JP5932120B1 - Suspension manufacturing apparatus and manufacturing method thereof - Google Patents

Abstract

Provided is a technique for efficiently producing a suspension having a fine and uniform dispersed phase in which the aggregate structure is eliminated without destroying the molecular structure of the dispersed phase. A suspension manufacturing apparatus includes a first pressure vessel filled with a mixture of solid particles and a liquid medium in a sealed state, and a mixture filled in the first pressure vessel. The first heating means 21 for heating the liquid, the second pressure vessel 12 from which the vapor 14 of the liquid medium generated by the heating is extracted through the first connection path 31, and the liquid extracted to the second pressure vessel 12 A second heating means 22 for heating the medium vapor 14; a second connection path 32 for communicating the second pressure vessel 12 and the first pressure vessel 11; And a take-off valve 17 for taking out a suspension 16 formed by finely pulverizing solid particles contained in 13 and dispersed in a liquid medium from the inside of the first pressure vessel 11 to the outside. [Selection] Figure 1

Description

  The present invention relates to a technique for producing a suspension in which fine solid particles are dispersed in a liquid medium.

  In a suspension obtained by dispersing solid particles in a liquid medium, the finer the solid particles, the lower the settling speed due to gravity, and the solid state is not separated and the stable state is maintained. In addition, when a solid substance is fermented or chemically reacted, the finer the solid particles, the larger the specific surface area of the solid particles, and the reaction can be promoted.

By the way, it is known that organic compounds containing biomass-derived components, fine powdered or fibrous inorganic compounds, etc. have high cohesiveness and are difficult to finely disperse in the matrix of other substances. Yes.
Examples of known techniques for finely dispersing such a compound in a liquid medium matrix include the following.

A technique is known in which a compound is coarsely pulverized with a mechanical pulverizer, subjected to particle size adjustment by sieving or air classification, and then mixed with a solvent such as water or alcohol to produce a suspension (for example, Patent Document 1).
Moreover, the technique of processing a biomass with a solvent with a high-pressure homogenizer and manufacturing a suspension is known (for example, patent document 2).

JP 2011-105893 A JP 2006-289164 A

However, since the technique of Patent Document 1 undergoes a process of pulverizing and solidifying solid particles independently, there is a problem that solid particles forming a dispersed phase reaggregate when mixed with a liquid medium.
Moreover, the technique of patent document 2 has the subject that there is little quantity of the suspension obtained by one process, and production efficiency is low including apparatus maintenance.

  The present invention has been made in view of such circumstances, and an object of the present invention is to provide a technique for efficiently producing a suspension having a fine and uniform dispersed phase in which the aggregate structure of the dispersed phase is eliminated. To do.

The suspension manufacturing apparatus according to the present invention includes a first pressure vessel in which a mixture of solid particles and a liquid medium is filled in a sealed state and a space filled with vapor of the liquid medium is formed; First heating means for heating the mixture filled in the pressure vessel to a temperature at which the internal pressure of the space becomes higher than atmospheric pressure, and the first on-off valve closes the vapor of the liquid medium generated by the heating. A second pressure vessel that is extracted from the space via the first connection path, a second heating unit that heats the vapor of the liquid medium that is extracted to the second pressure vessel, and the second A second connection path that communicates two pressure vessels and the first pressure vessel, and the second on-off valve switches from the closed state to the open state to spray the heated vapor of the liquid medium on the mixture, and is included in the mixture The solid particles are refined and dispersed in the liquid medium A takeout valve taken out from the inside of the first pressure vessel Nigoeki, characterized in that it comprises a.

  The present invention provides a technique for efficiently producing a suspension having a fine and uniform dispersed phase in which the aggregate structure of the dispersed phase is eliminated.

The block diagram of the manufacturing apparatus of the suspension which concerns on 1st Embodiment of this invention. The block diagram of the manufacturing apparatus of the suspension which concerns on 2nd Embodiment of this invention. The block diagram of the manufacturing apparatus of the suspension which concerns on 3rd Embodiment of this invention. The flowchart of the manufacturing method of the suspension which concerns on embodiment of this invention.

(First embodiment)
Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings.
As shown in FIG. 1, the suspension manufacturing apparatus 10A (10) according to the first embodiment includes a first pressure vessel 11 filled with a mixture 13 of solid particles and a liquid medium in a sealed state, A first heating means 21 for heating the mixture 13 filled in the one pressure vessel 11, a second pressure vessel 12 from which the vapor 14 of the liquid medium generated by this heating is extracted via the first connection path 31; The second heating means 22 for heating the vapor 14 of the liquid medium extracted into the second pressure vessel 12 and the second pressure vessel 12 and the first pressure vessel 11 communicate with each other to the mixture 13 to heat the liquid medium. A second connection path 32 for spraying 15, and a take-off valve 17 for taking out the suspension 16, in which the solid particles contained in the mixture 13 are refined and dispersed in a liquid medium, from the inside of the first pressure vessel 11 to the outside. I have.

The first pressure vessel 11 includes an open valve 23 that opens the internal sealed state to the outside based on the operation of the operator, a safety valve 24 that automatically leaks the vapor 14 of the liquid medium to the outside before exceeding the pressure resistance upper limit value, An opening 25 is closed by a detachable lid so that solid particles and a liquid medium can be introduced into the interior, and a take-out valve 17 for taking out the suspension 16 from the inside to the outside is provided.
Although not shown, a stirring unit that stirs the mixture 13 is disposed inside the first pressure vessel 11.
The solid particles and the liquid medium are each composed of one kind or two or more kinds of compounds.

The first pressure vessel 11 is provided with a heat exchanging portion 21a of a first heating means 21 for heating the filled mixture 13.
Since the first pressure vessel 11 is filled with the mixture 13 in a sealed state, the internal pressure P ₁ of the space filled with the vapor 14 of the liquid medium is saturated with the solvent at the temperature adjusted by the first heating means 21. Equal to vapor pressure.

Connection ends 31b and 31c of the first connection path 31 are connected to the first pressure vessel 11 and the second pressure vessel 12, respectively.
The second pressure vessel 12 communicates with the retention space of the vapor 14 of the first pressure vessel 11 through the first connection path 31, and communicates with the filling region of the mixture 13 of the first pressure vessel 11 through the second connection passage 32. Further, in the internal space of the second pressure vessel 12, a heat exchange part 22 a of the second heating means 22 for heating the vapor 14 of the liquid medium extracted from the first pressure vessel 11 is arranged.

The internal pressure P ₂ of the second pressure vessel 12 becomes equal to the internal pressure P ₁ of the first pressure vessel 11 when the setting of the on-off valve 31a of the first connection path is switched from closed to open.
Then, when the setting of the on-off valve 31a of the first connection path is switched from open to closed, and the setting of the on-off valve 32a of the second connection path is closed, the second heating means 22 is operated, whereby the second pressure vessel As the internal temperature of 12 rises, its internal pressure P ₂ also rises.

The pressure applied to the connection end 32 c on the first pressure vessel 11 side of the second connection path 32 takes a value obtained by adding the head pressure of the mixture 13 to the internal pressure P ₁ of the first pressure vessel 11.
Therefore, when the internal pressure P ₂ of the second pressure vessel 12 becomes sufficiently larger than the pressure applied to the connection end 32c of the second connection path, the setting of the on-off valve 32a of the second connection path is set from closed to open. To do.

Then, the heating steam 15 of the second pressure vessel 12 is sprayed to the mixture 13 filled in the first pressure vessel 11 through the second connection path 32.
In addition, since the non-return valve 32b is provided in the 2nd connection path 32, even if supply of the heating steam 15 stops, the mixture 13 with which the 1st pressure vessel 11 is filled will flow backward. There is no.

In addition, as shown in FIG. 1, by providing the first compressor 41 in the first connection path 31, the steam 14 generated in the first pressure vessel 11 is forced to flow toward the second pressure vessel 12, The internal pressure P ₂ of the two-pressure vessel 12 can be set higher.
The installation position of the first compressor 41 that functions as such is not limited to the first connection path 31, and may be disposed inside the second pressure vessel 12.
When such a first compressor 41 is provided, the on-off valve 31a of the first connection path and the on-off valve 32a of the second connection path are normally opened, and the heating steam 15 is continuously supplied to the first compressor 41. The mixture 13 filled in the pressure vessel 11 can be sprayed.

  The 1st heating means 21 and the 2nd heating means 22 can be suitably employ | adopted if each of the heat exchange part 21a and the heat exchange part 22a can be set to high temperature rather than ambient temperature. Specifically, it may be a power source that generates Joule heat by electric resistance, or may have a function of heating and forcing a heat medium to circulate. In addition, when the liquid medium or its vapor | steam 14 is combustible, the latter heat medium flow system is suitable.

Thus, the mixture 13 to which the heating steam 15 is sprayed has a strong mechanical action (shear pulverization action, collision destruction action, destruction action by cavitation, pressure action, etc.) on the two-phase system of solid particles and liquid medium. Is added, the solid particles are refined and dispersed in the liquid medium.
Here, the cavitation is a phenomenon in which a low pressure portion generated in the fluid flowing at high speed is vaporized to generate a vapor pocket, and the pocket disappears in a very short time. Due to the phenomenon that pockets are generated and disappeared in this way, very high pressure and destructive force are applied to the solid particles in the liquid medium to promote the miniaturization, and the mixture 13 is adjusted to a stable suspension.

The suspension obtained in this way may be distributed as a final product as it is, used as an intermediate material for producing the final product, or by further extracting useful substances contained therein. In some cases.
In addition, since the solid component from which the liquid medium is removed from such a suspension returns to the original suspension when mixed with the liquid medium again, it can be traded as a product in such a solid component state. Conceivable.

(Second Embodiment)
As shown in FIG. 2, the suspension manufacturing apparatus 10B (10) according to the second embodiment is arranged outside the first pressure vessel 11 and the circulation path 33 with both ends 33b and 33c communicating with each other. And a second compressor 42 that is provided in the circulation path 33 and forcibly flows the mixture 13 filled in the first pressure vessel 11 in one direction.
2 that have the same configuration or function as those in FIG. 1 are denoted by the same reference numerals, and redundant description is omitted.

  In the circulation path 33, one connection end 33 b is connected to the lower portion of the first pressure vessel 11, and the other connection end 33 c is connected to the upper portion of the first pressure vessel 11, and is routed outside the first pressure vessel 11. ing. The second compressor 42 provided in the circulation path 33 draws the mixture 13 from the lower portion of the first pressure vessel 11 and performs forced flow for reinjection from the upper portion. 11, the mixture 13 inside is stirred.

  Furthermore, the mixture 13 is subjected to a large shearing and grinding action from the inner wall surface of the circulation path 33 and the mechanical drive unit of the second compressor 42 in the process of passing through the narrow circulation path 33 at a high speed. Further promoted.

(Third embodiment)
As illustrated in FIG. 3, the suspension manufacturing apparatus 10 </ b> C (10) according to the third embodiment includes a supply container 51 that supplies solid particles 52, and a liquid medium 53 that is previously introduced into the first pressure container 11. And a mixing path 54 for mixing the supplied solid particles 52 while forcibly flowing through the outside.
In the first embodiment and the second embodiment, the solid particles and the liquid medium are collectively charged into the first pressure vessel 11 from the inlet 25. In the third embodiment, only the liquid medium 53 is introduced into the first pressure vessel 11 from the introduction port 25 in advance, and the solid particles 52 are introduced little by little from the outside of the first pressure vessel 11.

The solid particle supply container 51 stores solid particles roughly pulverized to an appropriate particle size by a mechanical pulverizer (not shown).
The mixing path 54 has one connection end 54 b connected to the lower portion of the first pressure vessel 11, and the other connection end 54 c connected to the upper portion of the first pressure vessel 11, and is routed outside the first pressure vessel 11. ing.

And the 3rd compressor 55 provided in this mixing channel 54 pulls out the liquid medium 53 from the lower part of the 1st pressure vessel 11, and performs the forced flow which reinjects from the upper part.
The supply container 51 supplies and mixes the solid particles 52 to the circulating liquid medium 53 at a mixing point 56 communicating with the mixing path 54.

According to the third embodiment, the solid particles 52 are continuously added in small amounts to the large amount of liquid medium 53 being stirred. Thereby, the solid particles 52 can be uniformly dispersed in the liquid medium 53 without agglomeration.
After the prescribed amount of solid particles 52 is introduced into the first pressure vessel 11, the third compressor 55 is stopped, and then the on-off valve 54 a of the mixing path is shut off to be in a sealed state. Thereafter, the heating means 21 and 22 are operated, and the operation described in the first embodiment or the second embodiment is performed.

Next, each embodiment of the suspension manufacturing method will be described with reference to the flowchart of FIG. 4 (see FIG. 1 as appropriate).
The mixture 13 of the solid particles and the liquid medium is filled in the first pressure vessel 11 and sealed (S11). The first heating means 21 is operated to heat the mixture 13 filled in the first pressure vessel 11 (S12). Then, the vapor 14 of the liquid medium generated by this heating is extracted to the second pressure vessel 12 through the first connection path 31 and heated by the second heating means 22 (S13).

  Then, the heated vapor 15 of the liquid medium further increases the pressure and is sprayed from the second pressure vessel 12 to the mixture 13 filled in the first pressure vessel 11 through the second connection path 32. (S14). As a result, the mixture 13 becomes a suspension 16 in which the contained solid particles are refined and dispersed in the liquid medium, and the take-off valve 17 is opened and taken out of the first pressure vessel 11 (S15 END).

Examples of the solid particles applicable to the present embodiment include organic compounds such as biomass-derived components and inorganic compounds.
The liquid medium is preferably used because highly polar water has excellent dispersibility. In addition, a solvent having a high affinity in relation to solid particles or a water-soluble hydroxide may be added to the solvent.
Particularly in woody biomass, the aggregated structure can be eliminated by a smaller shear stress by the swelling and plasticizing action of the boiled or immersed liquid medium. These circumstances also apply to layered clay minerals and highly cohesive nano-level fine powders (carbon materials / amorphous carbon, layered clay minerals, cellulose nanofibers, etc.).

Other solid particles that can be applied include food residues, waste bacteria beds, medicinal herbs, organic sludge, inorganic sludge, and organic-inorganic mixed sludge.
Furthermore, other applicable solid particles include metal hydroxides such as magnesium oxide and aluminum hydroxide. The final product using the suspension as an intermediate material can be flame retardant and non-flammable.

Further, other applicable solid particles include porous fine particles such as activated carbon, coal ash clinker ash, and volcanic ash. The final product using the suspension as an intermediate material can obtain characteristics with low density and excellent rigidity.
Further, other applicable solid particles include charcoal such as charcoal, bamboo charcoal, and rice husk charcoal, and activated carbon. The final product using the resulting suspension as an intermediate material can obtain electrical conductivity.

These solid particles can be dispersed in a small amount of liquid medium by mixing with the liquid medium in advance and stirring.
Further, a polymer compound can be added to the mixture of the solid particles and the liquid medium to form a composite. Such high molecular compounds include low density polyethylene (LDPE), high density polyethylene (HDPE), polypropylene (PP), ethylene-vinyl acetate copolymer (EVA), ethylene-acrylic, which are molded into pellets. A polyolefin-based resin such as an ethyl acid copolymer (EEA) is suitable, but is not limited thereto, and a thermoplastic resin can be applied and combined.

When the solid particles are an organic material and the liquid medium is a hydrocarbon oil or a fatty acid, the suspension can be used as a liquid fuel. Solid particles of organic material and liquid medium of hydrocarbon oil or fatty acid can be obtained by food recycling or the like. Furthermore, liquid fuel can be obtained from recycled resources by effectively utilizing waste oil and the like.
In addition, when the solid particles include carbides, even if the liquid medium includes water, since the combustion heat per weight is large, the suspension can be used as a liquid fuel.

  If the solvent contains phenols having an active group, polyhydric alcohols, cyclic esters such as ε-caprolactone, oxyacids such as lactic acid, cyclic carbonates such as ethylene carbonate and propylene carbonate, glycidyl compounds, etc. It can be used as a raw material for composite materials.

As phenols, phenol, o-cresol, m-cresol, p-cresol, 3,5-xylenol, 2,3-xylenol, α-naphthol and the like are monovalent phenols, and catechol and resorcinol are divalent phenols. And phloroglucin as a trivalent phenol.
Examples of bisphenols include bisphenol A, bisphenol F, bisphenol S, bisphenol AF, and halogenated bisphenol A.
Examples of polyhydric alcohols include ethylene glycol, propylene glycol, trimethylene glycol, 1.4-butanediol, 1.5-pentanediol, 1.6-hexanediol, 1.2-hexanediol, and 2.4-hexane. Diol, 1.7-heptanediol, 1.8-octanediol, 1.9-nonanediol, 1.10-decanediol, pinacol, cyclopentane1.2-diol, cyclohexane1.2-diol, cyclohexane Dihydric alcohols such as 4-diol, trihydric alcohols such as glycerin and trimethylolpropane, sugar alcohols such as sorbitol and sucrose, and polyethylene glycol (eg, polyethylene glycol 400), polyoxypropylene glycol, polyoxypropylene-polyoxye Glycol, polycaprolactone (PLACCEL 303) polymer such like.

From a suspension using a phenol as a solvent, a thermosetting molded article or adhesive composed of a phenol resin can be obtained.
By adding epichlorohydrin to a suspension using phenols having two or more phenolic hydroxyl groups as a solvent and reacting the hydroxyl groups in the liquid composition with epichlorohydrin in the presence of an alkali, An epoxy resin composite material can be obtained.

A suspension using a polyhydric alcohol as a solvent can be subjected to an isocyanate reaction to obtain a urethane-based composite material.
A photocurable composite material can be obtained, for example, by graft polymerization of a solvent of acrylic acid or methacrylic acid monomer in a suspension containing solid particles derived from biomass.
A fiber-reinforced composite material can be obtained by mixing a suspension in which cellulose-based long fibers are dispersed and an unsaturated polyester.

A reagent that reacts with the functional groups of the solid particles can be added to the suspension to provide a compatibilizer for the thermoplastic composite material. As such a reaction reagent, an active halogen compound, an aliphatic halogen compound, an unsaturated monomer and the like are preferably used.
When a thermoplastic composite material is produced as a final product, the solvent is selected from hydrocarbons, fatty acids, higher alcohols, aliphatic amides, and esters that have a high affinity for the synthetic polymer constituting the matrix.

  According to the suspension manufacturing apparatus of at least one embodiment described above, a mixture of solid particles and a liquid medium is heated, the generated steam is extracted, and the pressure is increased by reheating, and the heated steam is mixed. By spraying on the suspension, it is possible to efficiently produce a suspension having a fine and uniform dispersed phase.

  Although several embodiments of the present invention have been described, these embodiments are presented by way of example and are not intended to limit the scope of the invention. These embodiments can be implemented in various other forms, and various omissions, replacements, changes, and combinations can be made without departing from the scope of the invention. These embodiments and their modifications are included in the scope and gist of the invention, and are also included in the invention described in the claims and the equivalents thereof.

10 (10A, 10B, 10C) ... suspension manufacturing apparatus,
DESCRIPTION OF SYMBOLS 11 ... 1st pressure vessel, 12 ... 2nd pressure vessel, 13 ... Mixture, 14 ... Steam of liquid medium, 15 ... Heating steam, 16 ... Suspension, 17 ... Extraction valve, 21 ... 1st heating means, 21a ... heat exchange part of the first heating means, 22 ... second heating means, 22a ... heat exchange part of the second heating means, 23 ... release valve, 24 ... safety valve, 25 ... inlet, 31 ... first connection path, 31a ... Open / close valve of the first connection path, 31b, 31c ... Connection end of the first connection path, 32 ... Second connection path, 32a ... Open / close valve of the second connection path, 32b ... Check valve of the second connection path, 32c ... Connection end of second connection path, 33 ... Circulation path, 33a ... Open / close valve of circulation path, 33b, 33c ... Connection end of circulation path, 41 ... First compressor, 42 ... Second compressor, 51 ... Supply container, 52 ... Solid particles, 53 ... Liquid medium, 54 ... Mixing path, 54a ... Open / close valve of mixing path, 54b, 54c ... Connection , 55 ... third compressor, 56 ... mixing point.

Claims (10)

A first pressure vessel in which a mixture of solid particles and a liquid medium is filled in a sealed state and a space filled with the vapor of the liquid medium is formed ;
First heating means for heating the mixture filled in the first pressure vessel to a temperature at which the internal pressure of the space is higher than atmospheric pressure ;
A second pressure vessel in which the vapor of the liquid medium generated by the heating is extracted from the space through the first connection path when the first on-off valve is switched from closed to open ;
Second heating means for heating the vapor of the liquid medium extracted into the second pressure vessel;
A second connection path that communicates the second pressure vessel and the first pressure vessel, and blows the heating vapor of the liquid medium onto the mixture by switching the second on-off valve from closed to open ;
A suspension valve, wherein the solid particles contained in the mixture are refined and dispersed in the liquid medium to take out the suspension from the inside of the first pressure vessel. manufacturing device. In the suspension production apparatus according to claim 1,
Wherein the steam generated in the first pressure vessel, apparatus for producing a suspension, further comprising a first compressor to force flow to the first connection path toward the second pressure vessel. In the suspension production apparatus according to claim 1 or 2,
A circulation path disposed outside the first pressure vessel and having both ends communicating with each other;
A suspension manufacturing apparatus, further comprising: a second compressor that is provided in the circulation path and forcibly flows the mixture filled in the first pressure vessel in one direction. In the suspension production apparatus according to any one of claims 1 to 3,
A supply container for supplying the solid particles;
The suspension further comprising: a mixing path for forcibly flowing the liquid medium previously introduced into the first pressure vessel through the outside and mixing the supplied solid particles. Manufacturing equipment. In the suspension production apparatus according to any one of claims 1 to 4,
The first heating means and the second heating means have a function of heating and forcibly flowing a heating medium to circulate in each of the first pressure vessel and the second pressure vessel. Manufacturing equipment. In the suspension production apparatus according to any one of claims 1 to 5,
An apparatus for producing a suspension, further comprising: a stirring unit that is disposed inside the first pressure vessel and stirs the mixture. Filling the first pressure vessel in a sealed state with a mixture of solid particles and liquid medium and forming a space filled with vapor of the liquid medium ;
Heating the mixture filled in the first pressure vessel to a temperature at which the internal pressure of the space is higher than atmospheric pressure ;
The step of extracting the vapor of the liquid medium generated by the heating from the space to the second pressure vessel through the first connection path when the first on-off valve is switched from closed to open ;
Heating the vapor of the liquid medium extracted into the second pressure vessel;
Communicating the second pressure vessel and the first pressure vessel, and blowing the heating vapor of the liquid medium to the mixture by switching the second on-off valve from closed to open ;
And taking out the suspension formed by dispersing the solid particles contained in the mixture into the liquid medium from the inside of the first pressure vessel to the outside. Method. In the manufacturing method of the suspension of Claim 7,
A method for producing a suspension, further comprising the step of filling the first pressure vessel with a polymer compound in addition to the mixture. In the manufacturing method of the suspension of Claim 7 or Claim 8,
The solid particles include a suspension containing at least one selected from the group consisting of magnesium oxide, aluminum hydroxide, activated carbon, coal ash clinker ash, volcanic ash, charcoal, bamboo charcoal, and rice husk charcoal. Manufacturing method. In the manufacturing method of the suspension of Claim 7 or Claim 8,
The method for producing a suspension, wherein the solid particles are an organic material, the liquid medium is a hydrocarbon oil or a fatty acid, and the suspension is a liquid fuel.

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