dissolving the hydrophobic substance in an acidic liquid to impart hydrophilicity to the hydrophobic substance which is solid at normal pressure, and a vapor from the particle inlet. Particle supply means for supplying particles into the generator, first adjusting means for changing the temperature in the steam generating part, cooling pipe communicating with the steam generating part, and second adjusting means for changing the temperature of the cooling pipe A particle outlet for taking out particles from the cooling pipe, a particle discharging means for discharging the treated particles from the cooling pipe from the particle outlet, and supplying the particles into the steam generating part by the particle supplying means, and generating steam. The condensing agent vapor in the section is saturated by the first adjusting means, the condensing agent vapor in the cooling pipe is supersaturated by the temperature change by the second adjusting means, and the treated particles in which the condensing agent condenses on the surface are discharged by the particle discharging means. Cooling pipe As al discharged, and characterized in that a control means for controlling said respective means.

According to each of the above structures, the temperature in the processing space of the steam generating section and the temperature in the cooling pipe are respectively changed by the adjusting means or the control means, so that the particles are charged similarly to the above-described manufacturing apparatus. Without inconvenience, and with a simple device and operation, in a short time and at low cost,
An apparatus capable of producing hydrophilic particles having a relatively small particle diameter and uniformity can be provided.

In the above manufacturing apparatus, it is preferable that the cooling pipe is provided so as to extend upward from the upper portion of the steam generating section. In the above configuration, in order to make the condensing agent vapor in the steam generating section into a saturated state, the inside of the steam generating section is heated to generate a rising airflow in the steam generating section. , Particles and saturated vapors can be introduced. In addition, the condensing agent such as water condensed on the inner wall of the cooling pipe returns to the steam generating section by gravity and is reused. Therefore, in the above configuration, preparation of the particles after the treatment can be further simplified.

Further, in the above manufacturing apparatus, it is desirable that at least a part of the inner wall forming the processing space of the steam generating section has a porous material capable of containing a condensing agent. According to the configuration, since at least a part of the inner wall has a porous material, the surface area of the condensing agent can be increased, and the evaporation of the condensing agent can be promoted. Can be faster. Therefore, in the above configuration, preparation of the particles after the treatment can be further simplified.

Further, in the above-mentioned manufacturing apparatus, it is preferable that at least a part of the inner wall of the cooling pipe has a water-repellent material. According to the above configuration, even if the supersaturated vapor precipitates as a condensing agent on the inner wall of the cooling pipe in the cooling pipe, at least a part of the inner wall is made of a water-repellent material. It can be returned to the steam generator. Therefore, in the above configuration, the preparation of the particles after the treatment can be made more efficient.

Further, in the above manufacturing apparatus, it is preferable that the processing space of the steam generating section is formed in a tubular shape, and is set at an angle within a range of 90 degrees from horizontal. According to the above configuration, the particles and the saturated steam can be led to the cooling pipe without difficulty using the rising airflow generated in the steam generating section, and the preparation of the treated particles can be further simplified.

In order to solve the above-mentioned problems, still another hydrophilic particle producing apparatus of the present invention has a condensing apparatus for generating a condensing agent vapor, having a processing space that can be sealed inside. A process for introducing a solution obtained by dissolving a hydrophobic substance in an acidic liquid into particles to impart hydrophilicity to a hydrophobic substance which is solid at normal temperature and normal pressure into a processing space of a condenser. It is characterized by comprising a particle inlet, a particle outlet for taking out particles after processing from the processing space of the condenser, and pressure adjusting means for changing the pressure in the processing space of the condenser.

According to the above configuration, by providing the pressure adjusting means for changing the pressure in the processing space of the steam generating section, the above-mentioned supersaturated state of the steam is further reduced by the pressure change in the closed processing space. Can occur quickly.
As a result, in the above configuration, similarly to the above-described manufacturing apparatus, without charging the particles, and with a simple apparatus and operation, the particle diameter is relatively small and uniform, even more quickly and inexpensively. An apparatus for producing hydrophilic particles can be provided.

The pressure adjusting means comprises: a substantially polygonal column-shaped rotating rotor; and an inner wall portion abutting against each ridge end of the rotor, each outer surface between adjacent ridge ends of the rotor, and each outer surface thereof. Pressure processing means may be provided, in which each processing space formed between the processing space and the facing inner wall portion changes in accordance with the rotation of the rotor.

Further, it is preferable that the pressure adjusting means adiabatically changes the pressure in the processing space of the condenser. The pressure adjusting means for adiabatically changing the pressure in the processing space of the condenser is a piston type that reciprocates in the cylindrical part when the condenser has a cylindrical part communicating with the processing space. There may be.

The apparatus for producing hydrophilic particles according to the present invention further comprises a particle supply means for supplying particles from a particle inlet into the condenser, and a particle discharge means for discharging treated particles from a particle outlet. And supplying particles into the condenser by the particle supply means, and obtaining particles after treatment in which the condensing agent is condensed on the surface in a supersaturated state by adiabatic expansion due to a pressure change by the pressure adjusting means in the condenser. It is preferable that the apparatus further comprises control means for controlling each of the means so that the treated particles are discharged from the condenser by the particle discharge means.

According to each of the above structures, the particles are not charged, and furthermore, with a simple device and operation,
An apparatus for producing hydrophilic particles having a relatively small and uniform particle diameter in a short time and at low cost can be provided.

[0050] In the above manufacturing apparatus, it is preferable that at least a part of the wall for forming the processing space in the condensing device has a porous material capable of containing a condensing agent.
Thereby, the saturated vapor can be prepared in the condenser, and the preparation of the hydrophilic particles can be simplified.

In the above manufacturing apparatus, the transport gas supply device for supplying a gas (carrier) for transporting the liquid particles and the vapor is connected to the condenser through the impurity removing device for removing impurities in the gas. Is desirable. Thus, in the above configuration, the adverse effects of impurities in the gas can be suppressed, so that the production of hydrophilic particles can be further stabilized.

[0052]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS [First Embodiment of the Invention] The method for producing hydrophilic particles according to the first embodiment of the present invention is performed at room temperature.
A solution obtained by dissolving a hydrophobic substance which is a solid at normal pressure in an acidic liquid to impart hydrophilicity to a liquid is formed into particles (mist), and then the particles (hereinafter referred to as liquid particles) are formed. Is contacted with steam containing water vapor having a temperature higher than the temperature of the liquid particles (hereinafter, simply referred to as steam) to form a supersaturated atmosphere of the vapor and condense water on the surface of the liquid particles.

Further, the apparatus for producing hydrophilic particles according to the first embodiment of the present invention converts a solution obtained by dissolving the hydrophobic substance into an acidic solution into particles to impart hydrophilicity to the hydrophobic substance. And a condensing device that brings the liquid particles granulated by the granulating device into contact with supersaturated steam containing water to condense water on the surface of the liquid particles. The above-mentioned supersaturated steam containing water is obtained, for example, by contacting liquid particles with steam containing water having a temperature higher than the temperature of the liquid particles, preferably saturated, to form a supersaturated atmosphere of the steam. Can be. In the present invention, "normal temperature
“Normal pressure” means 20 ° C. and 1 atm.

The hydrophobic substance according to the present invention is soluble in an acidic solution without causing structural changes such as decomposition and polymerization, and can be imparted with the above-mentioned acidic solution, that is, hydrophilicity can be imparted. Any substance can be used as long as it can introduce a group, and is not particularly limited, but a pigment is most suitable. According to the production method of the present invention, pigment particles having hydrophilicity (hydrophilic particles) can be produced.

Further, the acidic liquid according to the present invention can dissolve a hydrophobic substance and can impart hydrophilicity to the hydrophobic substance, that is, it can introduce a hydrophilic group. Any liquid is possible as long as it is possible, and there is no particular limitation. For example, when the hydrophobic substance is a pigment, the acidic liquid is more preferably an aqueous solution containing chlorosulfonic acid and / or sulfuric acid. ADVANTAGE OF THE INVENTION According to the manufacturing method concerning this invention, the hydrophilic particle to which hydrophilicity was provided by introducing a sulfonic acid group (hydrophilic group) can be manufactured.

That is, when the hydrophobic substance is a pigment, the acidic liquid is preferably a so-called strong acid containing chlorosulfonic acid and / or sulfuric acid. The concentration of chlorosulfonic acid and the concentration of sulfuric acid in the acidic solution are not particularly limited, but higher ones are preferable. In the following description, when the hydrophobic substance is a pigment,
Let me give you an example.

The above-mentioned pigments need only have a structure capable of introducing a sulfonic acid group by reaction with chlorosulfonic acid or sulfuric acid, that is, a structure capable of performing sulfonation. is not. Examples of the pigment include an azo pigment, a condensed azo pigment, a phthalocyanine pigment, a perylene pigment, a perinone pigment, a quinacridone pigment, a dioxazine pigment, a thioindigo pigment, an isoindolinone pigment, and a quinophthalone pigment.

As the azo pigment, specifically, for example,
CI (Color Index) Pigment Orange 1,
5, 13, 14, 24, CI Pigment Yellow 1,
2,3,5,6,10,12,13,14,15,1
6, 65, 81, 83, CI Pigment Red 1, 2,
3,4,5,6,7,8,9,10,12,18,2
2,30,32,38,144,146,150,16
3,170, CI Pigment Violet 25, and the like. As the condensation azo pigment, specifically, for example, C.
I. Pigment Yellow 93,95, PO 31, PR
144, PR 166, P. Brown 23 and the like.

Specific examples of the phthalocyanine pigment include CI Pigment Blue 15, 16, and the like. Specific examples of the perylene pigment and the perinone pigment include, for example, CI Pigment Red 149, 17
8, 179, 190 and the like. As the quinacridone pigment, specifically, for example, CI Pigment Violet
19, CI Pigment Red 122, 207 and the like.

As the dioxazine pigment, specifically,
For example, CI Pigment Violet 23 and the like can be mentioned.
As the thioindigo pigment, specifically, for example, C.
I. Pigment Red 36, 38, 41, 88 and the like. Specific examples of the isoindolinone pigment include, for example, CI Pigment Yellow 109, 110, CI Pig
ment Orange 61 and the like. As the quinophthalone pigment, specifically, for example, CI Pigment Yellow
138 and the like.

These pigments may be used alone or as a mixture of two or more as necessary. The production method according to the present invention is most suitable for a pigment having a hue (attribute of color) of red, blue or yellow, whereby a pigment having hydrophilicity and a hue of red, blue or yellow is provided. Particles can be produced.

By dissolving the above pigment in an acidic solution containing chlorosulfonic acid and / or sulfuric acid, for example, at room temperature, the sulfonation of the pigment proceeds, and the pigment having a sulfonic acid group introduced therein, ie, the hydrophilicity is reduced A solution of the applied pigment (hereinafter simply referred to as a solution) is obtained. The concentration of the pigment in the solution is not particularly limited as long as it is not more than the saturation concentration. By appropriately adjusting the concentration,
The particle size of the resulting hydrophilic particles (pigment particles) can be arbitrarily adjusted.

When dissolving the pigment in the acidic liquid,
If necessary, heating and / or stirring may be performed. The higher the heating temperature or the longer the stirring time, the easier the sulfonation of the pigment proceeds. However, depending on the type of the pigment, there is a possibility that the color will change when exposed to a high temperature for a long time. Therefore, it is desirable to set the heating temperature and the stirring time according to the type of the pigment. For example, the heating temperature is
The temperature is more preferably in the range of room temperature (20 ° C) to 100 ° C. Further, the stirring time is more preferably in the range of 10 minutes to 6 hours. The method for preparing the solution is not particularly limited.

The method of forming the above solution into particles, that is, the method of obtaining liquid particles is not particularly limited.
The method of spraying the solution is simple. The particle size of the liquid particles may be set according to the desired particle size of the hydrophilic particles, and is not particularly limited.
The range of 0 μm is more preferable, and the range of 1 μm to 30 μm is particularly preferable.

The steam according to the present invention is not particularly limited as long as it contains water vapor and has a temperature higher than the temperature of the liquid particles. As a method of forming a supersaturated atmosphere (supersaturated steam) of the steam, specifically, for example, water or an azeotropic composition containing water is heated at normal pressure, under reduced pressure, or under pressure, to form steam, More preferably, a method of adiabatically expanding the steam after forming the saturated steam, a method of cooling the steam, and the like are included, but are not particularly limited. The above azeotropic composition is more preferably a composition that can generate steam containing steam as a main component. As the steam, steam is particularly preferable.

The method of bringing the liquid particles into contact with the vapor to form a supersaturated atmosphere of the vapor and condensing water on the surface of the liquid particles is not particularly limited. A method of condensing water into the water is preferred.

As the above method, specifically, for example,
A method of introducing liquid particles into a device (condenser) filled with steam, more preferably saturated steam, then adiabatically expanding the steam to form a supersaturated atmosphere and condensing water on the surface of the liquid particles; Is cooled to form a supersaturated atmosphere, and water is condensed on the surface of the liquid particles. Alternatively, by mixing the vapor with the cooled (lower temperature than the vapor) liquid particles, the vapor and the liquid particles are mixed. A method of forming a supersaturated atmosphere of the vapor using a temperature difference to condense water on the surface of the liquid particles, and the like, such as aggregation of liquid particles, aggregation and deterioration of hydrophilic particles (pigment particles), etc. The condition is not limited, and is not particularly limited.

As a result, when the vapor forms a supersaturated atmosphere and comes into contact with the liquid particles, the vapor condenses with the liquid particles as nuclei, thereby mixing with the acidic liquid and diluting the acidic liquid.
For this reason, hydrophilic substances (pigments) dissolved in acidic liquids
Are precipitated as hydrophilic particles (pigment particles) by dilution of the acidic liquid.

When the liquid particles are brought into contact with the vapor, it is sufficient that the vapor has a temperature higher than the temperature of the liquid particles. However, the temperature difference between the two is set so that water is more easily condensed. The larger, the better. That is, the liquid particles only need to have a temperature lower than the temperature of the steam, but are preferably cooled in order to make the temperature difference mixing proceed more smoothly.

The method for introducing the liquid particles into the apparatus filled with the vapor (more preferably saturated vapor) is not particularly limited, but the inert particles are used as a carrier and the liquid particles are introduced together with the inert gas. The blowing method is simple. That is, in the production method according to the present invention, the liquid particles can be brought into contact with the vapor in the presence of the inert gas.

Specific examples of the inert gas include, for example, nitrogen gas, helium gas, argon gas and the like, but are not particularly limited, and include liquid particles and liquid particles used in the production method according to the present invention. Steam, and
Any gas may be used as long as it is inert to the obtained hydrophilic particles. By using the inert gas as a carrier for the liquid particles, when the hydrophilic particles are formed by precipitation, an undesired reaction (for example, oxidation of the particle surface) or action to the hydrophilic particles due to the carrier is prevented. Can be eliminated.

The amount of water condensed on the surface of the liquid particles depends on the processing conditions such as the particle diameter and density of the liquid particles, the density of steam (supersaturated steam), the processing time, and the processing temperature (temperature difference between the liquid particles and the vapor). It can be adjusted by appropriate selection.
That is, the dilution rate at which the acidic liquid contained in the liquid particles is diluted, and the dilution ratio can be adjusted by appropriately selecting the above processing conditions.

The particle size of the hydrophilic particles precipitated by the dilution of the acidic solution depends on the concentration of the hydrophilic substance in the solution, the particle size of the liquid particles, the dilution ratio, and the like. Can be arbitrarily set by appropriately selecting. Processing time is usually
About one minute is sufficient, but not particularly limited.

For example, liquid particles having a particle size of 0.3 μm
When water condenses on the surface, the particle size becomes approximately 3μ.
m liquid particles (water droplets). Therefore, the solution (acid solution)
Is diluted approximately 1000 times, so that the hydrophilic substance dissolved in the solution is insolubilized and precipitated to become hydrophilic particles. The particle size of the hydrophilic particles can be arbitrarily set, but is more preferably in the range of 0.01 μm to 50 μm, and particularly preferably in the range of 0.01 μm to 5 μm. In the production method according to the present invention, since the hydrophilic particles are formed by precipitation, the particle size of the obtained hydrophilic particles does not depend on the particle size of the hydrophobic substance used first. Therefore, hydrophilic particles having a relatively small and uniform particle size can be obtained.

The hydrophilic particles obtained by the above method are:
After the collection, washing is performed using ultrapure water or the like, if necessary. Thereby, hydrophilic particles from which impurities have been removed can be produced. The washed hydrophilic particles may be dried, if necessary, to such an extent that the hydrophilic particles do not aggregate. Whether or not the impurities contained in the hydrophilic particles have been removed may be determined, for example, using the pH of the cleaning solution as a guide. The method for collecting the hydrophilic particles, the method for washing with water, and the method for drying are not particularly limited.

As described above, in the method for producing hydrophilic particles according to the present invention, a solution obtained by dissolving a hydrophobic substance in an acidic solution to impart hydrophilicity to the hydrophobic substance is formed into particles,
In this method, the liquid particles are brought into contact with steam having a temperature higher than the temperature of the liquid particles to form a supersaturated atmosphere of the steam, and water is condensed on the surface of the liquid particles.

According to the above method, the hydrophobic substance is given hydrophilicity by dissolving it in an acidic liquid, and the hydrophobic substance is made hydrophilic. Then, when the supersaturated atmosphere is formed and comes into contact with the liquid particles, the vapor condenses with the liquid particles as nuclei, mixes with the acidic liquid, and dilutes the acidic liquid.

For this reason, the hydrophilic substance dissolved in the acidic liquid (that is, the hydrophobic substance which has been hydrophilized) precipitates as the acidic liquid is diluted to become hydrophilic particles. Therefore, unlike the conventional method of stirring particles using a stirring device such as a stirring blade, there is no possibility that the particles are charged by friction or the like. In addition, since a device that can generate steam is used, the treatment can be performed in a short time with a simple device and operation.

Further, since the hydrophilic particles are formed by precipitation, the particle size of the obtained hydrophilic particles does not depend on the particle size of the hydrophobic substance used, and the particle sizes of the hydrophilic particles are compared. Can be small and aligned. This makes it possible to produce hydrophilic particles having a relatively small and uniform particle size without charging the particles, with a simple apparatus and operation, in a short time and at low cost.

In the above manufacturing method, the liquid particles are cooled and then brought into contact with the vapor, so that the vapor (supersaturated vapor) is more easily condensed with the liquid particles as nuclei. Therefore, hydrophilic particles can be produced in a much shorter time.

As described above, in the method for producing hydrophilic particles according to the present invention, a solution obtained by dissolving a hydrophobic substance in an acidic liquid to impart hydrophilicity to the hydrophobic substance is formed into particles. A step of contacting the liquid particles with a vapor having a temperature higher than the temperature of the liquid particles to form a supersaturated atmosphere of the vapor, and condensing water on the surface of the liquid particles; Collecting the particles and washing with water.

According to the above method, the obtained hydrophilic particles are collected and washed with water, so that impurities contained in the hydrophilic particles can be removed. This makes it possible to produce hydrophilic particles having a relatively small and uniform particle diameter and from which impurities have been removed without charging the particles, with a simple apparatus and operation, in a short time and at a low cost.

The hydrophilic particles obtained by the above production method are imparted with hydrophilicity by the introduction of a hydrophilic group on the particle surface, and thus have improved wettability with water. More specifically, for example, since the pigment particles have a sulfonic acid group introduced on the particle surface, the wettability to water is improved. The hydrophilic particles obtained by the above production method are suitably used for various applications such as paints, printing inks and toners (developers), for example, when the hydrophobic substance is a pigment.

An example of a manufacturing apparatus suitably used in the above manufacturing method will be described below with reference to FIG. As shown in FIG. 1, the manufacturing apparatus 21 includes a spraying apparatus (granulating apparatus) 10, a reforming tower (condensing apparatus) 22 including a steam generating section 22a and a tubular mixing section 22b, and optical measuring apparatuses 3A and 3B. Provided so that hydrophilic particles can be continuously produced.

The above optical measuring device (second detecting means, fourth
Detection means) 3A is provided inside each of the housings 3j, 3h, and 3i.
A light-transmitting plate 3e, which is a partition plate with a light source 3a, a lens 3b, a light-shielding plate (not shown), and a mixing unit 22b made of glass or the like
3f, a light detection unit 3g, and the like are provided. The optical measuring device 3A causes the light emitted from the light source 3a to enter the light detecting unit 3g via the lens 3b, the opening of the light shielding plate, the light transmitting plate 3e, the inside of the mixing unit 22b, and the light transmitting plate 3f. Has become.

The light emitted from the light source 3a is
The light quantity is changed by being scattered and dimmed by the hydrophilic particles inside b. Thereby, the optical measuring device 3A can determine the particle diameter of the hydrophilic particles and the number of liquid particles (unit of liquid particles) contained in a unit volume based on the signal output from the light detection unit 3g according to the amount of incident light. Density). By measuring the particle size of the hydrophilic particles using the optical measurement device 3A, the particle size can be controlled.

On the other hand, an optical measuring device (first detecting means, third detecting means)
The detection means 3B has the same configuration as the configuration of the optical measurement device 3A, and includes the particle diameter of the liquid particles supplied from the spray device 10 and the number of liquid particles contained in a unit volume (density of the liquid particles). ) Is to be measured.

The optical measuring devices 3A and 3B are configured to measure the particle diameter by using the photodialysis / scattering method. However, the measuring method is not particularly limited. A line transmission method, a sedimentation method, a laser diffraction / scattering method, a photon correlation method using dynamic scattering, or the like can also be employed. In addition to the optical measurement method, an image processing analysis method using an optical microscope or an electron microscope may be employed. By providing such optical measuring devices 3A and 3B, by controlling the production process of the hydrophilic particles based on the measurement results from the optical measuring devices 3A and 3B, it is possible to reduce the particle size and the particle size. It is possible to stably produce uniform hydrophilic particles.

The steam generating section 22a has an elongated cylindrical shape or a prism shape extending in the horizontal direction, and is constituted by an inner wall 2a and an outer wall 2b, and the inside is a steam generating space. At least a part of the inner wall portion 2a has an affinity for an aqueous solution such as water or an azeotropic composition containing water (hereinafter, simply referred to as water), and is made of a ceramic or nonwoven fabric capable of holding the aqueous solution. It is made of a porous material.

The inner wall 2a is preliminarily impregnated or impregnated with water, whereby the temperature and pressure inside the steam generator 22a are adjusted by a control means such as a microcomputer (not shown). This produces steam, more preferably saturated steam. On the other hand, the outer wall 2b is made of stainless steel or the like.

A heating device 7 is spirally wound and attached to the outer peripheral portion of the steam generating section 22a. Further, a thermometer 8 for measuring the temperature of the steam generation space is mounted above the steam generation section 22a. The shape of the steam generating portion 22a is not particularly limited. However, in order to efficiently produce hydrophilic particles using the present manufacturing apparatus, the steam generating portion 22a is more preferably the above-described horizontally long shape than the vertically long shape. .

The steam generating space extending in the longitudinal direction of the steam generating section 22a is formed, for example, in a cylindrical hole shape which is vertically inclined with respect to the axial direction of the steam generating section 22a. A storage section 2c for storing the water 20 is formed at a lower end inside the steam generation section 22a.

Since the inside of the steam generating portion 22a is inclined, the water 20 previously attached or impregnated to the inner wall portion 2a generates steam and a part of the water 20 is stored in the storage portion 2a.
Flow into c. Further, a clean gas supply pipe 2d for supplying a clean gas such as an inert gas into the reforming tower 22 as necessary is connected to a lower end portion inside the steam generating section 22a. The clean gas supply pipe 2d is connected to a clean gas supply device (not shown) via a valve 2e. still,
Instead of previously adhering or impregnating water to the inner wall 2a,
Water can be stored in the storage section 2c in advance.

A mixing section 22b having an elongated cylindrical shape extending in the up-down direction is connected to an upper portion of the steam generation section 22a so as to communicate with an upper end of a steam generation space inside the steam generation section 22a. I have. The mixing section 22b includes a mixing pipe 29 made of stainless steel or the like, and a cooling section 30 provided on an outer peripheral portion of the mixing pipe 29, and the inside is a processing space. For this reason, the processing space communicates with the steam generation space. A thermometer 8 for measuring the temperature of the processing space is mounted above the mixing section 22b.

The steam generating section 22a and the mixing section 22b
The particle supply pipe 4 is connected to the mixing pipe 29 in a state where the particle introduction port 4a, which is the opening thereof, is in the vicinity of the connection portion with the mixing pipe. On the other hand, the upper end of the mixing section 22b is
An optical measuring device 3A for optically measuring the particle diameter of the hydrophilic particles inside 2 and a particle collecting device (not shown) are connected via a particle take-out tube 5. Therefore, the manufacturing apparatus 21
Is mainly composed of the spraying device 10, the reforming tower 22, the optical measuring devices 3A and 3B, a particle collecting device and control means (not shown), and the like.

The particle supply pipe 4 is provided with an optical measuring device 3B for optically measuring the particle diameter of the liquid particles supplied to the reforming tower 22.
Is connected to the particle supply pipe 18 via the The particle supply pipe 18 is connected to the spray device 10. Particle supply pipe 4
Is equipped with a thermometer 8 for measuring the temperature in the pipe. The particle supply pipe 4 continuously supplies the liquid particles together with the inert gas into the mixing pipe 29.

The spraying device 10 includes a spraying container 10a, a nozzle 11, a solution supply pipe 15, a baffle (particle diameter adjusting section) 1
6, a particle supply pipe 18 and the like are provided so that liquid particles can be continuously supplied into the mixing pipe 29. The tip 11a of the nozzle 11 and the solution supply pipe 15
Of the baffle 16, and the opening of the particle supply pipe 18 are arranged substantially in a straight line and horizontally.

The spray container 10a is charged with a predetermined amount of a solution 14 obtained by dissolving a hydrophobic substance such as a pigment in an acidic liquid. When the hydrophobic substance is a pigment, the particle diameter of the pigment is usually about 1 μm to 2 μm, but is not particularly limited.

The solution supply pipe 15 is fixed to the nozzle 11 by a support member 17. The lower end of the solution supply pipe 15 is immersed in the solution 14, and an inert gas is sprayed horizontally on the upper end 15 a to reduce the pressure inside, so that the solution 14 is sucked up to the upper end 15 a. It has become.

The nozzle 11 is connected to a position facing the particle supply pipe 18 in the spray container 10a, and supplies an inert gas (carrier) into the spray container 10a. The nozzle 11 is connected to an inert gas supply device (not shown) via an air filter (impurity removing device) 13 and a mist removing portion (impurity removing device) 12. And
The nozzle 11 blows an inert gas horizontally from the tip 11 a thereof to the upper end 15 a of the solution supply pipe 15 so that the solution 14
Is sprayed to form the solution 14 in the form of particles (mist).
It is supposed to. The mist removing unit 12 and the air filter 13 remove impurities contained in the inert gas so that a clean inert gas is supplied to the spray container 10a.

The baffle 16 is fixed to the solution supply pipe 15, and has a spherical tip 16a. The baffle 16 removes the liquid particles having a relatively large particle diameter when the liquid particles granulated at the upper end 15a of the solution supply pipe 15 collide with the inert gas at the tip 16a. ing. That is, by adjusting the particle diameter of the liquid particles by the baffle 16, the spray device 1
0 is such that liquid particles having a relatively small and uniform particle diameter are supplied into the mixing tube 29.

The maximum particle size of the liquid particles to be supplied into the mixing tube 29 can be arbitrarily controlled by appropriately adjusting the size of the tip 16a of the baffle 16. The supply amount of the liquid particles per unit time can be arbitrarily controlled by adjusting the spraying conditions such as the diameter of the solution supply pipe 15, the flow rate and the flow rate of the inert gas, and the like. The liquid particles removed by the baffle 16 flow down the baffle 16 and are reused as the solution 14.

The particle supply pipe 18 is connected to a position facing the nozzle 11 in the spray container 10a. Also,
The particle supply pipe 18 is in communication with the particle supply pipe 4 connected to the mixing section 22b via the optical measurement device 3B.
At the end of the particle supply pipe 18 on the side of the optical measurement device 3B,
A cooling device 19 for cooling the liquid particles as needed is provided.

The cooling device 19 is provided with a Peltier element, and cools the inside of the particle supply pipe 18, that is, the liquid particles in the particle supply pipe 18 by the Peltier effect. The cooling device 19 may have a configuration corresponding to a desired cooling temperature, and is not particularly limited. The cooling device 19 may be configured to cool the liquid particles using an organic solvent (refrigerant) cooled by liquid nitrogen, water, dry ice, or the like, for example. Alternatively, the cooling device 1
9 may be, for example, a Liebig cooling pipe through which a coolant such as water or ice water flows.

In order to produce hydrophilic particles using the production apparatus 21 having the above-described configuration, first, a steam generation space is formed in the reforming tower 22 and then the heating apparatus 7 is used to attach or adhere to the inner wall 2a in advance. The steam of the impregnated water (or the water 20 stored in the storage unit 2c), more preferably, the saturated steam is generated. The steam generated in the steam generation section 22a is supplied to the inside of the mixing pipe 29, which is a processing space communicating with the steam generation space, by the clean gas (carrier) supplied from the clean gas supply pipe 2d.
Introduced by

Next, liquid particles are generated by the spray device 10 and the liquid particles are continuously supplied into the mixing pipe 29.
That is, the solution 14 is formed into particles by horizontally blowing an inert gas from the tip 11 a of the nozzle 11 to the upper end 15 a of the solution supply pipe 15, and the particle diameter of the liquid particles is adjusted by the baffle 16. Then, the obtained liquid particles are supplied (introduced) into the mixing tube 29 in the mixing section 22b via the particle supply tube 18, the optical measurement device 3B, and the particle supply tube 4. At this time, the particle supply pipe 1
The liquid particles passing through the inside of the cooling device 8 are cooled by the cooling device 1 if necessary.
Cool using 9.

The liquid particles supplied into the mixing pipe 29 are
It is mixed with the steam supplied from the steam generation part 22a. Further, by cooling the mixing tube 29 using the cooling unit 30, the steam is cooled, a further supersaturated atmosphere is formed, and water is condensed on the surface of the liquid particles. This allows
The hydrophilic substance contained in the liquid particles precipitates to form hydrophilic particles. Then, by measuring the particle size of the hydrophilic particles using the optical measurement device 3A, the device is controlled so as to obtain hydrophilic particles having a desired particle size, and the mixing tube 29 is connected via the particle extraction tube 5. From the hydrophilic particles.

[0108] The particle diameter of the hydrophilic particles is determined by the vapor generating portion 22a.
By appropriately setting the heating temperature, the flow rates of the inert gas and the clean gas (carrier), the temperature of the liquid particles, and the temperature of the mixing section 22b, the temperature can be easily controlled. In the mixing section 22b, the time for exposing the liquid particles to steam (supersaturated steam) can be easily adjusted by appropriately setting the flow rates of the inert gas and the clean gas, the length of the mixing pipe 29, and the like. Can be.

As a result, hydrophilic particles having a desired particle diameter, that is, hydrophilic particles according to the present invention can be easily and continuously produced. The above manufacturing apparatus 21
Since hydrophilic particles are continuously produced, continuous processing under the same conditions can be easily performed as compared with a batch-type production apparatus. Therefore, hydrophilic particles having certain physical properties can be stably mass-produced. When producing the hydrophilic particles using the production apparatus 21, it is desirable that the inside of the apparatus be replaced in advance with a clean gas such as an inert gas used as a carrier.

The hydrophilic particles taken out through the particle take-out tube 5 are collected (collected) by a particle collecting device (not shown). The collected hydrophilic particles are washed with ultrapure water or the like by a washing device (not shown) as necessary. Thereby, hydrophilic particles from which impurities have been removed are obtained. The washed hydrophilic particles are dried, if necessary, to such an extent that the hydrophilic particles do not aggregate.

In producing the hydrophilic particles using the production apparatus 21 having the above configuration, instead of supplying the liquid particles into the mixing tube 29 and then cooling the mixing tube 29 using the cooling unit 30, The liquid particles are cooled by the cooling device 19 (to a temperature lower than that of the steam) and introduced into the mixing tube 29, so that the supersaturated atmosphere of the steam is mixed by utilizing the temperature difference between the steam and the liquid particles. 29, water can be condensed on the surface of the liquid particles.

As described above, the apparatus 21 for producing hydrophilic particles according to the present invention converts the solution 14 obtained by dissolving a hydrophobic substance into an acidic solution into particles in order to impart hydrophilicity to the hydrophobic substance. The spray device 10 and the liquid particles granulated by the spray device 10 are brought into contact with steam having a temperature higher than the temperature of the liquid particles to form a supersaturated atmosphere of the steam and condense water on the surface of the liquid particles. And a mixing section 22b.

According to the above-mentioned structure, hydrophilic particles having a relatively small and uniform particle diameter can be produced without charging the particles, with a simple apparatus and operation, in a short time and at low cost. .

Further, since the hydrophilic particle producing apparatus 21 according to the present invention employs the spraying apparatus 10 as a granulating apparatus, it is possible to produce hydrophilic particles having a much smaller particle diameter. Further, the apparatus 21 for producing hydrophilic particles according to the present invention is provided with a cooling device 19 for cooling liquid particles. This makes it easier for water to condense on the surface of the liquid particles, so that hydrophilic particles can be produced in a shorter time. In addition, since the spray device 10 includes the baffle 16, hydrophilic particles having a smaller and uniform particle size can be manufactured.

In the above description, the manufacturing apparatus 21 capable of continuously manufacturing hydrophilic particles has been described as an example, but the specific configuration of the manufacturing apparatus is limited to the above-described configuration. It is not limited. The apparatus for producing hydrophilic particles according to the present invention may have a configuration capable of producing hydrophilic particles in a batch system. Each manufacturing process in the manufacturing apparatus is controlled by control means such as a microcomputer (not shown) with a built-in program.

In the above description, the manufacturing apparatus 21 having a configuration in which the steam is cooled to form a supersaturated atmosphere has been described as an example. However, the manufacturing apparatus performs a supersaturated atmosphere by adiabatically expanding the steam. (Supersaturated steam) may be provided. Further, in the above description, the spraying device 10 has been described as an example of the granulating device, but the configuration of the granulating device is not particularly limited.
The granulating device may be configured to make the solution into particles by, for example, scattering the solution by ultrasonic vibration.

[Embodiment 2] An apparatus for manufacturing hydrophilic particles according to Embodiment 2 of the present invention is shown in FIG. 4 as a modification of the manufacturing apparatus 21 described in Embodiment 1 above. The manufacturing apparatus 21a. In the second embodiment, members having the same functions as those of the manufacturing apparatus 21 described in the first embodiment in the manufacturing apparatus 21a are given the same member numbers in FIG. Was.

In the manufacturing apparatus 21a, the particle inlet 4a of the particle supply pipe 4 for supplying the liquid particles together with the inert gas is connected to the storage section 2 in the internal processing space of the steam generation section 22a.
An opening is provided above the c-side end.

The center axis of the cylindrical hole-shaped (straight tubular) steam generation space in the steam generation section 22a is vertically inclined with respect to the horizontal direction, as described above.
Is set within a range exceeding horizontal and up to 90 degrees.

Therefore, in the steam generating section 22a of the manufacturing apparatus 21a, liquid particles can be continuously supplied together with the inert gas into the steam generating section 22a from the particle supply pipe 4 through the particle introduction port 4a. ing.

In the manufacturing apparatus 21a, the mixing pipe 29 serving as a cooling pipe is connected to the central axis of the mixing pipe 29 and the steam generating section
A is attached to the steam generating section 22a so that the angle θ between the central axis of the tubular steam generating space in a and the vertical direction is in the range of 90 degrees to 1 degree, which is the vertical direction.

On the other hand, the above-described cooling device 19 for cooling the inside of the mixing tube 29 is attached to the outer peripheral portion of the mixing tube 29, and at least a part of the inner wall portion of the mixing tube 29 is provided with water or water. It is composed of a water-repellent material such as a fluororesin having a property of repelling an aqueous solution containing the same. On the other hand, a mixing pipe 29 is installed so as to communicate upward from the upper part of the steam generating part 22a and extend upward.

Thus, even if the steam in the mixing pipe 29 is condensed on the inner wall of the mixing pipe 29 to become water, the water is returned to the steam generating section 22a through the inner wall, so that it is used as a condensing agent. Water can be used efficiently.

The heating device 7 provided on the outer periphery of the steam generating section 22a and the cooling device 19 for the mixing pipe 29 also obtain the respective measurement results of the thermometers 8 provided in the steam generating section 22a and the mixing section 22b, respectively. In addition, an adjusting means (a first adjusting means and a second adjusting means, not shown), such as a microcomputer of a program type, for precisely controlling a predetermined temperature by a temperature adjuster is provided.

Further, in the manufacturing apparatus 21a, such a cooling device 19 supplies each inert gas to the outer circumference of the clean gas supply pipe 2d and the outer circumference of the inert gas supply pipe 11b to the nozzle 11, respectively. It may be provided in advance for cooling.

Also in such a manufacturing apparatus 21a, the same hydrophilic particles as described above can be obtained by the same operation and operation, except for the following operation different from that of the above-described manufacturing apparatus 21.

The different operation will be described below. First, the liquid particles prepared in the spraying device 10 are supplied by the particle supply pipe 4 to the upper part of the internal processing space in the steam generating part 22a at the end on the storage part 2c side. From the steam generator 22a, the configuration can be simplified.

Therefore, in the production apparatus 21a, water can be condensed on the surface of the liquid particles, and the water can be more uniformly condensed on the surface of the liquid particles as in the production apparatus 21 described above. Thus, the production of hydrophilic particles can be further stabilized.

In producing the hydrophilic particles using the production apparatus 21a having the above configuration, the vapor generation section 22a
After supplying the liquid particles to the inside, instead of cooling the vapor in the mixing pipe 29, before supplying the liquid particles to the vapor generation part 22a, the cooling device 1 provided on the outer peripheral part of the particle supply pipe 18
9 and introduced into the steam generator 22a (so that the temperature is lower than the saturated steam in the steam generator 22a), thereby forming a supersaturated atmosphere utilizing the temperature difference between the steam and the liquid particles. Then, water caused by the steam may be condensed on the surface of the liquid particles.

Alternatively, a cooling device 19 is arranged in front of the spray device 10 and the inert gas (carrier) to be supplied to the spray device 10 is cooled in advance, so that the liquid particles are cooled (the steam generating section 22a). (To be lower in temperature than the saturated steam in the inside) may be introduced into the steam generator 22a. In addition, the inert gas (carrier) supplied from the clean gas supply pipe 2d to the steam generator 22a may be similarly cooled in advance. As described above, when the inert gas is cooled in advance, the mixing section 22b including the mixing pipe 29 can be omitted, and the manufacturing apparatus 21a can be further simplified.

The manufacturing apparatus 21 and the manufacturing apparatus 2
1a, an example in which the spraying device 10 is used to prepare the liquid particles has been described. However, the method for preparing the liquid particles is not limited to the above, and for example, as shown in FIG. Alternatively, an atomizer-type granulator 10a that shakes off the liquid film to form liquid particles as droplets may be used. Such an atomizer type granulator 10a
Can produce liquid particles having a small particle diameter even when the solution 14 has a high concentration and a high viscosity.

In such a granulating apparatus 10a, the solution 14 in which the hydrophobic substance is dissolved in the acidic liquid is supplied to the introduction pipe 150.
The solution 14 is supplied onto the disk-shaped rotating part 160 rotating at high speed, and the solution 14 which has become a liquid film on the rotating part 160 is shaken outward from the outer edge of the rotating part 160 by centrifugal force to form a spray. (Mist shape). The liquid particles in the form of a spray are converted into an optical measurement device 3B by an inert gas (carrier).
To the reforming tower 22 via the Unwanted liquid particles having a too large particle size, for example, are separated and discharged.
Discharged by 0.

Further, instead of the spraying device 10, for example, as shown in FIG. 6, a granulating device 10b for preparing liquid particles from the solution 14 by applying ultrasonic vibration to the solution 14 blown out from the orifice. May be used. In such a granulating apparatus 10b, the solution 14 is introduced into the introduction pipe 150.
Is introduced into the orifice 161 by this orifice 1
Ultrasonic vibration is applied to the solution 14 coming out of 61 by a vibration member 170 such as a piezo element. The generation rate of the liquid particles is controlled by the vibration frequency of the vibration member 170. The formed liquid particles are conveyed to the reforming tower 22 by an inert gas (carrier) via the optical measuring device 3B.

Further, in place of the spraying device 10, for example, as shown in FIG. 7, a granulating device 10c, which is another method for preparing liquid particles by vibration, may be used. In such a granulator 10c, the solution 14 is introduced into the tank-shaped supply unit 162 by an introduction pipe (not shown). This supply unit 16
2, a vibration member 170 such as a piezo element is disposed, and between the supply unit 162 and the vibration member 170,
The medium 180 that transmits the vibration from the vibration member 170 is filled.

The bottom of the supply section 162 has a downwardly curved shape, and the vibration generated by the vibrating member 170 is applied to the solution 14 in the supply section 162 via the bottom.
The liquid 14 is concentrated by the above-mentioned convexly curved shape to promote the formation of particles of the solution 14, that is, the generation of liquid particles at the liquid surface. In addition, an inert gas (carrier) is supplied from above the device, and the generated liquid particles are transported to the reforming tower 22 via the optical measuring device 3B by the inert gas (carrier). ing. Each such granulator 1
0a, 10b, and 10c can be used also in the first embodiment and the third to fifth embodiments described later.

[Third Embodiment of the Invention] The apparatus for producing hydrophilic particles according to the third embodiment of the present invention is shown in FIG. 8 as a modification of the production apparatus 21 described in the first embodiment. The manufacturing apparatus 21b. In the third embodiment, members having the same functions as those of the manufacturing apparatuses 21 and 21a described in the first and second embodiments in the manufacturing apparatus 21b are given the same member numbers in FIG. The explanation was omitted.

In the manufacturing apparatus 21b, the first embodiment is used.
And a reforming tower 112 having a steam generating section 111 and a condensing section (pressure adjusting means) 112. Regarding the steam generator 111, the steam generator 2
It has the same configuration as 2a and can generate steam.

On the other hand, the condensing section 112 is of a rotary gasoline engine type, and performs compression and expansion sequentially in an adiabatic manner. That is, the condensing unit 11
2 is an approximately polygonal columnar rotating rotor 114 and an inner wall 113 abutting against each ridge end 114a of the rotor 114, respectively.
Each processing space 1 formed between each outer surface 114c between the outer surfaces 114a and the inner wall portion 113 facing each outer surface 114c.
Capacity 12b has as respectively according to the rotation of the rotor changes as that each processing space _{112b 1 · 112b 2 · 112b 3} .

The inner wall portion 113 has a gourd shape in which two circles are partially overlapped with each other in a cross-sectional shape in a direction perpendicular to the rotation axis of the rotor 114. Internal gear 11 inside
In the gear 114b, a drive gear 115 having external teeth smaller in diameter than the gear 114b is planetarily meshed internally. Thus, the rotor 114 can rotate the inner wall portion 113 while maintaining the respective ridge end 114a in contact with the inner wall portion 113.

At this time, each outer surface 114c of the rotor 114
May come into contact with the convex portion of the inner wall portion 113, but by the concave portion provided at the center portion of each outer surface 114c,
Is formed between the ridge end 114a adjacent each processing space 112b, for example, the processing space 112b ₂ is prevented from being separated by the protrusion at between ridge ends 114a adjacent.

Next, a method for producing hydrophilic particles using the production apparatus 21b will be described. First, the rotor 114 is set at the position shown in FIG.
2b, the steam generated by the steam generator 111 is
It is supplied via a steam supply pipe 73. On the other hand, liquid particles are introduced into the processing space 112b from the spray device 10 through the particle supply pipe 4 through the particle introduction port 4a. In this case, each opening 1 of the condensing agent inlet 72 and the particle inlet 4a
17 and 116 correspond to the processing space 112b (processing space 11).
2b ₁ ).

Subsequently, as the rotor 114 is rotated in the direction of the arrow (clockwise) in the figure by control means such as a microcomputer (not shown), the processing space 112 is rotated.
b of one ridge end 114 in the counterclockwise direction
When a passes through the openings 117 and 116, the processing space 112b is shut off from the steam supply pipe 73 and the particle introduction port 4a. Therefore, the processing space 112b is closed while moving inside the condenser 112 clockwise.

Next, in order to obtain a saturated vapor of the condensing agent in the condensing section 112, the processing space 112b is pressurized and heated. Pressurization is performed by rotating the rotor 114 clockwise (180 ° from the state in FIG. 8).
In this pressure to boost the processing space 112b (state of the processing space 112b ₂₎ at a predetermined pressure higher than the atmospheric pressure (atmospheric pressure). This processing space 112b (processing space 11
2b ₂ ) is measured by the pressure gauge 60,
The pressure is set to a predetermined pressure by the pressure regulator 50 based on the measured value.

The heating is performed by the heating device 7. Heating device 7
Is activated, the heat generated from the heater 7a is
c, the inside of each processing space 112b is heated via the inner wall portion 113. The temperature in each processing space 112b is measured by the thermometer 8, and the operation of the heating device 7 is controlled based on the measured value.

Thereafter, the rotor 114 is allowed to stand for an appropriate time until saturated vapor of the condensing agent is obtained. That is, the above state is maintained for the condensing section 112. In order to obtain a saturated vapor, at least the above-mentioned pressurization may be performed, and the heating may be performed supplementarily as necessary. This is the same in the other examples described below.

[0146] Through the above process, in the processing space 112b (state of the processing space 112b _2), the saturated vapor of the condensing agent is obtained. In this state, the vapor of the condensing agent exists so as to surround the liquid particles. Next, the rotor 114
Is further rotated, and the inside of the processing space 112b is adiabatically reduced to normal pressure, so that the saturated vapor of the condensing agent is brought into a supersaturated state. Thereby, the processing space 112 containing the liquid particles
In b, the saturated vapor of the condensing agent becomes supersaturated, and a condensation reaction of the condensing agent vapor occurs on the surface of the liquid particles. As a result, a liquid film is formed on the surface of the liquid particles, and the hydrophilic particles are precipitated as described above.

The precipitated hydrophilic particles further rotate the rotor 114 to rotate the processing space 112b (processing space 112b ₃ ).
Is opened to the particle outlet 95 of the condensing section 112, thereby being collected through the optical measuring device 3A and the particle outlet tube 5, washed and dried in the same manner as described above, and used.

In the above description, an example is described in which the condensing agent is introduced as vapor from the condensing agent introduction port 72.
2b, at least a portion of the porous material in the concave portion provided at the center of each outer surface 114c of the rotor 114 is installed on the porous material, and the porous material is preliminarily attached and impregnated with a condensing agent. Alternatively, saturated steam may be generated in the processing space 112b.

[Fourth Embodiment of the Invention] FIG. 9 shows a modification of the production apparatus 21 according to the fourth embodiment of the present invention. The manufacturing apparatus 21c is used. Embodiment 4
In the manufacturing apparatus 21c, members having the same functions as those of the manufacturing apparatuses 21, 21a, and 21b described in the first to third embodiments are given the same member numbers in FIG. Omitted.

The components of the production apparatus 21c will be described by describing a method for producing hydrophilic particles using the production apparatus 21c. First, in the above-described production method, a condensing agent such as water is preliminarily attached or impregnated to the inner wall portion 2a inside the reforming tower (condensing box) 22 fixed on the base 9 in an upright state, and the reforming tower 22 The inside of the steam generation space 22c is replaced with a clean gas, such as clean air, in which there is no impurity that can be a nucleus.

After that, the inside of the reforming tower 22 is sealed. In this case, the liquid particles are introduced from the spray device 10 through the particle supply pipe 4, for example, as an aerosol from the particle introduction port 4 a into the reformer 22. Therefore, the valves 30 and 40 of the particle supply pipe 4 and the particle discharge pipe 41 are opened when introducing the liquid particles, and the air in the reforming tower 22 is discharged by the spraying device 1.
After being replaced with the aerosol of liquid particles starting from 0, the valves 30 and 40 are closed, and the inside of the reforming tower 22 is closed.

Next, in order to obtain a saturated vapor of the condensing agent in the reforming tower 22, the inside of the reforming tower 22 is pressurized and heated. The pressurization is performed by opening the valve 70 and sending clean gas into the reforming tower 22 through the pressurizing and depressurizing pipe 71 and the pressurizing and depressurizing port 6. In this pressurization, the pressure inside the reforming tower 22 is increased to a predetermined pressure higher than the normal pressure. The pressure in the reforming tower 22 is measured by a pressure gauge 60,
When the predetermined pressure is reached, the valve 70 is closed.

The heating is performed using the heating device 7. When the heating device 7 operates, heat generated from the heater 7a is transmitted to the outer wall portion 2b, the inner wall portion 2a, and the steam generation space 22c, and they are heated. The temperature in the steam generation space 22c is measured by the thermometer 8, and the operation of the heating device 7 is controlled based on the measured value.

Thereafter, the reforming tower 22 is allowed to stand for an appropriate time until saturated vapor of a condensing agent such as water is obtained. In order to obtain saturated steam, at least the above pressurization may be performed,
Heating may be performed supplementarily as needed. This is the same in the other examples described below. Although not shown, the above-described operations are controlled by control means such as a microcomputer based on the detected values of the detected temperatures, particle diameters, number concentrations, pressures, and the like.

Through the above steps, saturated vapor of the condensing agent is obtained in the reforming tower 22. In this state, the vapor of the condensing agent exists so as to surround the liquid particles. Next, the inside of the reforming tower 22 is adiabatically reduced to normal pressure to make the saturated vapor of the condensing agent supersaturated. At this time, by opening the valve 70 of the pressurizing / depressurizing pipe 71 and opening the inside of the reforming tower 22 to the atmosphere, the saturated vapor of the condensing agent in the vapor generating space 22c is adiabatically expanded.

Thus, in the vapor generation space 22c containing the liquid particles, the saturated vapor of the condensing agent becomes supersaturated, and a condensation reaction of the condensing agent vapor occurs on the surface of the liquid particles. As a result, a liquid film is formed on the surface of the liquid particles, and the modified hydrophilic particles are deposited as described above. Valve 7
0 closes immediately after adiabatic expansion.

The precipitated hydrophilic particles are collected from the reforming tower 22 to the outside through the optical measuring device 3A and the particle take-out tube 5, washed and dried in the same manner as described above, and used. In such recovery, the valves 30 and 40 of the particle supply pipe 4 and the particle discharge pipe 41 are opened, and for example, a clean gas is introduced from the particle supply pipe 4 into the reforming tower 22, This is performed by discharging the hydrophilic particles in the steam generation space 22c from the particle discharge pipe 41 and replacing the inside of the steam generation space 22c with clean gas.

When the liquid particles are supplied (introduced) into the vapor generation space 22c via the particle supply pipe 4, the liquid particles passing through the particle supply pipe 18 are changed as necessary.
The cooling may be performed in advance by the cooling device 19. Alternatively, a cooling device 19 may be provided before the spray device 10 to cool the inert gas in advance so that the liquid particles supplied into the steam generation space 22c may be cooled in advance.

[Fifth Embodiment] In the manufacturing apparatus for hydrophilic particles according to the fifth embodiment of the present invention, FIG. 10 is a modification of the manufacturing apparatus 21 described in the first embodiment.
The manufacturing apparatus 21d shown in FIG. In the fifth embodiment, in the manufacturing apparatus 21d, the manufacturing apparatuses 21, 21a, 21b, and 21c described in the first to fourth embodiments are used.
The members having the same functions as those described above are given the same member numbers in FIG. 10 and the description thereof is omitted.

The components of the manufacturing apparatus 21d will be described by describing a method for manufacturing hydrophilic particles using the manufacturing apparatus 21d. First, in the above-described manufacturing method, the piston 75a of the pressurizing / depressurizing piston 75 is lowered by the crank portion 75b so as to increase the processing space volume of the steam generating space 22c, and sprayed into the steam generating space 22c of the reforming tower 22. Liquid particles conveyed from the apparatus 10 through the particle supply pipe 4 are introduced, for example, as aerosol from the particle inlet 4a, and a condensing agent such as water from the condensing agent inlet 72 as vapor.

Therefore, in this case, the valves 30 and 74 of the particle inlet 4a and the condensing agent inlet 72 are kept open, and the valve 50 of the particle outlet tube 5 is closed. In the lower part of the steam generating space 22c, the piston 75a has a cylinder shape so that the piston 75a can reciprocate and pressurize and depressurize the inside of the steam generating space 22c.

Subsequently, after the piston 75a has been lowered to the lowest position, the valves 30 and 74 are closed, and the steam generation space 22c is closed. Next, the steam generation space 22c
In order to obtain saturated vapor of condensing agent vapor at
2c is pressurized and heated. Pressurizing the piston 7
This is done by raising 5a. In this pressurization, the pressure inside the steam generation space 22c of the reforming tower 22 is increased to a predetermined pressure higher than the normal pressure. The pressure in the steam generation space 22c is measured by the pressure gauge 60, and is set to a predetermined pressure by the pressure regulator 50.

The heating is performed using the heating device 7. When the heating device 7 operates, heat generated from the heater 7a is applied to the outer wall portion 2b, the inner wall portion 2a, and the steam generation space 22c,
They are heated. The temperature in the steam generation space 22c is measured by the thermometer 8, and the operation of the heating device 7 is controlled based on the measured value.

Thereafter, the reforming tower 22 is allowed to stand for an appropriate time until saturated vapor of a condensing agent such as water is obtained. In order to obtain saturated steam, at least the above pressurization may be performed,
Heating may be performed supplementarily as needed. This is the same in the other examples described below. Although not shown, the above-described operations are controlled by control means such as a microcomputer based on the detected values of the detected temperatures, particle diameters, number concentrations, pressures, and the like.

Through the above steps, saturated vapor of the condensing agent is obtained in the reforming tower 22. In this state, the vapor of the condensing agent exists so as to surround the liquid particles. Next, the inside of the reforming tower 22 is adiabatically reduced to normal pressure to make the saturated vapor of the condensing agent supersaturated. At this time, the saturated vapor of the condensing agent in the vapor generation space 22c is adiabatically expanded by lowering the piston 75a to the lowermost position (initial position).

Thus, in the vapor generation space 22c containing the liquid particles, the saturated vapor of the condensing agent becomes supersaturated, and a condensation reaction of the condensing agent vapor occurs on the surface of the liquid particles. As a result, a liquid film is formed on the surface of the liquid particles, and the modified hydrophilic particles are deposited as described above. The particle diameter of the hydrophilic particles is measured by the optical measuring device 3A.

The precipitated hydrophilic particles are recovered from the reforming tower 22 to the outside via the particle take-out tube 5 and the particle discharge tube 41, washed and dried in the same manner as described above, and used.
Such recovery is performed by closing the valves 30 and 74 of the particle introduction port 4a and the condensing agent introduction port 72 while the particle extraction tube 5 is closed.
This is performed by opening the valve 40 and raising the piston 75a from the lowermost position to the uppermost position.

In the above description, the condensing agent is introduced as vapor from the condensing agent inlet 72. However, the inner wall 2a of the reforming tower 22 facing the vapor generation space (processing space) 22c is described.
At least a part of the porous material, a condensing agent is preliminarily attached and impregnated in the porous material, and the heating device 7 is used.
Saturated steam may be generated in the steam generation space 22c.

When the liquid particles are supplied (introduced) into the vapor generating space 22c via the particle supply pipe 4, the liquid particles passing through the particle supply pipe 18 are optionally replaced with
The cooling may be performed by the cooling device 19. Alternatively, a cooling device 19 may be provided before the spray device 10 to cool the inert gas in advance so that the liquid particles supplied into the steam generation space 22c may be cooled in advance.

[0170]

EXAMPLES The present invention will be described in more detail with reference to the following Examples, but it should not be construed that the invention is limited thereto.

Example 1 Using the above-described manufacturing apparatus 21 and the respective manufacturing apparatuses 21a to 21d, hydrophilic particles were manufactured. That is, a pigment as a hydrophobic substance (CI Pigmen
A solution was prepared by adding 1 g of t Red 2) to 20 ml of 98% sulfuric acid (concentrated sulfuric acid) as an acidic solution and stirring at room temperature (20 ° C.) for 30 minutes to dissolve. And
The solution was charged into the spray device 10.

On the other hand, after the water 20 is stored in the storage section 2c of the steam generation section 22a, the reforming tower 22 is closed, and the heating section 7 is used to heat the steam generation section 22a to 80 ° C. at normal pressure. Saturated steam was generated.

Next, liquid particles were formed under predetermined conditions in the spray device 10, and the liquid particles were cooled by the cooling device 19 and supplied into the mixing pipe 29 through the particle supply pipes 18.4. . After supplying the liquid particles, the cooling pipe 30 is used to cool the mixing pipe 29 to cool the saturated steam to form a supersaturated steam (supersaturated atmosphere), thereby condensing water on the surface of the liquid particles. . This allows
The pigment (hydrophilic substance) contained in the liquid particles was precipitated, and the pigment particles (hydrophilic particles) according to the present invention were generated.

In the first embodiment, a production example using the production apparatus 21 was described. However, similar hydrophilic particles were produced using the other production apparatuses 21a to 21d as described above. .

The obtained pigment particles were taken out of the inside of the reforming tower 22 through the particle take-out tube 5 and collected. Thereafter, the pigment particles were washed with ultrapure water and dried. And
The infrared absorption spectrum of the pigment before the treatment and the infrared absorption spectrum of the pigment (pigment particles) after the treatment were measured.

A chart of the infrared absorption spectrum of the pigment before the treatment is shown in FIG. 2, and a chart of the infrared absorption spectrum of the pigment after the treatment is shown in FIG. As is clear from both figures, the pigment after treatment has a wavelength of 1100 cm ^{-1 to} 1300.
In the vicinity of cm ⁻¹ , absorption by a sulfonic acid group, which was not observed in the pigment before treatment, was observed. Therefore, it was confirmed that a sulfonic acid group (hydrophilic group) was introduced into the pigment after the treatment, and that the pigment was given hydrophilicity.

Then, the pigment before the treatment and the pigment after the treatment were put into ultrapure water and stirred to evaluate the wettability with water. As a result, since the pigment before the treatment had hydrophobicity, it did not wet with water and floated on the water surface. On the other hand, the pigment after the treatment, that is, the pigment particles according to the present invention were wetted with water and dispersed (floated) in water because of being imparted with hydrophilicity. In other words, it was confirmed that the pigment particles obtained by the production method according to the present invention had excellent wettability to water since a sulfonic acid group was introduced on the particle surface.

Example 2 A pigment (C.
I. Pigment Orange 24) 1 g of 98% sulfuric acid 20m
The solution was prepared by adding the solution to 1 liter and stirring at room temperature (20 ° C.) for 1 hour to dissolve. Then, operations similar to those in Example 1 were performed except that the above solution was charged into the spraying device 10 instead of the solution used in Example 1. Thereby, pigment particles (hydrophilic particles) according to the present invention were obtained.

Then, in the same manner as in Example 1, the wettability of the pigment before the treatment and the pigment after the treatment with water was evaluated. As a result, the pigment before the treatment did not get wet with water and floated on the water surface. On the other hand, the treated pigment, that is, the pigment particles according to the present invention, were wetted with water and dispersed in water. That is,
It was confirmed that each pigment particle obtained by the production method according to the present invention had excellent wettability to water.

Example 3 A pigment (C.
I. Pigment Yellow 10) 1 g of 80% sulfuric acid 30 m
The solution was prepared by adding the mixture to 1 l and stirring at room temperature (20 ° C.) for 3 hours to dissolve. Then, operations similar to those in Example 1 were performed except that the above solution was charged into the spraying device 10 instead of the solution used in Example 1. Thereby, pigment particles (hydrophilic particles) according to the present invention were obtained.

The wettability of the pigment before the treatment and the pigment after the treatment with water were evaluated in the same manner as in Example 1. As a result, the pigment before the treatment did not get wet with water and floated on the water surface. On the other hand, the treated pigment, that is, the pigment particles according to the present invention, were wetted with water and dispersed in water. That is,
It was confirmed that each pigment particle obtained by the production method according to the present invention had excellent wettability to water.

Example 4 A pigment (C.
I. Pigment Red 144) 1 g, 90% sulfuric acid 20 ml
And a solution was prepared by stirring and dissolving at 50 ° C. for 3 hours. Then, operations similar to those in Example 1 were performed except that the above solution was charged into the spraying device 10 instead of the solution used in Example 1. Thereby, pigment particles (hydrophilic particles) according to the present invention were obtained.

Then, in the same manner as in Example 1, the wettability of the pigment before the treatment and the pigment after the treatment with water was evaluated. As a result, the pigment before the treatment did not get wet with water and floated on the water surface. On the other hand, the treated pigment, that is, the pigment particles according to the present invention, were wetted with water and dispersed in water. That is,
It was confirmed that each pigment particle obtained by the production method according to the present invention had excellent wettability to water.

Example 5 Pigment as hydrophobic substance (C.
I. Pigment Blue 16) 1 g of 98
% Chlorosulfonic acid was added to the mixture, and the mixture was dissolved by stirring at 90 ° C. for 4 hours to prepare a solution. Then, operations similar to those in Example 1 were performed except that the above solution was charged into the spraying device 10 instead of the solution used in Example 1. Thereby, pigment particles (hydrophilic particles) according to the present invention were obtained.

Then, in the same manner as in Example 1, the pigment before treatment and the pigment after treatment were evaluated for wettability with water. As a result, the pigment before the treatment did not get wet with water and floated on the water surface. On the other hand, the treated pigment, that is, the pigment particles according to the present invention, were wetted with water and dispersed in water. That is,
It was confirmed that each pigment particle obtained by the production method according to the present invention had excellent wettability to water.

Example 6 A pigment (C.
A solution was prepared by adding 1 g of I. Pigment Red 178) to 40 ml of 98% chlorosulfonic acid and stirring at 80 ° C. for 3 hours to dissolve. Then, instead of the solution used in Example 1, the above solution was sprayed with a spray device 10
The same operations and the like as those in the same example were performed except that they were prepared in the same manner. Thereby, pigment particles (hydrophilic particles) according to the present invention were obtained.

Then, in the same manner as in Example 1, the wettability of the pigment before the treatment and the pigment after the treatment with water was evaluated. As a result, the pigment before the treatment did not get wet with water and floated on the water surface. On the other hand, the treated pigment, that is, the pigment particles according to the present invention, were wetted with water and dispersed in water. That is,
It was confirmed that each pigment particle obtained by the production method according to the present invention had excellent wettability to water.

Example 7 A pigment (C.
A solution was prepared by adding 1 g of I. Pigment Red 122) to 40 ml of 98% chlorosulfonic acid and stirring at 50 ° C. for 3 hours to dissolve. Then, instead of the solution used in Example 1, the above solution was sprayed with a spray device 10
The same operations and the like as those in the same example were performed except that they were prepared in the same manner. Thereby, pigment particles (hydrophilic particles) according to the present invention were obtained.

Then, in the same manner as in Example 1, the wettability of the pigment before the treatment and the pigment after the treatment with water was evaluated. As a result, the pigment before the treatment did not get wet with water and floated on the water surface. On the other hand, the treated pigment, that is, the pigment particles according to the present invention, were wetted with water and dispersed in water. That is,
It was confirmed that each pigment particle obtained by the production method according to the present invention had excellent wettability to water.

Example 8 A pigment (C.
A solution was prepared by adding 1 g of I. Pigment Violet 23) to 30 ml of 98% chlorosulfonic acid and stirring at 50 ° C. for 2 hours to dissolve. And Example 1
The above solution was sprayed in place of the solution used in
The same operations and the like as those in the same example were performed except that they were charged to 0. Thereby, pigment particles (hydrophilic particles) according to the present invention were obtained.

The wettability of the pigment before the treatment and the pigment after the treatment were evaluated in the same manner as in Example 1. As a result, the pigment before the treatment did not get wet with water and floated on the water surface. On the other hand, the treated pigment, that is, the pigment particles according to the present invention, were wetted with water and dispersed in water. That is,
It was confirmed that each pigment particle obtained by the production method according to the present invention had excellent wettability to water.

Example 9 Pigment as hydrophobic substance (C.I.
A solution was prepared by adding 1 g of I. Pigment Red 41) to 30 ml of 98% chlorosulfonic acid and stirring and dissolving at 30 ° C. for 3 hours. Then, operations similar to those in Example 1 were performed except that the above solution was charged into the spraying device 10 instead of the solution used in Example 1. Thereby, pigment particles (hydrophilic particles) according to the present invention were obtained.

Then, in the same manner as in Example 1, the wettability of the pigment before the treatment and the pigment after the treatment with water was evaluated. As a result, the pigment before the treatment did not get wet with water and floated on the water surface. On the other hand, the treated pigment, that is, the pigment particles according to the present invention, were wetted with water and dispersed in water. That is,
It was confirmed that each pigment particle obtained by the production method according to the present invention had excellent wettability to water.

[Example 10] 1 g of a pigment (CI Pigment Orange 61) as a hydrophobic substance was added to 98% sulfuric acid 4
A solution was prepared by adding to 0 ml and stirring and dissolving at 80 ° C. for 3 hours. Then, operations similar to those in Example 1 were performed except that the above solution was charged into the spraying device 10 instead of the solution used in Example 1. Thereby, pigment particles (hydrophilic particles) according to the present invention were obtained.

Then, in the same manner as in Example 1, the wettability of the pigment before the treatment and the pigment after the treatment with water was evaluated. As a result, the pigment before the treatment did not get wet with water and floated on the water surface. On the other hand, the treated pigment, that is, the pigment particles according to the present invention, were wetted with water and dispersed in water. That is,
It was confirmed that each pigment particle obtained by the production method according to the present invention had excellent wettability to water.

Example 11 A solution was prepared by adding 1 g of a pigment (CI Pigment Yellow 138) as a hydrophobic substance to 40 ml of 90% sulfuric acid, and stirring and dissolving at 70 ° C. for 3 hours. Then, operations similar to those in Example 1 were performed except that the above solution was charged into the spraying device 10 instead of the solution used in Example 1. Thereby, pigment particles (hydrophilic particles) according to the present invention were obtained.

Then, in the same manner as in Example 1, the wettability of the pigment before the treatment and the pigment after the treatment with water was evaluated. As a result, the pigment before the treatment did not get wet with water and floated on the water surface. On the other hand, the treated pigment, that is, the pigment particles according to the present invention, were wetted with water and dispersed in water. That is,
It was confirmed that each pigment particle obtained by the production method according to the present invention had excellent wettability to water.

[0198]

As described above, the method for producing hydrophilic particles of the present invention comprises dissolving a hydrophobic substance which is solid at normal temperature and pressure in an acidic liquid so as to impart hydrophilicity to the liquid. In this method, the resulting solution is made into particles, and the particles are brought into contact with steam containing water vapor having a temperature higher than the temperature of the particles to form a supersaturated atmosphere of the steam, thereby condensing water on the surface of the particles. In the above method, the formation of the supersaturated atmosphere may be performed by cooling the particles after mixing with the steam containing steam, or after mixing the particles with the steam containing steam,
Adiabatic expansion may be performed.

Therefore, in the above-mentioned method, hydrophilic particles having a relatively small and uniform particle size can be produced without charging the particles, with a simple apparatus and operation, in a short time and at low cost. This has the effect.

In the method for producing hydrophilic particles of the present invention, the particles may be cooled and then brought into contact with steam. Thereby, there is an effect that the hydrophilic particles can be manufactured in a shorter time.

The method for producing hydrophilic particles of the present invention is a method wherein the hydrophobic substance is a pigment. This allows
There is an effect that pigment particles having hydrophilicity can be produced.

The method for producing hydrophilic particles of the present invention is a method wherein the hue of the pigment is red, blue or yellow. Thereby, there is an effect that pigment particles having hydrophilicity and a hue of red, blue or yellow can be produced.

[0203] The method for producing hydrophilic particles of the present invention is a method in which the acidic liquid further contains chlorosulfonic acid and / or sulfuric acid. Thereby, there is an effect that hydrophilic particles to which hydrophilicity has been imparted by introducing a sulfonic acid group can be produced.

The method for producing hydrophilic particles of the present invention is a method in which the particles are further brought into contact with a vapor in the presence of an inert gas. Thereby, for example, by using an inert gas as a carrier of the particles, when the hydrophilic particles are formed by precipitation, it is possible to eliminate undesired reactions and effects on the hydrophilic particles due to the carrier. It has the effect of being able to.

As described above, another method for producing hydrophilic particles according to the present invention is to dissolve a hydrophobic substance which is solid at normal temperature and pressure in an acidic liquid so as to impart hydrophilicity to the hydrophobic substance. A first step of forming a solution into particles, and contacting the particles with steam having a temperature higher than the temperature of the particles and containing steam, forming a supersaturated atmosphere of the steam, and condensing water on the particle surfaces. This is a method including two steps and a third step of collecting and washing the hydrophilic particles obtained in the second step with water. In the above method, the second step may be replaced with a step of mixing the particles with steam containing steam and then cooling, or a step of mixing the particles with steam containing steam and then performing adiabatic expansion. .

Therefore, in the above-mentioned method, the hydrophilic particles having a relatively small and uniform particle diameter and free of impurities can be obtained in a short time and at low cost with a simple apparatus and operation without charging the particles. Is produced.

As described above, the apparatus for producing hydrophilic particles of the present invention comprises a solution prepared by dissolving a hydrophobic substance which is solid at ordinary temperature and pressure in an acidic liquid so as to impart hydrophilicity to the substance. And a condensing device for bringing the particles granulated by the granulating device into contact with supersaturated steam containing water to condense water on the surface of the particles. In the above configuration, in order to form a supersaturated atmosphere, the particles are brought into contact with steam containing steam having a temperature higher than the temperature of the particles, or after the particles are mixed with steam containing steam. To cool, or the particles,
After mixing with steam containing water vapor, it may be configured to expand adiabatically.

Therefore, in the above configuration, hydrophilic particles having a relatively small and uniform particle size can be produced without charging the particles, with a simple apparatus and operation, in a short time and at low cost. The effect that a device can be provided is produced.

The apparatus for producing hydrophilic particles of the present invention further comprises a cooling device for cooling the particles granulated by the granulating device. Thereby, there is an effect that an apparatus capable of manufacturing hydrophilic particles in a shorter time can be provided.

[0210] The apparatus for producing hydrophilic particles of the present invention is further configured such that the granulating apparatus is a spray apparatus for forming the solution into particles by spraying the solution. This allows
This has the effect of providing an apparatus capable of producing hydrophilic particles having a smaller particle diameter.

[0211] The apparatus for producing hydrophilic particles of the present invention has a configuration in which the spraying apparatus further has a particle diameter adjusting section for adjusting the particle diameter. Thereby, there is an effect that an apparatus capable of producing hydrophilic particles having a smaller and uniform particle diameter can be provided.

[Brief description of the drawings]

FIG. 1 is a cross-sectional view illustrating a schematic configuration of a manufacturing apparatus according to a first embodiment relating to a method for manufacturing hydrophilic particles according to the present invention.

FIG. 2 is a chart of an infrared absorption spectrum of a pigment (CI Pigment Red 2) before treatment.

FIG. 3 is a chart of an infrared absorption spectrum of the pigment after treatment.

FIG. 4 is a cross-sectional view illustrating a schematic configuration of a manufacturing apparatus according to a second embodiment relating to a method for manufacturing hydrophilic particles according to the present invention.

FIG. 5 is a schematic cross-sectional view showing a modification of the granulating apparatus used in the manufacturing apparatus.

FIG. 6 is a schematic cross-sectional view showing another modified example of the granulating apparatus used in the manufacturing apparatus.

FIG. 7 is a schematic cross-sectional view showing still another modified example of the granulating apparatus used in the manufacturing apparatus.

FIG. 8 is a cross-sectional view illustrating a schematic configuration of a manufacturing apparatus according to a third embodiment relating to the method for manufacturing hydrophilic particles according to the present invention.

FIG. 9 is a cross-sectional view illustrating a schematic configuration of a manufacturing apparatus according to a fourth embodiment relating to the method for manufacturing hydrophilic particles according to the present invention.

FIG. 10 is a cross-sectional view illustrating a schematic configuration of a manufacturing apparatus according to a fifth embodiment relating to the method for manufacturing hydrophilic particles according to the present invention.

[Explanation of symbols]

 Reference Signs List 3A optical measuring device 3B optical measuring device 4a particle inlet 5 particle take-out tube (particle take-out port) 7 heating device 10 spraying device (granulating device) 11 nozzle 14 solution 15 solution supply tube 16 baffle (particle diameter adjusting section) 18 particles Supply pipe 19 Cooling device 21 Manufacturing device 21a Manufacturing device 21b Manufacturing device 21c Manufacturing device 21d Manufacturing device 22 Reforming tower 22a Steam generation unit 22b Mixing unit (condensing device) 29 Mixing tube (cooling tube) 30 Cooling unit 112 Condensing unit

Claims (33)

[Claims] An aqueous solution of a hydrophobic substance dissolved in an acidic liquid is formed into particles in order to impart hydrophilicity to a hydrophobic substance which is solid at normal temperature and normal pressure. A method for producing hydrophilic particles, comprising: bringing a supersaturated atmosphere of steam into contact with steam having a higher temperature than the steam containing steam to condense water on the particle surface. 2. A solution obtained by dissolving a hydrophobic substance, which is solid at normal temperature and pressure, in an acidic liquid so as to impart hydrophilicity to an acidic liquid, is formed into particles. A method for producing hydrophilic particles, comprising cooling after mixing with steam to form a supersaturated atmosphere of steam and condensing water on the surface of the particles. 3. A solution obtained by dissolving a hydrophobic substance, which is solid at normal temperature and pressure, in an acidic liquid so as to impart hydrophilicity to the acidic liquid, is formed into particles, and the particles are then mixed with water vapor. A method for producing hydrophilic particles, comprising adiabatically expanding after mixing with steam to form a supersaturated atmosphere of steam and condensing water on the surface of the particles. 4. The method for producing hydrophilic particles according to claim 1, wherein the particles are cooled and then brought into contact with steam. 5. The method for producing hydrophilic particles according to claim 1, wherein the hydrophobic substance is a pigment. 6. The method for producing hydrophilic particles according to claim 5, wherein the hue of the pigment is red, blue or yellow. 7. The method for producing hydrophilic particles according to claim 1, wherein the acidic liquid contains chlorosulfonic acid and / or sulfuric acid. 8. The method for producing hydrophilic particles according to claim 1, wherein the particles are brought into contact with steam in the presence of an inert gas. 9. A first step of forming a solution obtained by dissolving a hydrophobic substance, which is solid at normal temperature and pressure, in an acidic liquid so as to impart hydrophilicity to the acidic liquid, comprising: A second step of forming a supersaturated atmosphere of the vapor by contacting with a vapor containing water vapor having a temperature higher than the temperature of the particles, and condensing water on the particle surface; and the hydrophilic particles obtained in the second step. And a third step of collecting and washing with water. 10. A first step in which a solution obtained by dissolving a hydrophobic substance which is solid at normal temperature and pressure in an acidic liquid to impart hydrophilicity to an acidic liquid is formed into particles, After mixing with steam containing steam, the mixture is cooled to form a supersaturated atmosphere of steam, the second step of condensing water on the surface of the particles, and the hydrophilic particles obtained in the second step are collected and washed with water. A method for producing hydrophilic particles, comprising: a third step. 11. A first step of forming a solution obtained by dissolving a hydrophobic substance, which is solid at normal temperature and normal pressure, in an acidic liquid so as to impart hydrophilicity to the acidic liquid, comprising: After mixing with steam containing water vapor, adiabatic expansion is performed to form a supersaturated atmosphere of steam, and the second step of condensing water on the surface of the particles, and collecting the hydrophilic particles obtained in the second step And a third step of washing with water. 12. A granulating device for dissolving a hydrophobic substance which is a solid at normal temperature and normal pressure in an acidic liquid so as to impart hydrophilicity to an acidic liquid, and a granulating apparatus; And a condensing device for condensing water on the surface of the particles by bringing the particles granulated in (1) into contact with supersaturated steam containing water vapor. 13. The condenser according to claim 12, wherein said condenser is brought into contact with said particles and steam having a temperature higher than the temperature of said particles to form a supersaturated atmosphere of said steam. An apparatus for producing the hydrophilic particles according to the above. 14. The apparatus for producing hydrophilic particles according to claim 12, further comprising a cooling device for cooling the particles granulated by the granulating device. 15. The production of hydrophilic particles according to claim 12, wherein the granulating device is a spraying device for spraying the solution to form the solution into particles. apparatus. 16. The apparatus for producing hydrophilic particles according to claim 15, wherein the granulating apparatus has a particle diameter adjusting section for adjusting the particle diameter. 17. A steam generating part for generating a condensing agent vapor having a processing space therein, and a hydrophilic substance imparted to a hydrophobic substance which is solid at normal temperature and normal pressure and is connected to the vapor generating part. A cooling pipe for condensing a condensing agent vapor for particles obtained by dissolving the hydrophobic substance in an acidic liquid to form particles, and a particle introduction for introducing the particles into a processing space of a vapor generation unit. An opening, a particle outlet for taking out particles after processing from the cooling pipe, and a control means for changing the temperature in the processing space of the steam generating section and the temperature in the cooling pipe, respectively. Equipment for producing conductive particles. 18. A steam generating section for generating a condensing agent vapor having a processing space therein, and a hydrophobic substance which is solid at normal temperature and normal pressure is hydrophilic with respect to the processing space of the steam generating section. A particle introduction port for introducing particles obtained by dissolving the hydrophobic substance in an acidic liquid to give a particle, and a particle supply means for supplying particles from the particle introduction port into the steam generation section. First adjusting means for changing the temperature in the steam generating section, a cooling pipe communicating with the steam generating section, second adjusting means for changing the temperature of the cooling pipe, and a particle collecting section for extracting particles from the cooling pipe. An outlet, a particle discharging means for discharging the treated particles from the cooling pipe from the particle outlet, and supplying the particles into the steam generating section by the particle supplying means, and saturating the condensing agent vapor in the steam generating section by the first adjusting means. State and second tone Control means for controlling each of the means so that the condensing agent vapor in the cooling pipe is supersaturated by the temperature change due to the means and the condensing agent is condensed on the surface and the treated particles are discharged from the cooling pipe by the particle discharging means. An apparatus for producing hydrophilic particles, comprising: 19. A steam generator according to claim 17, wherein at least a part of an inner wall forming a processing space in the steam generator has a porous material capable of containing a condensing agent.
An apparatus for producing the hydrophilic particles according to the above. 20. The apparatus for producing hydrophilic particles according to claim 17, wherein at least a part of the inner wall of the cooling pipe has a water-repellent material. 21. The method according to claim 17, wherein the processing space of the steam generating section is formed in a tubular shape and is set at an angle within a range of 90 degrees from horizontal. An apparatus for producing the hydrophilic particles according to the above. 22. A condensing device having a processing space capable of being sealed therein for generating a condensing agent vapor, and a condensing device for imparting hydrophilicity to a hydrophobic substance which is solid at normal temperature and normal pressure. Particle inlet for introducing the particles of the solution obtained by dissolving the acidic substance in the acidic liquid into the processing space of the condenser, and a particle collection port for removing the processed particles from the processing space of the condenser. An apparatus for producing hydrophilic particles, comprising: an outlet; and pressure adjusting means for changing the pressure in the processing space of the condenser. 23. A pressure adjusting means comprising: a substantially polygonal column-shaped rotating rotor; and an inner wall portion abutting against each ridge end of the rotor, each outer surface between adjacent ridge ends of the rotor, 23. The apparatus for producing hydrophilic particles according to claim 22, wherein each processing space formed between the outer surface and the inner wall portion facing each other is changed so as to change according to rotation of the rotor. 24. A box-shaped condensing device for generating a condensing agent vapor having a processable space inside which can be sealed, and a hydrophobic solid which is solid at normal temperature and normal pressure with respect to the processing space of the condensing device. A particle inlet for introducing particles obtained by dissolving the hydrophobic substance in an acidic liquid to impart hydrophilicity to the substance, and a particle for supplying particles from the particle inlet to the condenser. Supply means, a rotor-type pressure adjusting means for changing the pressure in the processing space of the condenser, a particle outlet for extracting particles after processing from the processing space of the condenser, and particles processed from the particle outlet. The particles are supplied to the condensing device by the particle discharging means and the particle supplying means, and the condensing agent is condensed on the surface of the particles by changing the pressure of the condensing agent vapor in the condensing device into a supersaturated state by the pressure adjusting means. Let me, after processing Obtain particles, the particles after the treatment so as to discharge from the condenser at the particle discharge unit, the apparatus for producing hydrophilic particles characterized in that a control means for controlling each unit. 25. A condensing device having a processable space therein and generating a condensing agent vapor, and a condensing device for imparting hydrophilicity to a hydrophobic substance which is solid at normal temperature and normal pressure. Particle inlet for introducing the particles of the solution obtained by dissolving the acidic substance in the acidic liquid into the processing space of the condenser, and a particle collection port for removing the processed particles from the processing space of the condenser. An apparatus for producing hydrophilic particles, comprising: an outlet; and pressure adjusting means for adiabatically changing the pressure in the processing space of the condenser. 26. A box-shaped condenser for generating a condensing agent vapor having a processable space therein, and a hydrophobic solid which is solid at normal temperature and normal pressure with respect to the processing space of the condenser. A particle inlet for introducing a particle obtained by dissolving a solution obtained by dissolving the hydrophobic substance in an acidic liquid to impart hydrophilicity to the substance, and a particle for supplying particles from the particle inlet to the processing space. Supply means, pressure adjusting means for adiabatically changing the pressure in the processing space, a particle outlet for taking out the processed particles from the processing space of the condenser, and discharging the processed particles from the particle outlet. A process in which the particles are supplied into the processing space by the particle discharge means and the particle supply means, and the condensing agent vapor is condensed on the surface of the particles in a supersaturated state by the pressure change by the pressure adjusting means in the processing space. Obtain later particles and process After the particles to discharge from the condenser at the particle discharge unit, the apparatus for producing hydrophilic particles characterized in that a control means for controlling each unit. 27. A condensing device for generating a condensing agent vapor having a processing space that can be hermetically sealed therein and a cylindrical portion communicating with the processing space, and a hydrophobic material that is solid at normal temperature and normal pressure. A particle inlet for introducing particles obtained by dissolving a solution obtained by dissolving the hydrophobic substance in an acidic liquid to impart hydrophilicity to the hydrophobic substance into a processing space of the condenser; and a processing space of the condenser. And a piston-type pressure adjusting means that reciprocates in the cylindrical portion in order to adiabatically change the pressure in the processing space of the condensing device. An apparatus for producing hydrophilic particles, characterized in that: 28. A box-shaped condensing device for generating a condensing agent vapor having a processable space inside thereof, and a hydrophobic solid which is solid at normal temperature and normal pressure with respect to the processing space of the condensing device. Inlet for introducing particles obtained by dissolving a solution obtained by dissolving the hydrophobic substance in an acidic liquid to impart hydrophilicity to the hydrophobic substance, and supplying the particles from the particle inlet to the condenser. Particle supply means, pressure adjusting means for changing the pressure in the processing space by a piston type, a particle outlet for extracting the processed particles from the processing space, and a particle discharge for discharging the processed particles from the particle outlet. Means, supplying particles into the condenser by the particle supply means, and treating the particles after the condensing agent condensed on the surface in a supersaturated state by adiabatic expansion due to a pressure change by the pressure adjusting means in the condensing agent on the surface. Get The particles after physical to discharge from the condenser at the particle discharge unit, the apparatus for producing hydrophilic particles characterized in that a control means for controlling each unit. 29. The condensing device according to claim 22, wherein at least a part of a wall for forming a processing space in the condensing device has a porous material capable of containing a condensing agent. 5. An apparatus for producing hydrophilic particles according to any one of the above. 30. A transport gas supply device for supplying a gas (carrier) for transporting particles and vapor, the transport gas supply device including an impurity removing device for removing impurities in the gas. An apparatus for producing hydrophilic particles according to any one of claims 17 to 29. 31. The method for producing hydrophilic particles according to claim 17, wherein cooling means for cooling a gas (carrier) for transporting the particles and vapor is provided. apparatus. 32. A first detecting means for detecting a particle size of particles before being condensed by steam, and a second detecting means for detecting a particle size of particles after being condensed by steam.
The apparatus for producing hydrophilic particles according to any one of claims 17 to 31, further comprising a detection unit. 33. A system comprising: third detecting means for detecting the number concentration of particles before being condensed by steam; and fourth detecting means for detecting number concentration of particles after being condensed by steam. Claim 17
33. The apparatus for producing hydrophilic particles according to any one of the above items.