JP2022053935A - Vertical multi-stage contact separation apparatus and vertical multistage contact separation method using the same - Google Patents

Abstract

To improve the separation rate and separation efficiency of hydrophobic particles when the hydrophobic particles and hydrophilic particles are separated from a mixture of the hydrophobic particles and the hydrophilic particles.SOLUTION: In order to solve the above problem, according to an aspect of the present invention, there is provided a vertical multistage contact separation apparatus including: a plurality of settler portions; mixer portions disposed between the plurality of settler portions; a partition plate separating the settler portions and the mixer portions and having a through-hole; a light liquid introduction port that introduces light liquid into the mixer portion above the lowermost settler portion; a heavy liquid introduction port that introduces heavy liquid into the mixer portion below the uppermost settler portion; a slurry introduction port that introduces slurry in which pre-pulverized separation target mixture is dispersed in water into one of the mixer portions; and outlets that respectively discharge, among an aqueous phase, an emulsion phase, and a hydrophobic liquid phase formed in a vertical outer wall tube, at least the aqueous phase and the emulsion phase.SELECTED DRAWING: Figure 3

Description

The present invention relates to a vertical multi-stage contact separation device and a vertical multi-stage contact separation method using the same.

Fly ash generated during power generation at a coal-fired thermal power plant or the like is recycled into a raw material for concrete, a raw material for building materials, a raw material for cement, and the like. However, fly ash contains unburned carbon particles, which are unburned carbon components, in the ash composed of metal oxides such as Al ₂ O ₃ and SiO ₂ . Therefore, in order to improve the quality of the recycled fly ash, it is preferable to separate and remove the unburned carbon particles contained in the fly ash.

As a method for separating unburned carbon particles in fly ash, for example, an electrostatic separation method and a flotation method are known. The electrostatic separation method is a method in which charged unburned carbon particles are attracted to the positive electrode side and separated by introducing fly ash into the electrodes of the parallel plate in a dry state. In the flotation method, unburned carbon particles are attached to microair generated by using a foaming agent in a fly ash slurry via a collecting agent such as kerosene to obtain unburned carbon particles. It is a method of floating and separating.

For example, Patent Document 1 discloses a method for removing unburned carbon particles in fly ash by flotation. In the flotation method of Patent Document 1, first, water is added to stir the slurried fly ash to generate active energy on the surface of the unburned carbon particles, and the unburned carbon particles are made into oil. (Flottation). Next, a collecting agent such as kerosene and light oil and a foaming agent are added to the slurry containing the unburned carbon particles that have become lipophilic to attach the collecting agent to the unburned carbon particles, and the generated bubbles are not present. Flotation is performed by adhering fuel carbon particles. By such a flotation method, a mixture of unburned carbon particles (specific gravity: 1.3 to 1.5) which are hydrophobic particles and metal oxides (specific gravity: 2.4 to 2.6) which are hydrophilic particles. Unburned carbon particles are separated from the fly ash.

On the other hand, as a multi-stage contact separation device for separating liquids from each other, for example, a horizontal multi-stage contact separation device disclosed in Patent Document 2 and a vertical multi-stage contact separation device disclosed in Patent Document 3 are known. In the technique disclosed in Patent Document 2, the settler section (stationary chamber) and the mixer section (stirring chamber) are alternately arranged in the horizontal direction. In the technique disclosed in Patent Document 3, the settler section (separation chamber) and the mixer section (mixing chamber) are alternately arranged in the vertical direction. Further, the separation chamber and the mixing chamber below the separation chamber are connected by a descending pipe. The descending pipe supplies the heavy liquid in the separation chamber connected above the descending pipe to the mixing chamber connected below the descending pipe.

JP-A-2007-167825 Japanese Unexamined Patent Publication No. 11-244604 Japanese Unexamined Patent Publication No. 9-271649

However, in the flotation method in which unburned carbon particles contained in fly ash are attached to bubbles and floated as described in Patent Document 1, there is a problem that the separation speed of the unburned carbon particles is slow and the separation efficiency is poor. there were.

Specifically, in the flotation method described in Patent Document 1, as shown in FIG. 15, water in which many particles of metal oxide 102 are suspended in a state where water and fly ash are mixed and stirred. In the phase 105, the particles of the unburned carbon particles 101 adhere to the fine bubbles 103 via the collecting agent 104, and the unburned carbon particles 101 float in the aqueous phase 105 together with the bubbles 103. At this time, the unburned carbon particles 101 may be separated from the bubbles 103, and the unburned carbon particles 101 gradually rise in the aqueous phase 105 while repeating floating and settling, and gather on the surface layer portion of the aqueous phase 105. Therefore, since the separation rate of the unburned carbon particles 101 is slow, in order to separate the unburned carbon particles 101 from the metal oxide 102 and reduce the content of the unburned carbon particles 101 to the target value or less, for example, It takes a long time of about 1 hour.

Further, in the above flotation method, the separation efficiency of the unburned carbon particles 101 is the particle size of the unburned carbon particles 101, the degree of hydrophobicity (these depend on the type of coal used), and the existence form of the unburned carbon particles 101. It is considerably affected by such factors. For example, when the particles of the unburned carbon particles 101 are large, the weight of the unburned carbon particles 101 makes it difficult for the unburned carbon particles 101 to adhere to the bubbles 103, and also makes it difficult for the unburned carbon particles 101 to float in the aqueous phase 105. Further, when the unburned carbon particles 101 are in the existing form of being bitten into the metal oxide 102, the surface portion of the unburned carbon particles 101 to which the bubbles 103 can adhere becomes small, so that the unburned carbon particles 101 become the bubbles 103. It becomes difficult to adhere. Due to these causes, the separation rate of the unburned carbon particles 101 is lowered, the separation efficiency of the unburned carbon particles 101 is deteriorated, and the content of the unburned carbon particles 101 in the mixture cannot be lowered to the target value in many cases. The processing cost was also high.

On the other hand, the techniques disclosed in Patent Documents 2 and 3 are devices assuming that liquids are separated from each other. Attempts to remove unburned carbon particles from fly ash slurries using these techniques are expected to cause various problems. For example, when a fly ash slurry is introduced into the technique disclosed in Patent Document 2, there may be a problem that particles such as unburned carbon particles (particularly emulsion particles described later) precipitate in a static chamber and do not flow. .. When a fly ash slurry is introduced into the technique disclosed in Patent Document 3, there may be a problem that particles such as unburned carbon particles (particularly emulsion particles described later) settle in a separation chamber and do not flow. Further, there may be a problem that the descending tube is clogged with particles such as unburned carbon particles (particularly emulsion particles described later).

In the above, the problem of separating unburned carbon particles from fly ash, which is a mixture of unburned carbon particles (hydrophobic particles) and metal oxides (hydrophilic particles), has been described, but other hydrophobicities have been described. It is assumed that similar problems may occur even when each particle is separated from a mixture of particles and hydrophilic particles.

Therefore, the present invention has been made in view of the above problems, and an object of the present invention is to separate hydrophobic particles and hydrophilic particles from a mixture of hydrophobic particles and hydrophilic particles. The purpose is to improve the separation speed and separation efficiency of the particles.

In order to solve the above problems, according to a certain viewpoint of the present invention, it is a vertical multi-stage contact separation device that separates hydrophobic particles and hydrophilic particles from a mixture to be separated in which hydrophobic particles and hydrophilic particles are mixed. It contains hydrophobic particles, hydrophilic particles, a light liquid, and a heavy liquid having a higher specific gravity than the light liquid, and contains contents of the heavy liquid and the light liquid, one of which is water and the other of which is a hydrophobic liquid. A vertical outer wall tube, a plurality of settler sections arranged in the vertical direction in the vertical outer wall tube, and at least one mixer section and a settler section arranged between the plurality of settler sections to stir the contents. In the mixer section above and near the bottom settler section, which is the bottom settler section, and a partition plate that partitions the mixer section and has a through hole for distributing the contents between the mixer section and the settler section. The light liquid introduction port that introduces the light liquid into the mixer, the heavy liquid introduction port that introduces the heavy liquid into the mixer section below and near the top settler section, which is the top settler section, and the mixture to be separated and the mixture to be separated. A slurry introduction port for introducing a slurry dispersed in water or a slurry in which a pre-crushed mixture to be separated is dispersed in water into one of the mixer units, and an aqueous phase, an emulsion phase, and a hydrophobic phase formed in a vertical outer wall tube. Provided is a vertical multi-stage contact separation device comprising an discharge port for discharging at least an aqueous phase and an emulsion phase among the sexual liquid phases.

Here, in at least one region between the mixer section provided with the slurry introduction port and the uppermost settler section, and between the mixer section provided with the slurry introduction port and the lowermost settler section, 1 A pair or more of the mixer section and the settler section may be further arranged, and the mixer section and the settler section may be arranged alternately.

Further, the hole diameter of the through hole formed in the partition plate may be 8 to 50 mm, and the aperture ratio may be 10 to 50 area%.

Further, the vertical multi-stage contact separation device may further have an observation window capable of observing at least one of the interface between the aqueous phase and the emulsion phase and the interface between the emulsion phase and the hydrophobic liquid phase.

Further, the vertical multi-stage contact separation device has an observation window capable of observing the interface between the emulsion phase and the hydrophobic liquid phase, and the observation window is a transparent plate having no hydrophilic functional group on the surface. Alternatively, it may be a transparent plate covered with a transparent paint having no hydrophilic functional group.

Further, the vertical multi-stage contact separation device may have an umbrella that obstructs the distribution of the contents in the upper part or the lower part of any observation window inside the vertical multi-stage contact separation device.

Further, the light liquid may be water, the heavy liquid may be a hydrophobic liquid, and the mixture to be separated in which hydrophobic particles and hydrophilic particles are mixed may be fly ash.

Further, the light liquid may be a hydrophobic liquid, the heavy liquid may be water, and the mixture to be separated in which hydrophobic particles and hydrophilic particles are mixed may be fly ash.

According to another aspect of the present invention, there is provided a vertical multi-stage contact separation method using the above-mentioned vertical multi-stage contact separation device.

Here, in the vertical multi-stage contact separation method, at least one of the interface between the aqueous phase and the emulsion phase and the interface between the emulsion phase and the hydrophobic liquid phase may be maintained at a constant level.

Further, the light liquid is water, the heavy liquid is a hydrophobic liquid, and the mixture to be separated in which hydrophobic particles and hydrophilic particles are mixed is fly ash. The interface with the emulsion phase may be maintained at a constant level.

Further, the light liquid is a hydrophobic liquid, the heavy liquid is water, and the mixture to be separated in which hydrophobic particles and hydrophilic particles are mixed is fly ash. The interface with the emulsion phase may be maintained at a constant level.

Further, the mixture to be separated may be pre-pulverized with a bead mill and then introduced into a vertical multi-stage contact separation device.

According to the above viewpoint of the present invention, it is possible to improve the separation rate and separation efficiency of the hydrophobic particles when the hydrophobic particles and the hydrophilic particles are separated from the mixture in which the hydrophobic particles and the hydrophilic particles are mixed.

It is explanatory drawing which shows typically the fly ash which is an example of a mixture to be separated. It is sectional drawing which shows typically the surface state of fly ash. It is sectional drawing which shows typically the fly ash after pulverization. It is sectional drawing which shows typically the surface state of the fly ash after pulverization. It is explanatory drawing which shows typically the whole structure of the vertical multi-stage contact separation system which concerns on this embodiment. It is a top view which shows the upper end surface of the partition plate with different aperture ratios. It is explanatory drawing which shows the state of the contents of a mixer part schematically. It is explanatory drawing which shows the state of the contents of the settler part schematically. It is explanatory drawing which shows typically the flow | flow state of the particle between a mixer part and the settler part above and there. It is explanatory drawing which shows the function of an umbrella schematically. It is explanatory drawing which shows typically the modification of the vertical multi-stage contact separation apparatus which concerns on this embodiment. It is a flowchart for demonstrating the process of the vertical multi-step contact separation method which concerns on this embodiment. It is a graph which shows the correlation between the opening ratio of a partition plate and the unburned carbon content ( _CA ) in refined fly ash, or the unburned _carbon content (CC) in unburned carbon concentrate. It is a graph which shows the correlation between the aperture ratio of a partition plate and C _C / C _A. It is explanatory drawing which shows typically the whole structure of the vertical type multi-stage contact separation apparatus which concerns on the modification of this embodiment. It is explanatory drawing which shows typically the whole structure of the vertical multi-stage contact separation apparatus which concerns on Example 1. FIG. It is a schematic diagram which shows the flotation principle of unburned carbon in a conventional flotation method.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. In the present specification and the drawings, components having substantially the same functional configuration are designated by the same reference numerals, so that duplicate description will be omitted. Further, in the present embodiment, the numerical limitation range represented by using "-" means a range including the numerical values before and after "-" as the lower limit value and the upper limit value. Numerical values that indicate "greater than" or "less than" do not fall within the numerical range.

<1. Mixture to be separated>
First, a vertical multi-stage contact separation device according to an embodiment of the present invention and a mixture to be separated, hydrophilic particles, hydrophobic particles and the like to be treated by the vertical multi-stage contact separation method using the same will be described.

The mixture to be separated is a mixture of hydrophobic particles and hydrophilic particles. Examples of such a mixture to be separated include fly ash, blast furnace gas ash, coal and the like. Fly ash is a substance discharged from a coal-fired thermal power plant, contains unburned carbon particles (a type of carbon particles) as hydrophobic particles, and is a metal containing SiO ₂ and Al ₂ O ₃ as main components as hydrophilic particles. Contains oxide particles. Most fly ash contains, for example, about 50 to 95% by mass of metal oxide particles which are hydrophilic particles and about 5 to 50% by mass of unburned carbon particles which are hydrophobic particles.

Blast furnace gas ash is a collection of dust from raw materials charged into the blast furnace, dust generated by the metallurgical reaction in the blast furnace, in other words, blast furnace dust collection ash, and unburned carbon particles derived from coke as hydrophobic particles. It contains metal oxide particles containing Fe ₂ O ₃ as a main component as hydrophilic particles. The blast furnace gas ash contains, for example, 15 to 30% by mass of unburned carbon particles and 70 to 85% by mass of metal oxide particles.

By the way, in the mixture to be separated, which is the object to be treated in the present embodiment, the hydrophobic particles and the hydrophilic particles may exist independently of each other, or both may be integrated. An example of the case where both are integrated is a case where hydrophilic particles are mixed in the surface layer portion or the inside of the hydrophobic particles. Specifically, the hydrophobic particles are often porous. When the hydrophobic particles become porous, the hydrophilic particles are often mixed in the pores of the surface layer portion. Then, the hydrophilic particles mixed in the surface layer portion of the hydrophobic particles impart hydrophilicity to the hydrophobic particles. That is, a part of the surface layer portion of the hydrophobic particles is often hydrophilic. Further, the metal oxide particles may be mixed in the pores inside the hydrophobic particles.

1A and 1B (hereinafter collectively referred to as FIG. 1) schematically show fly ash. As shown in FIG. 1, the unburned carbon particles P2 are porous particles, and a large number of pores P20 are formed on the surface layer of the unburned carbon particles P2. Further, the metal oxide particles P1 are substantially spherical solid particles, and may be attached to the surface of the unburned carbon particles P2, or a plurality of fine particles formed on the surface layer of the unburned carbon particles P2. It may be present inside the hole P20. Further, although not shown in FIG. 1, the metal oxide particles P1 may be mixed in the pores inside the unburned carbon particles P2.

If hydrophilic particles are mixed in the surface layer or inside of the hydrophobic particles (especially if hydrophilic particles are mixed in the inside of the hydrophobic particles), simply stir the mixture to be separated with water and a hydrophobic liquid. It may be difficult to sufficiently separate the two by just doing so.

Therefore, in order to increase the separation efficiency of the hydrophobic particles and the hydrophilic particles, it is preferable to pre-pulverize the mixture to be separated. By such pre-grinding, the hydrophilic particles in the surface layer portion or the inside of the hydrophobic particles can be removed from the hydrophobic particles. However, even with such pre-grinding, hydrophilic particles may remain on the surface layer of the hydrophobic particles. Then, a part of the surface layer portion of the hydrophobic particles is made hydrophilic by the remaining hydrophilic particles. Further, such pre-grinding may be performed by wet pulverization using a bead mill, and in this case, water may remain on the surface layer portion of the hydrophobic particles. Water remaining on the surface layer of the hydrophobic particles also imparts hydrophilicity to the surface layer of the hydrophobic particles.

2A and 2B (hereinafter collectively referred to as FIG. 2) schematically show unburned carbon particles wet-milled with a bead mill. As shown in FIG. 2, the unburned carbon particles P2 in the fly ash are crushed, divided into a plurality of pieces at the fracture surface P21, and refined. As a result, the substantially spherical metal oxide particles P1 that have entered the pores P20 near the fracture surface P21 are released from the pores P20. Therefore, not only the metal oxide particles P1 adhering to the surface of the unburned carbon particles P2 but also the metal oxide particles P1 that have entered the pores P20 are separated and removed from the unburned carbon particles P2. , The unburned carbon particles P2 and the metal oxide particles P1 can be more preferably separated. However, even with such a treatment, as shown in FIG. 2B, the metal oxide particles P1 may remain on the surface layer portion of the unburned carbon particles P2.

In the present embodiment, hydrophilic particles (for example, metal oxide particles) and hydrophobic particles (for example, unburned carbon particles) are separated from the mixture to be separated in which hydrophilic particles and hydrophobic particles are mixed as described above. And collect. As a result, the metal oxide particles (for example, refined fly ash) are reused as raw materials for concrete (aggregate, admixture, etc.), building materials, etc., and unburned carbon particles (for example, unburned carbon concentrate). Is reused, for example, as a carbon material for power generation, iron making, cement clinker, and the like. At this time, if the carbon content in the recovered metal oxide particles can be reduced to, for example, 5% by mass or less, the quality of the metal oxide particles is improved and the recycling use is improved. In particular, if the carbon content in the recovered metal oxide particles can be reduced to 3% by mass or less, the ignition loss (carbon) in the quality regulation of fly ash I for concrete described in JIS A6201-2008. By adjusting the quality regulations such as other powderiness, the metal oxide particles can be recycled for a fee as fly ash for concrete, and the recycling use will be expanded. ..

<2. Hydrophobic liquid>
Next, the hydrophobic liquid used in the separation method according to the present embodiment will be described. The hydrophobic liquid is a liquid having hydrophobicity, that is, a liquid having a property of having a low affinity for water (difficult to dissolve in water or being difficult to mix with water). The hydrophobic liquid is, for example, a liquid having a solubility in water at 20 ° C. of 0 g / L or more and 5.0 g / L or less. The hydrophobicity in the present specification is a property including lipophilicity. The hydrophobic liquid may be, for example, an organic solvent having hydrophobicity (hereinafter referred to as “hydrophobic liquid”), various oils, or the like. Since the hydrophobic liquid has a low affinity for water, when the mixed liquid in which the hydrophobic liquid and water are mixed and stirred is allowed to stand, the aqueous phase mainly composed of water and the hydrophobic liquid phase mainly composed of the hydrophobic liquid are allowed to stand. It is separated into two phases. Although details will be described later, when a mixture (slurry) of a mixture to be separated, water, and a hydrophobic liquid to be treated is allowed to stand, an emulsion phase is formed between the aqueous phase and the hydrophobic liquid phase. .. A large amount of hydrophobic particles are contained in this emulsion phase.

Further, in the present embodiment, as the hydrophobic liquid, a liquid having a specific density different from that of water, that is, a liquid having a specific gravity greater than or less than 1, is used. By using a hydrophobic liquid having a specific gravity different from that of water, when the mixed solution of the hydrophobic liquid and water is stirred and then allowed to stand, it is separated into an aqueous phase and a hydrophobic liquid phase due to the difference in specific gravity between the two liquids. In the present embodiment, of the water and the hydrophobic liquid, the one having a smaller (lighter) specific gravity is also referred to as a "light liquid", and the one having a larger (heavy) specific gravity is also referred to as a "heavy liquid".

The specific gravity of the hydrophobic liquid is preferably 0.95 or less or 1.05 or more. As a result, after the mixture to be separated, water (specific gravity 1), and the hydrophobic liquid are mixed and allowed to stand, the mixed liquid quickly becomes an emulsion phase, an aqueous phase, and a hydrophobic liquid in a short time of, for example, about 1 to 30 seconds. It is separated into three phases, a liquid phase. Therefore, the separation rate of hydrophobic particles and hydrophilic particles is improved. Further, in the recovery step, after the hydrophobic particles are recovered by the solid-liquid separation device, the hydrophobic liquid adhering to the hydrophobic particles is evaporated. Therefore, the boiling point of the hydrophobic liquid is preferably less than 200 ° C, more preferably lower than the boiling point of water, specifically less than 90 ° C. The details of the recovery process will be described later.

Hydrophobic liquids are typically solvents, oils and the like. Examples of the hydrophobic liquid having a specific gravity of 0.95 or less include n-pentane, n-hexane, kerosene, gasoline, kerosene and the like, and examples of the hydrophobic liquid having a specific gravity of 1.05 or more include a bromine-based solvent. , Fluorine-based solvent, chlorine-based solvent and the like. More specifically, it is trichlorethylene, tetrachlorethylene, 1-bromopropane, hydrofluoroether and the like. Considering the difficulty of ignition, stability, ease of separation, etc. of the hydrophobic liquid, it is preferable to use a hydrophobic liquid having a specific gravity larger than that of water.

Next, hydrophilic particles and hydrophobic particles will be described. The hydrophilic particles are particles having an affinity for water and have a property of being more easily mixed with water than the above-mentioned hydrophobic liquid. On the other hand, the hydrophobic particles are particles having an affinity for the hydrophobic liquid, and have a property of being more easily mixed with the hydrophobic liquid than water.

As described above, the hydrophilic particles are, for example, particles of metal oxides such as Al ₂ O ₃ , SiO ₂ , and Fe ₂ O ₃ , but if the particles have hydrophilicity, they may be particles of other materials. There may be. On the other hand, the hydrophobic particles are, for example, coal powder such as unburned carbon or coke powder, but if the particles have hydrophobicity and a part of the surface thereof has hydrophilicity, the particles are made of other materials. May be. When a part of the surface of the hydrophobic particles is hydrophilic, for example, when the hydrophobic particles are introduced into a container containing an equal volume of a hydrophobic liquid having a specific gravity different from that of water, and the mixture is stirred and then allowed to stand, the specific gravity becomes higher than that of water. An emulsion phase is formed in the middle part with a different hydrophobic liquid, and hydrophobic particles are concentrated in the emulsion phase. Here, as a container that can be used for the above test (that is, a container in which the emulsion phase can be observed), for example, a closed glass container in which a plastic tape such as polyethylene is attached to a part of the inside of the container in the vertical direction. Can be mentioned. By using such a container, the interface between the aqueous phase and the emulsion phase can be recognized from the part where the wetted part is glass, and the emulsion phase and the hydrophobic liquid can be recognized from the part where the wetted part is a plastic tape. The interface with the phase can be recognized. The reason will be described later. By doing so, it is possible to determine whether or not a part of the surface of the hydrophobic particles is hydrophilic.

The content of hydrophilic particles and the content of hydrophobic particles contained in the mixture to be separated, which is the object to be treated, are not particularly limited, but for example, the content of hydrophilic particles in the mixture to be separated is 5 to 97 mass. The content of the hydrophobic particles may be about 3 to 95% by mass. However, the total content of the hydrophilic particles and the hydrophobic particles is 100% by mass or less. When the hydrophobic particles are unburned carbon particles, for example, when the mixture to be separated is fly ash or blast furnace gas ash, the ignition loss rate can be measured and the value can be used as the content of the hydrophobic particles. .. The ignition loss rate is the mass loss rate when a sample dried at 105 ° C. is held in an atmospheric atmosphere oven set at 975 ° C. for 15 minutes or more.

<3. Overview of separation method>
In this embodiment, hydrophilic particles and hydrophobic particles are separated from the mixture to be separated by using the vertical multi-stage contact separation system 10A described later. Therefore, first, an outline of a separation method (vertical multi-stage contact separation method) using the vertical multi-stage contact separation system 10A will be described with reference to FIGS. 3, 13, 5, and 6. 3 is an explanatory diagram showing a configuration example of a vertical multi-stage contact separation device 10 preferably used when the light liquid 100 is water and the heavy liquid 200 is a hydrophobic liquid, and FIG. 13 is an explanatory diagram showing the configuration example of the vertical multi-stage contact separation device 10. Is an explanatory diagram showing a configuration example of a vertical multi-stage contact separation device 10'in which is a hydrophobic liquid and the heavy liquid 200 is preferably used when the heavy liquid 200 is water. Of course, even when the light liquid 100 is a hydrophobic liquid and the heavy liquid 200 is water, the vertical multi-stage contact separation device 10 may be used, or the light liquid 100 is water and the heavy liquid 200 is hydrophobic. When liquid, the vertical multi-stage contact separation device 10'may be used. However, in these cases, at least, it is necessary to replace the vertical relationship between the first interface observation window 70 and the second interface observation window 80 shown in FIGS. 3 and 13. The reason will be described later.

The vertical multi-stage contact separation method according to the present embodiment is hydrophilic from the separation target mixture (for example, fly ash) 310 in which hydrophilic particles (for example, metal oxide particles) and hydrophobic particles (for example, unburned carbon particles) are mixed. This is a wet separation method for separating particles and hydrophilic particles.

In this vertical multi-stage contact separation method, water is used as a scavenger for hydrophilic particles, and a hydrophobic liquid having a specific gravity different from that of water is used as a scavenger for hydrophobic particles. Further, the mixture to be separated (solid content) is mixed with water and / and a hydrophobic liquid, stirred, and then wet-ground to produce a first slurry 300 in which the pre-ground mixture of the mixture to be separated is dispersed (. Pre-grinding process). The pre-pulverized product contains hydrophilic particles and hydrophobic particles, but hydrophilic particles may remain particularly on the surface layer portion of the hydrophobic particles. Therefore, a part of the surface layer portion of the hydrophobic particles is often hydrophilic. Next, the first slurry 300 is introduced into the vertical multi-stage contact separation device 10 from the slurry introduction port 10d installed in the middle of the vertical multi-stage contact separation system 10A (slurry introduction step).

On the other hand, a heavy liquid (water or a hydrophobic liquid having a larger specific gravity than water (heavy) than water) 200 is introduced into the vertical multi-stage contact separation device 10 from the upper part (heavy liquid introduction port 10c) of the vertical multi-stage contact separation device 10. (Heavy liquid introduction step), From the lower part (light liquid introduction port 10e) of the vertical multi-stage contact separation device 10, a light liquid (water or a hydrophobic liquid having a smaller specific gravity than water (lighter)) 100 is introduced into the vertical multi-stage contact separation device. Introduce within 10 (light liquid introduction step).

Here, as an example of a preferable combination of the light liquid 100, the heavy liquid 200, and the mixture to be separated 310, the light liquid 100 is water, the heavy liquid 200 is a hydrophobic liquid having a specific gravity of 1.05 or more, and the mixture to be separated 310 is a fly. It is a combination that becomes ash. As another combination, the light liquid 100 is a hydrophobic liquid having a specific gravity of 0.95 or less, the heavy liquid 200 is water, and the mixture 310 to be separated is fly ash. Of course, the combination of the light liquid 100, the heavy liquid 200, and the mixture to be separated 310 is not limited to these. For example, blast furnace gas ash or the like may be used as the mixture to be separated 310.

A plurality of settler portions 30 and a mixer portion 40 are alternately provided in the vertical multi-stage contact separation device 10 in the height direction. Then, the content 40c (see FIG. 5) in the mixer unit 40 is stirred by the mixer unit 40, and the content 30c is allowed to stand in the settler unit 30 (see FIG. 6). By performing the above-mentioned processing by each settler unit 30 and the mixer unit 40, the contents of the vertical multi-stage contact separation device 10 are separated into the light liquid phase 500, the emulsion phase 600, and the heavy liquid phase 700 from the top (specific gravity separation). Specific gravity separation step).

Of the light liquid phase 500 and the heavy liquid phase 700, one is an aqueous phase and the other is a hydrophobic liquid phase. That is, when the specific gravity of the hydrophobic liquid is larger than that of water, the light liquid phase 500 is the aqueous phase and the heavy liquid phase 700 is the hydrophobic liquid phase. On the other hand, when the specific gravity of the hydrophobic liquid phase is smaller than that of water, the light liquid phase 500 is the hydrophobic liquid phase and the heavy liquid phase 700 is the aqueous phase.

What is important here is that the first slurry 300 is not only separated into two phases, a light liquid phase 500 and a heavy liquid phase 700, but also an emulsion phase 600 is formed between these phases. The hydrophilic particles are mainly present in the aqueous phase, and the hydrophobic particles are mainly present in the emulsion phase 600.

Then, the light liquid phase 500 separated in the specific gravity separation step is recovered (first recovery step), the emulsion phase 600 separated in the specific gravity separation step is recovered (second recovery step), and further, the specific gravity separation step is performed. The heavy liquid phase 700 separated in 1 is also recovered (third recovery step). As a result, hydrophilic particles and hydrophobic particles can be separated quickly and efficiently, and the aqueous phase having a high content of hydrophilic particles and the emulsion phase having a high content of hydrophobic particles can be recovered and reused, respectively. can. The vertical multi-stage contact separation system 10A and the vertical multi-stage contact separation method using the vertical multi-stage contact separation system 10A will be described in detail below.

<4. Overall configuration of vertical multi-stage contact separation system>
Next, the overall configuration of the vertical multi-stage contact separation system 10A according to the present embodiment will be described with reference to FIG. The vertical multi-stage contact separation system 10A includes a pre-stirring mixer 1000, a bead mill 2000, and a vertical multi-stage contact separation device 10. The first slurry 300 in which the mixture to be separated is dispersed is produced by the pre-stirring mixer 1000 and the bead mill 2000 (pre-grinding step), and the first slurry 300 is the light liquid phase 500 and the emulsion phase 600 in the vertical multi-stage contact separation device 10. And the heavy liquid phase 700. Then, each phase is discharged from each discharge port. FIG. 3 is an explanatory diagram showing a configuration example of a vertical multi-stage contact separation device 10 preferably used when the light liquid 100 is water and the heavy liquid 200 is a hydrophobic liquid, and FIG. 13 is an explanatory diagram showing a configuration example in which the light liquid 100 is hydrophobic. It is explanatory drawing which shows the structural example of the vertical multi-stage contact separation apparatus 10 which is a sex liquid and is preferably used when the heavy liquid 200 is water.

<5. Configuration of mixer for pre-stirring and bead mill>
Next, the configurations of the pre-stirring mixer 1000 and the bead mill 2000 will be described. The pre-stirring mixer 1000 and the bead mill 2000 are a group of devices for manufacturing the first slurry 300 to be introduced into the vertical multi-stage contact separation device 10.

The pre-stirring mixer 1000 is a stirrer having a container 1010, a pre-stirring stirring blade 1020, and a pre-stirring motor 1050. The pre-stirring mixer 1000 is connected to the bead mill 2000 in the subsequent stage. The mixture 310 to be separated and water are introduced into the container 1010 of the pre-stirring mixer 1000. The pre-stirring mixer 1000 vigorously stirs the mixture 310 to be separated and the mixed solution 1030 of water by rotating the pre-stirring stirring blade 1020 by the pre-stirring motor 1050. As a result, the 0th slurry is produced. The 0th slurry is sent to the bead mill 2000 through a pipe (not shown). A pump (not shown) is connected to the pipe, and the 0th slurry in the pipe is sent to the bead mill 2000 by the pump.

The device for producing the 0th slurry is not limited to the above example, and any device may be used as long as it can vigorously stir the mixture 310 to be separated and water. Examples of other devices include line mixers, pumps capable of stirring the mixture internally, and the like.

Next, the bead mill 2000 will be described. As described above, hydrophilic particles may be mixed in the surface layer portion or the inside of the hydrophobic particles. For example, when the mixture is fly ash, the metal oxide particles in the fly ash are substantially spherical particles containing Al ₂ O ₃ and SiO ₂ as main components. Many metal oxide particles are independently present on the outside of the unburned carbon particles. However, the unburned carbon particles in fly ash are porous, and metal oxide particles may be mixed in the pores on the surface layer or inside of the unburned carbon particles. The proportion of metal oxide particles that have penetrated into the unburned carbon particles may reach the same amount as the mass of the unburned carbon particles.

Separation of hydrophobic particles and hydrophilic particles proceeds to some extent by stirring with the above-mentioned pre-stirring mixer 1000, but when hydrophilic particles are mixed inside many hydrophobic particles, separation of these particles Sex gets worse. The cause of the deterioration of the separability is that the metal oxide particles are mixed in the pores inside the hydrophobic particles, and if there are many such metal oxide particles, the separability is deteriorated. Therefore, even if the 0th slurry is introduced into the vertical multi-stage contact separation device 10 as it is, there is a possibility that the hydrophobic particles and the hydrophilic particles cannot be sufficiently separated. Therefore, in the present embodiment, the solid content (for example, hydrophobic particles containing hydrophilic particles inside) in the 0th slurry is further pulverized by the bead mill 2000. As a result, the first slurry 300 in which the solid content in the 0th slurry is further pulverized is produced. Further, since the hydrophobic particles are further refined by pulverization with the bead mill 2000, the hydrophobic particles can be easily concentrated in the emulsion phase 600.

In the present embodiment, by introducing the 0th slurry into the bead mill 2000, the solid content (for example, hydrophobic particles containing hydrophilic particles inside) in the 0th slurry is wet-ground and pulverized. As a result, the hydrophobic particles are crushed, and the hydrophilic particles mixed in the hydrophobic particles are removed from the hydrophobic particles. As a result, in the first slurry 300, many hydrophilic particles are removed from the hydrophobic particles. However, it is difficult to completely remove the hydrophilic particles from the hydrophobic particles, and the hydrophilic particles often remain in the pores on the surface layer of the hydrophobic particles. Therefore, a part of the surface layer portion of the hydrophobic particles is hydrophilized. Further, the hydrophobic particles are made finer by the bead mill 2000. On the other hand, hydrophilic particles are often harder than hydrophobic particles, and their sizes often do not change even after being pre-milled by the bead mill 2000. The first slurry 300 produced by pulverization by the bead mill 2000 is introduced into the vertical multi-stage contact separation device 10 from the slurry introduction port 10d.

The pre-grinding step does not necessarily have to be performed. However, when the mixture 310 to be separated is fly ash, the porous unburned carbon particles are easily crushed, but the metal oxide particles are spherical and dense and difficult to crush. Further, the unburned carbon particles are porous, and many metal oxide particles may remain in the surface layer portion and the pores inside. Therefore, it is particularly preferable to perform the pre-grinding step using the pre-stirring mixer 1000 and the bead mill 2000. As a result, brittle unburned carbon particles can be efficiently crushed in a short time without destroying the hard metal oxide particles contained in the fly ash. In addition, more metal oxide particles can be separated from the unburned carbon particles.

The larger the diameter of the beads (hereinafter referred to as the bead diameter), the harder the substantially spherical metal oxide particles in order to crush the unburned carbon particles having a smaller particle diameter between the substantially spherical metal oxide particles. Must be crushed, reducing the likelihood of collision between the beads and the smaller unburned carbon particles. On the other hand, the smaller the bead diameter, in other words, the larger the curvature of the bead, the more the bead can come into contact with the unburned carbon particles having a small particle size without colliding with the hard substantially spherical metal oxide particles. Therefore, the bead diameter is preferably 2 mm or less, more preferably 1 mm or less. When the other type of mixture is pre-ground by the bead mill 2000, the bead diameter is preferably 2 mm or less, more preferably 1 mm or less, for the same reason. On the other hand, the lower limit of the bead diameter is preferably larger than the maximum particle size of the powder after pulverization because it is necessary to separate the beads and the powder after pulverization, and it is determined by conducting a test. For example, in the case of fly ash, the particle diameter after pulverization is usually less than 200 μm, so that the diameter of the beads is preferably 200 μm or more.

The crushing method is not limited to the bead mill, and various methods can be applied. For example, a pulverizing medium other than beads (for example, a ball) may be used. Further, either one may be used, such as colliding with a high-speed shear blade of a high-shear homogenizer to pulverize, or irradiating ultrasonic waves with an ultrasonic crusher to pulverize. The hardness of each of the hydrophilic particles and the hydrophobic particles in the mixture, the state of integration of both particles, and the like may be observed, and finally the pulverization method may be tested to select the optimum method. Further, the pre-grinding may be performed by a dry method.

As described above, the pre-grinding step does not necessarily have to be performed. In this case, the mixture 310 to be separated may be directly introduced into the vertical multi-stage contact separation device 10 from the slurry introduction port 10d, or the mixture 310 to be separated may be dispersed in water to form a slurry and then slurryed from the slurry introduction port 10d. It may be introduced in the vertical multi-stage contact separation device 10. However, the hydrophobic particles and the hydrophilic particles contained in the mixture to be separated 310 are often bound to each other in a very complicated form as described above. Therefore, it is preferable to perform a pre-grinding step using the pre-stirring mixer 1000 and the bead mill 2000, and to introduce the first slurry 300 obtained by the pre-grinding step into the vertical multi-stage contact separation device 10.

<6. Configuration of vertical multi-stage contact separation device>
Next, the configuration of the vertical multi-stage contact separation device 10 which is a main component of the vertical multi-stage contact separation system 10A will be described. The vertical multi-stage contact separation device 10 includes a vertical outer wall tube 20, a plurality of settler sections 30, a mixer section 40, a stirring shaft 10a, a heavy liquid introduction port 10c, a slurry introduction port 10d, and a light liquid introduction port 10e. A light liquid discharge port 10f, an emulsion phase discharge port 10g, a heavy liquid discharge port 10h, a first interface observation window 70, and a second interface observation window 80 are provided.

(6-1. Vertical outer wall pipe)
The vertical outer wall pipe 20 is a substantially columnar pipe extending vertically, and the upper and lower end faces are closed. However, a through hole 10a-1 for passing the stirring shaft 10a, which will be described later, is formed in the center of the upper end surface. The material of the vertical outer wall tube 20 is not particularly limited, but does not affect each other with the contents of the vertical outer wall tube 20 (that is, hydrophobic particles, hydrophilic particles, water, hydrophobic liquid, etc.). It is preferably made of a material (not corroded, not melted, etc.), for example, stainless steel.

The inside of the vertical outer wall tube 20 is divided into a plurality of settler portions 30 and a mixer portion 40 in the vertical direction, and the settler portions 30 and the mixer portions 40 are alternately arranged. The uppermost region and the lowermost region are both settler portions 30. Therefore, the settler unit 30 is always arranged above and below the mixer unit 40. In other words, the mixer unit 40 is arranged between the settler units 30. A partition plate 35 for partitioning the mixer section 40 and the settler section 30 is arranged.

In the following description, the uppermost settler portion 30 is referred to as the uppermost settler portion 30a, the lowermost settler portion 30 is referred to as the lowermost settler portion 30b, and the other settler portions 30 are referred to as other settler portions 30d. There is. In the example of FIG. 3, the settler unit 30 is formed in a total of 6 stages and the mixer unit 40 is formed in a total of 5 stages, but it goes without saying that the number of stages of the settler unit 30 and the mixer unit 40 is not limited to this example. Further, the settler unit 30 and the mixer unit 40 are arranged alternately. For example, at least one of the settler unit 30 and the mixer unit 40 is continuously arranged in a plurality of stages at any position of the vertical multi-stage contact separation device 10. It may have been done.

Returning to the example of FIG. 3, the central mixer unit 40 constitutes the coarse separation mixer unit 40a, and the two sets of settler units 30 and the mixer unit 40 above the coarse separation mixer unit 40a constitute the heavy liquid cleaning unit 50. The two sets of settler units 30 and the mixer unit 40 below the coarse separation mixer unit 40a constitute the light liquid cleaning unit 60. The settler portion 30 above the heavy liquid cleaning portion 50 is the uppermost settler portion 30a, and the settler portion 30 below the light liquid cleaning portion 60 is the lowermost settler portion 30b. One or both of the heavy liquid cleaning unit 50 and the light liquid cleaning unit 60 may be omitted.

Here, when the heavy liquid 200 becomes water, the heavy liquid cleaning unit 50 moves the hydrophilic particles 300b (see FIG. 5) in the water (aqueous phase 100a) downward and rises in the light liquid 100. The hydrophilic particles 300b of the above are removed, and the proportion of the hydrophobic particles 300a (see FIG. 5) in the light liquid 100 is increased. When the heavy liquid 200 is a hydrophobic liquid, the hydrophobic particles 300a in the hydrophobic liquid are moved downward, the rising hydrophobic particles 300a in the light liquid 100 are removed, and the ratio of the hydrophilic particles 300b in the light liquid 100 is adjusted. increase. By increasing the number of washing stages, the content of hydrophobic particles 300a in the solid matter in the emulsion phase 600 obtained from the emulsion phase discharge port 10 g is increased. Or / and in the solid matter in the aqueous phase 100a obtained from the aqueous phase discharge port (light liquid discharge port 10f when water is light liquid 100, heavy liquid discharge port 10h when water is heavy liquid 200). Increases the content of the hydrophilic particles 300b in the water.

When the light liquid 100 becomes water, the light liquid cleaning unit 60 moves the hydrophilic particles 300b (see FIG. 5) upward, removes the hydrophilic particles 300b in the descending heavy liquid 200, and removes the hydrophilic particles 200b. Increase the proportion of hydrophobic particles 300a (see FIG. 5) in it. When the light liquid 100 is a hydrophobic liquid, the hydrophobic particles 300a in the hydrophobic liquid are raised, the falling hydrophobic particles 300a in the heavy liquid 200 are removed, and the proportion of the hydrophilic particles 300a in the heavy liquid 200 is increased. .. By increasing the number of washing stages, the content of hydrophobic particles 300a in the solid matter in the emulsion phase 600 obtained from the emulsion phase discharge port 10 g is increased. Or / and in the solid matter in the aqueous phase 100a obtained from the aqueous phase discharge port (light liquid discharge port 10f when water is light liquid 100, heavy liquid discharge port 10h when water is heavy liquid 200). Increases the content of the hydrophilic particles 300b in the water.

(6-2. Stirring shaft)
Inside the vertical outer wall tube 20, a stirring shaft 10a penetrating the settler portion 30, the partition plate 35, and the substantially center of the mixer portion 40 is provided. The upper end of the stirring shaft 10a penetrates to the outside from the upper end surface of the vertical outer wall tube 20. The upper end of the stirring shaft 10a is connected to a driving device (not shown), and is rotated in the direction of arrow A by the driving force of the driving device, for example. Further, of each portion of the stirring shaft 10a in the length direction, a stirring blade 10b is provided at a portion penetrating the mixer portion 40. The stirring blade 10b includes a stirring rod 10b-1 provided substantially perpendicular to the stirring shaft 10a, and stirring blades 10b-2 provided at both ends of the stirring rod 10b-1. When the stirring shaft 10a rotates, the stirring blade 10b rotates in conjunction with the rotation of the stirring shaft 10a. Therefore, in the mixer unit 40, the content 40c is stirred (see FIG. 5). The rotation speed of the stirring shaft 10a (in other words, the rotation speed of the stirring blade 10b) is not particularly limited, and the contents introduced in the vertical multi-stage contact separation device 10 are finally the light liquid phase 500 and the emulsion phase 600. , And it may be appropriately determined so that it can be separated into the heavy liquid phase 700. As an example, the rotation speed of the stirring shaft 10a may be determined so that the peripheral speed of the stirring blade 10b is about 0.8 to 2.8 m / sec. The materials of the stirring shaft 10a and the stirring blade 10b are not particularly limited, but do not affect each other with the contents of the vertical outer wall tube 20 (that is, hydrophobic particles, hydrophilic particles, water, hydrophobic liquid, etc.). It is preferably made of a material (not corroded, not melted, etc.), for example, stainless steel. In the example of FIG. 3 or 13, the stirring shaft 10a is provided from the upper end to the lower end of the vertical multi-stage contact separation device 10, but the stirring shaft 10a may be provided for each mixer unit 40, for example. good. In this case, for example, the rotation speed of the stirring blade 10b may be adjusted for each mixer unit 40.

(6-3. Each inlet)
The vertical multi-stage contact separation device 10 is provided with three introduction ports, that is, a heavy liquid introduction port 10c, a slurry introduction port 10d, and a light liquid introduction port 10e. The material of each inlet is not particularly limited, but does not affect each other with the contents of the vertical outer wall tube 20 (that is, hydrophobic particles, hydrophilic particles, water, hydrophobic liquid, etc.) (corrosion). No, does not dissolve, etc.) Material, for example, preferably made of stainless steel.

The heavy liquid introduction port 10c introduces the heavy liquid 200 into the mixer unit 40 directly below the uppermost settler portion 30a (that is, below and immediately before the uppermost settler portion 30a). Here, when the specific gravity of the hydrophobic liquid is larger than 1, the hydrophobic liquid becomes the heavy liquid 200, so that the hydrophobic liquid is introduced into the vertical multi-stage contact separation device 10 from the heavy liquid introduction port 10c. On the other hand, when the specific gravity of the hydrophobic liquid is less than 1, the water becomes the heavy liquid 200, so that the water is introduced into the vertical multi-stage contact separation device 10 from the heavy liquid introduction port 10c. The heavy liquid 200 introduced into the vertical multi-stage contact separation device 10 gradually moves downward due to its specific gravity.

The slurry introduction port 10d introduces the first slurry 300 into the coarse separation mixer unit 40a installed in the middle of the vertical multi-stage contact separation device 10 in the height direction. Hereinafter, the mixer unit 40 provided with the slurry introduction port 10d may be referred to as a coarse separation mixer unit 40a, and the other mixer units 40 may be distinguished as another mixer unit 40b. Instead of the first slurry 300, the separation target mixture 310 itself, or simply the slurry in which the separation target mixture 310 is dispersed in water may be introduced into the coarse separation mixer unit 40a. However, as described above, it is preferable to introduce the first slurry 300 obtained by the pre-grinding step into the vertical multi-stage contact separation device 10.

The light liquid introduction port 10e introduces the light liquid 100 into the mixer section 40 directly above the lowermost settler section 30b (that is, above and near the lowermost settler section 30b). Here, when the specific gravity of the hydrophobic liquid is less than 1, the hydrophobic liquid becomes the light liquid 100, so that the hydrophobic liquid is introduced into the vertical multi-stage contact separation device 10 from the light liquid introduction port 10e. On the other hand, when the specific gravity of the hydrophobic liquid is larger than 1, the water becomes the light liquid 100, so that the water is introduced into the vertical multi-stage contact separation device 10 from the light liquid introduction port 10e. The light liquid 100 introduced into the vertical multi-stage contact separation device 10 gradually moves upward due to its specific gravity.

Considering the difficulty of ignition, stability, ease of separation, etc. of the hydrophobic liquid, it is preferable to use a hydrophobic liquid having a specific gravity larger than that of water. Therefore, the hydrophobic liquid is introduced into the vertical multi-stage contact separation device 10 as the heavy liquid 200 from the heavy liquid introduction port 10c, and water is introduced into the vertical multi-stage contact separation device 10 from the light liquid introduction port 10e as the light liquid 100. It is preferable to do so.

(6-4. Partition plate)
A partition plate 35 for partitioning the mixer section 40 and the settler section 30 is arranged. Therefore, the configuration of the partition plate 35 will be described with reference to FIG. FIGS. 4A and 4B schematically show the upper end surface of the partition plate 35, but the aperture ratios of the partition plates 35 are different. The details of the aperture ratio will be described later, but the aperture ratio in FIG. 4 (a) is smaller than the aperture ratio in FIG. 4 (b). The partition plate 35 may or may not be fixed to the inner wall surface of the vertical outer wall pipe 20. When the partition plate 35 is not fixed to the inner wall surface of the vertical outer wall pipe 20, the position of the partition plate 35 is fixed by the support column 35c described later. The material of the partition plate 35 is not particularly limited, but does not affect each other with the contents of the vertical outer wall tube 20 (that is, hydrophobic particles, hydrophilic particles, water, hydrophobic liquid, etc.) (corrosion). No, does not dissolve, etc.) Material, for example, preferably made of stainless steel.

A through hole (first through hole, shaft hole) 35a for passing the stirring shaft 10a is formed at substantially the center of the partition plate 35. In order to suppress the contact between the first through hole 35a and the stirring shaft 10a, it is preferable that there is a gap between the peripheral surface of the stirring shaft 10a and the inner wall surface of the first through hole 35a. The contents 30c of the settler unit 30 (see FIG. 6) and the contents 40c in the mixer unit 40 (see FIG. 5) (that is, the contents introduced in the vertical multi-stage contact separation device 10) pass through this gap. Can be distributed to each other. The distance (the length of the gap) between the peripheral surface of the stirring shaft 10a and the inner wall surface of the first through hole 35a is not particularly limited, but considering that the stirring shaft 10a vibrates, it is approximately 5 to 30 mm. Is preferable.

A sleeve extending vertically may be provided on the wall surface of the first through hole 35a, and the stirring shaft 10a may be passed through the sleeve. In this case, the above-mentioned gap becomes unnecessary. With such a sleeve, it is possible to suppress blurring of the stirring shaft 10a during rotation.

Further, the partition plate 35 has a through hole (second through hole, through) for allowing the contents 30c of the settler portion 30 (see FIG. 6) and the contents 40c in the mixer portion 40 (see FIG. 5) to flow to each other. A liquid hole) 35b is also formed. A plurality of second through holes 35b are formed in the partition plate 35. The aperture ratio of the partition plate 35 can be adjusted by adjusting at least one of the hole diameter (diameter) and the number of the second through holes 35b. The hole diameter and aperture ratio of each through hole provided in the partition plate 35 efficiently distribute the contents in the vertical multi-stage contact separation device 10, and thus efficiently lighten the contents in the vertical multi-stage contact separation device 10. It can be said that it is important for separating into the liquid phase 500, the emulsion phase 600, and the heavy liquid phase 700. Suitable values for the hole diameter and aperture ratio of the second through hole 35b are determined by the contents 30c of the settler section 30 (see FIG. 6) and the contents 40c in the mixer section 40 (see FIG. 5), and these have been described. Later, a suitable value will be examined again.

The partition plate 35 may be formed with one or more columns 35c. The support column 35c can further firmly fix the position of the partition plate 35 by connecting the partition plates 35 adjacent to each other on the upper and lower sides. The upper end surface of the uppermost partition plate 35 may be provided with a support column 35c for connecting the upper end surface and the upper end surface of the vertical outer wall pipe 20. The lower end surface of the lowermost partition plate 35 may be provided with a support column 35c for connecting the lower end surface and the bottom portion of the vertical outer wall pipe 20. When the partition plate 35 is not fixed to the inner wall surface of the vertical outer wall pipe 20, the position of the partition plate 35 can be arbitrarily adjusted by adjusting the length of the support column 35c. Further, the support column 35c of the coarse separation mixer unit 40a and the support column 35c of the other mixer unit 40b act as a baffle plate to improve the mixing property in the mixer unit 40.

(6-5. Coarse separation mixer section)
Next, the operation of the coarse separation mixer unit 40a will be described in detail with reference to FIG. FIG. 5 is an explanatory diagram schematically showing the state of the contents 40c of the coarse separation mixer unit 40a and the other mixer unit 40b. The content 40c shown in FIG. 5 is in a state where stirring in the coarse separation mixer section 40a and the other mixer section 40b has progressed to some extent. The contents 40c of the other mixer unit 40b are also in almost the same state as in FIG. Further, in the example of FIG. 5, the water is the light liquid 100 and the hydrophobic liquid is the heavy liquid 200.

A stirring blade 10b is arranged in the coarse separation mixer unit 40a, and the contents 40c of the coarse separation mixer unit 40a are agitated by the rotation of the stirring blade 10b. Further, a partition plate 35 having a first through hole 35a and a second through hole 35b is provided above and below the rough separation mixer portion 40a.

Here, as described above, the first slurry 300 and the like are introduced into the coarse separation mixer unit 40a. Further, each substance is introduced from the upper and lower settler portions 30. A substance having a large specific gravity, for example, emulsion particles 600a, which will be described later, is introduced from the upper settler portion 30 (when the specific gravity of the hydrophobic liquid is larger than that of water). Further, the heavy liquid 200 is also introduced into the coarse separation mixer unit 40a. Here, the heavy liquid 200 is introduced from the heavy liquid introduction port 10c and then lowered in the vertical multi-stage contact separation device 10. The heavy liquid 200 is water or a hydrophobic liquid. When the heavy liquid 200 becomes a hydrophobic liquid, the heavy liquid 200 is introduced into the coarse separation mixer unit 40a as hydrophobic droplets 200a. The heavy liquid 200 is agitated by another mixer unit 40b while descending in the vertical multi-stage contact separation device 10. Further, the liberated hydrophobic particles 300a can also be introduced into the coarse separation mixer unit 40a. When the heavy liquid 200 becomes water, it is introduced into the coarse separation mixer unit 40a as the aqueous phase 100a. The aqueous phase 100a contains hydrophilic particles 300b derived from the first slurry 300.

On the other hand, a substance having a small specific density, for example, a light liquid 100, is introduced from the settler portion below the coarse separation mixer portion 40a. The light liquid 100 is introduced from the light liquid introduction port 10e and then raised in the vertical multi-stage contact separation device 10. The light liquid 100 is water or a hydrophobic liquid. When the light liquid 100 becomes a hydrophobic liquid, the light liquid 100 is introduced into the coarse separation mixer unit 40a as hydrophobic droplets 200a. This is because the light liquid 100 is agitated by another mixer unit 40b while ascending in the vertical multi-stage contact separation device 10. Further, the liberated hydrophobic particles 300a can also be introduced into the coarse separation mixer unit 40a. Further, the emulsion particles 600a may be introduced into the coarse separation mixer unit 40a by a jet flow generated in the settler unit 30 (a jet flow generated from another mixer unit 40b further below the settler unit 30). Such emulsion particles 600a are also agitated, but are eventually returned to the lower settler portion 30 (when the specific gravity of the hydrophobic liquid is larger than that of water).

Therefore, in addition to the first slurry 300, the crude separation mixer unit 40a contains emulsion particles 600a, water (aqueous phase 100a), hydrophobic liquid (hydrophobic droplets 200a), hydrophobic particles 300a, and hydrophilic particles 300b. It will be introduced.

The coarse separation mixer unit 40a stirs these contents 40c. As a result, as shown in FIG. 5, a large number of hydrophobic droplets 200a are dispersed in the aqueous phase 100a. Here, the aqueous phase 100a is derived from water introduced into the vertical multi-stage contact separation device 10 in addition to the first slurry 300. Many hydrophobic particles 300a are attached to the surface layer of the hydrophobic droplet 200a. As described above, the hydrophobic particles 300a in the present embodiment also have hydrophilic properties (more specifically, a part of the surface layer portion of the hydrophobic particles 300a is hydrophilized by the hydrophilic particles 300b or water). .. Therefore, many hydrophobic particles 300a adhere to the surface layer portion of the hydrophobic droplet 200a. In other words, the hydrophobic particles 300a hardly enter the inside of the hydrophobic droplet 200a. As a result, in the coarse separation mixer unit 40a, a large number of emulsion particles 600a to which many hydrophobic particles 300a are attached are formed on the surface layer portion of the fine hydrophobic droplets 200a. Since the surface layer portion of the emulsion particles 600a is covered with the hydrophobic particles 300a, it becomes difficult to unite with each other. Therefore, the emulsion particles 600a can stably exist in the vertical multi-stage contact separation device 10. Further, the specific gravity of the emulsion particles 600a is a value between water and a hydrophobic liquid. As described above, the emulsion particles 600a may be introduced into the coarse separation mixer unit 40a. The coarse separation mixer unit 40a may further refine the formed emulsion particles 600a by a shearing force.

The larger the peripheral speed of the stirring blade 10b, the stronger the shearing force of the stirring blade 10b, and the smaller the particle size of the emulsion particles 600a. If the particle size of the emulsion particles 600a is excessively small, the emulsion particles 600a are difficult to settle, and if the particle size of the emulsion particles 600a is too large, the emulsion particles 600a are provided in the partition plate 35 through the first through holes 35a and the second through holes 35a. It becomes difficult to pass through the hole 35b (when the specific gravity of the hydrophobic liquid is larger than that of water). When the specific gravity of the hydrophobic liquid is smaller than that of water, the specific gravity of the emulsion particles 600a becomes small, and the emulsion particles 600a move (rise) upward. If the particle size of the emulsion particles 600a is excessively small, the emulsion particles 600a are difficult to rise, and if the particle size is too large, the emulsion particles 600a pass through the first through hole 35a and the second through hole 35b provided in the partition plate 35. It becomes difficult to do. Therefore, the particle size of the emulsion particles 600a is preferably about 500 to 2000 μm. In other words, it is preferable to adjust the peripheral speed of the stirring blade 10b installed in each mixer unit 40 so that the particle size of the emulsion particles 600a is within such a range.

If the particle size of the emulsion particles 600a is less than 500 μm, the emulsion particles 600a may be difficult to settle (or rise) in the settler portion 30, and as a result, the aqueous phase 100a and the emulsion phase 600 may be difficult to separate. .. Further, when the particle size of the emulsion particles 600a exceeds 2000 μm, the specific surface area of the hydrophobic droplets 200a becomes small, so that the hydrophobic droplets 200a may have difficulty in capturing the hydrophobic particles 300a.

Considering that the particle sizes of the hydrophobic particles 300a and the hydrophilic particles 300b are approximately 100 μm or less, it can be said that the emulsion particles 600a are particularly large particles. The particle size of each particle in this embodiment is a sphere-equivalent diameter. The method of observing the particle size of the emulsion particles 600a will be described later.

On the other hand, the aqueous phase 100a contains hydrophilic particles 300b. The aqueous phase 100a contains a very small number of free hydrophobic particles 300a. Further, in the aqueous phase 100a, the hydrophobic liquid not covered with the hydrophobic particles 300a is dispersed as the hydrophobic droplets 200a.

Each substance constituting the content 40c moves upward or downward depending on the difference in their specific densities. Since the specific gravity of the emulsion particles 600a is a value between water and the hydrophobic liquid, it moves upward or downward depending on the specific gravity of the hydrophobic liquid. That is, when the specific gravity of the hydrophobic liquid is larger than that of water, the specific gravity of the emulsion particles 600a becomes large and moves downward (descends) in the aqueous phase 100a. On the other hand, when the specific gravity of the hydrophobic liquid is smaller than that of water, the specific gravity of the emulsion particles 600a becomes small and moves upward (increases) in the aqueous phase 100a.
When the specific gravity of the emulsion particles 600a is larger than that of the aqueous phase 100a (that is, when the specific gravity of the hydrophobic liquid is larger than that of water), the emulsion particles 600a are first penetrated by the partition plate 35 below the coarse separation mixer portion 40a. It is introduced into the lower settler portion 30 through the hole 35a and the second through hole 35b. When the specific gravity of the emulsion particles 600a is smaller than that of the aqueous phase 100a (that is, when the specific gravity of the hydrophobic liquid is smaller than that of water), the emulsion particles 600a are provided on the partition plate 35 above the coarse separation mixer unit 40a. It is introduced into the upper settler portion 30 through the first through hole 35a and the second through hole 35b.

On the other hand, when the specific gravity of the hydrophobic liquid is larger than 1, the aqueous phase 100a becomes the light liquid 100 and thus moves upward. Then, the aqueous phase 100a is introduced into the upper settler portion 30 through the first through hole 35a and the second through hole 35b provided in the partition plate 35 above the coarse separation mixer portion 40a. When the specific gravity of the hydrophobic liquid is less than 1, the aqueous phase 100a becomes the heavy liquid 200, and thus moves downward. Then, the aqueous phase 100a is introduced into the lower settler portion 30 through the first through hole 35a and the second through hole 35b provided in the partition plate 35 below the coarse separation mixer portion 40a. The hydrophilic particles 300b move following the aqueous phase 100a.

On the other hand, the hydrophobic droplet 200a (those not covered with the hydrophobic particles 300a) becomes the heavy liquid 200 when the specific gravity of the hydrophobic liquid is larger than 1, and thus moves downward. Then, the hydrophobic droplet 200a is introduced into the lower settler portion 30 through the first through hole 35a and the second through hole 35b provided in the partition plate 35 below the coarse separation mixer portion 40a. When the specific gravity of the hydrophobic liquid is less than 1, the hydrophobic droplet 200a becomes the light liquid 100, and thus moves upward. Then, the hydrophobic droplet 200a is introduced into the upper settler portion 30 through the first through hole 35a and the second through hole 35b provided in the partition plate 35 above the coarse separation mixer portion 40a.

On the other hand, the free hydrophobic particles 300a in the coarse separation mixer section 40a are introduced into the upper or lower settler section 30.

As described above, the coarse separation mixer unit 40a is roughly divided into the contents 40c with the emulsion particles 600a, the aqueous phase 100a (and the hydrophilic particles 300b mixed in the aqueous phase 100a), and the hydrophobic droplets 200a (hydrophobic particles 300a). (Uncovered) and free hydrophobic particles 300a are separated and each is moved to the upper and lower settler portions 30.

(6-6. Other mixer section)
The operation of the other mixer unit 40b is almost the same as that of the coarse separation mixer unit 40a. Hereinafter, the operation of the other mixer unit 40b will be described with reference to FIG. A stirring blade 10b is arranged in the other mixer unit 40b, and the coarse separation mixer unit 40a and the contents 40c are stirred by the rotation of the stirring blade 10b.

Each substance is introduced into the other mixer section 40b from the upper and lower settler sections 30. These substances are as described in the item of the coarse separation mixer unit 40a. Therefore, the emulsion particles 600a, water, the hydrophobic liquid (hydrophobic droplets 200a), the hydrophobic particles 300a, and the hydrophilic particles 300b are introduced into the other mixer unit 40b.

The light liquid 100 is further introduced from the light liquid introduction port 10e into another mixer unit 40b directly connected to the light liquid introduction port 10e. Further, the heavy liquid 200 is further introduced into the other mixer unit 40b directly connected to the heavy liquid introduction port 10c from the heavy liquid introduction port 10c.

In any case, as described above, the contents 40c of the other mixer unit 40b include emulsion particles 600a, water, a hydrophobic liquid (hydrophobic droplet 200a), hydrophobic particles 300a, and hydrophilic particles 300b. Will be included.

The other mixer unit 40b stirs these contents 40c. As a result, as shown in FIG. 5, a large number of hydrophobic droplets 200a are dispersed in the aqueous phase 100a. Here, the aqueous phase 100a is derived from water introduced into the vertical multi-stage contact separation device 10 in addition to the first slurry 300. Many hydrophobic particles 300a are attached to the surface layer of the hydrophobic droplet 200a. As a result, the emulsion particles 600a are formed. As described above, the emulsion particles 600a may be introduced into the other mixer unit 40b. The other mixer unit 40b may further refine the formed emulsion particles 600a by a shearing force. When the specific gravity of the emulsion particles 600a is larger than that of the aqueous phase 100a and the emulsion particles settle downward, the lower mixer unit 40 contains more emulsion particles 600a than the upper mixer unit 40 (that is, the concentration of the emulsion particles 600a is high). It can be said that. On the contrary, when the specific gravity of the emulsion particles 600a is smaller than that of the aqueous phase 100a and rises upward, the upper mixer unit 40 contains more emulsion particles 600a than the lower mixer unit 40 (that is, the concentration of the emulsion particles 600a is high). ).

On the other hand, the aqueous phase 100a contains hydrophilic particles 300b. The aqueous phase 100a contains a very small number of free hydrophobic particles 300a. Further, in the aqueous phase 100a, the hydrophobic liquid not covered with the hydrophobic particles 300a is dispersed as the hydrophobic droplets 200a.

Each substance constituting the content 40c moves upward or downward depending on the difference in their specific densities. The details are as described in the item of the coarse separation mixer unit 40a.

As described above, in the other mixer unit 40b, the contents 40c are roughly divided into emulsion particles 600a, aqueous phase 100a (and hydrophilic particles 300b mixed in the aqueous phase 100a), and hydrophobic droplets 200a (hydrophobic particles 300a). (Uncovered) and free hydrophobic particles 300a are separated and each is moved to the upper and lower settler portions 30.

(6-7. Settler section)
Next, the operation (function) of the settler unit 30 will be described in detail with reference to FIG. FIG. 6 is an explanatory diagram showing the contents 30c of the settler portion 30d other than the uppermost settler portion 30a and the lowermost settler portion 30b. Further, in the example of FIG. 6, the water is the light liquid 100 and the hydrophobic liquid is the heavy liquid 200.

A partition plate 35 having a first through hole 35a and a second through hole 35b is provided above and below the other settler portion 30d. Therefore, each substance is introduced into the other settler section 30d from the upper and lower mixer sections 40. As described above, from the upper mixer section 40, a substance having a large specific gravity, for example, emulsion particles 600a (when the specific gravity of the hydrophobic liquid is larger than water) is introduced into the other settler section 30d.

On the other hand, since the aqueous phase 100a becomes the light liquid 100 when the specific gravity of the hydrophobic liquid is larger than 1, it is introduced from the lower mixer section 40 into the other settler section 30d. Since the aqueous phase 100a becomes a heavy liquid 200 when the specific gravity of the hydrophobic liquid is less than 1, it is introduced from the upper mixer section 40 into another settler section 30d. The hydrophilic particles 300b move following the aqueous phase 100a.

On the other hand, the hydrophobic droplet 200a (those not covered with the hydrophobic particles 300a) becomes a heavy liquid 200 when the specific gravity of the hydrophobic liquid is larger than 1, so that the mixer section 40 above to another settler section. Introduced within 30d. Since the hydrophobic liquid droplet 200a becomes a light liquid 100 when the specific gravity of the hydrophobic liquid is less than 1, it is introduced into another settler unit 30d from the lower mixer unit 40.

On the other hand, the free hydrophobic particles 300a in the upper or lower mixer section 40 are introduced into the other settler section 30d from the upper or lower mixer section 40.

The other settler portion 30d separates the contents 30c by specific gravity by allowing them to stand still. For example, the emulsion particles 600a having a large specific density (when the specific gravity of the hydrophobic liquid is larger than that of water) settle on the lower partition plate 35 and concentrate at this position. After that, the settled emulsion particles 600a are introduced into the lower mixer section 40 through the first through hole 35a and the second through hole 35b provided in the partition plate 35. When the specific gravity of the emulsion particles 600a is small, the emulsion particles 600a are introduced from the lower mixer section 40 into the other settler section 30d and concentrated in the vicinity of the upper partition plate 35. After that, it is introduced into the upper mixer section 40 through the first through hole 35a and the second through hole 35b provided in the upper partition plate 35.

Since the aqueous phase 100a (and the hydrophilic particles 300b following it) becomes the light liquid 100 when the specific gravity of the hydrophobic liquid is larger than 1, it moves upward (floats) in the other settler portion 30d (Fig.). Example of 6). After that, the aqueous phase 100a is introduced into the mixer section 40 above from the first through hole 35a and the second through hole 35b provided in the upper partition plate 35. On the other hand, when the specific gravity of the hydrophobic liquid is less than 1, the aqueous phase 100a becomes a heavy liquid 200, and therefore settles downward in the other settler portion 30d. After that, the aqueous phase 100a is introduced into the mixer section 40 below from the first through hole 35a and the second through hole 35b provided in the lower partition plate 35.

The hydrophobic droplets 200a (those not covered with the hydrophobic particles 300a) become the heavy liquid 200 when the specific gravity of the hydrophobic liquid is larger than 1, and thus settle downward. Then, the hydrophobic droplet 200a is introduced into the lower mixer section 40 through the first through hole 35a and the second through hole 35b provided in the partition plate 35 below the other settler section 30d. When the specific gravity of the hydrophobic liquid is less than 1, the hydrophobic droplet 200a becomes the light liquid 100, and therefore moves upward (floats). Then, the hydrophobic droplet 200a is introduced into the upper mixer section 40 through the first through hole 35a and the second through hole 35b provided in the partition plate 35 above the other settler section 30d.

The liberated hydrophobic particles 300a are introduced into the mixer section 40 above or below the other settler section 30d due to its specific gravity.

FIG. 7 schematically shows the movement of the emulsion particles 600a and the aqueous phase 100a between the coarse separation mixer section 40a and the settler sections 30 (other settler sections 30d) above and below the coarse separation mixer section 40a. In this example, the aqueous phase 100a is the light liquid 100. Therefore, the specific gravity of the emulsion particles 600a is larger than that of the aqueous phase 100a. In this example, many emulsion particles 600a settle in the lower settler portion 30, but some of the emulsion particles 600a move to the upper settler portion 30 by the jet flow of the coarse separation mixer portion 40a. However, the emulsion particles 600a are separated by specific gravity in the upper settler portion 30 and returned to the coarse separation mixer portion 40a.

Similarly, many aqueous phases 100a float in the upper settler section 30, but some aqueous phases 100a settle in the lower settler section 30 due to the stirring flow by the coarse separation mixer section 40a. However, the aqueous phase 100a is separated by specific gravity in the lower settler section 30 and returns to the coarse separation mixer section 40a.

The function of the uppermost settler portion 30a is almost the same as that of the other settler portion 30d, but the substance moved upward is different from the function of the other settler portion 30d in that the substance stays in the uppermost settler portion 30a. The liquid level of the light liquid phase 500 may be formed on the uppermost settler portion 30a. In the example of FIG. 3, the liquid surface 500b of the light liquid phase 500 is formed in the uppermost settler portion 30a.

The heavy liquid 200 is settled at the bottom of the lowermost settler portion 30b (the bottom of the vertical outer wall tube 20), and the heavy liquid phase 700 is formed. Then, the emulsion phase 600 is formed above the emulsion phase 600. Therefore, the interface 110c of the emulsion phase 600 / heavy liquid phase 700 (in this embodiment, the upper and lower phases of the interface are connected by / is represented) is formed in the lowermost settler portion 30b. ..

(6-8. Each phase formed in the vertical multi-stage contact separation device)
When each settler unit 30 and the mixer unit 40 repeat the above-mentioned processing, the heavy liquid 200 gradually settles in the vertical multi-stage contact separation device 10 to form the heavy liquid phase 700. The light liquid 100 gradually rises in the vertical multi-stage contact separation device 10 to form the light liquid phase 500. On the other hand, the emulsion particles 600a form an emulsion phase 600 between the light liquid phase 500 and the heavy liquid phase 700 regardless of its specific gravity. As a result, as shown in FIG. 3 or FIG. 13, the contents in the vertical multi-stage contact separation device 10 are separated by specific gravity into the light liquid phase 500, the emulsion phase 600, and the heavy liquid phase 700 from above. However, the concentration distribution of the emulsion particles 600a is formed in the emulsion phase 600 due to the specific gravity of the emulsion particles 600a. When the specific gravity of the emulsion particles 600a is larger than that of the aqueous phase 100a (that is, when the specific gravity of the hydrophobic liquid is larger than that of water), the concentration of the emulsion particles 600a in the lower emulsion phase 600 is the concentration of the emulsion particles 600a in the upper emulsion phase 600. Greater than the concentration. On the other hand, when the specific gravity of the emulsion particles 600a is smaller than that of the aqueous phase 100a (that is, when the specific gravity of the hydrophobic liquid is smaller than that of water), the concentration of the emulsion particles 600a in the upper emulsion phase 600 is the emulsion particles in the lower emulsion phase 600. Greater than the concentration of 600a.

Here, the light liquid phase 500 is a phase in which the light liquid 100 is concentrated, and the heavy liquid phase 700 is a phase in which the heavy liquid 200 is concentrated. When the light liquid phase 500 or the heavy liquid phase 700 becomes the aqueous phase 100a, many hydrophilic particles 300b are contained in the aqueous phase 100a. The aqueous phase 100a may contain a very small amount of hydrophobic particles 300a. Therefore, the aqueous phase 100a contains more hydrophilic particles 300b than the hydrophobic particles 300a. That is, the solid matter obtained by recovering and drying the aqueous phase 100a contains many hydrophilic particles 300b. When the mixture 310 to be separated becomes fly ash, the solid matter becomes so-called refined fly ash. The carbon (that is, hydrophobic particle) content _CA in the purified fly ash is an index for evaluating the quality of the purified fly ash and, by extension, the separation performance of the vertical multi-stage contact separation device 10. The carbon content _CA in the refined fly ash is the mass% of carbon with respect to the total mass of the refined fly ash. The carbon content in this embodiment (and each of the examples described later) is measured as the ignition loss rate as described above. The ignition loss rate is the mass loss rate when a sample dried at 105 ° C. is held in an atmospheric atmosphere oven set at 975 ° C. for 15 minutes or more.

It can be said that the smaller the carbon content _CA in the refined fly ash, the higher the quality of the refined fly ash. When the light liquid phase 500 or the heavy liquid phase 700 is a hydrophobic liquid phase, the hydrophobic liquid phase contains almost no hydrophobic particles 300a and hydrophilic particles 300b. Since the hydrophobic liquid exists as hydrophobic droplets 200a in the vertical multi-stage contact separation device 10, it is covered with the hydrophobic particles 300a in the process of moving in the vertical multi-stage contact separation device 10 and becomes the emulsion particles 600a. Often becomes. However, there are also hydrophobic droplets 200a that reach the end of the vertical multi-stage contact separation device 10 without being covered with the hydrophobic particles 300a, and the hydrophobic droplets 200a coalesce with each other to form a light liquid phase. It becomes 500 or a heavy liquid phase 700.

The emulsion phase 600 is a phase in which the emulsion particles 600a are concentrated, and contains a large amount of the emulsion particles 600a. The emulsion particles 600a may contain at least one of the aqueous phase 100a (and the hydrophilic particles 300b following the aqueous phase 100a), the hydrophobic liquid, and the liberated hydrophobic particles 300a. Therefore, the solid matter obtained by recovering and drying the emulsion particles 600a contains a large amount of hydrophobic particles 300a. When the mixture 310 to be separated becomes fly ash, the carbon content CC in the solid matter (carbon concentrate) is an index for evaluating the quality of the unburned _carbon concentrate and the separation performance of the vertical multi-stage contact separation device 10. Will be. The carbon content _CC in the unburned carbon concentrate is the mass% of carbon with respect to the total mass of the unburned carbon concentrate. It can be said that the higher the _carbon content CC in the unburned carbon concentrate, the higher the quality of the unburned carbon concentrate.

(6-9. Regarding the hole diameter and aperture ratio of the partition plate)
As described above, the first through hole 35a and the second through hole 35b provided in the partition plate 35 are through holes necessary for passing each substance (particularly emulsion particles 600a, aqueous phase 100a, etc.). Therefore, in order to allow these substances to pass efficiently, the pore diameter and aperture ratio of these through holes are important. The preferable range of the distance (the length of the gap) between the peripheral surface of the stirring shaft 10a and the inner wall surface of the first through hole 35a is about 5 to 30 mm. Therefore, the hole diameter of the second through hole 35b and the opening ratio of the entire through hole will be examined again.

Of the water, hydrophobic liquid, hydrophobic particles 300a, hydrophilic particles 300b, and emulsion particles 600a, the emulsion particle 600a has the largest particle size, and the particle size is approximately 500 to 2000 μm as described above. .. As shown in FIG. 6, since a large number of emulsion particles 600a are concentrated on the lower partition plate 35 (when the specific gravity of the hydrophobic liquid is larger than that of water), one second through hole 35b is formed by the plurality of emulsion particles. 600a may pass at the same time. When the specific gravity of the emulsion particles 600a is smaller than that of the aqueous phase 100a, the emulsion particles 600a are concentrated in the vicinity of the upper partition plate 35, and one second through hole 35b in the upper partition plate 35 is formed in the plurality of emulsion particles 600a. May pass at the same time. Considering these facts, the pore diameter of the second through hole 35b is preferably about several times the particle size of the emulsion particles 600a, and is preferably 8 mm or more, for example. More preferably, it is 12 mm or more. On the other hand, if the hole diameter of the second through hole 35b becomes too large, the stirring flow generated in the mixer section 40 becomes an excessive jet and enters the settler section 30, and the emulsion particles 600a settle and partition in the settler section 30. Concentration on the plate 35 is less likely to occur (when the specific gravity of the hydrophobic liquid is greater than that of water). When the specific gravity of the emulsion particles 600a is smaller than that of the aqueous phase 100a, it becomes difficult for the emulsion particles 600a to concentrate in the vicinity of the upper partition plate 35. Therefore, it becomes difficult to separate the emulsion phase 600 and the light liquid phase 500. Therefore, the hole diameter of the second through hole 35b is preferably 50 mm or less, more preferably 30 mm or less. Therefore, the hole diameter of the second through hole 35b is preferably, for example, 8 to 50 mm.

Next, the aperture ratio of the partition plate 35 will be examined. In this embodiment, the aperture ratio of the partition plate 35 is defined as follows. That is, the denominator of the aperture ratio is the area of the area where the emulsion particles 600a may be concentrated (the area in the plan view), and the numerator of the aperture ratio is the area in the plan view of the entire through hole. Specifically, the area obtained by subtracting the column cross-sectional area and the stirring shaft cross-sectional area from the area (1 / 4πd ² ) of the partition plate 35 obtained from the plan-view diameter (d) of the partition plate 35 is used as the denominator and the first penetration. The opening area obtained by subtracting the cross-sectional area of the stirring shaft 10a from the cross-sectional area of the hole 35a and the opening area of the second through hole 35b was defined as the molecule, and the ratio of the molecule to the denominator (100%) was defined as the opening ratio. .. As shown in Examples described later, the preferred range of aperture ratio is 10 to 50 (area%). The aperture ratio is more preferably 20 to 40 area%. When the aperture ratio is within the above range, the quality of refined fly ash and unburned carbon concentrate is improved, for example. More specifically, the carbon content CA in the refined fly ash is small, the carbon content _{C C in} the unburned carbon concentrate is large, and these ratios (carbon content ratio) _CC / _CA The value is 20 or more. (See FIGS. 11 and 12). By setting the opening ratio to 20 to 40 area%, the carbon content _CA in the refined fly ash can be set to 2.0% by mass or less.

When the aperture ratio is less than 10%, the flow of each liquid or particle group (for example, emulsion particles 600a, liberated hydrophobic particles 300a, hydrophilic particles 300b, etc.) through the partition plate 35 cannot be stably performed. There is a possibility that the particle group is excessively deposited on the upper part of the partition plate 35 and the particle group is accumulated until it comes into contact with the upper mixer part 40, and the separation in the settler part 30 cannot be continued. .. On the other hand, when the aperture ratio exceeds 50%, the flow due to stirring in the mixer section 40 greatly affects the settler section 30, and the emulsion particles 600a are less likely to settle in the settler section 30 (the specific gravity of the hydrophobic liquid is high). If larger than water). For example, there is a possibility that the agitated flow generated in the mixer unit 40 becomes an excessive jet and is ejected from the first through hole 35a and the second through hole 35b, making it difficult for the emulsion particles 600a to concentrate on the lower partition plate 35. There is. When the specific gravity of the emulsion particles 600a is smaller than that of the aqueous phase 100a, it becomes difficult for the emulsion particles 600a to concentrate in the vicinity of the upper partition plate 35. When the aperture ratio is 10 to 50 area%, an appropriate jet is introduced into the settler portion 30 from the first through hole 35a and the second through hole 35b, so that the emulsion particles are placed on the upper or lower partition plate 35. While concentrating, clogging of the first through hole 35a and the second through hole 35b can be suppressed. Further, the emulsion particles 600a can be moved from the first through hole 35a and the second through hole 35b to the mixer portion 40 below. As a result, as described above, the carbon content CA in the refined fly ash is small, the carbon content C _C in the unburned carbon concentrate is large, and the carbon content ratio _{C C / CA} is 20. That is all.

The hole diameter of the first through hole 35a, the hole diameter, the number, and the aperture ratio of the second through hole 35b may be common to all the partition plates 35, or may be different for each partition plate 35. However, it is preferable that all the partition plates 35 satisfy the above-mentioned requirements. In order to set the carbon content ratio C _C / C _A to 20 or more, it is particularly preferable that the opening ratios of all the partition plates 35 are 10 to 50 area%.

(6-10. Interface position and observation method)
In the present embodiment, as shown in FIG. 3, the interface 110c of the emulsion phase 600 / heavy liquid phase 700 is formed in the lowermost settler portion 30b. A second interface observation window 80 is provided in the lowermost settler portion 30b.

On the other hand, an emulsion is placed in a settler section 30 directly under the coarse separation mixer section 40a (hereinafter, such a settler section 30 is also referred to as an observation settler section 30e. The observation settler section 30e is a kind of another settler section 30d). The interface 110b of the phase 600 / light liquid phase 500 is formed. The observation settler unit 30e is provided with a first interface observation window 70. The first interface observation window 70 is an observation window for observing the interface of the emulsion phase 600 / aqueous phase 100a, and the second interface observation window 80 is for observing the interface of the emulsion phase 600 / hydrophobic liquid phase. It is an observation window. Therefore, in the example shown in FIG. 3, the light liquid phase 500 is the aqueous phase 100a, and the heavy liquid phase 700 is the hydrophobic liquid phase. Therefore, first, an observation method will be described in which the light liquid phase 500 becomes the aqueous phase 100a and the heavy liquid phase 700 becomes the hydrophobic liquid phase.

The operator can observe the interface 110b of the emulsion phase 600 / light liquid phase 500 (that is, the emulsion phase 600 / aqueous phase 100a) through the first interface observation window 70, and can observe the interface 110b through the second interface observation window 80. The interface 110c of the emulsion phase 600 / heavy liquid phase 700 (that is, the emulsion phase 600 / hydrophobic liquid phase) can be observed. Of course, the position of each interface is not limited to the example shown in FIG. However, when the light liquid phase 500 becomes the aqueous phase 100a, the interface 110b can be easily recognized by forming the interface 110b at this position (that is, the position of the observation settler portion 30e directly under the coarse separation mixer portion 40a). There is a merit of becoming.

For example, when the mixture 310 to be separated becomes fly ash, the hydrophilic particles 300b become gray metal oxide particles, and the hydrophobic particles 300a become black unburned carbon particles. Therefore, the emulsion phase 600 is black and the light liquid phase 500 (ie, the aqueous phase 100a) is gray. Therefore, the operator can observe the interface 110b of the emulsion phase 600 / light liquid phase 500 (that is, the emulsion phase 600 / aqueous phase 100a) through the first interface observation window 70. Since the heavy liquid phase 700 (that is, the hydrophobic liquid phase) becomes transparent, the operator can use the emulsion phase 600 / heavy liquid phase 700 (that is, the emulsion phase 600 / hydrophobic liquid phase) through the second interface observation window 80. ) Interface 110c can be observed.

However, a large amount of the aqueous phase 100a and the metal oxide particles following the aqueous phase 100a are flowing above the coarse separation mixer unit 40a. Therefore, when the first interface observation window 70 is arranged above the coarse separation mixer unit 40a and the interface 110b of the emulsion phase 600 / light liquid phase 500 is maintained at this position, the black color of the emulsion phase 600 becomes a metal oxide. The gray color of the particles makes it difficult to recognize the interface 110b between the light liquid phase 500 (that is, the aqueous phase 100a) and the emulsion phase 600.

On the other hand, below the coarse separation mixer unit 40a, the amount of the aqueous phase 100a and the metal oxide particles following the aqueous phase 100a is significantly reduced. Therefore, when the interface 110b of the emulsion phase 600 / light liquid phase 500 (that is, the emulsion phase 600 / aqueous phase 100a) is arranged in the observation settler portion 30e directly under the coarse separation mixer portion 40a as in the example of FIG. 3, the emulsion The black color of the phase 600 is the gray color of the metal oxide particles, which makes it difficult to fade. Therefore, the operator can easily recognize the interface between the light liquid phase 500 (that is, the aqueous phase 100a) and the emulsion phase 600.

In the example of FIG. 3, the settler section 30 (the settler section 30 directly below the coarse separation mixer section 40a) in the fourth stage from the top is used as the settler section 30e for observation, and the emulsion phase 600 / light liquid phase 500 is located at this position. Although it was decided to maintain the interface 110b, the interface 110b may be maintained at the settler portion 30 further below.

Further, as shown in FIG. 8, on the upper part of the interface 110b of the emulsion phase 600 / light liquid phase 500 (that is, the emulsion phase 600 / aqueous phase 100a) (that is, the upper part of the first interface observation window 70 in the vertical outer wall tube 20). In), an umbrella 75 that suppresses the emulsion particles 600a falling from the upper part of the interface 110b may be provided. With such an umbrella 75, the emulsion particles 600a on the upper part of the interface 110b can be obstructed from flowing, and can be dropped to a position away from the first interface observation window 70. That is, in the example of FIG. 3, since the specific gravity of the emulsion particles 600a is larger than that of the aqueous phase 100a, the emulsion particles 600a settle (fall) downward in the multi-stage contact separation device 10. When such emulsion particles 600a fall in the vicinity of the first interface observation window 70, the interface 110b observed by the operator may be disturbed. However, by providing such an umbrella 75, it is possible to suppress the disturbance of the interface 110b observed by the operator. The material of the umbrella 75 is not particularly limited, but does not affect each other (that is, does not corrode) with the contents of the vertical outer wall tube 20 (that is, hydrophobic particles, hydrophilic particles, water, hydrophobic liquid, etc.). , Not melted, etc.) Material, for example, preferably made of stainless steel.

At the interface 110c of the emulsion phase 600 / heavy liquid phase 700 (that is, the emulsion phase 600 / hydrophobic liquid phase), the heavy liquid phase 700 is the hydrophobic liquid phase, so that an umbrella is not always necessary. This is because there is almost no movement of the emulsion particles 600a between these phases.

Next, a case where the light liquid phase 500 becomes the hydrophobic liquid phase and the heavy liquid phase 700 becomes the aqueous phase 100a will be described. In this case, the positions of the first interface observation window 70 and the second interface observation window 80 may be simply exchanged, but it is preferable to use the vertical multi-stage contact separation device 10'shown in FIG. Note that FIG. 13 shows only the configuration of the vertical multi-stage contact separation device 10'of the vertical multi-stage contact separation system 10A. The pre-stirring mixer 1000 and the bead mill 2000 shown in FIG. 3 are also connected to the vertical multi-stage contact separation device 10'.

The vertical multi-stage contact separation device 10'has almost the same configuration as the vertical multi-stage contact separation device 10 shown in FIG. 3, but has a first interface observation window 70, a second interface observation window 80, an emulsion phase discharge port 10 g, and the like. And the arrangement of the umbrella 75 is different. Further, the interface 110b of the emulsion phase 600 / light liquid phase 500 (that is, the emulsion phase 600 / hydrophobic liquid phase) is formed in the uppermost settler portion 30a, and the emulsion phase 600 / heavy liquid phase 700 (that is, the emulsion phase 600 / water) is formed. The interface 110c of the phase 100a) is formed in the settler portion 30 directly above the coarse separation mixer portion 40a.

Therefore, the observation window for observing the first interface observation window 70, that is, the interface 110c of the emulsion phase 600 / heavy liquid phase 700 (more specifically, the emulsion phase 600 / aqueous phase 100a) is directly above the coarse separation mixer unit 40a. (Therefore, this settler portion 30 becomes the observation settler portion 30e). A second interface observation window 80, that is, an observation window for observing the interface 110b of the emulsion phase 600 / light liquid phase 500 (more specifically, the emulsion phase 600 / hydrophobic liquid phase) is provided in the uppermost settler portion 30a. Be done.

The method of observing the interfaces 110b and 110c using each observation window is the same as the method described with reference to FIG. By arranging each observation window as described above, the amount of the aqueous phase 100a (here, the heavy liquid phase 700) and the metal oxide particles following the aqueous phase 100a is significantly reduced above the coarse separation mixer unit 40a. Therefore, when the interface between the emulsion phase 600 and the aqueous phase 100a (that is, the interface 110c) is arranged above the coarse separation mixer unit 40a, the black color of the emulsion phase 600 is less likely to fade due to the gray color of the metal oxide particles. Therefore, the operator can easily recognize the interface between the emulsion phase 600 and the aqueous phase 100a. It should be noted that the position of each interface is not limited to the example of FIG. 13, which is the same as the example of FIG. The arrangement of each observation window may be adjusted according to the position of the interface.

As shown in FIG. 13, the umbrella 75 is arranged below the interface 110c in the observation settler portion 30e. That is, in the example of FIG. 3, since the specific gravity of the emulsion particles 600a is smaller than that of the aqueous phase 100a, the emulsion particles 600a rise (float) in the multi-stage contact separation device 10. Such an umbrella 75 can prevent the emulsion particles 600a floating from below the interface 110c from flowing, and can be floated at a position away from the first interface observation window 70. That is, when such emulsion particles 600a float in the vicinity of the first interface observation window 70, the interface 110c observed by the operator may be disturbed. However, by providing such an umbrella 75, it is possible to suppress the disturbance of the interface 110c observed by the operator.

The emulsion phase discharge port 10g is installed slightly closer to the emulsion phase 600 than, for example, the interface 110b between the light liquid phase 500 and the emulsion phase 600. The emulsion phase 600 is discharged from the emulsion phase discharge port 10 g. In the example of FIG. 13, the specific gravity of the emulsion particles 600a is smaller than that of the aqueous phase 100a (that is, the specific gravity of the hydrophobic liquid is smaller than that of water). Therefore, the concentration of the emulsion particles 600a in the upper emulsion phase 600 is higher than the concentration of the emulsion particles 600a in the lower emulsion phase 600. Therefore, by providing the emulsion phase discharge port 10 g at this position, the emulsion phase 600 can be efficiently recovered. The details of the emulsion phase discharge port 10 g will be described later.

The materials of the first interface observation window 70 and the second interface observation window 80 are also very important for the operator to clearly observe each of the interfaces 110b and 110c. Hereinafter, the case where the separation target mixture 310 becomes fly ash will be described as an example, but even when the separation target mixture 310 becomes the above-mentioned other substances, the first interface observation window 70 and the second interface observation window 80 are appropriate. The material is the same.

First, since the first interface observation window 70 is an observation window for observing the interface of the emulsion phase 600 / aqueous phase 100a, it is preferably made of glass. As a result, the operator can recognize the emulsion phase 600 as black and the aqueous phase 100a as gray through the first interface observation window 70. That is, the interface between the emulsion phase 600 and the aqueous phase 100a can be recognized. Further, the imaging device can image the interface between the emulsion phase 600 / aqueous phase 100a. That is, the image pickup apparatus can image the emulsion phase 600 in black and the aqueous phase 100a in gray.

When the first interface observation window 70 is made of another material, for example, an arbitrary organic resin, the emulsion phase 600 spreads toward the aqueous phase 100a due to the influence of the meniscus, and the interface 110b between the aqueous phase 100a and the emulsion phase 600, There is a possibility that 110c will be difficult to distinguish.

Next, since the second interface observation window 80 is an observation window for observing the interface of the emulsion phase 600 / hydrophobic liquid phase, it does not have a hydrophilic functional group on the surface, that is, it is compatible with the hydrophobic liquid. It is preferable to use a transparent plate having a high thickness. Here, the transparent plate having no hydrophilic functional group on its surface is, for example, a plastic plate whose surface itself is made of a resin having no hydrophilic functional group, as well as at least an emulsion phase 600 and a hydrophobic liquid phase. Examples thereof include a transparent plate (for example, a transparent plate made of glass) whose contact surface is covered with a transparent paint having no hydrophilic functional group.

Here, examples of the hydrophilic functional group include a hydroxyl group (OH), an amino group (NH ₂ ), a carboxyl group (COOH), and a sulfonic acid group (SO ₃ H). Whether or not the surface of the transparent plate has a hydrophilic functional group can be determined by whether or not the signal of the corresponding functional group is detected by the measurement by surface contact type infrared spectroscopy.

Materials for plastic plates include polyethylene terephthalate (PET), polyethylene (PE), polypropylene (PP), vinyl chloride, acrylic, polystyrene, ABS resin, nylon resin, polycarbonate, Teflon (registered trademark), biethylene acid copolymer, and phenol. Examples thereof include resin, melamine, unsaturated polyester and epoxy. Specific examples of the transparent paint include acrylic synthetic resin paint, polyurethane synthetic resin paint, acrylic silicon synthetic resin paint, fluorine synthetic resin paint and the like. Since some materials cannot be used depending on the type of hydrophobic liquid, it is preferable to select a material suitable for the hydrophobic liquid to be used.

For example, when the mixture 310 to be separated becomes fly ash, the second interface observation window 80 may be a polypropylene plate or a glass plate coated with polypropylene resin.

As a result, the operator can recognize the emulsion phase 600 as black and the hydrophobic liquid phase as transparent through the second interface observation window 80. That is, the interface of the emulsion phase 600 / hydrophobic liquid phase can be recognized. Further, the imaging device can image the interface of the emulsion phase 600 / hydrophobic liquid phase. That is, the imaging device can image the emulsion phase 600 in black and the hydrophobic liquid phase transparently.

When the second interface observation window 80 is made of another material, for example, a glass plate, the emulsion phase 600 spreads toward the hydrophobic liquid phase due to the influence of the meniscus, and the interface 110b between the hydrophobic liquid phase and the emulsion phase 600, There is a possibility that 110c will be difficult to distinguish.

As described above, either one of the light liquid phase 500 and the heavy liquid phase 700 becomes the aqueous phase 100a, and the other becomes the hydrophobic liquid phase. Therefore, for example, when the light liquid phase 500 becomes the aqueous phase 100a and the heavy liquid phase 700 becomes the hydrophobic liquid phase, it is preferable to observe each interface using the vertical multi-stage contact separation device 10 shown in FIG. On the contrary, when the light liquid phase 500 becomes the hydrophobic liquid phase and the heavy liquid phase 700 becomes the aqueous phase 100a, it is preferable to observe each interface using the vertical multi-stage contact separation device 10'shown in FIG.

The lengths of the first interface observation window 70 and the second interface observation window 80 in the vertical direction are not particularly limited, but are two to three times the length considering the fluctuation of the interfaces 110b and 110c (for example, the displacement amount of the interfaces 110b and 110c). Degree) is preferable.

(6-11. Method for measuring the particle size of emulsion particles)
The particle size (sphere equivalent diameter, pseudo particle size) of the emulsion particles 600a can be measured using an captured image. Specifically, the vertical multi-stage contact separation device 10 (or vertical type) uses the total volume of water in the first slurry 300 used in the actual operation and the water to be used as the light liquid 100 or the heavy liquid 200. It is introduced in the multi-stage contact separation device 10'). Further, the hydrophobic liquid to be used as the light liquid 100 or the heavy liquid 200 is introduced into the vertical multi-stage contact separation device 10 (or the vertical multi-stage contact separation device 10'). Then, the stirring shaft 10a is rotated at the same peripheral speed as in the actual operation. Then, the inside is imaged from the first interface observation window 70, that is, the observation window serving as a glass plate, and the captured image is acquired. Then, about 500 hydrophobic droplets 200a reflected in the captured image are extracted, and their average particle size (arithmetic mean value of the sphere equivalent diameter) is calculated. It may be the particle size of the emulsion particles 600a.

Although it depends on which phase is particularly desired to be recovered, for example, unburned carbon particles and hydrophobic liquid can be recovered from the emulsion phase 600, and water and hydrophilic particles can be recovered from the aqueous phase 100a. can. Therefore, it is preferable to recover at least the emulsion phase 600 and the aqueous phase 100a.

The interface between the emulsion phase 600 and the aqueous phase 100a does not necessarily have to be recognized. For example, when the heavy liquid phase 700 becomes the aqueous phase 100a, the first interface observation window 70 in the vertical multi-stage contact separation device 10'is not always necessary. Even in such a case, the heavy liquid phase 700 (that is, the aqueous phase 100a) is always formed at the lower end of the vertical multi-stage contact separation device 10', and therefore the heavy liquid discharge port (details will be described later). By providing 10h, the aqueous phase 100a can be recovered.

On the other hand, when the light liquid phase 500 becomes the aqueous phase 100a, the first interface observation window 70 in the vertical multi-stage contact separation device 10 is not always necessary. Even in such a case, the light liquid phase 500 (that is, the aqueous phase 100a) is always formed at the upper end of the vertical multi-stage contact separation device 10, so that the light liquid discharge port (details will be described later) is at this position. ) By providing 10f, the aqueous phase 100a can be recovered. Of course, even in these cases, it is preferable that the interface between the emulsion phase 600 and the aqueous phase 100a is also recognized. For example, when continuous treatment is continued, the interface between the emulsion phase 600 and the aqueous phase 100a may fluctuate significantly. In this case, the emulsion phase 600 may also be recovered from the discharge port for recovering the aqueous phase 100a. For example, when the light liquid phase 500 becomes the aqueous phase 100a and the interface between the emulsion phase 600 and the aqueous phase 100a moves to the vicinity of the upper end of the vertical multi-stage contact separation device 10, the emulsion phase 600 is recovered from the light liquid discharge port 10f. There is a possibility. Further, when the heavy liquid phase 700 becomes the aqueous phase 100a and the interface between the emulsion phase 600 and the aqueous phase 100a moves to the vicinity of the lower end of the vertical multi-stage contact separation device 10, the emulsion phase 600 is recovered from the heavy liquid discharge port 10h. There is a possibility. Therefore, it is preferable that the interface between the emulsion phase 600 and the aqueous phase 100a is also recognized.

(6-12. Each outlet)
The vertical multi-stage contact separation device 10 is provided with three discharge ports, that is, a light liquid discharge port 10f, an emulsion phase discharge port 10g, and a heavy liquid discharge port 10h. The material of each discharge port is not particularly limited, but does not affect each other with the contents of the vertical outer wall tube 20 (that is, hydrophobic particles, hydrophilic particles, water, hydrophobic liquid, etc.) (corrosion). No, does not dissolve, etc.) Material, for example, preferably made of stainless steel.

The light liquid discharge port 10f is provided near the liquid level of the light liquid phase 500, for example, and discharges the light liquid phase 500. Of course, the installation position of the light liquid discharge port 10f is not limited to this position. The light liquid phase 500 is, for example, an aqueous phase 100a or a hydrophobic liquid. Thereby, the aqueous phase 100a or the hydrophobic liquid can be recovered. The recovered hydrophobic liquid can be reused as the light liquid 100. The recovered hydrophobic liquid may be reused as it is, but since it may contain liberated hydrophobic particles 300a and the like, it is preferable to reuse it after washing by any method. Examples of the method for cleaning the hydrophobic liquid include so-called centrifugation and distillation.

On the other hand, many hydrophilic particles 300b are concentrated in the aqueous phase 100a. Therefore, first, the aqueous phase 100a is separated into water and solid content using a centrifuge, a centrifuge having a filtration function, or an arbitrary settler. The separated water can be reused as the light liquid 100. The centrifuge having a filtering function is a centrifuge having a rotating body having a large number of pores through which the filtered liquid passes on the wall surface in the direction in which the centrifugal force acts, and the dehydrated liquid has pores. It passes through and moves to the outside of the rotating body, but the solid matter remains in the rotating body. On the other hand, since water remains in the solid content, it is preferable to dry the solid content. The water evaporated by drying can be reused as the light liquid 100 after being condensed. On the other hand, the dried solid can be appropriately reused depending on its components. For example, when the mixture 310 to be separated becomes fly ash, the solid matter becomes refined fly ash. The refined fly ash has many uses, and examples thereof include raw materials for concrete, raw materials for building materials, and raw materials for cement. Since the carbon content _CA in the refined fly ash is very low (for example, the carbon content _CA can be reduced to less than 2% by mass by setting the opening ratio of the partition plate 35 to 10 to 50%). The quality of refined fly ash is very high.

In FIG. 3, when the light liquid phase 500 is the aqueous phase 100a and the heavy liquid phase 700 is the hydrophobic liquid phase, coarse hydrophilic particles having a large particle size (for example, 200 μm or more) settle in the emulsion phase 600. However, it may be concentrated near the interface 110c between the emulsion phase 600 and the heavy liquid phase 700. In such a case, the liquid near the interface 110c between the emulsion phase 600 and the heavy liquid phase 700 is recovered little by little, and the coarse hydrophilic particles are separated by a sieve or the like to recover the emulsion phase 600 including the emulsion particles 600a. can do.

The emulsion phase discharge port 10g is provided slightly closer to the emulsion phase 600 than, for example, the interface 110c between the emulsion phase 600 and the hydrophobic liquid phase (heavy liquid phase 700 in the example of FIG. 3). Thereby, the emulsion phase 600 can be recovered. Of course, the installation position of the emulsion phase discharge port 10g is not limited to this position. However, in the example of FIG. 3, the specific gravity of the emulsion particles 600a is larger than that of the aqueous phase 100a (that is, the specific gravity of the hydrophobic liquid is larger than that of water). Therefore, the concentration of the emulsion particles 600a in the lower emulsion phase 600 is higher than the concentration of the emulsion particles 600a in the upper emulsion phase 600. Therefore, by providing the emulsion phase discharge port 10 g at this position, the emulsion phase 600 can be efficiently recovered. The recovered emulsion phase 600 is first separated into a solid content and a liquid phase using a centrifuge, a centrifuge having a filtration function, or an arbitrary settler. Most of the liquid phase is a hydrophobic liquid, but since a small amount of water is also mixed, these can be separated by distillation or the like and then reused as a light liquid 100 or a heavy liquid 200. Alternatively, since the water and the hydrophobic liquid are finally mixed, the recovered liquid phase may be reused as it is as the light liquid 100 or the heavy liquid 200.

On the other hand, since the liquid remains in the solid content, it is preferable to dry the solid content. The liquid evaporated by drying is condensed and then separated into a hydrophobic liquid and water (or as it is) by the method described above, and can be reused as a light liquid 100 or a heavy liquid 200. On the other hand, the dried solid can be appropriately reused depending on its components. For example, when the mixture 310 to be separated becomes fly ash, the solid matter becomes an unburned carbon concentrate. The carbon content C _C in the unburned carbon concentrate is very high (for example, the carbon content C _C can be increased by setting the opening ratio of the partition plate 35 to 10 to 50%, for example, light liquid cleaning. The quality of the unburned carbon concentrate is very high because it can be increased to more than 70% by mass when the portion is made into two stages). The unburned carbon concentrate can be reused as a carbon material for power generation, iron making, cement clinker and the like, for example.

The heavy liquid discharge port 10h is provided, for example, at the lower end of the vertical multi-stage contact separation device 10. The heavy liquid phase 700 is, for example, an aqueous phase 100a or a hydrophobic liquid. Thereby, the aqueous phase 100a or the hydrophobic liquid can be recovered. The recovered aqueous phase 100a or hydrophobic liquid can be reused by the method described above (that is, described in the item of the light liquid discharge port 10f). For example, when the mixture 310 to be separated becomes fly ash, purified fly ash having a very low carbon content _CA can be recovered from the aqueous phase 100a. For example, by setting the opening ratio of the partition plate 35 to 10 to 50%, the carbon content _CA can be reduced to less than 2% by mass at the minimum.

Therefore, for example, when the mixture 310 to be separated becomes fly ash, the fly ash can be separated into purified fly ash and unburned carbon concentrate by the vertical multi-stage contact separation device 10 according to the present embodiment. Here, the purified fly ash contains the metal oxide particles which are hydrophilic particles 300b at a high content (in other words, the unburned carbon particles at a low content), and the unburned carbon concentrate is not the hydrophobic particles 300a. Contains high carbon particles. Therefore, fly ash can be separated into metal oxide particles and unburned carbon particles with a high separation rate and a high separation efficiency.

<7. Modification example of vertical multi-stage contact separation device>
The vertical multi-stage contact separation device 10 shown in FIG. 3 has a 5-stage mixer unit 40 and a 6-stage settler unit 30, but the vertical multi-stage contact separation device 10 is not limited to such an example. .. FIG. 9 shows a modified example of the vertical multi-stage contact separation device 10. The vertical multi-stage contact separation device 10 according to this modification has a one-stage rough separation mixer unit 40a as the mixer unit 40, and has an uppermost settler unit 30a and a lowermost settler unit 30b as the settler unit 30. .. That is, the number of the mixer unit 40 and the settler unit 30 is the minimum. The partition plate 35 is provided above and below the coarse separation mixer unit 40a, respectively.

The other components are almost the same as the example shown in FIG. That is, in the vertical multi-stage contact separation device 10 according to this modification, in addition to the above, the vertical outer wall tube 20, the stirring shaft 10a, the stirring blade 10b, the heavy liquid introduction port 10c, the slurry introduction port 10d, and the light liquid introduction port 10e , A light liquid discharge port 10f, and an emulsion phase discharge port 10 g. The heavy liquid discharge port 10h, the first interface observation window 70 and the second interface observation window 80 are omitted. When these are provided, the heavy liquid discharge port 10h may be provided below the emulsion phase discharge port 10g. On the other hand, the first interface observation window 70 and the second interface observation window 80 may be appropriately installed according to the types of the light liquid phase 500 and the heavy liquid phase 700. For example, when the light liquid phase 500 is the aqueous phase 100a and the heavy liquid phase 700 is the hydrophobic liquid phase, the first interface observation window 70 is the uppermost settler portion 30a, and the second interface observation window 80 is the lowermost settler portion. It may be provided in each of 30b. On the other hand, when the light liquid phase 500 becomes a hydrophobic liquid phase and the heavy liquid phase 700 becomes an aqueous phase 100a, the first interface observation window 70 is in the lowermost settler portion 30b, and the second interface observation window 80 is in the uppermost settler portion. It may be provided in each of 30a (see also Example 1 described later).
Also in this modification, the contents of the vertical multi-stage contact separation device 10 are separated into a light liquid phase 500, an emulsion phase 600, and a heavy liquid phase 700, and these phases can be discharged from each discharge port. ..

<8. Vertical multi-stage contact separation method>
Next, a vertical multi-stage contact separation method using the vertical multi-stage contact separation system 10A will be described with reference to FIGS. 3 to 10 and 13. FIG. 10 is a flowchart showing a rough procedure of the vertical multi-stage contact separation method.

(8-1. Pre-grinding process)
In step S10, a pre-grinding step is performed. In this pre-grinding step, the first slurry 300 is produced by pre-stirring and pulverizing the mixture 310 to be separated by the pre-stirring mixer 1000 and the bead mill 2000. Since the details are as described above, only the outline will be described here.

First, the mixture 310 to be separated and water are introduced into the container 1010 of the pre-stirring mixer 1000. Then, by rotating the pre-stirring stirring blade 1020, the mixture 310 to be separated and the mixture of water or / and the hydrophobic liquid 1030 are vigorously stirred. As a result, the 0th slurry is produced. The 0th slurry is sent to the bead mill 2000 through a pipe (not shown).

Then, using the bead mill 2000, the solid content (for example, hydrophobic particles containing hydrophilic particles inside) in the 0th slurry is wet-ground and pulverized. As a result, the first slurry 300 is manufactured. That is, the hydrophobic particles are crushed, and the hydrophilic particles mixed in the hydrophobic particles are removed from the hydrophobic particles. As a result, in the first slurry 300, many hydrophilic particles are removed from the hydrophobic particles.

After the pre-grinding step (S10), the hydrophobic liquid is mixed in advance in the 0th slurry, and most of the liberated hydrophobic particles (for example, unburned carbon particles) 300a adhere to the surface layer portion of the hydrophobic droplets 200a. May be allowed to form emulsion particles 600a.

(8-2. Slurry introduction process, light liquid introduction process, and heavy liquid introduction process)
In step S20, a slurry introduction step, a light liquid introduction step, and a heavy liquid introduction step are performed. That is, first, the first slurry 300 produced by the pre-grinding step using the pre-stirring mixer 1000 and the bead mill 2000 is introduced into the vertical multi-stage contact separation device 10 from the slurry introduction port 10d (slurry introduction step). On the other hand, the heavy liquid (water or a hydrophobic liquid having a specific gravity larger than that of water) 200 is introduced into the vertical multi-stage contact separation device 10 from the heavy liquid introduction port 10c (heavy liquid introduction step). Further, the light liquid (water or a hydrophobic liquid having a specific gravity smaller than that of water) 100 is introduced into the vertical multi-stage contact separation device 10 from the light liquid introduction port 10e (light liquid introduction step).

(8-3. Specific gravity separation step)
In step S30, the specific gravity separation step is performed. Specifically, the stirring shaft 10a is rotated. As a result, the content 40c (see FIG. 5) in the mixer unit 40 is stirred by the mixer unit 40, and the content 30c is allowed to stand in the settler unit 30 (see FIG. 6). By performing the above-mentioned processing by each settler unit 30 and the mixer unit 40, the contents of the vertical multi-stage contact separation system 10A are separated into the light liquid phase 500, the emulsion phase 600, and the heavy liquid phase 700 from the top.

Since the details of the functions of the settler unit 30 and the mixer unit 40 are as described above, only the outline will be described here. First, in the coarse separation mixer unit 40a, the first slurry 300 is stirred together with the hydrophobic liquid (hydrophobic droplet 200a) and the like. As a result, especially the emulsion particles 600a are generated in the coarse separation mixer unit 40a.

The hydrophobic droplets 200a and the hydrophobic particles 300a released in the coarse separation mixer section 40a move to the upper or lower settler section 30 depending on their specific densities. Then, these are separated by specific gravity in the settler section 30 and further moved to another mixer section 40b. Then, the hydrophobic particles 300a adhere to the surface layer portion of the hydrophobic droplets 200a in the other mixer unit 40b, and become emulsion particles 600a.

The emulsion particles 600a generated in any of the mixer units 40 gradually settle or rise in the vertical multi-stage contact separation device 10, and finally concentrate in the emulsion phase 600. Therefore, when the specific gravity of the hydrophobic liquid is larger than that of water, the concentration of the emulsion particles 600a in the lower mixer section 40 is higher than the concentration of the emulsion particles 600a in the upper mixer section 40. Alternatively, when the specific gravity of the hydrophobic liquid is smaller than that of water, the concentration of the emulsion particles 600a in the upper mixer section 40 is higher than the concentration of the emulsion particles 600a in the lower mixer section 40.

The hydrophobic droplets 200a that do not take in the hydrophobic particles 300a move to the upper end or the lower end in the vertical multi-stage contact separation device 10 and coalesce to form a light liquid phase 500 or a heavy liquid phase 700. On the other hand, the aqueous phase 100a moves to the upper end or the lower end in the vertical multi-stage contact separation device 10 depending on its specific gravity and coalesces to form a light liquid phase 500 or a heavy liquid phase 700. Hydrophilic particles 300b are concentrated in the aqueous phase 100a. For example, when the specific gravity of the hydrophobic liquid is larger than that of water, the light liquid phase 500 becomes the aqueous phase 100a and the heavy liquid phase 700 becomes the hydrophobic liquid phase.

In the specific gravity separation step, in order to stably perform the first to third recovery steps described later, the operator observes the interface 110b of the emulsion phase 600 / light liquid phase 500 through the first interface observation window 70. It is preferable to maintain the position (height) of the interface 110b at a constant level as much as possible (when the light liquid phase 500 becomes the aqueous phase 100a). Similarly, it is preferable to observe the interface 110c of the emulsion phase 600 / heavy liquid phase 700 through the second interface observation window 80 and maintain the position (height) of the interface 110c at a constant level as much as possible (heavy liquid phase). When 700 is a hydrophobic liquid phase). When the light liquid phase 500 becomes the hydrophobic liquid phase and the heavy liquid phase 700 becomes the aqueous phase 100a, the positions of the first interface observation window 70 and the second interface observation window 80 are exchanged, or the vertical type shown in FIG. The same process as that shown in FIG. 10 may be performed using the multi-stage contact separation device 10'.

Here, as a method of maintaining the interface 110b of the emulsion phase 600 / light liquid phase 500 at a constant level, there is a method of adjusting the emulsion discharge amount (drawing amount) from the emulsion phase discharge port 10 g. Further, as a method of maintaining the interface 110c of the emulsion phase 600 / heavy liquid phase 700 at a constant level, a method of adjusting the heavy liquid discharge amount (drawing amount) from the heavy liquid discharge port 10h can be mentioned.

(8-4. 1st to 3rd recovery steps)
In step S40, the first to third recovery steps are performed. Specifically, the light liquid phase 500 separated in the specific gravity separation step is recovered (first recovery step), the emulsion phase 600 separated in the specific gravity separation step is recovered (second recovery step), and further, the above. The heavy liquid phase 700 separated in the specific gravity separation step is also recovered (third recovery step). Since the specific contents of each process are as described above, only the outline will be described here.

The aqueous phase 100a is recovered as a light liquid phase 500 or a heavy liquid phase 700. The recovered aqueous phase 100a is separated into water and solid content. The water can be reused as a light liquid 100 or a heavy liquid 200. It is preferable that the solid content is further dried. The dried solid can be reused as appropriate depending on its components. For example, when the mixture 310 to be separated becomes fly ash, the solid matter becomes refined fly ash. The refined fly ash has many uses, and examples thereof include raw materials for concrete, raw materials for building materials, and raw materials for cement. Since the carbon content _CA in the refined fly ash is very low (for example, the carbon content _CA can be reduced to less than 2% by mass by setting the opening ratio of the partition plate 35 to 10 to 50%). The quality of refined fly ash is very high.

The hydrophobic liquid phase is also recovered as the light liquid phase 500 or the heavy liquid phase 700. The recovered hydrophobic liquid can be reused as a light liquid 100 or a heavy liquid 200. The recovered hydrophobic liquid may be reused as it is, but since it may contain liberated hydrophobic particles 300a and the like, it is preferable to reuse it after washing by any method. Examples of the method for cleaning the hydrophobic liquid include so-called centrifugation and distillation.

On the other hand, the recovered emulsion phase 600 is first separated into a solid content and a liquid phase using a centrifuge, a centrifuge having a filtration function, or an arbitrary settler. Most of the liquid phase is a hydrophobic liquid, but since a small amount of water is also mixed, these can be separated by distillation or the like and then reused as a light liquid 100 or a heavy liquid 200. Alternatively, since the water and the hydrophobic liquid are finally mixed, the recovered liquid phase may be reused as it is as the light liquid 100 or the heavy liquid 200.

On the other hand, since the liquid remains in the solid content, it is preferable to dry the solid content. The liquid evaporated by drying is condensed and then separated into a hydrophobic liquid and water (or as it is) by the method described above, and can be reused as a light liquid 100 or a heavy liquid 200. On the other hand, the dried solid can be appropriately reused depending on its components. For example, when the mixture 310 to be separated becomes fly ash, the solid matter becomes an unburned carbon concentrate. The carbon content C _C in the unburned carbon concentrate is very high (for example, the carbon content C _C can be increased by setting the opening ratio of the partition plate 35 to 10 to 50%, for example, light liquid cleaning. If the number of parts 60 is increased to more than 70% by mass), the quality of the unburned carbon concentrate is very high. The unburned carbon concentrate can be reused as a carbon material for power generation, iron making, cement clinker and the like, for example.

As described above, the vertical multi-stage contact separation device 10 according to the present embodiment has, for example, a configuration as shown in FIG. 3, particularly a plurality of settler units 30 and at least one or more mixer units 40. Can be separated into a light liquid phase 500, an emulsion phase 600, and a heavy liquid phase 700. Here, since the light liquid phase 500 or the heavy liquid phase 700 becomes the aqueous phase 100a, a solid substance having a very low content of hydrophobic particles (for example, a carbon particle content _CA ) from the aqueous phase 100a (for example, purified). Fly ash) can be collected. Further, from the emulsion phase 600, a solid substance (for example, unburned carbon concentrate) having a very high content of hydrophobic particles (for example, a _carbon particle content CC) can be recovered. Therefore, the hydrophobic particles and the hydrophilic particles can be efficiently separated from the mixture to be separated in which the hydrophobic particles and the hydrophilic particles are mixed. Further, unlike the flotation method as described in Patent Document 1, phase separation can be performed by simply stirring the contents containing the first slurry 300, as shown in Examples described later. , Phase separation is done in tens of seconds. Then, the desired substance can be recovered from each phase. In particular, a large amount of hydrophobic particles 300a can be recovered from the emulsion phase 600. Therefore, the separation rate of the hydrophobic particles 300a can also be increased.

More specifically, in the conventional flotation method described in Patent Document 1, a relatively large amount of hydrophobic liquid is not used as in the present embodiment, but a collecting agent such as kerosene and light oil and foaming are used. Hydrophobic particles (unburned carbon particles 101) having a relatively small specific gravity were attached to the bubbles 103 and floated by using a small amount of an agent (see FIG. 15). At this time, the amount of the collecting agent and the foaming agent added to the water is as small as several mass% with respect to the mass of the fly ash. However, in such a conventional method, when the particle size of the unburned carbon particles 101 is large, even if the unburned carbon particles 101 adhere to the bubbles 103, they are easily peeled off from the bubbles 103, so that they are difficult to float and separate. .. In this conventional method, bubbles are attached to the unburned carbon particles 101 that are about to settle, and the particles are forced to levitate against gravity. Therefore, the ascent rate is very slow, and it takes about one hour to reduce the carbon content to a low content (for example, 3% by mass or less), and also the recovered hydrophilic particles (metal oxides). ), The content of the unburned carbon particles 101 may not be reduced to the target value or less (for example, 3% by mass or less), and there is a problem that the separation efficiency is poor.

On the other hand, in the separation method according to the present embodiment, hydrophobic particles (for example, unburned carbon particles) 300a are efficiently separated into the emulsion phase 600 as compared with the conventional flotation method described in Patent Document 1. Therefore, it is excellent in the ability to separate the hydrophobic particles 300a from the mixture 310 to be separated. Therefore, the separation rate of the hydrophobic particles 300a can be significantly increased, and the separation efficiency can also be improved. Therefore, the content of the hydrophobic particles 300a in the solid matter (for example, purified fly ash) recovered from the aqueous phase 100a (for example) For example, the carbon content _CA ) in refined fly ash can be significantly reduced.

Further, in the vertical multi-stage contact separation device 10 according to the present embodiment, the coarse separation mixer unit 40a provided with the slurry introduction port 10d and the uppermost settler unit 30a, the coarse separation mixer unit 40a, and the lowermost portion are provided. A pair or more of the other mixer section 40b and the settler section 30d are further arranged in at least one region between the settler section 30b and the settler section 30b. The mixer section 40 and the settler section 30 are arranged alternately. Therefore, the separation rate and separation efficiency of the hydrophobic particles 300a can be further increased.

Further, the hole diameter of the second through hole 35b formed in the partition plate 35 may be 8 to 50 mm, and the aperture ratio may be 10 to 50 area%. In this case, the separation rate and separation efficiency of the hydrophobic particles 300a can be further increased.

Further, the vertical multi-stage contact separation device 10 has an observation window (first interface observation) capable of observing at least one of the aqueous phase / emulsion phase interface and the emulsion phase / hydrophobic liquid phase interface (interfaces 110b and 110c). It further has a window 70 or a second interface observation window 80). Therefore, the operator can more easily observe the interface (interface 110b, 110c).

Further, the observation window capable of observing the interface (interface 110b or interface 110c) of the emulsion phase / hydrophobic liquid phase is a transparent plate having no hydrophilic functional group on the surface or a transparent plate having no hydrophilic functional group. It is a transparent plate covered with paint. Therefore, the operator can observe the interface more easily.

Further, the vertical multi-stage contact separation device 10 has contents in the upper part or the lower part of any observation window (first interface observation window 70 in the example of FIG. 3) inside the vertical multi-stage contact separation device 10. It has an umbrella 75 that obstructs distribution. Therefore, the operator can observe the interface more easily.

Further, the light liquid 100 may be water, the heavy liquid 200 may be a hydrophobic liquid, and the mixture 310 to be separated may be fly ash. In this case, unburned carbon particles are separated from the fly ash at a higher separation rate and separation efficiency. , Can be recovered.

Further, the light liquid 100 may be a hydrophobic liquid, the heavy liquid 200 may be water, and the mixture 310 to be separated may be fly ash. In this case, unburned carbon particles are separated from the fly ash at a higher separation rate and separation efficiency. , Can be recovered.

Further, in the vertical multi-stage contact separation method, at least one of the interface of the aqueous phase / emulsion phase and the interface of the emulsion phase / hydrophobic liquid phase is maintained at a constant level, so that these phases should be recovered stably. Can be done.

Further, the light liquid 100 is water, the heavy liquid 200 is a hydrophobic liquid, and the mixture to be separated 310 is fly ash, and the interface between the aqueous phase / emulsion phase is maintained at a constant level below the coarse separation mixer unit 40a. May be good. This allows the operator to more easily observe the interface between the aqueous phase / emulsion phase and thus easily keep it at a constant level.

Further, the light liquid 100 is a hydrophobic liquid, the heavy liquid 200 is water, and the mixture to be separated 310 is fly ash, and the interface between the aqueous phase / emulsion phase is maintained at a constant level above the coarse separation mixer unit 40a. May be good. This allows the operator to more easily observe the interface between the aqueous phase / emulsion phase and thus easily keep it at a constant level.

Further, the mixture to be separated may be pre-pulverized (pre-pulverized) with a bead mill and then introduced into the vertical multi-stage contact separation device 10. In this case, the separation rate and separation efficiency of the hydrophobic particles 300a can be further increased.

Next, an embodiment of the present embodiment will be described. In this example, the following experiments were carried out in order to confirm the effect of this embodiment. Of course, the present invention is not limited to the examples described below. It is clear that a person having ordinary knowledge in the field of technology to which the present invention belongs can come up with various modifications or modifications within the scope of the technical ideas described in the claims. , These are also naturally understood to belong to the technical scope of the present invention. In particular, the specifications of the vertical multi-stage contact separation device shown as specifications are merely an example of this embodiment.

<1. Common specifications of vertical multi-stage contact separation device>
First, the common specifications of the vertical multi-stage contact separation device described below will be described. These specifications are as follows.
・ Inner diameter of vertical outer wall pipe: 81.1 mm
-Height of mixer unit 40: 50 mm
Height of settler portion: 50 mm, 100 mm, or 150 mm (Since the jet flow from the mixer portion 40 is estimated to be about 30 mm, the interface is controlled to be at least 50 mm in order to promote the sedimentation of 600a of the emulsion particles. The height of the settler portion 30 was set to 100 mm or 150 mm.)
・ Partition plate 35
-Hole diameter of the first through hole 35a: 20 mm
-Hole diameter of the second through hole 35b: 12 mm
(The number per partition plate is adjusted for each example between 0 and 24, and the aperture ratio of the partition plate 35 is adjusted for each example between 5 and 60 area%).
-Strut 35c: Diameter 6 mm x 3 locations (per partition plate)
・ Stirring shaft 10a and stirring blade 10b
As shown in FIG. 3, the stirring shaft 10a extends from at least the upper end to the lower end of the vertical multi-stage contact separation device 10, and further extends upward from the upper end of the vertical multi-stage contact separation device 10.
-Diameter of stirring shaft 10a: 8 mm
(Therefore, the gap between the peripheral surface of the stirring shaft 10a and the inner wall surface of the first through hole 35a is 12 mm).
Diameter of stirring blade 10b (distance between tips of opposing stirring blades 10b-2): 50 mm
The height of the stirring blade 10b-2: 10 mm, the width of the stirring blade 10b-2 (the length in the length direction of the stirring rod 10b-1 (the radial direction of the stirring blade 10b)): 12.5 mm.
-Number of stirring blades 10b: 1 for each mixer section (6 stirring blades 10b-2 for each stirring blade 10b)

<2. Example 1>
In Example 1, fly ash was used as the mixture to be separated 310, and the separation efficiency and the separation rate according to the present embodiment were considered.

(2-1. Specifications of vertical multi-stage contact separation device)
FIG. 14 shows the configuration of the vertical multi-stage contact separation device 10 according to the first embodiment. As shown in FIG. 14, the vertical multi-stage contact separation device 10 according to the first embodiment has a simplified configuration of the vertical multi-stage contact separation device 10'. Specifically, in this vertical multi-stage contact separation device 10, the mixer unit 40 has only one stage of the coarse separation mixer unit 40a, and the uppermost settler unit 30a and the lowermost settler unit 30b are arranged above and below the mixer unit 40a. The heights of the uppermost settler portion 30a, the coarse separation mixer portion 40a, and the lowermost settler portion 30b were set to 150 mm, 50 mm, and 100 mm, respectively.

The partition plate 35 was formed with 12 second through holes 35b per partition plate, and the opening ratio of each partition plate 35 was 32 area%. The rotation speed of the stirring shaft 10a was set to 500 rpm (peripheral speed: 1.28 m / sec).

The second interface observation window 80 was provided in the uppermost settler portion 30a, and the first interface observation window 70 was provided in the lowermost settler portion 30b. The second interface observation window 80 was a glass plate coated with polypropylene, and the first interface observation window 70 was a glass plate.

The heavy liquid introduction port 10c, the slurry introduction port 10d, and the light liquid introduction port 10e are all provided in the coarse separation mixer section 40a. However, the order of installation was the heavy liquid introduction port 10c, the slurry introduction port 10d, and the light liquid introduction port 10e from the top. The heavy liquid 200 was water, and the light liquid 100 was n-hexane (specific gravity: 0.65). Therefore, the light liquid phase 500 becomes the hydrophobic liquid phase, and the heavy liquid phase 700 becomes the aqueous phase 100a.

The light liquid discharge port 10f is near the upper end of the uppermost settler portion 30a, and the emulsion phase discharge port 10g is near the lower end of the uppermost settler portion 30a (a little closer to the emulsion phase 600 than the interface 110b between the light liquid phase 500 and the emulsion phase 600). ), The heavy liquid discharge port 10h is provided near the lower end of the lowermost settler portion 30b, respectively. Specifications other than these are described in <1. The specifications are the same as those described in> Common specifications for vertical multi-stage contact separation devices.

(2-2. Operation using a vertical multi-stage contact separation device)
An operation was performed to separate fly ash into purified fly ash and unburned carbon concentrate using the vertical multi-stage contact separation device 10 having the above specifications. Specifically, water is 0.3 L / min, the first slurry (fly ash slurry) 300 is 0.2 L / min, n- from the heavy liquid introduction port 10c, the slurry introduction port 10d, and the light liquid introduction port 10e. The hexane was introduced into the coarse separation mixer unit 40a at a flow rate of 0.4 L / min. Here, the first slurry 300 is manufactured by performing the above-mentioned pre-grinding step (pre-grinding step using the pre-stirring mixer 1000 and the bead mill 2000) on the fly ash. The concentration of the first slurry 300 was 250 g / L. The carbon content of the fly ash used in Example 1 was 8.5% by mass.

In the pre-grinding step, the fly ash was made into the 0th slurry by mixing the fly ash and water using the pre-stirring mixer 1000. Then, 1 L of the 0th slurry was put into a bead mill 2000 containing 1 kg of zirconia beads having a diameter of 500 μm, and the mixture was stirred at 1500 rpm for 10 minutes. As a result, the fly ash was crushed to produce the first slurry 300. The method for producing the first slurry 300 was the same as in Examples 2 and 3 described later.

During the operation, the operator observed the interface 110b of the emulsion phase 600 / light liquid phase 500 (here, the interface of the emulsion phase / hydrophobic liquid phase) through the second interface observation window 80. Then, the operator can make the interface 110b a constant level in the uppermost settler portion 30a (that is, the interface 110b to be a constant level above the emulsion phase discharge port 10g) so that the emulsion phase discharge port 10g. The amount of emulsion phase 600 drawn from was adjusted. At this time, the operator was careful that the liquid level 500b of the light liquid phase 500 was arranged directly above the light liquid discharge port 10f.

On the other hand, the operator observed the interface 110c of the emulsion phase 600 / heavy liquid phase 700 (here, the interface between the emulsion phase and the aqueous phase) through the first interface observation window 70. Then, the operator causes the interface 110c to have a constant level in the lowermost settler portion 30b (that is, the interface 110c has a constant level above the heavy liquid discharge port 10h), so that the heavy liquid discharge port 10h The amount of the aqueous phase 100a (that is, the heavy liquid phase 700) drawn from the water phase 100a was adjusted. At this time, the operator was careful that the liquid level 500b of the light liquid phase 500 was arranged directly above the light liquid discharge port 10f.

The emulsion phase 600 drawn from the emulsion phase discharge port 10 g is solid-liquid separated by a centrifuge having a filtration function, and the recovered dehydrated cake (solid content) is dried at 105 ° C. to obtain a solid substance (unburned carbon concentrate). ) Was recovered. Then, the carbon content CC in the unburned _carbon concentrate was measured.

Further, the aqueous phase 100a drawn from the heavy liquid discharge port 10h is solid-liquid separated by a centrifuge having a filtration function, and the recovered dehydrated cake (solid content) is dried at 105 ° C. to obtain a solid substance (refined fly ash). ) Was recovered. Then, the carbon content _CA in the refined fly ash was measured. The carbon content _{C C} in the unburned carbon concentrate is 43% by mass, and the carbon content CA in the refined fly ash is 1.2% by mass, so that the unburned carbon particles in the fly ash can be efficiently separated. It turned out that. Further, the contents of the vertical multi-stage contact separation device 10 were separated into the light liquid phase 500, the emulsion phase 600, and the heavy liquid phase 700 within a few tens of seconds after the start of the operation, so that the separation speed was also high. ..

<3. Example 2>
In Example 2, the same operation as in Example 1 was performed except that the first interface observation window 70 and the second interface observation window 80 were both made of stainless steel plates. Therefore, in the second embodiment, the operator cannot observe the interfaces 110b and 110c, and thus cannot control the interfaces 110b and 110c as described above.

At the beginning of the operation of Example 2, the carbon content CC in the unburned _carbon concentrate was 45% by mass, the carbon content _CA in the refined fly ash was 1.4% by mass, and the carbon content in the fly ash was 1.4% by mass. The unburned carbon particles could be separated efficiently. However, as the operation was continued, a part of the emulsion phase 600 came to be discharged from the heavy liquid discharge port 10h of the lowermost settler portion 30b. It is considered that this is because the interface 110c of the emulsion phase 600 / heavy liquid phase 700 (here, the interface of the emulsion phase / aqueous phase) has decreased from the beginning of the operation.

Therefore, the carbon content CC in the unburned _carbon concentrate was almost the same as 43% by mass, but the carbon content in the refined fly ash increased to 4.3% by mass from the beginning of the operation. Therefore, the separation efficiency of unburned carbon particles in fly ash was slightly lower than that of Example 1. However, considering that the carbon content of the fly ash is 8.5% by mass, it means that the unburned carbon particles can be efficiently separated from the fly ash in the second embodiment as well.

<4. Example 3>
In Example 3, a preferable aperture ratio was confirmed by varying the aperture ratio of the partition plate 35. The specific test method is as follows.

(4-1. Specifications of vertical multi-stage contact separation device)
The overall configuration of the vertical multi-stage contact separation device 10 according to the third embodiment was the same as that of the example of FIG. That is, one stage of the coarse separation mixer section 40a was formed, and two sets of the mixer section 40 and the settler section 30 were provided above the coarse separation mixer section 40a, respectively. The upper two sets of the mixer section 40 and the settler section 30 of the coarse separation mixer section 40a serve as the heavy liquid cleaning section 50, and the lower two sets of the mixer section 40 and the settler section 30 serve as the light liquid cleaning section 60. Further, the uppermost settler portion 30a is arranged above the heavy liquid cleaning portion 50, and the lowermost settler portion 30b is arranged below the light liquid cleaning portion 60. A partition plate 35 was arranged between the mixer unit 40 and the settler unit 30.

The heights of the uppermost settler portion 30a and the lowermost settler portion 30b were both set to 100 mm. The height of the other settler portion 30d was set to 50 mm. The height of the mixer unit 40 including the coarse separation mixer unit 40a was set to 50 mm.

In Example 3, a plurality of different levels with different aperture ratios of the partition plate 35 between 5 and 60% were set, and operations were performed at each level. The aperture ratio was adjusted by varying the number of second through holes 35b between 0 and 24. The aperture ratio of each partition plate 35 was set to be the same within the same level. The stirring shaft 10a was rotated at 500 rpm (peripheral speed: 1.28 m / sec) at any level.

The first interface observation window 70 was installed in the settler section 30 (that is, the observation settler section 30e) directly under the coarse separation mixer section 40a, and the second interface observation window 80 was provided in the lowermost settler section 30b. The material of the first interface observation window 70 was a glass plate, and the material of the second interface observation window 80 was a glass plate coated with polypropylene.

The heavy liquid introduction port 10c was installed in the mixer section 40 directly below the uppermost settler section 30a, the slurry introduction port 10d was installed in the coarse separation mixer section 40a, and the light liquid introduction port 10e was provided in the lowermost settler section 30b. The heavy liquid 200 was 1-bromopropane (specific gravity 1.35), and the light liquid 100 was water. Therefore, the light liquid phase 500 becomes the aqueous phase 100a, and the heavy liquid phase 700 becomes the hydrophobic liquid phase.

The light liquid discharge port 10f is near the upper end of the uppermost settler portion 30a, the emulsion phase discharge port 10g is slightly upward in the height direction of the lowermost settler portion 30b, and the heavy liquid discharge port 10h is the lower end of the lowermost settler portion 30b. Each was provided in the vicinity.

When the operator observed the interface 110c of the emulsion phase 600 / heavy liquid phase 700 through the second interface observation window 80 during the operation described later, the heavy liquid phase 700 (that is, the hydrophobic liquid phase) and the emulsion phase 600 were observed. At the interface 110c with, almost no particles flowing between the phases were found. Therefore, an umbrella was not installed in the lowermost settler portion 30b.

On the other hand, in the upper part of the observation settler portion 30e (more specifically, the upper part of the interface 110b of the emulsion phase 600 / the light liquid phase 500), an umbrella is used to suppress the emulsion particles 600a falling from the upper part of the interface 110b. 75 was provided. Specifications other than these are described in <1. The specifications are the same as those described in> Common specifications for vertical multi-stage contact separation devices.

(4-2. Operation using a vertical multi-stage contact separation device)
An operation was performed to separate fly ash into purified fly ash and unburned carbon concentrate using the vertical multi-stage contact separation device 10 having the above specifications. Since a plurality of levels of vertical multi-stage contact separation devices 10 are prepared in Example 3, the same operation was performed on these vertical multi-stage contact separation devices 10.

Specifically, from the heavy liquid introduction port 10c, the slurry introduction port 10d, and the light liquid introduction port 10e, 1-bromopropane is 0.4 L / min and the first slurry (fly ash slurry) is 0.2 L / min, respectively. , Water was introduced into the vertical multi-stage contact separation device 10 at a flow rate of 0.3 L / min. Here, the first slurry 300 is manufactured by performing the above-mentioned pre-grinding step (pre-grinding step using the pre-stirring mixer 1000 and the bead mill 2000) on the fly ash. The concentration of the first slurry 300 was 250 g / L. The carbon content of the fly ash used in Example 3 was 8.5% by mass.

During the operation, the operator observed the interface 110b of the emulsion phase 600 / the light liquid phase 500 (here, the interface of the emulsion phase / the aqueous phase 100a) through the first interface observation window 70. Then, the operator adjusted the amount of the emulsion phase 600 drawn from the emulsion phase discharge port 10 g so that the interface 110b was at a constant level below the umbrella 75. At this time, the operator was careful that the liquid level 500b of the light liquid phase 500 was arranged directly above the light liquid discharge port 10f.

On the other hand, the operator observed the interface 110c of the emulsion phase 600 / heavy liquid phase 700 (here, the interface of the emulsion phase / hydrophobic liquid phase) through the second interface observation window 80. Then, the operator makes the interface 110c a constant level in the lowermost settler portion 30b (that is, the interface 110c becomes a constant level below the emulsion phase discharge port 10g and above the heavy liquid discharge port 10h). The amount of the heavy liquid phase 700 drawn out from the heavy liquid discharge port 10h was adjusted. At this time, the operator was careful that the liquid level 500b of the light liquid phase 500 was arranged directly above the light liquid discharge port 10f.

The emulsion phase 600 drawn from the emulsion phase discharge port 10 g is solid-liquid separated by a centrifuge having a filtration function, and the recovered dehydrated cake (solid content) is dried at 105 ° C. to obtain a solid substance (unburned carbon concentrate). ) Was recovered. Then, the carbon content CC in the unburned _carbon concentrate was measured.

Further, the aqueous phase 100a drawn from the light liquid discharge port 10f is solid-liquid separated by a centrifuge having a filtration function, and the recovered dehydrated cake (solid content) is dried at 105 ° C. to obtain a solid substance (refined fly ash). ) Was recovered. Then, the carbon content _CA in the refined fly ash was measured.

The above operations were performed for all standards. At any level (HRT (hydraulic residence time) is as short as about 70 seconds), the contents of the vertical multi-stage contact separation device 10 are the light liquid phase 500, the emulsion phase 600, and the heavy liquid phase 700. It can be said that the separation speed is high because it was separated into.

Furthermore, the carbon content CC in the unburned carbon concentrate and the _carbon content CA in the refined fly _ash were calculated for each level. Furthermore, these ratios, that is, the carbon content ratio C _C / _CA , were calculated. The results are shown in FIGS. 11 and 12.

The horizontal axis of FIG. 11 shows the opening ratio (area%) of the partition plate 35 at each level, and the vertical axis shows the carbon content CC in the unburned carbon concentrate or the _carbon content _CA in the refined fly ash. .. The point P100 shows the measured value of the aperture ratio of the partition plate 35 and the _carbon content CC in the unburned carbon concentrate at each level, and the graph L10 is a connection of the points P100. The point P200 shows the measured value of the aperture ratio of the partition plate 35 and the carbon content _CA in the refined fly ash at each level, and the graph L20 is a connection of the points P200.

The horizontal axis of FIG. 12 shows the opening ratio (area%) of the partition plate 35 at each level, and the vertical axis shows the _carbon content ratio CC / _CA (mass% / mass%). The point P300 shows the measured value of the aperture ratio of the partition plate 35 and the carbon content ratio _{C C} / CA at each level, and the graph L30 is a connection of the points P300.

According to FIGS. 11 and 12, when the aperture ratio is 10 to 50 area%, the emulsion particles 600a are concentrated below the settler portion 30 (that is, on the partition plate 35) in each settler portion 30, and the settler portion 30 is formed. In the upper part of the water phase 100a and oxide particles were mostly present (see FIG. 6).

Further, the emulsion particles 600a concentrated under the settler section 30 are concentrated under the settler section 30 while flowing due to an appropriate jet flow sent from the mixer section 40, and are concentrated under the settler section 30 without being deposited on the settler section 30. It was found that the particles were moved to the lower mixer section 40 via the first through hole 35a and the second through hole 35b provided in the lower partition plate 35.

As a result, the carbon content CA in the refined fly ash was low, and the carbon content _{C C in} the unburned carbon concentrate was high. That is, the value of these ratios (carbon content ratio) _{C C} / CA was 20 (mass% / mass%) or more. For example, when the aperture ratio is 32%, the carbon content ratio _{C C} / CA is as high as 45.0 (mass% / mass%).

On the other hand, even when the aperture ratio is less than 10%, the emulsion particles concentrated under the settler portion 30 are concentrated at the lower part of the settler portion 30, but these emulsion particles 600a move to the mixer portion 40 below. It became difficult. Therefore, the emulsion particles 600a gradually move above the vertical multi-stage contact separation device 10 (due to the jet flow provided from the mixer unit 40 below the settler unit 30), and are finally discharged from the light liquid discharge port 10f. Emulsion particles 600a are now mixed with the aqueous phase 100a. Therefore, the carbon content _CA in the refined fly ash was high. On the other hand, the amount of unburned carbon particles recovered from the hydrophobic liquid phase discharged from the heavy liquid discharge port 10h is small, and the carbon content CC in the unburned _carbon concentrate has an aperture ratio of 10 to 50 area%. It wasn't much different from the case. Therefore, the carbon content ratio C _C / C _A decreased. Nevertheless, considering that the carbon content _CA in the refined fly ash is less than 8.0% by weight and the carbon content of the initial fly ash is 8.5% by weight, even in this case the fly It means that the unburned carbon particles have been removed from the ash.

On the other hand, when the aperture ratio exceeds 50%, the jet flow given from the mixer section 40 to the settler section 30 becomes large, so that the emulsion particles 600a are less likely to settle in the settler section 30. As a result, for this reason, the emulsion particles 600a gradually move above the vertical multi-stage contact separation device 10 (due to the jet flow provided from the mixer unit 40 below the settler unit 30), and finally the light liquid discharge port 10f. Emulsion particles 600a came to be mixed with the aqueous phase 100a discharged from the water phase 100a. Therefore, the carbon content _CA in the refined fly ash was high. Furthermore, the carbon content CC in the unburned _carbon concentrate was also reduced. Therefore, the carbon content ratio C _C / C _A decreased. Nevertheless, considering that the carbon content _CA in the refined fly ash is less than 6.0% by weight and the initial fly ash has a carbon content of 8.5% by weight, even in this case the fly It means that the unburned carbon particles have been removed from the ash.

Therefore, unburned carbon particles can be efficiently removed from the fly ash regardless of the opening ratio of the partition plate 35, but the separation efficiency is particularly good when the opening ratio of the partition plate 35 is 10 to 50 area%. It can be said that it will be.

Although the preferred embodiments of the present invention have been described in detail above, the present invention is not limited to such examples. It is clear that a person having ordinary knowledge in the field of technology to which the present invention belongs can come up with various modifications or modifications within the scope of the technical ideas described in the claims. , These are also naturally understood to belong to the technical scope of the present invention.

10A Vertical multi-stage contact separation system 10 Vertical multi-stage contact separation device 10a Stirring shaft 10b Stirring blade 10c Heavy liquid introduction port 10d Slurry introduction port 10e Light liquid introduction port 10
10f Light liquid discharge port 10g Emulsion phase discharge port 10h Heavy liquid discharge port 20 Vertical outer wall tube 30 Settler part 30a Top settler part 30b Bottom settler part 35 Partition plate 35a First through hole 35b Second through hole 35c Strut 40 Mixer Part 40a Coarse separation mixer part 70 1st interface observation window 75 Umbrella 80 2nd interface observation window 100 Light liquid 100a Aqueous phase 200 Heavy liquid 200a Hydrophobic droplets 300a Hydrophobic particles 300b Hydrophilic particles 500 Light liquid phase 600 Emulsion phase 600a Emulsion particles 700 heavy liquid phase

Claims (13)

A vertical multi-stage contact separation device that separates the hydrophobic particles and the hydrophilic particles from the mixture to be separated in which the hydrophobic particles and the hydrophilic particles are mixed.
A content containing the hydrophobic particles, the hydrophilic particles, a light liquid, and a heavy liquid having a higher specific gravity than the light liquid, and one of the heavy liquid and the light liquid is water and the other is a hydrophobic liquid. With a vertical outer wall tube that houses
A plurality of settler portions arranged in the vertical direction in the vertical outer wall tube,
At least one mixer unit arranged between the plurality of settler units and agitating the contents, and a mixer unit.
A partition plate that partitions the settler portion and the mixer portion and has a through hole for distributing the contents between the mixer portion and the settler portion.
A light liquid introduction port for introducing the light liquid into the mixer section above and near the bottom settler section, which is the lowermost settler section.
A heavy liquid introduction port for introducing the heavy liquid into the mixer part below and near the uppermost settler part, which is the uppermost settler part.
A slurry introduction port for introducing the mixture to be separated, a slurry in which the mixture to be separated is dispersed in water, or a slurry in which the pre-pulverized mixture to be separated is dispersed in water into any of the mixer units.
Among the aqueous phase, emulsion phase, and hydrophobic liquid phase formed in the vertical outer wall tube, at least the aqueous phase and the discharge port for discharging the emulsion phase are provided. Contact separation device. At least one region between the mixer section provided with the slurry introduction port and the uppermost settler section, and between the mixer section provided with the slurry introduction port and the lowermost settler section. The vertical multi-stage contact separation device according to claim 1, wherein one or more pairs of the mixer section and the settler section are further arranged, and the mixer section and the settler section are alternately arranged. .. The vertical multi-stage contact separation device according to claim 1 or 2, wherein the through hole formed in the partition plate has a hole diameter of 8 to 50 mm and an opening ratio of 10 to 50 area%. The vertical multi-stage contact separation device is further characterized by further having an observation window capable of observing at least one of the interface between the aqueous phase and the emulsion phase and the interface between the emulsion phase and the hydrophobic liquid phase. The vertical multi-stage contact separation device according to any one of claims 1 to 3. The vertical multi-stage contact separation device has an observation window capable of observing the interface between the emulsion phase and the hydrophobic liquid phase.
The observation window according to claim 4, wherein the observation window is a transparent plate having no hydrophilic functional group on its surface, or a transparent plate covered with a transparent paint having no hydrophilic functional group. Vertical multi-stage contact separation device. The vertical multi-stage contact separation device is characterized in that, inside the vertical multi-stage contact separation device, an umbrella that obstructs the distribution of the contents is provided at the upper part or the lower part of any of the observation windows. Item 6. The vertical multi-stage contact separation device according to Item 4 or 5. One of claims 1 to 6, wherein the light liquid is water, the heavy liquid is a hydrophobic liquid, and the mixture to be separated in which the hydrophobic particles and the hydrophilic particles are mixed is fly ash. The vertical multi-stage contact separation device described in the section. One of claims 1 to 6, wherein the light liquid is a hydrophobic liquid, the heavy liquid is water, and the mixture to be separated in which the hydrophobic particles and the hydrophilic particles are mixed is fly ash. The vertical multi-stage contact separation device described in the section. A vertical multi-stage contact separation method using the vertical multi-stage contact separation device according to any one of claims 1 to 8. The vertical multi-stage contact separation method is characterized in that at least one of the interface between the aqueous phase and the emulsion phase and the interface between the emulsion phase and the hydrophobic liquid phase is maintained at a constant level. Item 9. The vertical multi-stage contact separation method according to Item 9. The light liquid is water, the heavy liquid is a hydrophobic liquid, and the mixture to be separated in which the hydrophobic particles and the hydrophilic particles are mixed is fly ash.
The vertical multi-stage contact separation method according to claim 10, wherein the interface between the aqueous phase and the emulsion phase is maintained at a constant level below the mixer portion provided with the slurry introduction port. The light liquid is a hydrophobic liquid, the heavy liquid is water, and the mixture to be separated in which the hydrophobic particles and the hydrophilic particles are mixed is fly ash.
The vertical multi-stage contact separation method according to claim 10, wherein the interface between the aqueous phase and the emulsion phase is maintained at a constant level above the mixer portion provided with the slurry introduction port. The vertical multi-stage contact separation method according to any one of claims 9 to 12, wherein the mixture to be separated is pre-pulverized with a bead mill and then introduced into the vertical multi-stage contact separation device.

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